Method for producing thin films

Abstract

Thin films are produced by a method wherein a material is heated in a furnace placed inside a vacuum system. An inert gas is flown over/through the heated material. The vapors of the material are entrained in the carrier gas which is then directed onto a substrate heated to a temperature below that of the furnace temperature and placed in close proximity to the exit of the furnace.

Description

BACKGROUND OF THE INVENTION

[0002] U.S. Pat. No. 5,945,163 discloses an apparatus and method for depositing a material on a substrate. In that patent a distributor is utilized which includes a heated permeable member through which a carrier gas and a material are passed to provide a vapor that is deposited on a conveyed substrate. The permeable member is tubular and has an electrical voltage applied along its length to provide the heating and the carrier gas and the material as a powder are introduced into the tubular permeable member for flow outwardly therefrom as the vapor. A shroud extends around the tubular permeable member and has an opening through which the vapor flows for the deposition.

[0003] It would be desirable if improved techniques could be provided for producing thin film.

SUMMARY OF THE INVENTION

[0004] An object of this invention is to provide improved methods for producing thin film.

[0005] In accordance with this invention the material to be produced as a thin film is heated to a sufficient temperature T in a furnace placed inside of a vacuum system. An inert carrier gas is flown over/through the heated material and the vapors of the material are entrained in the carrier gas. Carrier gas containing the vapors of the material is directed onto a substrate heated to a temperature below that of the furnace temperature and placed in close proximity to the exit of the furnace.

[0006] Carrier gas flow is adjusted to give:

[0007] A sufficient degree of entrainment of the material during contact with the source,

[0008] A pressure inside the vacuum enclosure that would be high enough to suppress any re-evaporation from the substrate,

[0009] The desired deposition rate.

[0010] The vacuum system could be pressurized by a secondary inert gas inlet not going through the source to give more flexibility for the adjustment of the carrier gas flow going through the furnace.

THE DRAWINGS

[0011] FIG. 1 is a schematic showing of the inert carrier gas flow used for deposition in accordance with this invention;

[0012] FIG. 2 is an exploded isometric view of a prototype source in accordance with this invention;

[0013] FIG. 3 is a side view of the source shown in FIG. 2;

[0014] FIG. 4 is an end view with the substrate of the source shown in FIGS. 2-3;

[0015] FIG. 5 is an SEM Image of example 2002 at the center of the deposition zone;

[0016] FIG. 6 is an X-Ray diffraction pattern of example 2002;

[0017] FIG. 7 is an SEM Image of example 2008 at the center of the deposition zone;

[0018] FIG. 8 is an AFM Image of example 2008 at the center of the deposition zone; and

[0019] FIG. 9 is an X-Ray diffraction pattern of example 2008.

DETAILED DESCRIPTION

[0020] All of the details of application Serial No. 60/193,662 are incorporated herein by reference thereto.

[0021] The invention enables high substrate temperature deposition of materials that have high vapor pressure, which would otherwise not stick to the substrate. Material utilization rate is very close to 100%. Such high utilization rate would reduce operational cost by:

[0022] Reducing material cost—no wastage,

[0023] Low maintenance and reduced downtime.

[0024] The method of the present invention does not require capital cost intensive high vacuum system; rather a low cost, mechanical pump generated low vacuum system is acceptable. The invention allows precise control of deposition rate by controlling gas flows both into the furnace and/or into the system. In fact, the deposition can be initiated and stopped by respectively reducing and increasing the pressure inside the system.

[0025] The invention also allows deposition of multi-layer films by placing multiple furnaces one after another in a vacuum system without costly schemes of physically separating deposition zones from each other. This is because 100% material utilization in each zone prevents any possibility of cross-contamination.

[0026] The invention is particularly useful for the deposition of CdTe films at high rates and at high substrate temperature. Other possible uses include high substrate temperature deposition of:

[0027] Any other congruently evaporating compounds such as CdS,

[0028] other high vapor pressure compounds such as In2Se3, CuCl,

[0029] Other high vapor pressure single component materials.

[0030] The following description provides first-order design calculations for CdTe deposition by a carrier gas. Following the description of the first-order design calculation is a description relating to vapor-resistant evaporation source in prototype experiment.

[0031] The following description provides first-order design calculations for CdTe deposition by a carrier gas. Following the description of the first-order design calculation is a description relating to vapor-resistant evaporation source in prototype experiment.

