the aerosol-assisted cvd of silver films from single-source precursors

DOI: 10.1002/cvde.200806729

Full Paper

The Aerosol-Assisted CVD of Silver Films fromSingle-Source Precursors**

By Arunkumar Panneerselvam, Mohammad A. Malik, Paul O’Brien,* and Madeleine Helliwell

Thin films of silver are deposited from tetraphenyldioxoimidodiphosphinato silver(I) [Ag{(OPPh2)2N}]4 � 2H2O (1) and silver(I)triflouoroacetate CF3COOAg (2) single-source precursors (SSPs) by the aerosol-assisted (AA)CVDmethod. The complex (1)is a tetramer with linear and distorted tetrahedral coordination modes at silver. Two types of films, silvery and brownish, are

observed from both SSPs due to the temperature gradient in the AACVD reactor. The as-deposited films are characterized by

X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, and ultraviolet/visible

(UV-vis) spectroscopy methods.

Keywords: AACVD, Silver, Thin films, Single-source precursors, Temperature gradient

1. Introduction

Silver thin films have many potential applications

including, as dopants in high-temperature superconducting

materials, bactericidal coatings (e.g., used in catheters),[1]

ultrafast optical switches, optical filters,[2] electrodes for

dielectric layers,[3] and surface-enhanced Raman sub-

strates.[4] Silver has the highest electrical conductivity at

room temperature, however its use in microelectronics is

often limited by its diffusion into semiconducting sub-

strates.[5] Thin films of silver have been deposited by many

non-vacuum techniques including electrodeposition,[6]

photochemical deposition,[7] electroless deposition,[8] and

sol-gel.[9] Physical vapor deposition techniques include

vacuum evaporation,[10] sputtering,[5,11,12] pulsed laser

deposition,[13] electron beam evaporation,[14] and molecular

beam epitaxy.[15] Among these various techniques, CVD has

the advantage of potentially superior step-coverage, and is a

single-step process which can easily be scaled up to deposit

high purity films over large areas. Compared to copper[16] or

gold,[17] there are relatively few reports on the CVD of

silver. The reported silver precursors for CVD are silver(I)

salts (AgF,[18] AgI,[19] CH3COOAg[20]), organometallic and

coordination compounds with fluorinated or non-fluori-

nated b-diketonates, carboxylates along with neutral donor

[*] A. Panneerselvam, Dr. M. A. Malik, Prof. P. O’BrienSchool of Chemistry and the School of Materials,University of ManchesterOxford Road, Manchester, M13 9PL. (UK)E-mail: [email protected]

Dr. M. HelliwellSchool of Chemistry, University of ManchesterOxford Road, Manchester, M13 9PL (UK)

[**] A. P. would like to thank the University of Manchester for financialsupport. The authors also thank BBSRC, UK for the grant to P.O’B thathave made some of this research possible.

Chem. Vap. Deposition 2009, 15, 57–63 � 2009 WILEY-VCH Verlag Gmb

ligands such as olefins, alkyl isocyanides, and tertiary

phosphines (PMe3, PEt3, and PPh3) adducts. However,

these precursors have either poor volatility or low thermal

stability, or cause contamination (usually carbon, fluorine,

or phosphorus) in the as-deposited silver films thereby

limiting their suitability for conventional CVD pro-

cesses.[1,2,21,22] In an attempt to overcome these difficulties,

the synthesis and evaluation of new classes of silver

precursors are under investigation.[23]

Recent developments of alternative precursor delivery

systems, like powder flash evaporation,[24] the powder feed

method,[19] AACVD,[25] and direct liquid injection CVD,[26]

circumvent the need for thermally stable and/or volatile

precursors. Molloy and co-workers deposited silver films by

AACVD using silver carboxylates, fluorocarboxylates,

b-diketonates, b-diketoiminates, and aryloxides as phosphine

adducts to give useful precursors which were, however,

considered unsuitable for conventional CVD.[27]

Recently, we have reported the synthesis of a single-

source precursor [Ag{(SPiPr2)2N}]3. AACVD from the

complex yielded a mixture of silver sulfide and silver thin

films, or pure silver films, depending upon the deposition

temperature.[28] In the present work, AACVD was used to

grow silver films from (1) and the readily available (2). The

SSP (1) was synthesized from the tetraphenyldioxoimido-

diphosphinate [Ph2P(O)NHP(O)Ph2] (TPOIP) ligand, an

inorganic analogue of the b-diketonate. To the best of our

knowledge, dioxoimidodiphosphinato silver complexes have

not previously been evaluated for the deposition of silver.

