processing and manufacturing technology of special sensors · 2020-04-08 · perature co-fired...

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Processing and Manufacturing Technology of Special Sensors Qiulin Tan Contents Introduction ....................................................................................... 2 Ceramic MEMS Device Processing and Manufacturing Methods .............................. 4 L/HTCC Micro-assembly Technology ....................................................... 5 Heterogeneous Material Co-ring Technology .................................................. 13 Co-ring of Heterogeneous Substrate Materials ............................................. 14 Electronic Paste Heterogeneous Co-ring .................................................... 16 Integration of Multiple Processing Technologies ................................................ 17 C-MEMS High-Temperature Device ............................................................. 18 Langasite Device Processing and Manufacturing Methods ..................................... 21 High Temperature Forming Mechanism ......................................................... 23 Wet Etching Mechanism ...................................................................... 23 Dry Etching Mechanism ...................................................................... 25 Bonding Mechanism .......................................................................... 26 LGS Device Sealed Cavity Manufacturing Technology ......................................... 27 Wet Etching Process .......................................................................... 27 Inductively Coupled Plasma (ICP) Etching Process ......................................... 28 Surface Polishing and Bonding Process ...................................................... 29 LGS Device Surface Graphic Manufacturing Technology ...................................... 30 SAW Temperature and Pressure Integrated Devices ............................................. 32 Summary .......................................................................................... 32 References ........................................................................................ 33 Q. Tan (*) Key Laboratory of Instrumentation Science & Dynamic Measurement, Ministry of Education, North University of China, Taiyuan, China Science and Technology on Electronic Test and Measurement Laboratory, North University of China, Taiyuan, China e-mail: [email protected] © Springer Nature Singapore Pte Ltd. 2019 S. Yang, Z. Jiang (eds.), Precision Machines, Precision Manufacturing, https://doi.org/10.1007/978-981-10-5192-0_23-1 1

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Page 1: Processing and Manufacturing Technology of Special Sensors · 2020-04-08 · perature co-fired ceramic) micro-assembly technology, heterogeneous material co-firing technology, integration

Processing and Manufacturing Technologyof Special Sensors

Qiulin Tan

ContentsIntroduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2Ceramic MEMS Device Processing and Manufacturing Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

L/HTCC Micro-assembly Technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5Heterogeneous Material Co-firing Technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

Co-firing of Heterogeneous Substrate Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14Electronic Paste Heterogeneous Co-firing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

Integration of Multiple Processing Technologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17C-MEMS High-Temperature Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18Langasite Device Processing and Manufacturing Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21High Temperature Forming Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Wet Etching Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23Dry Etching Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25Bonding Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

LGS Device Sealed Cavity Manufacturing Technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27Wet Etching Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27Inductively Coupled Plasma (ICP) Etching Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28Surface Polishing and Bonding Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

LGS Device Surface Graphic Manufacturing Technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30SAW Temperature and Pressure Integrated Devices . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

Q. Tan (*)Key Laboratory of Instrumentation Science & Dynamic Measurement, Ministry of Education,North University of China, Taiyuan, China

Science and Technology on Electronic Test and Measurement Laboratory, North University ofChina, Taiyuan, Chinae-mail: [email protected]

© Springer Nature Singapore Pte Ltd. 2019S. Yang, Z. Jiang (eds.), Precision Machines, Precision Manufacturing,https://doi.org/10.1007/978-981-10-5192-0_23-1

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AbstractAt present, the development of aerospace technology is changing with eachpassing day, which has greatly promoted the scientific and technological progressof human society. Among them, spacecrafts play an important role. For aero-space, industrial metallurgy, and other fields and for the testing requirements ofvarious parameters in special environments such as high temperature, highrotation, and small space, traditional silicon-based sensors have problems suchas PN junction failure, solder joint dropout, and ohmic contact failure inultrahigh-temperature environments, so this chapter takes ceramic MEMSdevices and langasite devices as examples to introduce the processing andmanufacturing methods for special sensors suitable for harsh environmentssuch as high temperature and high rotation, to realize the preparation of devicesand parameter testing in special environments. Among them, ceramic MEMSdevice processing and manufacturing methods include L/HTCC (low-/high-tem-perature co-fired ceramic) micro-assembly technology, heterogeneous materialco-firing technology, integration of multiple processing technologies, etc.;langasite device processing and manufacturing methods include wet etching,inductively coupled plasma etching, bonding, surface graphic manufacturing,and other technologies. From the aspects of mechanism, common equipment,and process, the processing methods of each special sensor are elaborated.Through the abovementioned processing and manufacturing methods, the prep-aration of special sensors is realized, the test of the sensors in special applicationenvironments is completed, and the working ability in harsh environments isverified.

KeywordsCeramic MEMS devices · Langasite devices · L/HTCC micro-assemblytechnology · Heterogeneous material co-firing technology · Integration ofmultiple processing technologies · Wet etching · Inductively coupled plasmaetching · Bonding · Surface graphic manufacturing

Introduction

Exploring space has always been a dream that mankind has pursued for a long time,and the development of aerospace technology has promoted the progress of mankindto the universe. Among them, spacecraft play a key role. The United States hassuccessively issued IHPTET plans, VAATE plans, etc. for aviation engines; inChina’s 13th 5-year national science and technology innovation plan, aeroengineand gas turbine “two aircraft” are listed as major science and technology specialprojects, making them become key problems in the aerospace field together withaerospace aircraft and hypersonic aircraft projects.

The aerospace vehicle is often accompanied by harsh environments such as hightemperature and high rotation, especially for key parts such as hypersonic aircraft

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surfaces, aeroengines, and gas turbines. The local temperature even exceeds 800 �C.However, in situ real-time acquisition of parameters such as temperature, pressure,and vibration in harsh environments is of great significance for material selection,structural design, and protective measures of spacecraft (George et al. 2005; Jatlaouiet al. 2011). For example, when the spacecraft is running at high speed, the surfaceskin is rubbed against the atmosphere, generating a lot of heat. The temperature,aerodynamic load, and vibration test of the skin surface are essential for skinstructure design and protection measures (Zhao et al. 2009); aircraft engine com-bustion chamber temperature is over 800 �C, and the working pressure is greater than1.2 MPa. Combustion chamber internal temperature and pressure parameters real-time monitoring is of great significance to the material selection and failure analysis(Anonymous 2017); aerospace engine turbine blades with ultrahigh temperature,strong turbulence, and severe vibration environment, vulnerable to damage or evengenerate crack, directly decide the quality of the aerospace engine performance, sothe turbine blades, such as temperature, pressure, and vibration parameters of realtime monitoring in situ for space is especially important to the safe operation of theengine (Sabol et al. 2009).