[0032] This document presents a methodology and quantitative results for the design of a CdTe deposition system using a carrier gas. In the design, the carrier gas is saturated with CdTe vapor (actually Cd and Te2) then flowed through the deposition zone. By maintaining the CdTe source at a higher temperature than the substrate, the vapor above the substrate becomes supersaturated, and deposits on the substrate. A conceptual schematic of the process is shown in FIG. 1. A key advantage of an inert atmosphere CdTe process over a vacuum CdTe process is the suppression of film re-evaporation during substrate cooldown.

[0033] By maintaining Tsource>Tplaten>Tsubstrate, CdTe vapor generated in the source becomes supersaturated in the deposition zone, and deposits on the substrate. Argon has been arbitrarily chosen as the carrier gas.

[0034] 1. Mass-Transfer Characterization

[0035] A first design design (to determine feasibility of the proposed process) requires the development of a mass balance and a worst-case estimate of the mass transfer rates in the system. As a first cut, mass transfer rates are estimated by calculating the diffusion characteristic time, given by

[0036] The following discussion has as its objective to demonstrate the viability of carrier-assisted CdTe deposition with grown rate of −0.1 to 1.0 μm/min at system pressures of 10 to 100 Torr.

[0037] 1. Prototype Source Schematic Diagrams

[0038] FIGS. 2-4 are views of the prototype source equipment.

[0039] 2. Power Ratings for 6 Loop Kanthal Filament, 90 cm L, 0.032 Gauge (0.8 mm dia)

[0040] Initial Resistance, R=3.5Ω

[0041] After Heating @44 V for 10 min in N2, R=4.5Ω.

TABLE 2.1
Filament power at different settings.
	Measured	Measured	Measured	Estimated
Variac	Voltage	Current	Power	Current
Setting	(V)	(A)	(W)	from P = I2R
10	11	3.3	36	2.8
20	22	6.6	145	5.7
30	33	9.7	320	8.4
40	44	12.5	550	11.0

[0042] Prototype Source #1—Circular Effusion Aperture, “Floating” Substrate Temperature

[0043] 20001

[0044] Base Pressure=18 mTorr

[0045] Deposition Pressure 20-23 Torr

[0046] Carrier Gas Flow Rate=20 sccm Argon

[0047] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0048] “Steady-State”Internal Source Temperature=945° C.

[0049] Sample to Orifice Distance=1.5 cm

[0050] Deposition time (at T>880° C.)=2 minutes

[0051] Substrate=1″×2″ L.O.F. 3.5 mm SL/SnO2

[0052] Comment: Sample touched heat shield and broke during deposition. Grey deposit 0.5 μm thick, XRD=>CdTe; growth rate˜0.25 μm/min. Rapidly raised system pressure to 200 Torr—seemed to stop deposition on exposed metal surface.

[0053] 20002

[0054] Base Pressure=8 mTorr

[0055] Deposition Pressure 20-21 Torr

[0056] Carrier Gas Flow Rate=20 sccm Argon

[0057] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0058] “Steady-State” Internal Source Temperature=935° C. Sample to Orifice Distance=1.7 cm

[0059] Deposition time (at T>880° C.)=6.5 minutes

[0060] Substrate=2″×3″ Corning 1.5 mm 7059/ITO/CBD CdS

[0061] Comment: Sample remained intact, developed grey coating at minute 6 (T=899° C.). Central 2 cm diameter region measured 7.5 μm thick; growth rate—1.1 μm/min. Band of pinholes and progressively thinner towards edges. 1$\begin{array}{cc}{\tau }_D=\frac{h^2}{D_{\mathrm{CdTe},\mathrm{Ar}}}& \left(\mathrm{eqn}.1\right)\end{array}$

[0062] where τD is the diffusion characteristic time (sec), h is the height of the gas phase above the CdTe source/sink (cm), and DCdTeAr is the diffusivity of CdTe vapor in argon (cm2/sec).