The silver trifluoroacetate (2) precursor was used in the

deposition of silver films by powder-feed,[19] and laser

assisted CVD.[29] As both precursors are soluble in common

organic solvents, AACVD is a suitable technique.[25] Herein

we report the deposition of silver thin films from (1) and (2)

by the AACVD method.

H & Co. KGaA, Weinheim 57

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Fig. 1. The molecular structure of [Ag{(OPPh2)2N}]4 � 2H2O. Hydrogen

atoms are omitted for clarity.

Table 2. Crystal data and structure refinement for [Ag{(OPPh2)2N}]4.2H2O.

Empirical formula C96H84N4Ag4P8O10

Formula weight 2132.91

Temperature 100(2) K

Wavelength 0.71073 A

Crystal system Triclinic

Space group P-1

a 12.3883(7) A

b 13.278(6) A

c 15.963(10) A

a 68.414(12)8b 67.605(10)8g 72.271(13)8Volume 2214(2) A3

Z 1

Density (calculated) 1.599 mg/m�3

Absorption coefficient 1.078 mm�1

F(000) 1076

Crystal size 0.35� 0.12� 0.12 mm

u range for data collection 1.68 to 20.818Limiting indices �12� h� 11, �12� k� 13, �15� l� 15

Reflections collected 6836

Unique reflections 4575

Completeness to u¼ 20.818 98.5%

Max. and min. transmission None

Refinement method Full-matrix least-squares on F2

Data/restraints/parameters 4575/490/550

Goodness-of-fit on F2 0.867

Final R indices [I> 2s(I)] R1¼ 0.0724, wR2¼ 0.1377

R indices (all data) R1¼ 0.1602, wR2¼ 0.1632

Largest difference peak and hole 1.290 and �0.747 A�3

2. Results and Discussion

The TPOIP ligand was prepared using a modification of

the method of Wang et al.[30] Deprotonation of the ligand

upon treatment with sodiummethoxide, and in-situ reaction

with silver trifluoroacetate in methanol, gave an off-white

powder (1).

The method described in the literature[31] for the

preparation of (1) used silver nitrate rather than silver

trifluoroacetate. The product we obtained from the reaction

of silver nitrate with sodium dioxoimidodiphosphinate salt

was a brown insoluble powder. Our repeated attempts to

prepare the required complex resulted in the same brown

insoluble powder, obviously not the required product.

However, when we used silver trifluoroacetate, the silver

complex (1) was readily formed. The compound is air,

moisture, and light stable. It can be stored over a period of

months without any decomposition.

Table 1. Selected bond lengths (A) and bond angles (8) for

[Ag{(OPPh2)2N}]4.2H2O.

Bond distances Bond angles

Ag(1)-N(1) 2.10(1) N(1)-Ag(1)-N(2) 172.2(5)

Ag(1)-N(2) 2.11(1) N(1)-Ag(1)-P(2) 29.7(3)

Ag(1)-P(2) 3.03(1) N(2)-Ag(1)-P(2) 143.6(3)

Ag(1)-Ag(2) 3.12(0) N(1)-Ag(1)-Ag(2) 95.8(3)

Ag(2)-O(2) 2.25(1) N(2)-Ag(1)-Ag(2) 77.9(3)

Ag(2)-O(4) 2.33(1) P(2)-Ag(1)-Ag(2) 66.1(1)

Ag(2)-O(3) 2.38(1) O(2)-Ag(2)-O(4) 151.7(3)

Ag(2)-O(4A) 2.52(1) O(2)-Ag(2)-O(3) 105.1(4)

P(1)-O(1) 1.48(1) O(4)-Ag(2)-O(3) 98.2(3)

P(1)-N(1) 1.68(1) O(2)-Ag(2)-O(4) 105.6(4)

P(2)-O(2) 1.52(1) O(4)-Ag(2)-O(4A) 91.3(3)