However, traditional silicon-based testing technology is difficult to achieveaccurate real-time monitoring of various parameters in the above harsh environment(Jatlaoui et al. 2007, 2008a, b, 2009; Scott and Peroulis 2009). On one hand,traditional sensors usually take silicon as the base, and silicon material higher than500 �C will appear as plastic deformation. So silicon sensors cannot meet therequirements of ultrahigh-temperature application (Diem et al. 1995).On the otherhand, the traditional wired sensor has problems such as aging at high temperature,ohmic contact failure, etc., and the active sensor has insufficient endurance, whichare not suitable for working under high-temperature and high-rotation environment.

Therefore, the current multiparameter test technology for temperature, pressure,and vibration in critical environments such as high temperature and high rotation hasbecome one of the main bottlenecks restricting the development of spacecraft. Thereis an urgent need for substrate material selection, test sensitivity mechanism, devicestructure, manufacturing process, packaging, and other aspects to break through thetraditional restrictions and to develop new special sensors to achieve real-time in situaccurate testing of multiple parameters in harsh environments.

Special sensors refer to sensors with new structures, new functions, etc., whichare manufactured by new principles, new technologies, new materials, and newprocesses. They are used for multiparameter real-time in situ accurate measurementunder high-temperature, high-pressure, high-rotation, and other harsh environments.

First of all, in the selection of materials, materials are required to have good high-temperature stability, chemical stability, and other characteristics (Yanjie et al. 2018).On the one hand, raw ceramics are flexible materials. Compared with silicon-basedmaterials, raw ceramics have the advantages of high-temperature resistance, highelectrical insulation performance, low dielectric constant and dielectric loss, highthermal conductivity, good chemical stability, close to the thermal expansion coef-ficient of components, etc. and are very suitable for application in harsh environ-ments such as high temperature and high rotation. On the other hand, langasite

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(LGS) is one kind of hard and brittle materials. LGS crystal has good high-temperature stability and chemical stability, and its electromechanical couplingcoefficient is two to three times of quartz. It can achieve remote wireless passivemonitoring and be suitable for high-temperature and high-rotation environmentparameters test (Zhang and Yu 2011).

Secondly, the sensor components are required to be able to work normally underthe environment of high-speed rotation. Wireless passive sensor can effectivelyavoid the problems of ohmic contact failure of wired sensor and insufficient batterylife of active sensor in harsh environment. Therefore, the wireless passive sensorcomponents based on high-temperature-resistant materials have significant advan-tages in testing various parameters in harsh environments such as high temperature,high rotation, and vibration. At present, wireless passive sensing technology ismainly divided into three categories: LC resonance mutual inductance couplingtechnology, surface acoustic wave (SAW) technology, and microwavetelemetry technology. The LC resonant wireless passive sensor adopts near-fieldcoupling technology, which can realize fast reading and energy coupling of test datain a harsh environment, and has a simple and reliable structure (Ren et al. 2012;Rodriguez and Jia 2011; Tan et al. 2017a); wireless passive sensor based on theprinciple of surface acoustic wave testing has simple structure, small volume, high Qvalue, and good stability and can realize long-distance, multiparameter wirelesspassive monitoring (Cheng et al. 2011, 2012; Ren et al. 2011); the microwave-based sensor has the advantages of long transmission distance and strong anti-metalinterference, which can be dynamically monitored to realize real-time data pro-cessing (Liu and Tong 2015). Since the preparation process of the chip-type micro-wave sensor is substantially similar with the LC resonance-type sensor. Therefore,this chapter mainly takes the preparation process of LC sensor and SAW sensor asexamples.

Finally, due to the special application environment of special sensors, typicalstructure requires miniaturization and integration. Therefore, it is very importantto realize the miniaturization and integrated manufacturing of sensors throughcontrollable micro-machining technology. This chapter introduces the technologyof wireless passive special sensor processing and manufacturing suitable for high-temperature and high-rotation and other harsh environments, taking typical high-temperature-resistant materials such as ceramic and LGS as is depicted in Fig. 1.

Ceramic MEMS Device Processing and Manufacturing Methods

The ceramic MEMS devices are mainly based on flexible low-/high-temperatureco-fired ceramic (L/HTCC) raw ceramic tape and integrate the manufacturingprocess of MEMS micromechanical structure. By means of micro-assembly andsintering technology, it forms highly integrated electronic circuits in three-dimensional space. The flexible L/HTCC raw porcelain belt is easy to realizemultilayer wiring, and each layer of circuit is connected through an interconnectionthrough the hole, ensuring the integrated density of the device prepared from this. In

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addition, the flexible substrate is easier to form cavity, beam, microchannel, andother micromechanical structure, compared with the hard substrate, more conduciveto the control of processing accuracy. In addition, sintered L/HTCC-based devicescan realize self-packaging. Ceramic substrates with high-temperature resistance andgood corrosion performance can form good self-protection for the circuit encapsu-lated in them, thus further reducing the volume of devices and enhancing thereliability of devices under special circumstances. The wireless passive devicesformed by C-MEMS and LC coupling RF sensing and signal reading technologycan realize multiparameter wireless telemetry in special environment and have greatapplication prospects in aerospace, industrial manufacturing, metallurgy, mining,and other fields.

L/HTCC Micro-assembly Technology

The C-MEMS wireless passive sensor mainly involves the microstructure cavity,beam structure, microchannel structure, and curved surface structure. It integrates asingle or several different microstructures on the same substrate through theL/HTCC micro-assembly process and combines with LC coupling resonance loopto realize parameter detection of different functions. L/HTCC micro-assemblyprocess mainly includes raw porcelain with cutting, filling, silk screen printing,lamination, laminating, sintering molding, and so on, according to the need toimplement the function of the device, corresponding to the micromechanical

Fig. 1 Special sensor application background

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structure design, by adjusting the preparation process, thus forming a ceramicsubstrate of cavity, the beam structure, the microchannel structure, and surfacestructure and microstructure.

Porcelain Belt Punching ProcessThe punching process of raw porcelain belt is mainly to cut the L/HTCC flexible rawporcelain belt formed by convection to form the structure of through-hole, cavity,beam, and microchannel with different shapes and sizes. As shown in Fig. 2, thethrough-hole structure is mainly used for interlayer interconnection of multilayercircuit and lamination positioning of L/HTCC substrate. For interconnect vias, areserved via is formed at a corresponding location on each layer of the flexibleceramic substrate for filling the paste to achieve a three-dimensional integratedinterconnection, depending on the design requirements of the interlayer intercon-nection of the device circuitry. Multilayer electronic circuit. For the positioning hole,the positioning hole of the corresponding size must be reserved according to the stateof the laminating mold to ensure that the positional deviation of each layer structuredoes not occur during the lamination process. Common cavity structures mainlyinclude quadrilateral cavities, hexagonal cavities, and circular cavities. They aresimilar to the through-hole structure, and the cavity of a specified size and shape iscut by laser at a specified position, combined with self-encapsulation technology ofL/HTCC, which can form a closed cavity structure.

