CA1242165A - Method and apparatus for plasma-assisted deposition of thin films - Google Patents

Method and apparatus for plasma-assisted deposition of thin films

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Publication number
CA1242165A
CA1242165A CA000479799A CA479799A CA1242165A CA 1242165 A CA1242165 A CA 1242165A CA 000479799 A CA000479799 A CA 000479799A CA 479799 A CA479799 A CA 479799A CA 1242165 A CA1242165 A CA 1242165A
Authority
CA
Canada
Prior art keywords
substrate
plasma
electrode means
chamber
thin film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
CA000479799A
Other languages
French (fr)
Inventor
Prem Nath
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Energy Conversion Devices Inc
Original Assignee
Energy Conversion Devices Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Energy Conversion Devices Inc filed Critical Energy Conversion Devices Inc
Application granted granted Critical
Publication of CA1242165A publication Critical patent/CA1242165A/en
Expired legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32422—Arrangement for selecting ions or species in the plasma
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching
    • H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Abstract

ABSTRACT

An improved method of and apparatus for depositing thin films, such as indium tin oxide, on substrates. The method includes electron beam vaporization of a solid material source and radio frequency plasma ionization of the evaporated material and of at least one reactant gas that is separately supplied. By passing the vaporized solid material and reactant gas through the plasma, they are ionized and react to form the desired compound prior to its deposition.

Description

S0-~56 2 METHOD AND APPARATUS FOR PLASMA-ASSISTED
DEPOSITION OF THIN FILMS

! The present invention concerns a plasma-assisted, electron beam ! evaporation process for depositing films, particularly electrically conductive, light transmitting films. Such films may be deposlted by simple vacuum evaporatlon, but it is difficult to control the composition of such deposited films when they contain a number of constituents, such as indium tin oxide films. In reactive evaporation, a residual atmosphere chemically reacts with other film constituents to produce the film compound. For example, oxygen may react with vaporized tin and lndium for depositing an indium tin oxide film. However, since such reactions are generally very slow, film deposition rates are undesirably low.
The rate of a reactive evaporation process may be accelerated by an activated evaporation process such as is disclosed in U.S. Patent No. 4,336,277 and Preparation of In203 and Tin-doped In20~
Films by a Novel Activated Reactive Evaporation Technique , Thin Solid Films, (1980), both by Bunshah and Nath. These references disclose reslstive heating of ~ndium and tln metals on the presence of an ¦ electron flux to produce a plasma. The process is performed at a pressure about 13 x 10-3 pascal in the presence of argon and a magnetic field.

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It is kn~ Nat solid deposition sources may be heated by electron beam bombardment. Secondary electrons produced ln thus process Jay be used to lonlze the evaporated material. See Bunshah Processes of the Activated Reactive Evaporatlon Type and Their Trlbolog~cal Applicatlons 107 Thln Solld Films page 26 (1983).
U.S. Patent No. 4 361 114 dlscloses radio frequency ~onlzatlon of oxygen in vapor deposltlon of lndium tln oxlde. The oxygen 10nlzatlon occurs at a point remote and lsolated from the tin and ~ndium vapors.
one of these processes produces sufflc1ent depos~tlon rates or rates that are lndependent of the evaporatlon rate or temperature of the solld source mater7als. The lnvention provldes a plasma actlvated evaporation process that overcomes these prevlously unsolved problems.
In the lnventlon solld source materlal ls vaporlzed by heatlng ln a vacuum. The evaporated materlal ls lonlzed ln a radlo frequency plasma establlshed near the source or sources. A react1ve gas lntroduced lnto the plasma near the solld source and is also ionized.
The lonlzed specles react to form the compound to be deposlted. The process ls partlcularly useful ln the formatlon and deposltlon of a multlple constltuent fllm such as indlum tln oxlde. The substrate on whlch the fllm ls condensed may be heated to 300C. In a preferred i. ' ., .
j:
x.

, .