[0063] An estimate of the diffusivity for a 2 component mixture is obtained using Chapman-Enskog theory: 2$\begin{array}{cc}{D}_{\mathrm{AB}}=0.0018583\frac{\sqrt{T^3\left(\frac{1}{M_A}+\frac{1}{M_B}\right)}}{P{{\sigma }_{\mathrm{AB}}}^2{\Omega }_{D,\mathrm{AB}}}& \left(\mathrm{eqn}.2\right)\end{array}$

[0064] where T is in K, P is the pressure in atm, σAB2 is the effective molecular diameter in Å, M1 is the molecular weight of component i, and ΩDAB is a tabulated dimensionless correction factor which accounts for intermolecular attraction/repulsion. ΩDAB varies between 0.5 and 2—for these calculations it has been assumed equal to unity. Values for the other parameters are shown in the section 3.

[0065] As a rule of thumb, a system reaches equilibrium after a time of about 4τ. Therefore, for a carrier gas either unsaturated or supersaturated, it will reach the saturation pressure of CdTe at a time of 4τD. Since a continuously flowing system is under examination, the requirement for saturation is that

⊖≧4τD  (eqn. 3)

[0066] where ⊖ is the residence time given by 3$\begin{array}{cc}\theta =\frac{L}{v}& \left(\mathrm{eqn}.4\right)\end{array}$

[0067] where v is the linear gas velocity (cm/sec), and L is the length.

[0068] In reality, the mass transfer of any system is typically enhanced by the presence of velocity gradients, thereby reducing the characteristic time. The approach exemplified by eqns. 3 and 4 therefore places an upper bound on the minimum required residence time.

[0069] At this stage, only two characterizations of the flow regime have been made, the Reynolds number 4$\begin{array}{cc}\mathrm{Re}=\frac{\rho \mathrm{vh}}{\mu }& \left(\mathrm{eqn}.5\right)\end{array}$

[0070] where ρ is the gas density (g/cm3) and μ is the gas viscosity (g/cm/sec), and the mean free path 5$\begin{array}{cc}\lambda =\frac{\mathrm{RT}}{\sqrt{2}{{\mathrm{\pi \sigma }}_{\mathrm{AB}}}^2{\mathrm{pN}}_{\mathrm{AV}}}& \left(\mathrm{eqn}.6\right)\end{array}$

[0071] where R is the ideal gas constant and NAV is Avogadro's number, 6.022×1023/mol. The gas viscosity (g/cm/sec) is independent of the system pressure and is given by Chapman-Enskog theory: 6$\begin{array}{cc}\mu =2.6693\times {10}^{-5}\frac{\sqrt{\mathrm{MT}}}{{\sigma }^2{\Omega }_{\mu }}& \left(\mathrm{eqn}.7\right)\end{array}$

[0072] As with ΩDAB, Ωμ is a tabulated dimensionless value ranging from about 0.5 to 2.

[0073] The primary purpose in calculating Re is to determine whether the flow regime is turbulent or laminar. For flow through a smooth tube, turbulence occurs for Re>103, orders of magnitude greater than the situation here (the calculation will be shown in section 3). The presence of laminar flow allows a solution of the velocity and concentration profiles in the system. This is beyond the scope of this document, however.

[0074] Further useful characterizations are the Peclet number (Pe), which indicates whether mass transport is primarily diffusive or convective, and the Grashof number (Gr), which is used in estimating free convection driven by thermal gradients. 7$\begin{array}{cc}{\mathrm{Pe}}_{\mathrm{AB}}=\frac{\mathrm{hv}}{D_{\mathrm{AB}}}& \left(\mathrm{eqn}.8\right)\\ \mathrm{Gr}=\frac{h^3{\rho }^{2}g\mathrm{\beta \Delta T}}{{\mu }^2}& \left(\mathrm{eqn}.9\right)\end{array}$

[0075] where g is a gravitational constant and β is the thermal expansion coefficient (easily calculated for a gas).

[0076] 2. Mass Balance

[0077] The mass balance relates the desired CdTe deposition rate (μm/cm2/min) to the physical design of the CdTe source and deposition zone, as well as the required flow rate of carrier gas.