Typical beam structures include single cantilever beam, double cantilever beam,double end beam, double island five beam, double end four beam, four side beam,and eight side beam. Different from the punching technology of through-hole andcavity structure, only when the beam and the substrate form a whole, its

location hole

L/HTCC substrate integrated hole

L/HTCC substrate integrated cavity

L/HTCC substrate integrated beam

L/HTCC substrate integrated

microchannel

L/HTCC flexible substrate

L/HTCC flexible substrate

L/HTCC flexible substrate

L/HTCC flexible substrate

Connectinghole

Spiral-channel

Circular cavity

Quadrilateralcavity

Hexagonalcavity

Square-channel

Double-endedbeamcross beam

suspensionbeamsDoublecantilever beam

Fig. 2 L/HTCC substrate microstructure

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microstructure is effective; therefore, the beam structure needs to be removed inreverse. Figure 2 shows the L/HTCC substrate with integrated through-hole, cavity,beam structure, and microchannel, and the raw porcelain belt laser punchingmachine and its cutting schematic diagram as shown in Fig. 3.

At present, micron ceramic microstructure can be achieved by mechanicalpunching or laser punching, and machining precision can be controlled by control-ling cutting times and feed quantity. However, to meet the higher precision and sizeof micro devices requirements, automation equipment is difficult to finish at presentstage, for example, in the microchannel structure processing, if can be implementedin single layer ceramic substrate arbitrarily deep punching, makes the size ofmicrochannel is not limited to raw porcelain thickness, will greatly improve theceramic base microchannel processing and application ability.

Filling and Screen Printing ProcessThe filling process is mainly set up for the interconnection of circuits betweenmultilayer L/HTCC substrates. According to the device circuit design, interlayerinterconnection through-hole is cut at the corresponding position of each layer ofsubstrates through the punching process. However, it is impossible to achieve circuitinterconnection only through the through-hole, only in the through-hole filled withthe corresponding electronic paste, in order to ensure the formation of current path inthe insulation medium. Figure 4 shows the filling equipment and filling diagram ofL/HTCC microhole.

Generally, there are three different situations in the filling process. When thefilling slurry is insufficient, the gap filling is formed. At this time, the connectingthrough-hole and the slurry cannot be fully fitted, resulting in slurry falling off and

Fig. 3 L/HTCC substrate punching process

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filling failure in the subsequent process. When the slurry is overfilled, the through-hole cannot fully accommodate the slurry. In the subsequent lamination and lami-nation processes, the slurry is squeezed by the outside world, and the connectedthrough-hole wall is subjected to uneven stress from the slurry, resulting in thedestruction of the flexible substrate structure and the weakening of mechanicalproperties. When the slurry is filled with the interconnecting through-hole, a com-plete filling is formed, which is an ideal filling condition. The slurry can completelyfit the through-hole substrate without excessive extrusion on the through-hole walland damaging the structure of raw porcelain belt.

Screen printing in L/HTCC process is a simple process in which electronic metalpaste is formed on the base material through screen printing plate. According to thedesigned circuit layout, the screen printing plate is prepared, and the mesh ofthe screen printing plate can print the slurry to ceramic substrate. During printing,the pulp is put into one end of the screen printing plate, and a scraper is used to applycertain pressure on the pulp part of the screen printing plate. At the same time, thescraper moves toward the other end of the screen printing plate at a constant speed.During the movement, the electronic pulp is squeezed by the scraper from the layoutholes to the substrate, as shown in Fig. 5. Due to the limitations of sintering process,different substrate materials need to choose corresponding electronic pastes forprinting. For example, LTCC ceramic substrate can be co-fired with silver pastes,while HTCC ceramic substrate can be co-fired with platinum, tungsten, and otherelectronic pastes. Screen-printing technology has the advantages of low-cost, simplemethod and, through the automatic screen printing machine, can accurately controlcircuit part printing precision, thus forming electronic components or circuit design,such as planar spiral inductor and a parallel plate capacitor; fork refers to the capacityas well as passive components such as integrated circuit, the circuit design ofdifferent functions such as gate. As shown in Fig. 5, it is a fully automatic screenprinting machine. Currently, the common equipment repetition accuracy is 10 μm,the screen size is 550 � 550 � 25 mm, and the maximum scraper pressure is 300 N.

Limited by the screen printing plate manufacturing process, screen printing canachieve the minimum printing line width of 50 μm, for the smaller size of the circuit

Feedopening

Substrate

micro-vias

Ceramic tape Slurry

Incompletefilling

Perfect filling

Excessive fillingFilling diagramMicrospore filling machine

Fig. 4 Filling process and its coordination

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pattern, through the screen printing technology to achieve the metallization ofceramic substrate will become very difficult. In addition, due to the fluidity of thepaste itself, the circuit pattern printed on the substrate surface will spread, resultingin the actual printing size larger than the design size. For narrow wire, the fluidity ofthe paste may lead to short circuit of adjacent wire. Therefore, the consistency of thepaste is important for screen printing. As shown in Fig. 6, the thick slurry cannot passthrough the screen mesh, thus it is unable to complete the substrate metallization;However, if the slurry is too thin, the short circuit or open circuit of adjacentconductors will be caused by the fluidity.

Lamination ProcessLamination process is an important part of the interconnection between the layers ofthe electronic circuits of the C-MEMS devices, the self-packaging of the devices,and the microstructure forming. After the perforation process, filling process, and

Fig. 5 Screen printing technology

Sparseslurry Mesh Screen

plate

DenseSlurry Mesh

SubstrateSubstrate

Fig. 6 Effect of paste consistency on silk screen

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screen printing process, the sequence superposition of printed circuit patterns andmicrostructure flexible ceramic raw ceramic tape layers was carried out. The circuitpatterns of different raw porcelain belt layers are connected to each other throughfilled connection holes to ensure that the whole circuit pattern forms a path and ishighly integrated in the three-dimensional space, as shown in Fig. 7. Interconnectionlayer 1, interconnection layer 2, and interconnection layer 3 are connected to eachother through sequential lamination.

Lamination technology can realize the self-encapsulation of device circuit whilerealizing the interconnection of different substrate circuits. In Fig. 7, interconnectionlayer 3, as the top metallized ceramic layer, is extremely vulnerable to corrosion byhigh temperature, corrosion, and other harsh environments. In the long run, thecircuit part will fail, resulting in device damage. L/HTCC material has a goodanticorrosion performance, covering a layer of substrate above the top layer ofmetallized ceramic. Through lamination process, the circuit part is completelyencapsulated in the substrate, so as to avoid damage to the device by the externalenvironment. In addition, since L/HTCC raw porcelain belt itself is flexible, chang-ing the laminated mold can change the base material forming. By designing thesurface laminated mold and laminating the base material, the surface device blanksample can be obtained.