P(2)-N(1) 1.60(1) O(3)-Ag(2)-Ag(1) 159.2(2)

P(3)-N(2) 1.68(1) O(4)-Ag(2)-Ag(1) 113.2(2)

P(3)-O(3) 1.53(1) O(1)-P(1)-N(1) 117.4(6)

O(3)-Ag(2) 2.38(1) O(2)-P(2)-N(1) 110.9(7)

58 www.cvd-journal.de � 2009 WILEY-VCH Verlag GmbH

2.1. X-ray Single Crystal Structure of[Ag{(OPPh2)2N}]4 � 2H2O

The molecular structure of [Ag{(OPPh2)2N}]4 � 2H2O is

shown in Figure 1. The asymmetric unit contains half of a

molecule and one water molecule. The water may have

come from the wet THF used to recrystallize the crude

Fig. 2. XRD patterns of silver (Ag) films deposited on glass by AACVD from

(1) at a flow rate of 160 sccm and substrate temperatures of (a) 375 8C,brownish matt film, (b) 425 8C, brownish reflective film, (c) 425 8C, silveryfilm, (d) 475 8C, brownish reflective film, and (e) 475 8C, silvery film.

& Co. KGaA, Weinheim Chem. Vap. Deposition 2009, 15, 57–63

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product. Selected bond lengths and bond angles are listed in

Table 1 and the crystallographic data are listed in Table 2.

This structure is similar to the reported [Ag{(OPPh2)2N}]4 �2EtOH[31] and [Ag4(m-Ph2PNHPPh2)2 (m-OPh2PNPPh2O)2] �(PF6)2 �CH3COCH3.

[32] The molecule is built up of four

Ag(TPOIP) units which are arranged as pairs, and has a centre

of symmetry. The two Agþ cations [Ag(1) and Ag(1A)] adopt

the preferred linear coordination with two TPOIP ligands

giving Ag(TPOIP)2�, with N(1)-Ag(1)-N(2) 172.2(5)8, and

leaving three pendent PNO groups. The absence of interaction

from the water molecule present in the unit cell is reflected

mainly in the P-O bond distance, 1.52 A, and also in the N-P-O

bond angles (117.48) which are larger than the bond distances

(�1.49 A) and bond angles (�116.88) reported for the

structures containing solvent molecules.[31,32]

The two Agþ cations [Ag(2) and Ag(2A)] share six PNO

moieties and thus hold two Ag(TPOIP)2 moieties together.

Fig. 3. SEM images of silver films deposited on glass by AACVD from (1) at flow

b) 425 8C, silvery film, c) 425 8C, brownish reflective film, d) 475 8C, silvery film and,

Chem. Vap. Deposition 2009, 15, 57–63 � 2009 WILEY-VCH Verlag Gm

Moreover, these two units are coupled by a pair of Ag��Ag

contacts (3.121 A), which is shorter than the sum of van der

Waals radii (3.4 A) for silver, suggesting the presence of a

weak Ag-Ag bonding interaction. In addition, the Ag-Ag

bond distance is shorter than the reported structure with

solvent units (3.24 A), but the Ag-Ag bond distance is still

longer than (2.816 A) found in the di-silver complex [Ag2(m-

Ph2PNHPPh2)(m-Ph2PNPPh2)2].[33] The coordination of the

two silver atoms to the six suitably oriented PNO groups

occurs in such a way as to lead a planar central Ag2O2 ring

{O(4)-Ag(2)-O(4A), 91.3(3)8}. The two oxygen atoms are

asymmetrically bonded to the Ag atoms {Ag(2)-O(4),

2.33(1) and Ag(2)-O(4A), 2.52(1) A}. The coordination

around silver is thus distorted tetrahedral with the oxygen

atoms of the PNO groups as neighboring atoms. The

shortest bond distance between silver and a terminal oxygen

atom is 2.245 A {Ag(2)-O(2)}. A salient feature in this

a rate of 160 sccm and growth temperatures of a) 375 8C, brownish matt film,

e) 475 8C, brownish reflective film.

bH & Co. KGaA, Weinheim www.cvd-journal.de 59

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structure is that the Ag atoms adopt both linear and

tetrahedral geometries.