[0078] The mass rate of CdTe carried to the deposition zone is given by

{dot over (N)} CdTe =c Cd q= 2cTe2q  (eqn. 10)

[0079] where NCdTe is in moles (dot above indicates rate), q is the volumetric flowrate in cm3sec, and ci is the concentration of species i in mol/cm3. The thickness deposition rate assuming 100% utilization of NCdTe is given by 8$\begin{array}{cc}\frac{d{z}_{\mathrm{CdTe}}}{dt}=\frac{{\stackrel{.}{N}}_{\mathrm{CdTe}}^{{}^{{}^{}}}{\mathrm{MW}}_{\mathrm{CdTe}}}{{\rho }_{{\mathrm{CdTe}}^A\mathrm{substrate}}}& \left(\mathrm{eqn}.11\right)\end{array}$

[0080] Alternately, eqn. 11 can be easily modified to express the area per time that a film of zCdTe thickness can be deposited on: 9$\begin{array}{cc}\frac{d{A}_{\mathrm{substrate}}}{dt}=\frac{{\stackrel{.}{N}}_{\mathrm{CdTe}}^{{}^{{}^{}}}{\mathrm{MW}}_{\mathrm{CdTe}}}{{\rho }_{\mathrm{CdTe}}{z}_{\mathrm{CdTe}}}& \left(\mathrm{eqn}.12\right)\end{array}$

[0081] where zCdTe is the film thickness and Asubstrate is the substrate area.

[0082] The concentrations of Cd and Te2 are determined by the saturation pressure curve of CdTe:

Log(PCdTesat/bar)=−10650/T−2.56 Log(T)+15.80  (eqn. 13)

[0083] Where T is in K and 1 bar=1 atm=760 torr. Since the vapor phase stoichiometry is Cd:Te2=2:1, the saturation pressures of Cd and Te2 respectively are

P Cd sat =0.67 PCdTesat(T)  (eqn. 14)

and PTe2sat=0.33 PCdTesat(T)  (eqn. 15)

[0084] Concentration is directly correlated to pressure by the ideal gas law: 16) 10$\begin{array}{cc}c=\frac{N_{\mathrm{AV}}}{V}=\frac{P}{\mathrm{RT}}& \left(\mathrm{eqn}.16\right)\end{array}$

[0085] In the source and deposition zone, the rate of accumulation/depletion of CdTe into/out of the carrier gas behaves exponentially:

[0086] Source: 11$\begin{array}{cc}{P}_{\mathrm{Cd}\mathrm{Te}·\mathrm{exit}}=P_{\mathrm{Cd}\mathrm{Te}}^{\mathrm{sat}}\left(T_{\mathrm{source}}\right)\left[1-\exp \left(-\frac{{\theta }_{\mathrm{source}}}{{\tau }_{D,\mathrm{source}}}\right)\right]& \left(\mathrm{eqn}.17\right)\end{array}$

[0087] Dep. zone: 12$\begin{array}{cc}{P}_{\mathrm{Cd}\mathrm{Te}·\mathrm{exit}}=\left(P_{\mathrm{Cd}\mathrm{Te}}^{\mathrm{sat}}\left(T_{\mathrm{source}}\right)-P_{\mathrm{Cd}\mathrm{Te}}^{\mathrm{sat}}\left(T_{\mathrm{substrate}}\right)\right)\left[1-\exp \left(-\frac{{\theta }_{\mathrm{dep}·\mathrm{zone}}}{{\tau }_{D,\mathrm{dep}·\mathrm{zone}}}\right)\right]& \left(\mathrm{eqn}.18\right)\end{array}$

[0088] These equations assume no pressure drop through the system. These equations are coupled by the requirement that the volumetric flow rate of carrier gas be the same for the source and deposition zone (this assumes that the partial volume of CdTe vapor is negligible).

[0089] 3. Sample Calculations

[0090] Clearly, a spreadsheet is best used to study the influence of the design variables (P, T, h, L, q) on the deposition rate. The following sample calculations are useful in placing an order of magnitude estimate on the design variables, however.

[0091] The diffusion coefficient was calculated using the following values: 13$\begin{array}{cc}{D}_{\mathrm{AB}}=0.0018583\frac{\sqrt{T^3\left(\frac{1}{39.9g\text{/}\mathrm{mol}}+\frac{1}{200g\text{/}\mathrm{mol}}\right)}}{{P\left(3.5\stackrel{.}{A}\right)}^2\left(1\right)}& \left(\mathrm{eqn}.19\right)\end{array}$

[0092] For T=600° C.=873 K and P=50 torr=0.066 atm, DAB=10.3 cm2/sec. Note that the diffusivity is determined primarily by argon, since it is much lighter than Cd or Te—as a result, the vapor phase stoichiometry of CdTe does not have a significant influence on the diffusivity.