Lamination process is an important step in the preparation of C-MEMS devices.Therefore, the process and precision errors in the lamination process will reduce theyield of devices. As the circuit part first, printing with a raw porcelain layer iscovered for the preparation of microstructure flexible ceramic raw porcelain layer, inorder to prevent subsequent laminated microstructure has been damaged by the highpressure in the process, need to fill microstructure by sacrifice layer materials, asshown in Fig. 8, and filling process are similar, too big a sacrifice layer materials willsqueeze the edge of microstructure, its mechanical performance degradation, whilethe sacrifice layer materials is too small will be caused by a lack of bearing capacity,causes in the process of laminated microstructure to collapse. In addition, laminatedpositioning accuracy also affects device performance. Interlayer circuit connectionhole size is small, so even a small positioning error will lead to interlayer circuit

Package layer

InterconnectionLayer 3

InterconnectionLayer 2

InterconnectionLayer 1

lamination mold

Microstructurelayer

Package layer

InterconnectionLayer 3

InterconnectionLayer 2

InterconnectionLayer 1

lamination mold

Surface laminationPlanar lamination

Microstructurelayer

Fig. 7 Lamination process of L/HTCC substrate

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connection break. Figure 8 shows a fully automatic laminating machine with amaximum number of lamination layers of 80 and a maximum stack thickness of5 mm. The lamination accuracy can be controlled within 10 μm.

Lamination and Sintering ProcessLamination is one of the key technologies in the L/HTCC micro-group process.Appropriate lamination conditions can make each raw ceramic layer physicallyinterconnected, and then through the sintering process, the layers of the greenporcelain strip and the electronic paste are completely viscous. The principle ofbonding the raw ceramic is shown in Fig. 9. The raw ceramic is composed of ceramicparticles, glass components, and organic components, wherein the organic compo-nents are mainly binders. During the lamination process, the raw ceramic is phys-ically bonded together under a certain temperature and pressure, the organiccomponents become plastic, and the ceramic particles and the glass components ofthe respective layers are diffused and aggregated together with the applied pressure.The setting of the lamination conditions also affects the performance of the device ormicrostructure. Excessive pressure can cause the microstructure to collapse, whiletoo little pressure can’t compress the layers of the raw ceramic strip, resulting in theseparation of the layers of raw ceramic, as shown in Fig. 10. It is a laminator with amaximum applied pressure of 5000 Psi, a maximum pressure control accuracy of�50 Psi, a maximum application temperature of 85 �C, and a temperature controlaccuracy of �3 �C.

After lamination, the device is sintered at a high temperature, the filled sacrificiallayer is burned together with the organic matter in the ceramic sheet to become a gasdischarge, and the glass component is melted, so that the ceramic particles arebonded together, and at the same time, the glass composition in the metal pasteand the organic binder volatilizes, and the metal particles gradually expand to form aconductor. In the sintering process, it is necessary to explore and grasp the temper-ature curve, so that the timing of the rubber discharge is consistent with the high-temperature evaporation of the carbon film. The final purpose of the sintering is toturn the laminated raw ceramic into a dense whole and perfect the solid phase.During the sintering process, the melting of the glass components plays a crucial rolein the viscous flow of all the components in the raw sheets.

Cavityfilling

Beamfilling

Microchannel filling

Sacrificiallayer

Substrate

Microstructure collapse

Extrusion microstructureAutomatic laminating machine

Fig. 8 Fully automatic laminating machine and sacrificial layer filling

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The discharge of the sacrificial layer is related to the high-temperature changecharacteristics of the green porcelain strip. The green porcelain strip exhibits a looseporous surface state during the debinding process, and when the glass phase in thegreen belt is completely melted, the green ceramic sheet begins to become dense;therefore, the sacrificial layer needs to be completely discharged at the critical pointwhere the green tape is completely dense. The sacrificial layer volatilizes prema-turely, the flexible ceramic layer on the microstructure will collapse, and the sacri-ficial layer will evaporate too late, the ceramic layer will be dense, and the sacrificiallayer will not be discharged. This leads to cracks in the microstructure and evenbreaks up, as shown in Fig. 11. Therefore, in the sintering process, by adopting asuitable sintering process curve, it is necessary to ensure that the sacrificial layer isfully volatilized before the ceramic sheet becomes dense, and at the same time, thesacrificial layer is prevented from being volatilized too quickly, so that the flexiblemicrostructure cannot be self-supporting to collapse. The equipment shown inFig. 10 is a LTCC raw belt sintering furnace with a maximum sintering temperatureof 1050 �C, a maximum heating rate of 30 �C/min, and a temperature controlaccuracy of �3 �C.

For the curved structure, it is necessary to pay attention to the placement of thedevice during the sintering process and horizontally. Because the curved shape iswarped and suspended on both sides, the curvature of the sample will graduallychange or even become flat under the influence of gravity during the sintering

Alumina

Greentape

BinderWater pressure

Initialsintering

Particle

Solvent

Impurities

Conductor

Impurities

latersintering

Sintering of substrate and slurryLaminatedPunching

Lay 3

Lay 2

Lay 1

Pore

Fig. 9 Interlayer adhesion mechanism of L/HTCC

Fig. 10 L/HTCC laminator and its influencing factors

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process. In response to this problem, the effect of gravity on the surface can bereduced by placing it vertically, as shown in Fig. 12.

Based on the above preparation technology, a C-MEMS device with integratedtemperature, pressure, and vibration parameters was prepared, as shown in Fig. 13.In the device, three independent LC-sensitive loops interact with the test antennathrough the near-field coupling, respectively. When external factors cause the sen-sitive capacitance to change, the resonant frequency of the corresponding sensitiveloop drifts, thereby detecting the change of the external environment. In the layoutdesign of the sensor, the overlap between the coils is avoided, which is beneficial toweaken the electromagnetic interference between different resonant signals. Thefinal sensor has a test temperature of 20–800 �C and a temperature responsesensitivity of 9.13 kHz/�C. After testing, the current vibration signal period is1.89 s, and the pressure response sensitivity is 13.6 kHz/kPa.

