study of functional coating preparation on ceramic materials

STUDY OF FUNCTIONAL COATING PREPARATION

ON CERAMIC MATERIALS

E. I. Suzdal’tsev,1 D. V. Kharitonov,1 and A. A. Anashkina1

Translated from Novye Ogneupory, No. 10, pp. 38 – 47, October 2011.

Original article submitted August 8, 2011.

Results are presented for a study of functional coating application, for example with increased blackness coef-

ficient, on ceramic and glass ceramic materials. Various methods for coating application used currently are

considered. A coating is proposed based on methyl phenyl spirocyloxane polymer (product MFSS-8).

Keywords: quartz ceramic, glass ceramic, coating, blackness coefficient, modified material surface, product

MFSS-8.

In the construction of objects experiencing the action of

high-temperature gas streams there has been extensive use of

composite, ceramic, and glass ceramic materials. Particular

interest in this case are rocket nose cones, which during oper-

ation experience action of high-temperature (above 1000°C)

and pressure, which cause significant destruction of a struc-

ture, including simultaneous evaporation, sublimation, com-

bustion, and movement of cracked and melted material parti-

cles. In view of this a basic requirement which is laid down

for the materials indicated above is absorption by a compara-

tively small volume of removed mass of a considerable part

of the heat, entering a structure due to aerodynamic heating.

This requirement may be fulfilled with use of materials ex-

hibiting:

– good heat insulation properties, a capacity to localize

heat in a thin surface layer and thereby retain the main

physicotechnical properties of the whole thickness without

change. In this connection favorable material properties are

porosity, property anisotropy, opaqueness for thermal beams;

the most promising materials are based on SiO2, ZrO2, Si3N4,

SiC, etc.;

– the possibility of a change-over from a solid or vis-

cous liquid condition into a gaseous condition, when the

gases formed increase the thickness of a boundary layer and

are capable of shifting the thermal fluxes applied. The best

ablation materials are those with considerable heat of evapo-

ration: graphite, boron nitride, silicon oxide;

– a capacity for formation at a heated surface of a liquid

film with high viscosity, preventing blowing away (removal)

of a liquid phase by a thermal flux; the most promising mate-

rial is silicon oxide, whose viscosity above 2000°C is at the

level of 106 Pa·sec;

– good radiating capacity. Secondary radiation from a

surface leads to a reduction in the overall amount of heat en-

tering a structure. Even a small increase in material radiation

capacity (~0.1) is capable of reducing the rate of mass re-

moval in the entry path of a satellite into the dense atmo-

sphere by about 20% [1, 2].

It should be noted in considering the question of using

ceramic materials in structures for nose cones that quartz ce-

ramic and glass ceramic, having a series of favorable proper-

ties (high mechanical strength, low level of thermophysical

property indices, high heat resistance), exhibit a low degree

of blackness (the blackness coefficient for these material is

within the limits 0.15 – 0.17 un.). In view of this a require-

ment arises for increasing their radiating capacity in order to

increase their stability under the action of high-temperature

gas streams. In this case with quartz ceramic, having open

porosity of 8 – 10%, and additionally with an increase in

blackness coefficient, it is necessary to resolve questions

with respect to material water repellence.

Quartz ceramic has been used in production for quite a

long time (almost from the middle of the last century), and

therefore questions of increasing its operating capacity have

received much attention. One method used for increasing the

blackness coefficient was introduction into original quartz

glass of various alloying additions. In [3 – 10] there is a de-

tailed study of the possibility of alloying quartz glass with

additions of different oxides. The possibility has been dem-

onstrated of a marked change in its physicotechnical proper-

Refractories and Industrial Ceramics Vol. 52, No. 5, January, 2012

340

1083-4877�12�05205-0340 © 2012 Springer Science+Business Media, Inc.

1FGUP ONPP Tekhnologiya, Obninsk, Kaluga Region, Russia.

ties, including radiation capacity. However, as shown in [11],

the radiation intensity is determined not only by the degree

of material blackness, i.e., its transparency, but also surface

temperature. As applied to quartz glass the surface tempera-

ture determines melt viscosity. Here additions introduced,

with a capacity to effectively “darken” the quartz glass,

could not reduce its viscosity, and this is almost impossible

to achieve.