[0093] The viscosity of the Ar carrier gas (neglecting the CdTe vapor) is easily calculated: 14$\begin{array}{cc}\mu =2.6693\times {10}^{-5}\frac{\sqrt{\left(39.9g\text{/}\mathrm{mol}\right)T}}{{\left(3.5\stackrel{.}{A}\right)}^2\left(1\right)}& \left(\mathrm{eqn}.20\right)\end{array}$

[0094] For T=600° C.=873 K, m=4.07×10−4 g/cm/sec.

[0095] For a gas velocity of v=10 cm/sec, a zone height of h=1 cm, and a pressure of 50 torr, the gas density and Re are calculated as follows: 15$\begin{array}{cc}\rho =\frac{\left(50\mathrm{torr}\right)\left(39.9g\text{/}\mathrm{mol}\right)}{\left(6.24\times {10}^4{\mathrm{cm}}^3\mathrm{torr}\text{/}\mathrm{mol}\text{/}K\right)\left(873K\right)}=3.66\times {10}^{-5}g\text{/}{\mathrm{cm}}^3& \left(\mathrm{eqn}.21\right)\\ \mathrm{Re}=\frac{\left(3.66\times {10}^{-5}g\text{/}{\mathrm{cm}}^3\right)\left(10\mathrm{cm}\text{/}\sec \right)\left(1\mathrm{cm}\right)}{\left(4.07\times {10}^{-4}g\text{/}\mathrm{cm}\text{/}\sec \right)}=0.90& \left(\mathrm{eqn}.22\right)\end{array}$

[0096] Now that the basic physical constants have been estimated, it is possible to proceed with the source design. The first-cut design assumes that the CdTe vapor exits the source at its saturation pressure—this condition is approximated by 16$\frac{\theta }{{\tau }_D}\ge 4.$

[0097] This condition is met by limiting the velocity of the carrier gas through the source to sufficiently increase the residence time. Since this is a worst case design, the physical situation is a carrier gas flowing above a planar source. The source could be designed for better performance by flowing the carrier gas through a packed bed of CdTe chunks, for example. After the saturation condition has been implemented, the velocity and maximum theoretical deposition rate (based on assumption of 100% utilization of CdTe in the deposition zone) can be estimated as a function of source geometry (height, width, and length), system pressure, and CdTe saturation pressure.

[0098] Assuming a source width of 10 cm and height of 1 cm, the following estimates for gas velocity, flow rate, and deposition rate were calculated:

TABLE 1
Effect of design variables on deposition rate.
cm	torr	torr	° C.	cm2/sec	sec	cm/sec	cm3/sec	sccm	μm/min/cm2	100 cm2 basis
L	pCdTe	pT	Tsource	DAB	char.time	velocity	q	qSTP	dep rate	dep rate, μm/min
1	1	10	775	67.83318	0.014742	16.95829	169.5829	38.31931	42.57248477	0.425725
1	1	50	775	13.56664	0.07371	3.391659	33.91659	38.31931	8.514496955	0.085145
1	1	100	775	6.783318	0.14742	1.695829	16.95829	38.31931	4.257248477	0.042572
1	10	50	900	16.0645	0.062249	4.016128	40.16128	40.5399	90.07910192	0.900791
1	10	100	900	8.032252	0.124498	2.008063	20.08063	40.5399	45.03955096	0.450396
10	1	10	775	67.83318	0.014742	169.5829	1695.829	383.1931	425.7248477	4.257248
10	1	50	775	13.56664	0.07371	33.91659	339.1659	383.1931	85.14496955	0.85145
10	1	100	775	6.783318	0.14742	16.95829	169.5829	383.1931	42.57248477	0.425725
10	10	50	900	15.0645	0.062249	40.16126	401.6126	405.399	900.7910192	9.00791
10	10	100	900	8.032252	0.124498	20.08063	200.8063	405.399	450.3955096	4.503955

[0099] These results suggest that sufficient deposition rates can be achieved using a carrier gas system. Furthermore, the results suggest that successful operation is achievable over a wide range of pressures.

[0100] Determination of actual operating parameters will be based on further analysis. Calculation of Pe, for example, indicates the ability of the carrier gas to “confine” the flow of the CdTe. This is useful not only in confining the CdTe vapor during source heat up, but also in reducing re-evaporation of the CdTe film after the substrate has passed through the deposition zone.