Heterogeneous Material Co-firing Technology

In many special application environments, a single base material or electronic metalpaste is difficult to meet the test requirements. For example, during the high-temperature test, the sensitivity of the sensor is not high enough because the

Fig. 11 L/HTCC sintering furnace and sintering influencing factors

Horizontal placement

Surface structure

Surface structure

Gravity

Gravity

Burnt board

Burnt board

Vertical placement After sintering

After sintering

Fig. 12 Influence of placement mode on sintering

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dielectric constant of the L/HTCC substrate itself changes slowly with temperature.If a high-temperature substrate whose partial dielectric constant changes rapidly withtemperature can be co-fired with the L/HTCC substrate, the high-temperature testproblem can be solved, and high-sensitivity sensing can be realized. Heterogeneoussintering of electronic paste is also a very important technology. For example, in theultrahigh-temperature test, the thermocouple pair composed of different electronicpastes is tested for temperature. Therefore, the co-firing technology of heterogeneousmaterials plays a very important role in the testing of special environmentalparameters.

Co-firing of Heterogeneous Substrate Materials

The co-firing of the heterogeneous substrate material is a combination of two ormore base materials having different compositional compositions by micro-assembly and sintering processes to make them self-contained. Due to the different

Fig. 13 C-MEMS devices with integrated temperature, pressure, and vibration parameters

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thermal and mechanical properties of different materials, in the sintering process, asthe temperature increases gradually, the heterogeneous materials may be warped anddeformed. In order to avoid the above situation, it is necessary to study the sinteringmechanism of the heterogeneous material. Combining thermal material analysis andsintering kinetics analysis, the sintering kinetics model of heterogeneous co-firingwas established to provide a basis for the optimization of multi-material heteroge-neous co-firing system. The composition and microstructure of the co-firing inter-face of heterogeneous materials were studied. The interface behavior during theco-firing process of the material is combined with the electrical-mechanical perfor-mance test to study the influence mechanism of the interface properties of theheterogeneous material on the mechanical and electrical properties of the L/HTCCceramic MEMS device. The specific heterogeneous material co-firing researchprocess is shown in Fig. 14.

The biggest difficulty in co-firing of heterogeneous ceramic materials lies in thedifferent heat shrinkage rates and shrinkage directions of different materials. For thesame ceramic material, it is only necessary to face the same surface of each layer ofsubstrate in one direction during lamination, so that it can be guaranteed. During thesintering process, the green tape shrinks in the same direction without arching orcracking. For heterogeneous materials, different shrinkage rates result in differentrates of shrinkage and shrinkage of the foreigner strip, resulting in shear stress in thehorizontal direction, resulting in tearing of the substrate. In addition, if the hetero-geneous layer material shrinks in the opposite direction, the critical surfaces of thetwo materials will generate vertical stress, causing the substrate to swell and rupture.Figure 15 shows the situation after the zirconia green tape is laminated and sinteredwith the alumina green tape. After lamination, the heterogeneous layer is physicallybonded, and the substrate appears to have formed a whole, but after the sinteringprocess, due to the different heat shrinkage rate and shrinkage direction, the

Fig. 14 Study on heterogeneous co-firing mechanism

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aluminum oxide layer is completely separated from the zirconia layer, and theheterogeneous layer is broken due to the existence of shear stress, as shown inFig. 15.

Electronic Paste Heterogeneous Co-firing

The heterogeneous slurry is formed on the surface of the medium by screen printing.Due to the different thermodynamic properties of the different slurry and thesubstrate medium, the substrate may even rupture during the sintering process, asshown in Fig. 16. Different pastes are in contact with each other by a silk screenprocess, and after high-temperature sintering, different thermal stresses cause theheterogeneous electrodes to fall off, causing the device to fail.

In the sintering process, on the one hand, the sintering process curve should beadjusted to ensure that the chemical changes between different slurries and betweenthe slurry and the substrate can be carried out slowly and stably, preventing exces-sive chemical reactions and reducing the mechanical properties of the materials.Slowing the sintering rate of the substrate or slurry during the debinding process, theorganic matter discharged through the block causes the metal electrode to warp oreven fall off; on the other hand, it can be offset by the external physical pressure tooffset the high temperature between different materials. Thermal stress plays animportant role in the preparation of sensors, as shown in Fig. 17, since the weight ofthe base material itself is much larger than that of the electronic paste, in the sinteringprocess, the electronic paste may be placed facing the burning plate and the substratefacing upward, using the substrate itself.

The weight is used to offset the thermal stress between the different electrodes. Itshould be noted that when placed in this way, the setter is to be polished, as shown inFig. 18, to prevent the metal paste and the setter during the sintering process.Bonding results in damage to the circuit structure. Generally, in order to ensure themetal electrode and the debinding of the substrate, the substrate is placed facing theburning plate downward and the metal electrode upward, and at the same time,the metal electrode and the substrate material are pressed by the hole-bearing plate.

Fig. 15 Co-firing of alumina and zirconia

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This can offset the thermal stress from different materials due to the difference inthermodynamic properties while ensuring that the metal paste is fully degreased.

Integration of Multiple Processing Technologies

L/HTCC process technology can realize the preparation of ceramic-based devices,screen printing technology reduces the cost of ceramic metallization, and thesintering process can achieve complete bonding of metal circuits and ceramic sub-strates. However, for some metal or heterogeneous substrates with low melting point

Fig. 16 Heterogeneous co-fired electronic paste

Fig. 17 Heterogeneous co-firing placement

Fig. 18 Plate for heterogeneous co-firing

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or poor matching ability with ceramic substrates, bonding cannot be achieved bysintering process. Therefore, only a combination of various MEMS processingtechnologies can solve the above problems.

In the special test environment, traditional silicon-based integrated circuit com-ponents are prone to failure. Various types of gate circuits composed of ceramic-based diodes and transistors can replace silicon-based circuit components, solvingthe problem that silicon-based devices cannot achieve normal operation and opera-tion under special environments. However, in the preparation process of the transis-tor, due to the limitation of the material itself, the heterogeneous material cannot beformed by the sintering process, and the photolithography sputtering process canavoid the erosion of the material by the high temperature and achieve the bonding ofdifferent materials. This part takes ceramic-based transistors as an example toillustrate the C-MEMS devices formed by the combination of L/HTCC processand photolithography and sputtering processes.

The ceramic-based film diode needs to integrate different metal materials andsemiconductor materials on the ceramic substrate. Due to the characteristics of thesemiconductor material and the thickness of the metal layer, it cannot be formed byscreen printing and high-temperature sintering. The ceramic-based thin film diodestructure is shown in Fig. 19. The ideal barrier height of Schottky diode is thedifference between the metal and semiconductor work function, but the actual barrierheight is not only related to the preparation material but also affected by thepreparation conditions and process. Although the alumina ceramic sheet has a highhardness, it is brittle and brittle when the thickness is thin, so care must be takenduring cleaning. In addition, the cleanliness and roughness of the substrate have agreat influence on the workability of the semiconductor device. When cleaning, aplurality of ceramic sheets was placed in a petri dish. Figure 20 is a surface top viewof a mirror-polished 96% Al2O3 ceramic observed by SEM. It can be seen that evenwith mirror polishing, there are many micropores of about 2–3 μm on the surface ofalumina, which is three orders of magnitude larger than that of standard polishedsilicon wafers and silicon carbide. This is also one of the challenges in fabricatingMEMS devices on high-temperature-resistant alumina ceramics.