2.2. Thermogravimetric Analysis

Thermogravimetric analysis (TGA) for precursor (1)

shows a sharp single decomposition step between 344 and

384 8C. The observed residue (35%) is higher than the

calculated residue (21%) for silver. XRD analysis of

the TGA residue showed impurity peaks which appear to

be due to decomposed ligand. Precursor (2) decomposed by

a single step between 313 and 354 8C. The residue (46%) is in

fair agreement with the calculated residue (49%) for silver.

Fig. 4. UV-vis spectra of silvery films deposited on glass by AACVD from (1)

at substrate temperatures of (a) 425 8C and (b) 475 8C; brownish matt

films deposited on glass at substrate temperature of (c) 375 8C and

brownish reflective films deposited at substrate temperatures of (d) 425 8Cand (e) 475 8C.

Fig. 5. XRD patterns of silver (Ag) films deposited on glass by AACVD from

(2) at a flow rate of 140 sccm and substrate temperatures of (a) 300 8C,brownish reflective film, (b) 300 8C, brownish matt film, (c) 325 8C, brownishreflective film, (d) 325 8C, silvery film, (e) 375 8C, brownish reflective film, and

(f) 375 8C, silvery film.

2.3. Silver Films from (1)

Deposition was carried out at temperatures between 375

and 475 8C, with an argon flow rate of 160 sccm. While no

deposition occurred below 375 8C, brownish matt films were

deposited at 375 8C. As-prepared films at 425 and 475 8Cwere of two colors; silvery film on the substrate closer to the

precursor inlet, and brownish reflective films on the adjacent

substrate towards the centre of the reactor. This difference is

most probably caused by a temperature gradient in the

reactor, or possibly by precursor decomposition as it moves

through the reactor.

XRD analysis (Figs. 2a–e) of brownish matt films

deposited at 375 8C, silvery and brownish films deposited

at 425 and 475 8C correspond to cubic silver (JCPDS 04-

0783). The as-obtained silvery and brownish films at all

deposition temperatures (375–475 8C) have preferred

orientation along the (111) plane. The crystallinity of the

deposited films increases at higher deposition temperatures.

The thickness of the brownish films was in the range 0.3–

0.6mm, whereas the silvery films varied between 1.2 and

1.5mm.

SEM of the as-deposited brownish matt films at 375 8Cconsists of spherical particles (Fig. 3a) composed of only

silver, as shown by EDX. Silvery films deposited at 425 8Cwere composed of fused silver particles of irregular shapes

(Fig. 3b), whereas spherical particles were the major

component in the brownish reflective film (Fig. 3c). The

morphology of the silvery film deposited at 475 8C appears to

be a mixture of rods grown vertically and cubic particles

(Fig. 3d). The size of the rods and particles were in the range

0.2–0.3mm. Similar features were observed in the brownish

film deposited at the same temperature, but the sizes of the

rods and particles were in the range 0.05–0.1mm (Fig. 3e).

EDX analysis of the silvery films deposited at 425 and 475 8Cshows the presence of silver alone, whereas the brownish

films deposited at these temperatures were composed of

97% silver with 3% phosphorus.

The UV-vis spectra (Fig. 4a) of the silvery films deposited

at 425 8C shows a surface plasmon resonance (SPR)[34] peak

at ca. 456 nm. The absorption maximum is red shifted to

60 www.cvd-journal.de � 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim Chem. Vap. Deposition 2009, 15, 57–63

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475 nm for the silvery films grown at

475 8C (Fig. 4b) which can be attrib-

uted to the increase in the particle size.

The as-deposited brownish matt film

at 375 8C exhibits absorption maxima

at ca. 420 nm (Fig. 4c). The absorption

peak of the brownish reflective (mirror-

like) films deposited at 425 and 475 8Cundergoes blue shift to ca. 406 nm

(Figs. 4d, e) which is due to the

microstructure of the film.

Fig. 6. SEM images of silver films deposited on glass by AACVD from (2) at a flow rate of 140 sccm at growth

temperatures of a) 300 8C, brownish matt film, b) 300 8C, brownish reflective film, c) 325 8C, silvery film,

d) 325 8C, brownish reflective film, e) 375 8C, silvery film, f) 375 8C, brownish reflective film, g) 425 8C, silvery film,

and h) 425 8C, brownish reflective film.