All of the above-mentioned effects, capable of leading to

an increase in the radiating capacity of quartz glass, may ade-

quately be extended to quartz ceramic. In [1] it is proposed to

introduce chromium oxide into a quartz glass slip. On intro-

ducing up to 2% Cr2O3 into a slip the rheological behavior of

the suspension and porosity of castings remains at the previ-

ous level. A subsequent increase in them due to bonding of

Cr2O3 particles with free water causes an increase in viscos-

ity, and therefore starting with an addition in an amount of

3% water was added at the rate of 20% of the weight of an

addition, and with 5% addition it was 50% water. A conse-

quence of introducing an additional amount of water is a re-

duction in slip solid phase consistency, increasing casting po-

rosity and reducing strength.

Based on results of work for increasing the radiating ca-

pacity of quartz glass, similar work was carried out for in-

creasing the blackness coefficient of glass ceramic. In [12]

modification of glass ceramic with addition of Cr2O3 is pro-

posed. The addition is made directly to a slip before molding

billets. Thereby there is a reduction in temperature and soak-

ing time [5]. In addition, as studies have shown, addition of

Cr2O3 does not effect the dielectric properties of glass ce-

ramic and increase the blackness coefficient. However, intro-

duction of an addition in an amount mote than 0.7 wt.%, the

same as in the case of quartz ceramic, has a marked effect on

the original porosity, significantly increasing it. In view of

this in order to resolve the problem of increasing blackness

coefficient for glass ceramic billets before firing it was pro-

posed to apply Cr2O3 to the surface of a molded billet with a

concentration of it in water from 40 to 60 wt.% [13]. This

method appears to be quite effective for reducing the firing

temperature (by about 100°C), although its use for increasing

the blackness coefficient for finished objects is problematic

due to lack of adhesion of Cr2O3 to shell material.

In view of this it is interesting to carry out work for mod-

ifying the surface of ceramic and glass ceramic objects.

Surface modification is a change in surface properties

and material surface zone with the aim of improving a broad

range of functional properties and material and object char-

acteristics (physical, chemical, optical, electrical, electronic,

magnetic, etc.) [14]. Available methods for surface differen-

tiation may be separated into two main groups: a change in

the surface layer and coating application.

In the first group there are also methods such as anodic

oxidation, diffusion impregnation, ion nitriding, ion implan-

tation, and ion atomization. This field of surface modifica-

tion is used during ion-volumetric strengthening of lithium

aluminosilicate glass ceramic in sodium nitrate salt [14, 16].

In view of existing limitations for the choice of materi-

als, suitable for use in technology of changing a surface, of

greatest interest are methods for coating application, i.e., ar-

tificially formed at the surface of an object, or a structure of

layers differing from the base material with respect to com-

position and physicochemical properties.

With respect to the position at a surface of a coating they

are separated into stratified, i.e., formed at the outer surface

of an object or structure having a sharp interface with the

base, and diffusion (or substitution), i.e., coatings formed

due to introduction into a material base without a marked

change in the initial object dimensions.

With respect to purpose coatings are divided into protec-

tive, production, and structural. Protective coatings provide

more prolonged component operation under working condi-

tions, production coatings protect the surface of an object

during production processing; by means of a structural coat-

ing the size and shape of an article is restored, the properties

are provided for its surface, and these coatings may fulfil the

role of structural materials. From most interest from the point

of view of use for coating application on ceramic materials

are the following methods: CVD. PVD, gasothermal deposi-

tion, application of paint and varnish materials.

CVD-coating (chemical vapor deposition) is a chemical

coating applied by a vapor [17]. The coating application pro-

cess is carried out by supply of gaseous reagent in a treat-

ment chamber, where it is in contact with the surface of a bil-

let. The CVD method has almost no limitations with respect

to coating chemical composition. All particles present may

be deposited at a material surface. What coatings form de-

pends on a combination of material and process parameters.

If the process proceeds with filling of space with a reaction

gas (oxygen, nitrogen, or hydrocarbon), then there is forma-

tion of oxide, nitride, and carbide coatings. There is chemical

reaction between atoms of deposited metals and molecules of

reaction gas. The composition of a coating depends on the

partial pressure oft eh reaction gas and coating deposition

rate.

For occurrence of required chemical reactions a tempera-

ture is necessary up to 1100°C. This condition markedly lim-

its the number of materials to which it is possible to apply

coatings by the CVD method. Due to the high deposition

temperature, providing partial diffusion of coating material

into a material base, CVD coatings have the best adhesion to

the base material.