C-MEMS High-Temperature Device

Based on the above process and manufacturing technology, C-MEMS high-temper-ature devices were fabricated and tested at high temperature to confirm that theC-MEMS devices based on the above manufacturing process can meet the parametertesting requirements in special environments.

C-MEMS devices with integrated microstructures and circuits: Based on theL/HTCC process, an LC wireless passive temperature-pressure dual-parameter sen-sor is designed and fabricated (Ji et al. 2018; Li et al. 2014; Lu et al. 2018; Qiulinet al. 2018; Tan et al. 2015, 2017b, 2018).

The sensor compensates the temperature drift of the pressure signal through thetemperature-sensitive unit to achieve accurate calibration and measurement of the

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sensor. The sensor structure and test results are shown in Fig. 21. The sensorpressure-sensitive film thickness is 100 μm, so the sensor pressure response sensi-tivity is higher. The temperature-sensitive loop does not overlap spatially with thepressure-sensitive loop, which greatly facilitates weakening crosstalk between thecoils. The sensor temperature response sensitivity is 11.33 kHz/�C, and the pressureresponse sensitivity at room temperature is 73.59 kHz/kPa. At 1100 �C, the pressureresponse sensitivity increases to 92.98 kHz/kPa.

Heterogeneous substrate co-fired C-MEMS devices: The LTCC/ferroelectricceramic heterogeneous co-fired LC wireless passive temperature sensor enableslonger test distances and higher sensitivity temperature tests. On the basis of theL/HTCC ceramic micro-assembly process, the ferroelectric ceramic is filled into theLTCC substrate. Since the dielectric constant of the ferroelectric ceramic changeswith temperature, when the external temperature changes, the capacitance in thesensor LC circuit changes, causing the sensor resonance frequency to change.

Fig. 19 Ceramic-based thinfilm diode structure

Fig. 20 Ceramic-based thin film diode

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Sen

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Figure 22 shows the structure of a LTCC-based temperature sensor filled withferroelectric ceramics. By adjusting the sintering process, the ferroelectric ceramicsand the LTCC substrate are completely bonded. The two materials permeate eachother, and there is no deformation or crack due to different materials. The heteroge-neous co-fired C-MEMS device finally achieved a 700 �C high-temperature test, andthe sensor frequency sensitivity was 12.14 KHz/�C over the entire test range (Tanet al. 2014).

Heterogeneous slurry co-fired C-MEMS devices: The heat flow sensor struc-ture formed by co-firing platinum and platinum rhodium paste is composed ofthermocouple, distributed on the top and bottom of the ceramic substrate. The sensorstructure is shown in Fig. 23 (Lyu et al. 2018). Low thermal conductivity insulatorsare used to create temperature differences, which increase the electromotive forceoutput and increase sensitivity. The Pt electrode and the Pt/Rh electrode were wellconnected after sintering at 1350 �C, and the thickness and width of the thermocou-ple electrode were 22.59 μm and 195.71 μm, respectively. The test results show thatthe sensor’s maximum electromotive force output is as high as 6.74 mv and thetemperature sensitivity is about 8.9 μV/�C, which has high sensitivity in a given heatflow range.

C-MEMS devices combined with photolithography and sputtering pro-cesses: The Pt/a-IGZO/Al diode was successfully fabricated on Al2O3 substrateand tested by I-V at 20–400 �C (Guo et al. 2019). The diode can work stably at21–400 �C. At the same time, a thin film transistor suitable for up to 250 �C wasfabricated on an alumina ceramic substrate using MEMS technology, and a thin filmtransistor based on a ceramic material is shown in Fig. 23. The test results show thatthe device has good electron mobility and stability, the mobility μsat decreases from263.1 (293 K) to 250.3 (523 K), and the subthreshold swing SS increases withtemperature, increased from 83.4 mV/dec to 136.4 mV/dec, and on this basis, digitallogic circuits such as inverters, NAND gates, and AND gates that can operate athigher temperatures are designed and tested (Fig. 24).

Langasite Device Processing and Manufacturing Methods

Langasite (LGS) devices are mainly based on hard and brittle materials, such asplatinum (Pt), rhodium (Rh), iridium (Ir), and PtIr, TiN, WC, and other compositematerials which are commonly used at high temperatures as electrode materials

Fig. 22 LC temperature sensor for co-firing of heterogeneous substrates

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Low

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(Hornsteiner et al. 1998). This kind of device is mainly manufactured by hot pressingprocess in high temperature, mainly involving the manufacturing process includingetching, polishing, bonding, and other technologies.

High Temperature Forming Mechanism

Wet Etching Mechanism

Wet etching refers to the process of systematically removing materials by immersingsolid materials in liquid. Its removal rate can be adjusted by temperature. It is easy tocontrol the shape and thickness of the film. Wet etching can be divided into two

Fig. 24 Ceramic-based thin film transistor structure

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categories: isotropic etching and anisotropic etching. Isotropic etching refers to theremoval of materials in all directions at the same speed. Most etchants belong to thiscategory. Anisotropic etching is a process in which etchants remove materials atdifferent speeds according to the exposed crystal plane (Gaura and Newman 2006).

Wet chemical etching of La3Ga5SiO14 is usually carried out in a mixed solution ofHCL and HF. The specific process is as follows: Firstly, La3Ga5SiO14 reactswith HCL.

La3Ga5SiO14 þ HClþ H2 ! SiO2 þ LaCl3 þ H2Oð Þ þ GaCl3 (1)

Then, hydrofluoric acid removes silicon oxide.

SiO2 þ 6HF ! H2SiF6 þ 2H2O (2)

Therefore, the total reaction equation is obtained by etching langasite in themixed solution of HCL and HF, as shown in Fig. 25.

La3Ga5SiO14 þ HClþ HFþ H2O ! H2SiF6 þ LaCl3 þ 7H2Oð Þ þ GaCl3 (3)

The effects of hydrofluoric acid and hydrochloric acid solutions with differentconcentrations on corrosion rate and roughness were studied. The results show thatthe combined corrosion rate of hydrofluoric acid and hydrochloric acid can reachabout 60 mm/h when HF accounts for 10% of the solution, and the batch micro-fabrication can be realized. At this time, the roughness is about 200 nm, which still

Fig. 25 Wet etchingschematic of LGS

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meets the design requirements. In addition, the mixed solution of hydrofluoric acidand hydrochloric acid can achieve isotropic corrosion of La3Ga5SiO14, which helpsto reduce the roughness of the device (Ansorge et al. 2011).