[0101] 4. Conclusions

[0102] The results of this simple analysis indicate that a CdTe/carrier gas deposition process is very robust—that is, there is sufficient room for error in both the design and operation of such processes.

APPENDIX

[0103]

Values Used in Calculations
Variable	Value	Units	Name
R	0.08206	L-atm/mol-K	Ideal gas constant
	62.4	L-torr/mol-K
	6.24 × 104	cm3-torr/mol-K
NAV	6.022 × 1023	l/mol	Avogadro's number
MWAr	39.95	g/mol	Molecular weight - Argon
MWCd	112.4	g/mol	Molecular weight -
			Cadmium
MWTe	127.6	g/mol	Molecular weight -
			Tellurium
MWCdTe	240.0	g/mol	Molecular weight -
			CdTe
ρCdTe	5.85	g/cm3	CdTe density
σ	3.5	Å	Molecular diameter
			assumed same for all gas-
			phase species)
χμ	1	[dimensionless]	Intermolecular interaction
			correction for
			viscosity calculations
χAB	1	[dimensionless]	Intermolecular interaction
			correction for
			diffusivity calculations.

OTHER VARIABLES

[0104] P Pressure

[0105] T Temperature

[0106] v linear velocity

[0107] q True volumetric flow rate

[0108] qSTF Standardized volumetric flowrate (sccm)

[0109] N Molar mass

[0110] L Length

[0111] h Height of atmosphere above CdTe source/sink

[0112] ⊖ Residence Time

[0113] τD Characteristic time for diffusion

[0114] λ Mean free path

[0115] ρ Density

[0116] μ Viscosity

[0117] DAB Diffusivity of mixture of A and B

[0118] Re Reynold's number

[0119] Pe Peclet number

[0120] Gr Grashof number

TABLE 3.1
X-ray diffraction peak data and assignments of 20002.
		Raw	2θ	d
	Peak	Counts	(± 0.05 deg)	(Å)	Assignment
	1	48	21.40	4.15	111 kβ
	2	169	22.80	3.90	W
	3	6566	23.75	3.74	111
	4	385	39.30	2.29	220
	5	605	46.45	1.953	311
	6	58	56.80	1.619	400
	7	313	62.45	1.486	331
	8	504	71.25	1.322	422
	9	315	76.30	1.247	511
	10	43	84.55	1.145	440
	11	109	89.40	1.095	531

[0121] Texture coefficient=1.76 (111)=>slight (111) texture.

[0122] Precision lattice parameter=6.478 ű0.002 Å.

[0123] 4. Prototype Source 2—Slit Effusion Orifice, “Floating” Substrate Temperature

[0124] 20003

[0125] Base Pressure=15 mTorr

[0126] Deposition Pressure 20-21 Torr

[0127] Carrier Gas Flow Rate=20 sccm Argon

[0128] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0129] “Steady-State” Internal Source Temperature=694° C.

[0130] Sample to Orifice Distance=1.5 cm

[0131] Deposition time (at T>880° C.)=0 minutes

[0132] Substrate=3″×3 LOF TEC-15 SL/SnO2/Double Coat CBD CdS (P041+P028)/CdCl2 HT

[0133] Comment: Sample shattered after 4 minutes, run aborted.

[0134] 20004

[0135] Base Pressure=15 mTorr

[0136] Deposition Pressure 20-21 Torr

[0137] Carrier Gas Flow Rate=20 sccm Argon

[0138] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0139] “Steady-State” Internal Source Temperature=880° C.

[0140] Deposition time (at T>850° C.)=6 minutes

[0141] Substrate=4″×2.5″ Solarex 7059/SnO2/Single Coat CBD CdS (P038)

[0142] Comment: Non-uniformly colored deposit. Average thickness based on mass gain=2 μm

[0143] Prototype Source 2—Slit Effusion Orifice, “Controlled” Substrate Temperature

[0144] 20005

[0145] Base Pressure=10 mTorr

[0146] Deposition Pressure 20-21 Torr

[0147] Carrier Gas Flow Rate=20 sccm Argon

[0148] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0149] Target “Steady-State” Internal Source Temperature=880° C.

[0150] Sample to Orifice Distance=1.7 cm

[0151] Deposition time (at T>850° C.)=0 minutes

[0152] Substrate Temperature: Monitored at edge with wide-gauge TC, set˜500° C.