In addition, in order to obtain uniform coating properties

it is necessary to provide optimum gas flow throughout the

whole volume of a device. A special system is used in this

case for gas supply, a so-called shower, and in order to pre-

vent dangerous gas discharges into the atmosphere the device

is fitted with a filter system.

A PVD coating (physical vapor deposition) is deposited

by condensation from a gas phase or as it is still called, the

method of physical deposition [14, 17]. The coating material

is converted into a gas phase from a solid state as a result of

evaporation under the action of thermal energy or as a result

Study of Functional Coating Preparation on Ceramic Materials 341

of atomizing due to kinetic energy of material particle colli-

sion. Energy, and the distribution of density of a particle

stream, are determined by application and process parame-

ters, and the shape of a particle source. The process occurs in

three stages: creation of vapor phase particles, transfer of

particles to a surface, and growth of a film at a surface.

Coating by the PVD method is performed at low temper-

ature (up to 450°C), which does not lead to significant limita-

tions with respect to material, to which a coating is applied.

All of the processes occur in a vacuum or in a working gas

atmosphere at quite low pressure (about 10–2 mbar), which is

necessary in order to facilitate transfer of particle from a

source (target) to an object (substrate) with the minimum

amount of collisions with gas atoms or molecules. This con-

dition also determines the necessity of direct particle flow.

As a result of this a coating is only applied to that part of an

object that is aimed at the particle source. The deposition rate

(rate of coating application) depends in this case on the rela-

tive position of source material. For uniform coating applica-

tion it is necessary to move the material systematically or use

some specific way of positioning sources. At the same time a

coating is only applied at the surface “in direct view of a

source”, leaving an adjacent region of a surface without a

coating. This is absolutely impossible with use of a chemical

deposition method [17].

Coating quality, applied by physical deposition, is deter-

mined by the basic purity of the starting materials, required

level of vacuum, and reaction gas purity.

Gasothermal deposition (thermal spraying) is a process

of heating, dispersal, and transfer of condensed particles of

atomized material by a gas or plasma stream in order to from

at a substrate a layer of a specific material [18]. Under the

general term “gasothermal deposition” (GTD) the following

deposition methods are combined: gas flame, high-velocity

gas flame, detonation, plasma, deposition with facing, elec-

tric metallization, and activated electric arc metallization.

The essence of gasothermal deposition involves fusion of

coating material (wire or powder) followed by application

(deposition) of it on a base in a gas stream. In the microzone

of particle impact of a melt over a coated surface they de-

form and spread, subsequently adhering to each other; by so-

lidifying, the material forms a flat coating layer. The bond of

deposited particles with a base occurs due to thermal and ki-

netic energy, which are determined by the temperature and

movement velocity of the particles. A bond of coating with a

base is adhesive. It is accomplished due to intermolecular

forces and mechanical adhesion of a coating with roughness

of a developed surface. The same as in the PVD method,

coatings are only applied to that part of an object that is

aimed towards the particle source.

In spite of the fact that by all of the methods in question

it is possible to apply different forms of coating on objects

and structures made of ceramics and glass ceramic materials,

they are not free from a marked disadvantage, i.e., the com-

plexity and expense of industrial equipment. This situation is

complicated by the fact that production of ceramic nose

cones is as a rule small scale with existence of a considerable

range of objects, and different standard sizes, which also

complicates the construction of the devices described above.

The simplest and cheapest in use and introduction into coat-

ing application technology on nose cones are paint and var-

nish coatings.

Paint and varnish materials (PVM) are multicomponent

compositions (liquid, paste, or powder), which on applica-

tion by a thin layer to a solid substrate provide formation of a

painted coating with prescribed properties. With respect to

composition and purpose PVM are separated into lacquers,

primers, putties, paints (including enamel). The main re-

quirements for a protective coating are high adhesion to a

substrate, absence of gas and water permeability, mechanical

strength, wear resistance and resistance under operating con-

ditions (atmospheric chemical resistance, etc.).

As film-forming organosilicon enamels lacquers are used

containing different substitutions for the silicon atom, i.e.,

methyl, ethyl, phenyl. It is possible to obtain polyorganosilo-

xanes from elastic to soluble with a different polyorgano-

siloxane structure in relation type and ratio of substitute. The

CH3 group in polyorganosiloxanes gives a coating atmo-

sphere resistance and hydrophobicity. With introduction of

C6H5 groups to polyorganosiloxane there is an increase in

heat resistance and hardness [19].