I

s .
, . I, ., apparatus for carrying out the process, a solid source or sources are heated by an electron beam and the plasma is formed between the solid sources and an electrode. A preferred electrode has three spaced plates, the intermediate one of which acts to sustain the plasma, while the outer plates are electrically grounded to confine the volume of the plasma. Preferably, the plates are spaced at a distance less than the dark space of the plasmaO The electrodes contain aligned central apertures that may be of different diameters or may be covered with a screen to confine the plasma. The invention is more easily understood with reference to certain embodlments shown in the drawings and described in more detail.
The present invention provides an improved method of depositing a thin film onto a substrate, said method including the steps of:
vacuumdæing a chamber;
providing an electrically unbiased substrate in the chamber;
providing a supply of solid vaporizable material in the chamber;
heating -the solid material with electron beam means so as to vaporize said material in a vapor zone formed k~hween the substrate and the supply of solid material;
disposing electrode means in the vapor zonel said electrode means operatively disposed in electrical communication with a source of alternating current;

z'~
SO-156 4a providing an ionizable gas; and activating the source of alternating current so as-*D
energize the electrode means and develop an ion-ized pla3ma fran at least the ionized gas, said ion-ized plasma developed in a pla3na region formed proximate the electrode means; whereby the vaporized solid material is activated by the plasma and deposi-ted as a thin firm onto the substrate.
In the drawings appended to this specification:
Figure 1 is a fragmentary, cross-sectional view of a stacked photovoltaic device o~mprising a plurality of p-i-n type cells, each layer of the cells formed, in the preferred embodiment, fram an amorphous semiconductor alloy, the device including a transparent thin film conductive oxide electrode layer formed according to the invention.
Figure 2 is a cross-sectional view illustrating a preferred embodlmYnt of an apparatus for depositing the thin film electrode of Figure 1 onto a continuously moving substrate.
Figure 3A is a fragmentary, cross-sectional, perspective view of a preferred electrode assembly for use in the practice of the invention.
Figure 3B is a fragmentary, cross-sectional, perspective view of a seoond preferred electrode assembly, similar to the assembly of Figure 3A, and for use in the practice of the invention.

~L2 Figure 1 shows a p-i-n type photovoltaic device 10, such as a solar cell, made up of individual p-l-n type cells 12a, 12b and 12c. A
substrate 11 forms a surface of cell 10 and functions as the first electrode. Substrate 11 may be transparent or formed from a metallic material such as stainless steel, aluminum, tantalum, molybdenum or chromium, with or without an insulating layer thereon, or may be an insulating material such as glass with or without embedded metallic particles. Certain applications may require the deposition of a thin conductive oxide layer and/or a thin, resistive barrier layer, and/or a series of base contacts prior to deposition of the semiconductor material. The term "substrate" includes not only a flexible film, but also any elements added to it by preliminary processing.
Each of cells 12a, 12b and 12c is preferably fabricated with an amorphous semiconductor body containing at least a silicon or germanium alloy. Each of the semiconductor bodies includes a n-type conductivity semiconductor layer 20a, 20b and 20c; an intrinsic semiconductor layer laa, 18b and 18c; and a p type conductivity semiconductor layer 16a, 16b and 16c. As illustrated, cell 12b is an intermediate cell and additional intermediate cells may be stacked on the illustrated cells.
A transparent conductive oxide (TC0) layer 22, formed in the preferred embodiment of indium tin oxide, forms a second electrode on device 10. A metallic electrode grid 24 may be applied to layer 22 to shorten the carrier path through the TC0 and increase current collection efficiency.