2.4. Silver Films from (2)

Deposition was carried out at tem-

peratures from 300 to 425 8C with an

argon flow rate of 140 sccm. XRD

patterns of the films deposited at 300–

375 8C, correspond to cubic silver

(JCPDS 04-0783) with a preferred

orientation along the (111) direction

(Figs. 5a–f). At 300 8C, brownish matt

films were deposited along with

brownish reflective films. Two types

of films were deposited at 325 and

375 8C; silvery films on the substrates

placed at the front region of the

reactor, and brownish reflective films

on the substrates placed in the middle

part of the reactor. As expected, the

size of the crystallites increased at

higher deposition temperatures.

The microstructure of the as-depos-

ited films exhibits obvious differences

depending on the growth tempera-

tures. Cubic silver crystallites were

observed on the brownish matt films

deposited at 300 8C (Fig. 6a), but the

mirror-like films deposited at the same

temperature were observed as dots

(Fig. 6b) on the surface of the

substrate. Silvery films deposited at

325 and 375 8C showed well-defined

blocky crystallites (Figs. 6c, e). The

brownish specular films were com-

posed of dots at 325 8C (Fig. 6d)

and spherical crystallites at 375 8C
(Fig. 6f). According to EDX measurements, the silvery
and brownish films deposited at the above-mentioned

temperatures (300–375 8C) showed the presence of silver

alone. Films deposited at 425 8C also show silvery and

brownish reflective (specular) films. XRD of both the films

matched with cubic silver with preferred orientation along

the (111) plane, but the brownish reflective films showed

additional peaks corresponding to silver fluoride (JCPDS


47-1355). The morphology of the silvery film deposited at

425 8C was observed as fused crystallites (Fig. 6g) and the

brownish specular films were composed of small particles

(Fig. 6h). EDX analysis showed the presence of fluorine

(6%) for the brownish films whereas the silvery films showed

no contamination. The film thickness varied from 2 to 3mm

for the silvery, and 0.7 to 0.9mm for the brownish films at all

deposition temperatures.


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Fig. 7. UV-vis spectra of brownish matt film deposited on glass by AACVD

from (2) at substrate temperature of (a) 300 8C; silvery films deposited at

substrate temperatures of (b) 325 8C and (c) 375 8C, and brownish reflective

films deposited at substrate temperatures of (d) 300 8C, (e) 325 8C, and

(f) 375 8C.

The UV-vis absorption spectra of the as-deposited

brownish matt film at 300 8C showed broad peak at

420 nm (Fig. 7a). The absorption of the as-deposited silvery

films at 325 and 375 8C was red shifted towards 433 and

464 nm, respectively (Figs. 7b, c). The brownish reflective

films deposited at 300 8C exhibited a SPR peak at 410 nm

(Fig. 7d) whereas as-grown films at 325 and 375 8C were red

shifted to 425 and 451 nm, respectively (Figs. 7e, f). The peak

broadness is due to dipole-dipole interactions of the Ag

particles.[34]

Fig. 8. Scheme of the AACVD reactor.

3. Conclusions

Silver films were deposited from (1) and (2)

by AACVD. Both precursors gave two types of

films, silvery and brownish, depending upon the

deposition temperatures and the position of the

glass substrates in the reactor. The morphology

of the silver films obtained from the imido-

precursor (1) varied from spherical particles

(375, 425 8C) to rods (475 8C) for both the silveryand brownish films. Phosphorus contamination

was observed on the brownish films (425,

475 8C) whereas the silvery films were devoid

of contamination. Silver trifluoroacetate (2)-

deposited silver films at temperatures from as

low as 300 8C up to 425 8C. The microstructure

62 www.cvd-journal.de � 2009 WILEY-VCH Verlag GmbH

of the silvery films exhibited cubic (300 8C), blocky (325,

375 8C), and fused crystallites (425 8C). The brownish films

were composed of dots (300, 325, 425 8C) and spherical

particles (375 8C). The brownish films deposited at 425 8Cshowed traces of silver fluoride whereas all other films were

composed of only silver.