[0153] Variac˜12%).

[0154] Substrate 3″×3″ Solarex 7059/SnO2/Single Coat CBD CdS (P045)

[0155] Comment: Sample shattered during substrate heat-up, run aborted.

[0156] 20006

[0157] Base Press=10 mTorr

[0158] Deposition Pressure 20-21 Torr

[0159] Carrier Gas Flow Rate=20 sccm Argon

[0160] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0161] Target “Steady-State” Internal Source Temperature=880° C.

[0162] Sample to Orifice Distance=1.7 cm

[0163] Deposition time (at T>850° C.)=0 minutes

[0164] Substrate Temperature: Monitored at edge with wide-gauge TC, set˜500° C.

[0165] (Variac˜12%).

[0166] Substrate=3″×3″ Solarex 7059/SnO2/Single Coat CBD CdS (P044)

[0167] Comment: Sample shattered during substrate heat-up, run aborted. Thermal gradient across sample judged to be excessive—sample touched heater clips.

[0168] 20006

[0169] Base Pressure=15 mTorr

[0170] Deposition Pressure 20-21 Torr

[0171] Carrier Gas Flow Rate=20 sccm Argon

[0172] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0173] Target “Steady-State” Internal Source Temperature=900° C.

[0174] Sample to Orifice Distance=1.7 cm

[0175] Deposition time (at T>850° C.)=6 minutes

[0176] Substrate Temperature: Monitored at edge with wide-gauge TC, set˜465° C.

[0177] Variac˜12%).

[0178] Substrate=1″×1″ and 1″×0.5″ IEC 7059/ITO/Evap CdS samples.

[0179] Comment: Samples directly on Vycor heater plate. Deposit thicker in edge band—we don't know the exact temperature in deposition zone. Also, there is significant thermal coupling between source and substrate.

[0180] 20008

[0181] Base Pressure=10 mTorr

[0182] Deposition Pressure 20-21 Torr

[0183] Carrier Gas Flow Rate=20 sccm Argon

[0184] Variac Setting=40% (44 V, 12.5 A, 550 W)

[0185] Target “Steady-State” Internal Source Temperature 880° C.

[0186] Sample to orifice Distance=1.7 cm

[0187] Deposition time (at T>850° C.)=8 minutes

[0188] Substrate Temperature: Monitored at center with narrow gauge TC, set˜500° C.

[0189] (Eurotherm). Rose to 600° C. during deposition.

[0190] Substrate=1″×1″ and 1″×0.5″ IEC 7059/ITO/Evap CdS samples.

[0191] Comment: Deposition observed from left side to right (left 3 cm is where sparge nozzles are located inside source). Mass gain thickness of longitudinally-centered substrates=2.9 μm; growth rate˜0.4 μm/min.

TABLE 5.1
X-ray diffraction peak data and assignments of 20008.
		Raw	2θ	d
	Peak	Counts	(± 0.05 deg)	(Å)	Assignment
	1	6566	23.75	3.74	111
	4	385	39.25	2.29	220
	5	605	46.45	1.953	311
	6	58	56.80	1.619	400
	7	313	62.40	1.487	331
	8	504	71.25	1.322	422
	9	315	76.30	1.247	511
	10	43	84.50	1.145	440
	11	109	89.40	1.095	531

[0192] Texture coefficient=0.31 (111) and 1.19 (311)=>slight (311) texture.

[0193] Precision lattice parameter=6.478 Å=0.002 Å.

[0194] 6.0 Summary and Conclusions

[0195] For source to substrate distance˜1-2 cm, achieved depositions at 0.2 to 1 μm/min (20001, 20002, 20008);

[0196] Deposits in central band are pure CdTe films having˜5 μm grains and ˜random texture (20002 and 20008);

[0197] Sparge holes inside source DO affect longitudinal film thickness (all runs);

[0198] Deposition can be quickly halted by increasing total system pressure (20001).

Claims

1. A method for producing thin film comprises heating a material to a sufficient temperature in a furnace placed inside a vacuum system, flowing an inert gas carrier over through the heated material and entraining the vapors of the material in the carrier gas, and directing the carrier gas containing the vapors onto a substrate heated to a temperature below that of the furnace temperature and placed in close proximity to the exit of the furnace.