Dry Etching Mechanism

Dry etching refers to the removal of materials by chemical reaction between alow-pressure gas and the base (Gaura and Newman 2006). Inductively coupledplasma etch (ICPE) is the result of the interaction of chemical and physical pro-cesses. Its basic principle is that the RF generated by ICP RF power supply is outputto the ring coupling coil under vacuum and low pressure. A high-density plasma isproduced by coupling glow discharge of coil etched gas in a certain proportion. Theplasma bombards the substrate surface under RF (radio frequency) of the lowerelectrode. The chemical bond of the semiconductor material in the pattern area of thesubstrate is interrupted, and the volatile substance is formed with the etched gas,which is separated from the substrate in the form of gas and extracted from thevacuum pipeline. Figure 26 shows an Oxford instruments ICP CVD.

Dry etching of La3Ga5SiO14 is usually done by Cl2/Ar ICP. As the rate of vaporphase corrosion increases linearly with the increase of chlorine content in plasma(from 20% to 70%), it is inferred that Cl2 is chemically corroded to the material.Physical sputtering of La3Ga5SiO14 and corrosion residues is caused by Ar gas(Giehl et al. 2003). The reaction equation is described as follows (Cho et al. 2007).

La3Ga5SiO14 þ 13Cl2 ! 3LaCl3 þ 3GaCl3 þ 2GaCl2 þ SiCl4 þ 7O2 (4)

In the process of Cl2/Ar ICP discharge, the etching rate of single crystalLa3Ga5SiO14 wafer is affected by plasma composition, plasma source power, andradio frequency chuck power. The maximum corrosion rate can reach 160 nm/min atrelatively high source power (~1000 w) or high Cl2 content. In most cases, the

Fig. 26 Oxford instrumentsICP CVD

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surface roughness of etched La3Ga5SiO14 is similar to or even better than that ofnon-etched wafers.

Bonding Mechanism

Bonding refers to the process of making patterns on the substrates of severalmaterials and contacting them closely to form a complex structure (Gaura andNewman 2006). The most commonly used wafer bonding types in microstructuralfabrication can be divided into three categories: direct bonding, anodic bonding, andinterlayer bonding. Among them, direct bonding is most commonly used. Directbonding refers to the direct contact of wafers .There is no intermediate layer,adherence of smooth surfaces, and some form of thermal cycle after contact toimprove bonding strength. The highest annealing temperature is below 450 �C orabove 800 �C (Schmidt 1998).

Direct bonding consists of three steps: surface preparation, pre-bonding, andpermanent bonding. The first step is surface preparation. The process is to cleantwo wafers to make their surfaces smooth enough to form a hydrated surface. Thesecond step is pre-bonding. In a clean environment, two wafer surfaces are contactedand pressed together by gentle pressure at a central point to form a bond between OHbases on the relative surface. The contact points are bound by the surface gravity oftwo water-bearing surfaces. The contact waves start from this point and sweep acrossthe wafer surface to make them close to each other on the whole surface. The thirdstep permanent bonding is to heat the wafer and expel water molecules from thesystem to form strong bonds. The usual annealing temperature is between roomtemperature and 1200 �C.

According to the above direct bonding process, the LGS bonding process is asshown in Fig. 27, firstly performing hydrophilic treatment, so that the surface of thesubstrate adheres to the -OH group, and then pre-bonding, so that the two surfacesare in close contact, and finally the high-temperature annealing is performed toachieve permanent bonding.

Among them, the pre-bonding and high-temperature bonding process is com-pleted in the temperature-pressure integrated controllable loading vacuum

Substrate 1

Substrate 2

0.5 MPa

1000°c

Atomic diffusion

150°c

O OO

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Fig. 27 Inductively coupled plasma etching of LGS

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hot-pressing furnace independently developed by North University of China, asshown in Fig. 28. The furnace can also be used for pressure sintering of variousceramics and nano-materials. The high-temperature furnace device heats the LGSsubstrate through an electrode and adjusts the heating rate by controlling the power.Pressure is applied to the workpiece by a hydraulic pump and pressure headdisplacement control system. In addition, in order to ensure the verticality, a columnconnection is also provided on the table and the movable beam of the hot pressfurnace. Most importantly, the hot press furnace can provide a vacuum environmentfor the substrate bonding to form a vacuum-sealed cavity, which is beneficial toimprove the performance of the sensor device.

LGS Device Sealed Cavity Manufacturing Technology

The formation of LGS sealed cavity is a key problem that SAW multiparametersensor needs to solve urgently in harsh environments such as high temperature, highrotation, and high pressure. First, the etching of the LGS cavity can be achieved bytwo methods: wet etching and inductively coupled plasma (ICP) etching, followedby surface polishing and bonding to complete cavity fabrication.

Wet Etching Process

The specific process steps of wet etching are shown in Fig. 29:

1. First, the gallium silicate lanthanide wafer was cleaned with acetone, isopropylalcohol, and a mixed solution of H2O2 and H2SO4 and heated at 150 �C for

Fig. 28 The temperature-pressure integrated controllable loading vacuum hot-pressing furnace(Li et al. 2017)

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20 min to remove the organic matter remaining on the surface of the galliumsilicate.

2. SU-8 photoresist was spin coated onto the surface of the gallium silicate germa-nium wafer. Among them, the thickness of the photoresist is 200 μm, whichprevents the adhesion problem caused by the passage of acidic molecules throughthe photoresist. In order to solve the problem of poor adhesion of the photoresistto the edge of gallium silicate, an HDMS layer is deposited on the surface of thegallium silicate wafer to enhance the adhesion of the photoresist.

3. Place a reticle, perform photolithography, develop, and clean it with deionizedwater.

4. Prepare a mixed solution of hydrochloric acid and hydrofluoric acid (HCl:HF:H2O = 1:1:2), and heat to 80 �C. The LPS coated with photoresist is etched. Thisacid mixture makes the surface of LGS smooth and has a faster corrosion rate; HFcan dissolve the SiO2 formed by the reaction, maintaining the surface flatness ofthe LGS wafer. The temperature in the reaction tank has an important influence onthe corrosion rate.

5. After the gallium silicate ruthenium is etched for a period of time, it is cleaned bydeionization, then the SU-8 photoresist is peeled off, the corrosion effect isobserved by a microscope, repeated tests are performed to determine the optimaletching time of the LGS, and finally the obtained LGS cavity is required.

Inductively Coupled Plasma (ICP) Etching Process

Using inductively coupled plasma (ICP) etching, as shown in Fig. 30, the substrate iscleaned with deionized water, alcohol, and acetone to remove dust, oil, and organicmatter from the surface of the piezoelectric substrate; using silicon dioxide as a hardmask material, the LGS wafer with a mask is placed in a plasma etching zone, andions in the gas in the reaction chamber are bombarded by the flat pressure of thereaction chamber to form a damaged layer.