As protective LVM for rocket noses there is currently

widespread use of enamels FP-566 and KO-5189. In spite of

the fact that the blackness coefficient of these materials is

0.80 – 0.90 un., their operating temperatures do not exceed

250 – 450°C, and under the action of high temperature com-

bined with considerable aerodynamic loads, during operation

of objects these coatings are removed from a cone surface.

Monitoring of contemporary LVM has not revealed ma-

terials with a capacity to increase markedly the blackness co-

efficient of objects made of ceramic materials, to retain high

adhesion to a material substrate under conditions of action of

a high temperature, to provide their water repellence, and di-

electric property stability. A search for ways and methods for

obtaining coatings on ceramic and glass ceramic materials

with a set of functional properties remains important.

In choosing a film-forming component for a proposed

coating many years of operating experience with use of

quartz glass was considered, which requires sealing and

moisture repellence, since after firing this material it has

open porosity of 8 – 10%. For example, in [1; 20 – 24, pp.

302 – 307; 25 – 27] versions are presented for strengthening

and moisture repellence for quartz ceramic with different

organosilicon resin compositions. Most widespread is im-

pregnation of quartz ceramic with products TMFT (solution

of titanium organosilicon oligomer of phenolformaldehyde resin

and butyl ester of boric acid in acetaone, TU 6-02-933–79)

and MFSS-8 (solution of polymethyl spirocyloxane in ace-

tone, TU 6-02-1352–87 or TU 2229-001-64570284–2011).

Here strengthening and moisture repellence of ceramic

occurs due to forming within pores and at the surface of im-

pregnated material a thin polymer film, which covers the

342 E. I. Suzdal’tsev et al.

pore channels formed, and which also provides reliable pro-

tection of the ceramic from moisture. As a result of this

moisture repellence process due to surface impregnation

with products TMFT and MFSS-8 they are used extensively

in the production of cones made of glass ceramic [1].

In spite of the fact that both products are well recom-

mended as impregnating solutions for preparing sealed and

moisture repellent quartz ceramic, of greatest interest is

product MFSS-8, and this is due to the fact that during opera-

tion of objects in the range 250 – 700°C as a result of de-

struction TMFT with formation of carbon there is loss of ra-

dio transparency of an object, and at above 700°C the mate-

rial acquires its original values [1]. Destruction of product

TMFT at elevated operating temperature has led to the situa-

tion that impregnation of cones made of quartz ceramic is

only accomplished from the inner side, whose temperature is

markedly lower than that of the outer surface [21, 22].

The product MFSS-8 also burns at above 700°C, al-

though during its destruction there is no substance formed

perceptible for radio transparency, which makes it possible to

MFSS-8 for impregnating the outer surface of shells [23].

Similar impregnation of quartz ceramic by other impregna-

tion substances with product MFSS-8 provides sealing of

material only due to a thin surface film, whereas during poly-

merization there is “cross linking” of the polymer structure

with formation of a spatial siloxane skeleton [1].

In order to evaluate the possibility of using these coat-

ings for ceramic and glass ceramic materials, a mixture of

product MFSS-8 and an oxide, i.e., CoO, Cr2O3, TiO2, was

used. The mixture obtained was applied to specimens of

quartz ceramic and glass ceramic in order to determine the

ultimate strength in static bending �ben, and dielectric proper-

ties: dielectric permittivity � and the dielectric loss angle tg�.

Then polymerization was performed in order to fix the

layer on a specimen. Data for the change in basic material

properties before and after coating application are presented

in Table 1. Data are also given there for water absorption w

of an applied layer.

As seen from the data presented in Table 1, by applying

coatings of CoO and Cr2O3 it is possible to increase consid-

erably (up to 0.85 – 0.90) the blackness coefficient. Use of

TiO2 as a filler material does not lead to such a marked re-

sult, and the blackness coefficient obtained for a coating is

0.33 – 0.34. Here dielectric properties of both quartz ceramic

and glass ceramic in relation to form of coating are un-

changed. The ultimate strength in bending increases by about

10% of the original for glass ceramic and by 30 – 40% for

quartz ceramic.

Then the ceramic and glass ceramic specimens obtained

with coatings applied to them were subjected the action of

the temperature range 500 – 1250°C with soaking at the

maximum temperature for 60 sec. Property indices were de-

termined for specimens treated in this way (Table 2).