Chile cell 10 is a stacked assembly of p-l-n type pho-tovoltaic cells, the invention may be used in the fabrication of other electronic devices such as single p-i-n cells, stacked or single n-i-p cells, p-n cells, Schottky barrier cells, transistors, diodes, integrated circuits, photodetectors, and other semiconductor devices, as well as any other application requiring the deposition of a thin film of materlal, such as the manufacture of interference filters, the preparation of optical coatings, etc.
In Figure 2, a preferred embodiment of an apparatus 30 for depositing films according to the invention is shown in cross section.
A vacuum chamber 32 is evacuated through a conduit 34 by a vacuum pump 36. Vacuum chamber 32 i5 divided into three communicating regions: the substrate supply region 32a; the deposition region 32b; and the substrate take-up region 32c. Substrate supply region 32a houses a supply roll 38 of web substrate material 11 and substrate take-up roller 40 about which web substrate 11 may be wound. Deb substrate material 11 extends from substrate supply reel 3~ through deposition region 32b and to take-up roller 40. Motors (not illustrated) continuously advance the web substrate 11 through deposition region 32b.
- A solid precursor material is disposed ln a crucible 42. An electron beam source 44 provides a beam 4~ focused by a conventional ? magnetic f7eld to impinge upon the precursor material in crucible 42.
Electron beam 46 is attracted to crucible 42 by maintaining a positive , potential on the cruclble. By controlling the beam current and voltage, Lit 5 the rate of evaporation of the solid precursor material from crucible 42 may be controlled. Precursor materials disposed in a single crucible may be vaporized by multiple electron beams; or, multiple crucibles and multiple electron beams may be employed to evaporate precursor materials having different melting points. Or a single electron beam may be rapidly switched between several crucibles to vaporize precursor material in each of them.
An electrode assembly 48 disposed between substrate 11 and crucible 42 is used to transmit electromagnetic energy to the precursor material vaporized from crucible 42 and to the reactant gas introduced into chamber 32b. Electrode assembly 48 comprises three planar, generally parallel electrically conductive plates 50, 52 and 54 spaced prom one another by a distance "d". Each of conductive plates 50, 52 and 54 includes a central opening 50a, 52a and 54a, respectively. In apparatus 30, plates 50, 52 and 5~ are generally horizontal. Outer plates 50 and 54 are electrically grounded, while central plate 52 is energized by a radio frequency power supply 55, operating at a conventional frequency, e.g., 13.56 MHz, or at a microwave frequency.
Electrode assembly 48 restricts the activating plasma to a relatively small reglon 56 (indicated in Figure 2 in phantom outline) proximate the central openings 50a, 52a and 54a ln the conductive plates, 50, 52 and 54, to limit ionlc bombardment of substrate 11. The distance separating each of the conductive plates is chosen to be less than the cathode dark space distance of the central plate 52 at the operating conditions to prevent formation of a plasma between the planar surfaces of the contiguous plates. Central opening 52a in the central plate 52 is slightly smaller than openings 50a and 5~a in the contiguous grounded plates 50 and 54. This geometrical arrangement also helps confine the plasma.
Apparatus 30 includes a reactant gas inlet 58 in communication with a gas supply source 60 and deposition region 32b directing reactant gas toward plasma region 56. Gaseous reactant materials, such as oxygen, nitrogen, hydrogen, ammonia, hydrogen sulfide, nitrous oxide, carbon tetrafluoride etc., may be introduced into evaporation apparatus 30 for activation by electrode assembly 48 and combination with precursor material evaporated from crucible 42 to produce a compound.
The compound is deposited on substrate 11. Apparatus 30 may preferably include a substrate heater 62, such as a plurality of radiant heating lamps 64 and an associated radiant heat reflector 66 for heating substrate 11. A thickness monitor 68, such as an optical or piezoelectric monitoring device, may be used to measure the thickness of the thin film deposited on web substrate 11.
As an example of the materials that can be deposlted by apparatus 30, a thin film of indium tin oxide may be deposited on a body of amorphous silicon semiconductor materlal that has been deposited on a web of stainless steel substrate material 11. In this example, web substrate material 11 is threaded through deposition apparatus 30 from supply roll 38 through deposition region 32b and to take-up roll 40. A

3~2~,f2 solid metallic precursor material comprising 85 atomic percent indium and 15 atomic percent tin is disposed in crucible 42. Apparatus 30 is evacuated to a pressure of about 1.33 x 10 3 pascal and backfilled through inlet 58 with oxygen, the reactant gas, to a pressure of about .13 pascal. A power of about 100 watts at a frequency of 13.56 MHz is delivered to cathode plate 52 to form an ionized oxygen plasma in region 56. Heater assembly 62 heats substrate 11 in chamber 32b to approxlmately 150C to 300C. Electron beam source 44 bombards the material in crucible 42 and evaporates the indium tin precursor material. The indium and tin vapors diffuse into region 56 where they are activated by the plasma and react with the oxygen gas to produce the desired indium tin oxide compound that is deposited on continuously advancing web 11. Indium tin oxide deposited in this manner to a thickness of about 60 nanometers exhibits a sheet resistance of about ~0-40 ohms per square, and a light transmission (integrated average percent from about 400 to 800 nanometers) of greater than 90 percent when deposited on glass.
In Figure 3A an electrode assembly 48a, similar to that depicted in Figure 2, includes three generally planar, parallel plates 50, 52, 54, wormed of an electrically conductive material such as aluminum or stainless steel. Each of conductive plate includes a central generally circular aperture 50a, 52a and 54a, respectively.