Fig. 29 Wet etching process flow chart of LGS

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Thereby, the free reactive groups in the plasma are accelerated on the surfacethereof, and the ion bombardment reflects the anisotropy of the dry etching, and thereaction of the free radicals is well suppressed due to the deposition of the sidewalls.The LGS cavity is etched by continuously adjusting the process chamber pressure,the upper RF source power, the lower RF source power, the helium back pressure,and the flow rate. Due to the unique combination of physical and chemical reactionsof dry etching, the size and shape of the pattern can be precisely controlled under theinteraction of anisotropic and isotropic.

Surface Polishing and Bonding Process

The three-dimensional structure of the LGS with the sealed cavity is realized bybonding with the etched LGS cavity. Prior to bonding, the pre-bonded LGS substrateis first surface-polished to reduce the surface roughness of the substrate, followed bya hydrophilic surface treatment including wet cleaning and plasma treatment. TheLGS substrate was wet-cleaned with acetone, alcohol, piranha solution (SPM),standard cleaning solution No. 1 (SC1), diluted hydrofluoric acid solution, anddeionized water. Subsequent surface activation of the LGS substrate by oxygenplasma can also achieve the purpose of eliminating wafer surface contaminationand further reducing surface roughness.

After the above surface treatment, direct pre-bonding is performed by using thepolished surfaces of the two LGS substrates, as shown in Fig. 31a. The pre-bondedsample is fixed in a graphite mold and then placed in a sleeve and fixed in a sinteringfurnace to pressurize the upper and lower surfaces in the vertical direction, and thewhole is subjected to a heating experiment to achieve permanent bonding of thesample, thereby obtaining a sealed LGS cavity. In the pre-bonding process, the -OHgroups of the two bonding faces are bonded, and in a high-temperature environment,water molecules between the two bonding faces are ejected to form a permanentbond. As shown in Fig. 31b, a sealed cavity is formed.

Fig. 30 Plasma etching process of LGS

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LGS Device Surface Graphic Manufacturing Technology

Integrated design of SAW multiparameter resonator/antenna is based on LGS pie-zoelectric material. The three-dimensional structure of LGS with sealed cavity isrealized by inductively coupled plasma etching technology and bonding process, theback-receiving antenna is fabricated by screen printing process, and the electrodesurface acoustic wave resonator is fabricated by ion plating process. Figure 32 is aprocess flow diagram of the SAW multiparameter resonator/antenna integratedfabrication. This method is applicable to the manufacture of all surface acousticwave sensors. The specific steps are as follows:1. Experimental preparation and pretreatment: The base piezoelectric material used

in the experiment was washed with freshly prepared piranha solution for 15 min,ultrasonically washed with ethanol for 5 min, and ultrasonically cleaned withacetone for 5 min. Finally, the surface of the deionized water is ultrasonicallycleaned for 5 min to clean the surface, which can effectively remove the adhesionof organic substances (such as grease) on the surface of the piezoelectric substrateand enhance metal adhesion in subsequent metal sputtering.

2. The fabrication of the cavity: the manufacture of the LGS sealed cavity by wetetching and plasma etching combined with bonding process.

3. Mask electrode fabrication: A photoresist is coated on the surface of the piezo-electric material, and a mask having an electrode pattern is overlaid on the surfaceof the photoresist and exposed to ultraviolet light. After the exposed photoresist issubjected to development processing, a mask pattern window is formed on thephotoresist.

Substrate 1

Substrate 2

AtomicdiffusionLGS crystal

SiLaGaO

Pressure

High temperature&

High pressure

Pressure

LGS

Graphite molda

b

Fig. 31 (a) Bonding process of LGS cavity; (b) schematic diagram of atomic diffusion

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4. Fabrication of the antenna: The screen printing process was carried out by using aplatinum-rhodium paste to realize the antenna printing on the lower surface of thepiezoelectric material and placed in a muffle furnace at a low temperature of100 �C for low-temperature sintering.

5. Lead connection: The through hole is filled with platinum paste to realize theelectrical connection between the antenna and the SAW sensor, and the wholedevice is placed in a high-temperature sintering furnace to be sintered accordingto a specific heating curve.

6. Fabrication of surface electrode: The metallization of the surface acoustic wavesensor platinum-ruthenium electrode is realized by ion plating process, and theion plating device is developed in acetone to obtain a complete metallizedelectrode.

7. Annealing treatment: The surface acoustic wave device is treated by annealing.First, rapid annealing is performed in an N2 atmosphere to form an ohmic contactbetween the electrode and the substrate material, thereby improving the electricalperformance of the electrode. Then, the device is placed in a high-temperaturefurnace for conventional annealing, and the electrode is aged to improve thestability of the electrode in a high-temperature environment.

8. A protective layer film and an absorbing material are applied to the surface ofthe LGS.

Fig. 32 Integrated multiparameter SAW sensor/antenna integrated manufacturing process

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SAW Temperature and Pressure Integrated Devices

The lithium niobate-based SAW temperature and pressure integrated sensor based onthe above process are shown in Fig. 33. Among them, the temperature sensor canmeasure 25–325 �C. The resonance frequency decreases with the increase of tem-perature, showing a negative temperature change trend. The temperature sensitivityof the temperature resonator is 1.41 KHz/�C, and the temperature sensitivity of thepressure resonator is 1.34 KHz/�C. The test range of the pressure sensor is0–1000 gf, and the maximum sensitivity of the pressure at 25–200 �C is10.6 KHz/100 gf.

Summary

This chapter introduces the flexible material processing and manufacturing technol-ogy represented by C-MEMS devices and the hard and brittle material processingand manufacturing technology represented by LGS devices. C- MEMS devices canbe fabricated by a mature L/HTCC micro-assembly process. Combined with hetero-geneous co-firing and traditional MEMS processes, multifunctional integrateddevices can be fabricated. However, compared to conventional silicon devices,the miniaturization process of C-MEMS devices still needs to be improved. LGSdevices currently have processing techniques such as wet etching, inductivelycoupled plasma etching, bonding, etc. Although LGS devices can be processed,how to process high-precision, miniaturized, and integrated devices still facesserious challenges. For example, in the process of wet etching, how to configurethe solution ratio so that the corrosion rate can be controlled and the surface

Fig. 33 SAW temperature and pressure integrated device

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roughness can be reduced to realize the balance between work efficiency andfinished product quality is one of the difficulties; in inductively coupled plasmaetching, it is also a difficult problem that how to control the composition of theetching gas, the power of the plasma source, and the power of the RF chuck to realizethe precise etching of the langasite micro-/nano-structure, and in the bondingprocess, how to eliminate the voids formed during the high-temperature annealingis also an urgent problem to be solved.

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