Analysis of data presented in Table 2 makes it possible to

conclude that all the coatings proposed are capable of operat-

ing up to 1250°C. Here neither strength nor dielectric proper-

ties of material undergo any marked changes (all of the

amount of deviations are within the limits of procedural er-

ror). Water absorption of the coating layer itself is also un-

changed. However, with visual examination of specimens of

glass ceramic with a coatings based CoO and TiO2 treated

from 900°C and above it is possible to observe breakdown of

coating integrity (swelling and crumbling), particularly for

cobalt oxide (Fig. 1). At the same time, a coating based on

Cr2O3 does not lose its high adhesion properties even with a

heat treatment temperature of 1250°C.

Worsening of adhesive capacity of the test coatings is

connected with the fact that at 900°C there is destruction of

product MFSS-8 and all of the organic phase evaporates.

This is indicated by data in Table 2, in which it may be seen

that there is an insignificant increase in tg� at 900°C. Up to

this temperature MFSS-8 is present within the system and

this unites coating particles into a single system. Above


TABLE 1. Dependence of the Level of Change in Glass Ceramic OTM 357 and Quartz Ceramic NIASIT Properties and Coating Quality

Material Coating on baseBlackness

coefficient

Specimen properties

original* with coating

tg� � tg� � �ben

, MPa Wcoating

, 10–3 %

OTM 357 Uncoated 0.16 0.011 7.21 — — — —

MFSS-8 + CoO 0.90 0.011 7.08 0.011 7.10 136 4

MFSS-8 + TiO2 0.33 0.011 7.14 0.010 7.12 141 6

MFSS-8 + Cr2O3 0.85 0.012 6.94 115 6.94 140 2

NIASIT Uncoated 0.14 <0.0005 3.40 0.0003 3.41 64 5

MFSS-8 + CoO 0.91 <0.0005 3.41 0.0003 3.40 58 3

MFSS-8 + TiO2 0.34 <0.0005 3.42 0.0010 3.42 67 2

MFSS-8 + Cr2O3 0.84 <0.0005 3.41 0.0003 3.42 60 4

* Ultimate strength in bending for original OTM 357 material specimen is 130 MPa, and for original NIASIT material specimen it is 46 MPa.

900°C, when all of the acetone has evaporated, within the

system only SiO2 remains, being in a nanodispersed condi-

tion within the composition of the product MFSS-8. Due to

the high specific surface of SiO2 nanoparticles a considerable

number of siloxane bonds form with the surface of substrate

material and Cr2O3 particles.

Thus, most promising from the point of view of effective

increase in blackness coefficient (up to 0.85 un.) and high

adhesive capacity, is a coating based on product

MFSS-8 modified with Cr2O3 addition.

However, an attempt to apply a coating with chromium

oxide, showing good adhesion on glass ceramic specimens,


TABLE 2. Dependence of the Level of Change in Glass Ceramic OTM 357 and Quartz Ceramic NIASIT with Coating Properties on Test Tem-

perature

Material

Specimen treatment

temperature, °C

(60 sec)

Specimen properties

original* with coating

tg� � tg� � �ben

, MPa Wcoating

, 10–3 %

Coating based on MFSS-8 + Cr2O3

OTM 357 500 105 7.05 105 7.02 140 5

700 102 7.14 109 7.08 146 0

900 104 7.09 112 7.13 138 0

1100 108 7.12 114 7.11 136 2

1250 103 7.13 111 7.07 99 2

NIASIT 500 <5 3.40 3 3.41 64 5

700 <5 3.42 9 3.43 57 1

900 <5 3.44 17 3.42 60 7

1100 <5 3.42 4 3.43 75 7

1250 <5 3.40 4 3.41 51 8

Coating based on MFSS-8 + CoO

OTM 357 500 105 6.99 117 6.91 134 7

700 110 7.00 114 6.99 123 7

900 110 7.18 118 7.13 123 11

1100 105 7.05 111 7.14 134 6

1250 104 7.16 109 7.12 100 11

NIASIT 500 <5 3.41 3 3.46 66 1

700 <5 3.43 7 3.41 58 4

900 <5 3.43 16 3.44 60 1

1100 <5 3.44 6 3.42 74 3

1250 <5 3.41 6 3.44 53 4

Coating based on MFSS-8 + TiO2

OTM 357 500 103 7.03 105 7.02 152 2

700 103 7.12 119 7.07 130 2

900 105 7.19 119 7.16 153 1

1100 106 7.21 101 7.15 99 1

1250 103 7.03 109 7.17 99 2

NIASIT 500 <5 3.44 10 3.44 57 1

700 <5 3.42 22 3.39 62 2

900 <5 3.45 19 3.45 48 1

1100 <5 3.42 11 3.45 57 2

1250 <5 3.39 16 3.40 45 5

* Ultimate strength in bending for original OTM 357 material specimen is 136 MPa, and for original NIASIT material specimen it is 60 MPa.