4. Experimental

All reactions were performed under an inert atmosphere of dry nitrogen

using standard Schlenk techniques. All reagents were purchased from theSigma-Aldrich chemical company and used as received. Solvents weredistilled prior to use. 1H and 31P NMR studies were carried out using a BrukerAC300 FTNMR instrument. Microanalysis was performed at the Universityof Manchester microanalytical laboratory. Infrared spectra were recorded ona Perkin Elmer Spectrum BX FTIR spectrometer. The ligand [Ph2P(O)NH-P(O)Ph2] was prepared by the reported method [30]. TGA measurementswere carried out using a Seiko SSC/S200 model at a heating rate of10 8Cmin�1 under nitrogen.Melting points were recorded on a Stuart meltingpoint apparatus and are uncorrected.

[Ag{(OPPh2)2N}]4: Sodiummethoxide (0.18 g, 3.4 mmol) was added to a

stirred solution of [Ph2P(O)NHP(O)Ph2] (1.5 g, 3.4 mmol) in anhydrousmethanol (50mL). The resulting solution was stirred at room temperature for15min. Silver trifluoroacetate (0.74 g, 3.4 mmol) dissolved in methanol wasadded, and the reaction stirred at room temperature for 30min. It was thenfiltered and dried under vacuum. Recrystallization from THF at roomtemperature yielded off-white crystals. Yield: 1.2 g (63%), mp: 243–246 -C, IR(cmS1): n(PNP) 1226(s), 743(m); n(PO) 1121(m). 1HNMR (300MHz; CDCl3;Me4Si): 7.8 ppm (m, 8H), 7.2 ppm (m, 12H). 31P NMR (162MHz): d¼23.58 ppm. Elemental analysis: calculated for C24H20N1P2O2Ag: C, 54.9; H,3.9; N, 2.7; P, 11.8; Ag, 20.6%. Found: C, 54.3; H, 3.9; N, 2.6; P, 11.6; Ag,20.1%.

X-Ray Crystallography: Single-crystal XRD data for the compound wascollected using graphite monochromatedMoKa radiation (l¼ 0.71073 A) ona Bruker APEX diffractometer. The structure was solved by direct methodsand refined by full-matrix least squares on F2 [35]. All non-H atoms wererefined anisotropically. H atoms were included in calculated positions,assigned isotropic thermal parameters, and allowed to ride on their parentcarbon atoms. All calculations were carried out using the SHELXTL package[36].CCDC number 692341 contains the supplementary crystallographic data

for this paper. These data can be obtained free of charge fromThe CambridgeCrystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.

Deposition of Films by AACVD: In a typical deposition, ca. 0.20 g of theprecursor was dissolved in 20mL toluene in a two-necked 100mL round-bottom flask. Argon was used as a carrier gas with a flow rate of 140 or160 sccm, and the deposition was carried out for 120min. The flow rate wascontrolled by a Platon flow gauge. Seven glass substrates (approx.1 cmT 3 cm) were placed inside the reactor tube. The precursor solutionwas kept in a water bath above the piezoelectric modulator of a PIFCO

& Co. KGaA, Weinheim Chem. Vap. Deposition 2009, 15, 57–63

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ultrasonic humidifier (Model No. 1077) where aerosol droplets weregenerated and transferred into the hot-wall deposition zone by carrier gas(Fig. 8). Both solvent and precursor were evaporated and the precursor vaporreached the substrate surface where thermally induced reactions and filmdeposition took place [37].

Characterization of Thin films: XRD studies were performed on a BrukerAXS D8 diffractometer using a monochromated Cu Ka radiation. Thesamples were mounted flat and scanned between 20 and 80- in a step size of0.05-with a count rate of 9 s. Films were carbon coated using Edward’s E306Acoating system before carrying out SEM and EDX analyses. SEM analysiswas performed using a Philips XL 30FEG and EDX was carried out using aDX4 instrument. The thickness of the films was measured with a Dektak 8Stylus surface profilometer. UV-vis spectra were measured using a Helios-Beta Thermospectronic spectrophotometer.

Received: July 21, 2008

Revised: October 07, 2008

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the aerosol-assisted cvd of silver films from single-source precursors

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