Plates 50, 52 and 54 are spaced from one another by a distance d which is less than the dark space distance for an electrode operating at a particular frequency and in a particular pressure. Dark space means that region of a glow discharge immediately adjacent the electrode in which little or no plasma discharge or light ls produced. Aperture 52a in plate 52 is of a smaller diameter than are the apertures 50a and 54a. By making aperture 52a somewhat smaller than those in the grounded plates 50 and 54, a plasma may be formed in the region extending through the apertures. It has been found that a very weak plasma, or no plasma at all, ls formed when all of the apertures are uniformly sized.
Electrode assembly 48b in Flgure 3B is similar to electrode assembly 48a, except apertures 50a, 52b and 54a in conductive plates 50, 52 and 54 are all of approximately the same diameter. However, a pair of crcssed, substantially perpendicular, electrically conductive wires 70 and 72 extend across the aperture 52b. Crossed conductlve wires 70 and 72 function to confine the plasma in substantially the same manner as the small central aperture in the plate 52 of assembly 48a.
Similarly an electrically conductive wire grid or wire mesh could extend across the aperture of the central conductive plate 52. Other aperture configurations may be employed to conflne the plasma region to the immediate vicinlty of the apertures. For example, central conductive plate 52 may have a star-shaped aperture. In that conflguration, the inward projecting portions of the aperture confine and sustain the plasma.

Claims (13)

1. An improved method of depositing a thin film onto a substrate, said method including the steps of:
vacuumizing a chamber;
providing an electrically unbiased substrate in the chamber;
providing a supply of solid vaporizable material in the chamber;
heating the solid material with electron beam means so as to vaporize said material in a vapor zone formed between the substrate and the supply of solid material;
disposing electrode means in the vapor zone, said electrode means operatively disposed in electrical communication with a source of alternating current;
providing an ionizable gas; and activating the source of alternating current so as to energize the electrode means and develop an ion-ized plasma from at least the ionized gas, said ion-ized plasma developed in a plasma region formed proximate the electrode means; whereby the vaporized solid material is activated by the plasma and deposited as a thin film onto the substrate.
2. A method as in claim 1, including the further steps introducing a reactive gas proximate the plasma region;
and activating the reactive gas in the plasma region, whereby the activated gas and the reactive vapor of the solid material react for the deposition thereof as a thin film.
3. A method as in claim 1, including the further step of:
maintaining the substrate at a temperature of about room temperature to 300°C. during the deposition of the thin film thereonto.
4. A method as in claim 1, including the further step of:
selecting the solid material from the group consisting essentially of: In, Sn, Cd, Zn, Ti, Si, Ge and mixtures thereof.
5. A method as in claim 2, including the further step of:
selecting the reactive gas from the group consisting essentially of: O2, N2, NH3, CH4, H2S N2O, CF4 and mixtures thereof.
6. A method as in claim 1, wherein the step of energizing the electrode means with alternating current comprises: energizing the electrode means with radio frequency energy.
7. A method as in claim 1, wherein the step of energizing the electrode means with alternating current comprises: energizing the electrode means with micro-wave energy.
8. A method as in claim 1, including the further step of:
maintaining the pressure within the chamber in the range of 10-2-10-4torr.
9. A method as in claim 1, including the further step of:
continuously advancing the substrate through the chamber, whereby a thin film is continuously deposited upon the advancing substrate.
10. A method as in claim 2, wherein:
the step of heating the solid vaporizable material with electron beam means comprises the heating of an indium:tin alloy;
the step of introducing a reactive gas comprises the introduction of oxygen; and the method includes the further step of maintaining the substrate at a temperature from about room temperature to 300°C.
11. A method as in claim 2, wherein:
the step of heating the solid vaporizable material comprises heating indium with electron beam means;
the step of introducing a reactive gas comprises the introduction of oxygen; and the method includes the further step of maintaining the substrate at a temperature of up to 300°C.
12. A method as in claim 2, wherein the substrate in the chamber includes a body of semiconductor material thereupon.
13. A method as in claim 1, wherein the substrate in the chamber includes having a plurality of amorphous semiconductor layers thereupon.
CA000479799A 1984-05-02 1985-04-23 Method and apparatus for plasma-assisted deposition of thin films Expired CA1242165A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/606,014 US4514437A (en) 1984-05-02 1984-05-02 Apparatus for plasma assisted evaporation of thin films and corresponding method of deposition
US606,014 1984-05-02

Publications (1)

Publication Number Publication Date
CA1242165A true CA1242165A (en) 1988-09-20

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Country Status (5)

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US (1) US4514437A (en)
EP (1) EP0161088B1 (en)
JP (1) JPS60243268A (en)
CA (1) CA1242165A (en)
DE (1) DE3563224D1 (en)

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JPS60243268A (en) 1985-12-03
US4514437A (en) 1985-04-30
EP0161088B1 (en) 1988-06-08
JPH0475314B2 (en) 1992-11-30
DE3563224D1 (en) 1988-07-14
EP0161088A1 (en) 1985-11-13

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