did not give a favorable result on quartz ceramic specimens

(Fig. 2). With an increase in heat treatment temperature there

was separation of all of the test coatings from a quartz ce-

ramic specimen surface. Whereas for coatings based on CoO

and TiO2, this effect was predictable, for a coating based on

Cr2O3, a lack of adhesion was entirely unexpected.

Analysis of the specimens obtained makes it possible to

propose that the reason for crumbling of a coating with

Cr2O3 from the surface of a quartz ceramic specimen is the

quite high porosity of ceramic specimens (8 – 10%). Pres-

ence of porosity in substrate material leads to a situation that

with application at its surface of a mixture of product

MFSS-8 and Cr2O3 there is impregnation of pores with

MFSS-8 material. Here Cr2O3 particles do not penetrate into

pores and remain at the surface. All of this leads to impover-

ishment of the mixture, which in total does not provide for-

mation of a sufficient number of siloxane bonds for joining

with the surface layers of substrate material.

Emerging from this complicated situation it appeared

preferable to impregnate porous substrate material with

MFSS-8 in order to seal its surface. Specimens of quartz ce-

ramic are shown in Fig. 3 with prior impregnation and with-

out it, coated with Cr2O3 and heat treated at 1250°C. It is evi-

dent that introduction of additional impregnation of porous

materials is capable of increasing markedly coating adhesion

to substrate material.

A result of these studies was preparation of a coating

based on product MFSS-8 and Cr2O3 capable of markedly in-

creasing the blackness coefficient for ceramic and glass ce-

ramic materials. Here a coating retains it properties, and also

with short-term action of high temperature. At the same time

operation of objects of ceramic materials for which the coat-

ings are being developed, occurs under the action of severe

climatic conditions: alternating temperature, increased mois-

ture content, rain, dust, etc. Therefore it is desirable to pro-

duce verification of retention of property stability for the

proposed coatings under these conditions, and also the stabil-

ity of a coating based on MFSS-8 and Cr2O3 compared with

materials used currently: enamels FP-566, KO-5189,

ÉP-140, and products MFSS-8 and TMFT, used for water

repellence of quartz ceramic. For complete information

about the protective properties of these products studies were

carried out for resistance to action of cyclic thermal loads

and prolonged action of sea water.

In order to determine the resistance of different coating

versions thermal cycling of specimens was performed at

temperatures from -60 to +300°C (50 cycles). After 25 cy-

cles specimens were selected for determination of water ab-

sorption, �, and tg�. Then specimens were returned for fur-


Fig. 1. Specimens of glass ceramic OTM 357 with different coatings after heat treatment at 500 and 1250°C with soaking for 60 sec.

ther testing. The results of measurements are presented in Ta-

ble 3.

Practically all of the coatings applied to quartz ceramic,

did not withstand cyclic temperature drops, and after 25 cy-

cles there is a marked increase in water absorption, and cor-

respondingly the dielectric loss angle. Only a coating based

on MFSS-8 with Cr2O3 filler behaved well. It is interesting

that a coating of pure MFSS-8 was subject to surface failure

after 50 thermal cycles. A specimen is presented in Fig. 4 of

quartz ceramic impregnated with product MFSS-8 after ther-

mal cycling. In contrast to specimens with a coating of


TABLE 3. Dependence of Change in Coated Quartz and Glass Ceramic Properties on Thermal Cycling*

Coating

Original uncoated specimen parameters

Coated specimen parameters after thermal cycling, cycles

with coating 25 50

�, g/cm3 W, % � tg�, 104� tg�, 104 W, % � tg�, 104 W, % � tg�, 104 W, %

NIASIT quartz ceramic

MFSS-8 1.972 5.372 3.43 <5 3.40 12 0.005 3.40 11 0.062 3.59 308 0.175

TMFT 1.959 5.777 3.39 <5 3.39 10 0.007 3.37 16 0.048 3.57 437 0.250

FP-566 1.974 5.380 3.39 <5 3.39 7 0.008 3.39 12 0.012 3.24 201 0.083

KO-5189 1.984 5.054 3.42 <5 3.48 10 0.000 3.48 10 0.019 3.47 95 0.208

MFSS-8 + Cr2O3 1.976 5.219 3.42 <5 3.40 10 0.003 3.44 9 0.008 3.42 9 0.007

OTM 357 glass ceramic

MFSS-8 + Cr2O3 2.50 0.003 7.02 110 7.02 115 0.002 7.03 109 0.003 7.02 116 0.005

* Cycle from –60 to +300°C, soaking at final temperature for 60 min.

Fig. 2. Specimens of quartz ceramic with different coatings after heat treatment at 500 and 1250°C with soaking for 60 sec.

MFSS-8 and Cr2O3, which has a form similar to that pre-

sented in Fig. 3b, all of the specimens surface impregnated

only with MFSS-8 is a fine network of cracked structure.

Proceeding from the fact that MFSS-8 destruction occurred

at 700 – 900°C, it may be suggested that the action of low

temperature led to this unfavorable effect. In the case of test-

ing specimens impregnated with chromium oxide, apparently

a favorable result is connected with formation of a stronger

coating carcase.

Another batch of specimens was subjected for verifica-

tion of coating stability to the action of sea water. Specimens

impregnated with product MFSS-8 and TMFT, and also

painted with enamels FP-566 and KO-5169, were placed in

saline water. The change in dielectric properties and water

absorption under the action of sea water are presented in Ta-

ble 4. After 150 h for specimens in sea water there is a sharp

increase in tg� for specimens coated with enamels FP-566

and KO-5169, and also impregnated with TMFT solution. A

further increase in exposure to 550 h only aggravates this

change. Thus, only specimens of glass ceramic and quartz

ceramic with coatings of MFSS-8 and a composite based on

product MFSS-8 modified with chromium oxide withstood

testing.

Thus, as a result of these studies a new functional coating

has been prepared having as a film-forming component prod-

uct MFSS-8 and chromium oxide as a filler. The coating ob-


Fig. 3. Specimens of quartz ceramic coated with

MFSS-8 + Cr2O3 heat treated at 1250°C for 60 sec: a)

substrate material without prior impregnation; b ) pre-

vious impregnation of substrate with product MFSS-8.

Fig. 4. Quartz ceramic specimen impregnated with MFSS-8 prod-

uct after 50 thermal cycles –60 to +300°C.

TABLE 4. Dependence of Change in Coated Quartz Ceramic NIASIT and Glass Ceramic OTM 357 Properties on Prolonged Exposure in Sea

Water

Coating

Original uncoated specimen parameters

Coated specimen parameters after exposure, h

coated 150 550

�, g/cm3 W, % � tg�, 104� tg�, 104 W, % � tg�, 104 W, % � tg�, 104 W, %

NIASIT quartz ceramic

MFSS-8 1.975 5.380 3.43 <5 3.40 7 0.004 3.43 8 0.004 3.44 10 0.005

TMFT 1.962 5.657 3.43 <5 3.43 6 0.005 3.46 78 0.170 3.46 121 0.370

FP-566 1.970 5.480 3.44 <5 3.43 5 0.009 3.71 613 0.750 No signal 3.020

KO-5189 1.981 5.244 3.42 <5 3.42 9 0.016 3.47 97 0.120 3.52 283 0.350

MFSS-8 + Cr2O3 1.980 5.283 3.43 <5 3.43 8 0.004 3.44 9 0.006 3.43 9 0.007

OTM 357 glass ceramic

MFSS-8 + Cr2O3 2.50 0.003 7.02 115 7.02 118 0.004 7.03 116 0.004 7.03 121 0.005

tained is capable of increasing markedly ceramic and glass

ceramic material blackness coefficient. A coating exhibits

good adhesion capacity, it may be operated under the action

of temperatures up to 1250°C, withstand thermal cycling in

the range from –60 to +300°C, and also maintain its proper-

ties with prolonged action of sea water.

The results of these studies may be used not only for im-

proving the blackness coefficient of objects made from ce-

ramic and glass ceramic materials, but also in order to re-

solve other important problems, for example a change in ma-

terial dielectric permittivity, an increase in object wall radio

transparency, etc. All of these problems are resolved by

choice of the required component for introduction of product

MFSS-8.

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study of functional coating preparation on ceramic materials

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