# US 8,858,713 B2 · Apparatus for depositing a thin film of material on a substrate and regeneration process for such an apparatus

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- Number: US 8,858,713 B2
- Document ID: US8858713B2
- Status: Granted
- Kind: B2
- Application number: 13/379,220
- Filed: 2010-06-17
- Published: 2012-04-26
- Granted: 2014-10-14
- Earliest claimed: 2009-06-18
- Assignees: Riber
- Applicants: Jerome Villette; Valerick Cassagne; Catherine Chaix
- Inventors: Jerome Villette; Valerick Cassagne; Catherine Chaix
- Web page: https://patentgrep.com/patent/US8858713B2

## CPC

- C30B 23/02: Epitaxial-layer growth
- C23C 16/4401: {Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber}
- C23C 16/4408: {by purging residual gases from the reaction chamber or gas lines}
- C23C 16/455: characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C 16/45502: {Flow conditions in reaction chamber}
- C23C 16/45544: {characterized by the apparatus}
- C30B 23/002: {Controlling or regulating}
- C30B 29/403: {AIII-nitrides}
- Y10T 29/49718: Repairing
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR
- 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 (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

Disclosed is an apparatus for depositing a thin film of material on a substrate and a regeneration process. The apparatus includes a chamber, a cryogenic panel disposed inside the chamber, a sample holder able to support a substrate, a gas injector able to inject a gaseous precursor into the chamber, a first trap connected to the vacuum chamber and able to trap a part of the gaseous precursor released by the cryogenic panel, the first trap having a fixed pumping capacity S1. The apparatus for depositing a thin film of material on a substrate includes a second trap having a variable pumping capacity S2 able to be regulated in function of the gaseous precursor partial pressure, the first and second trap providing a total pumping capacity S=S1+S2 sufficient to maintain the gaseous precursor partial pressure in the vacuum chamber under a determined pressure PL.

## Claims

### Claim 1

An apparatus for depositing a thin film of material on a substrate comprising:
a vacuum chamber,
a sample holder disposed inside said vacuum chamber, said sample holder being configured to support said substrate,
a gas injector configured to inject a gaseous precursor into the vacuum chamber, a part of said gaseous precursor being configured to react at the surface of the substrate,
at least a first cryogenic panel positioned inside the vacuum chamber, and configured to adsorb a part of said gaseous precursor which has not reacted at the surface of the substrate and to release said adsorbed gaseous precursor,
a first trap connected to said vacuum chamber and configured to trap a part of said gaseous precursor released by said first cryogenic panel, said first trap having a fixed pumping capacity S1, and a second trap configured to trap an other part of said gaseous precursor released by said first cryogenic panel, during the trapping of the part of said desorbed gaseous precursor by the first trap, said second trap having a variable pumping capacity S2, and configured to be regulated in function of the gaseous precursor partial pressure,
said first trap and said second trap providing a total pumping capacity S=S1+S2 sufficient to maintain the gaseous precursor partial pressure in the vacuum chamber under a determined pressure PL.

### Claim 2 (depends on 1)

The apparatus according to claim 1, wherein said second trap comprises:
a regulating cryogenic element positioned inside said vacuum chamber, said regulating cryogenic element configured to be supplied by a cryogenic fluid,
a pressure gauge configured to measure the gaseous precursor partial pressure inside the vacuum chamber, generating a measured pressure PM,
a valve configured to adjust the cryogenic fluid flow into said regulating cryogenic element, and
a control unit configured to receive said measured pressure PM and compare said pressure PM to the determined pressure PL,
wherein when the measured pressure PM is different from the determined pressure PL, said control unit is configured to command said valve to adjust the cryogenic fluid flow in said regulating cryogenic element, such that the measured pressure PM reaches the determined pressure PL.

### Claim 3 (depends on 2)

The apparatus according to claim 2, wherein said regulating cryogenic element is an additional cryogenic element.

### Claim 4 (depends on 2)

The apparatus according to claim 2, wherein said regulating cryogenic element is positioned in said at least one first cryogenic panel positioned inside the vacuum chamber.

### Claim 5 (depends on 2)

The apparatus according to claim 2, wherein said sample holder is surrounded by a secondary cryogenic panel, and said regulating cryogenic element is positioned in said secondary cryogenic panel.

### Claim 6 (depends on 1)

The apparatus according to claim 1, wherein said first trap comprises a pumping duct having a wall, said pumping duct being connected to a pumping device by a first ends and emerging into the vacuum chamber by a second ends, and the wall inner surface of said pumping duct is covered by a second cryogenic panel.

### Claim 7 (depends on 6)

The apparatus according to claim 6, wherein said first trap comprise a closing means configured to isolate the volume of the pumping duct of said first trap from the volume of the vacuum chamber.

### Claim 8 (depends on 1)

The apparatus according to claim 1, further comprising a molecular beam epitaxy system for producing wafers of semiconductor material comprising a substrate,
said vacuum chamber being a growth chamber including further a lateral wall having an inner surface, a cryogenic panel covering the inner surface of said lateral wall,
said apparatus comprising at least one effusion cell configured to evaporate atoms or molecules of elements or compounds, a part of said gaseous precursor being configured to react with the evaporated atoms or molecules of elements or compounds on the surface of the substrate to form a layer of semiconductor or insulating compound.

### Claim 9

A process for regenerating cryogenic panels of an apparatus for depositing a thin film of material on a substrate, said apparatus comprising:
a vacuum chamber;
a sample holder disposed inside said vacuum chamber, the sample holder being configured to support the substrate;
a gas injector configured to inject a gaseous precursor into the vacuum chamber, a part of the gaseous precursor being configured to react at the surface of the substrate;
at least a first cryogenic panel positioned inside the vacuum chamber, and configured to adsorb a part of the gaseous precursor which has not reacted at the surface of the substrate and to release the adsorbed gaseous precursor;
a first trap connected to the vacuum chamber and configured to trap a part of the gaseous precursor released by the first cryogenic panel, the first trap having a fixed pumping capacity S1, and a second trap configured to trap an other part of the gaseous precursor released by the first cryogenic panel, the second trap having a variable pumping capacity S2 and configured to be regulated in function of the gaseous precursor partial pressure;
the first trap and the second trap providing a total pumping capacity S=S1+S2 sufficient to maintain the gaseous precursor partial pressure in the vacuum chamber under a determined pressure PL;
the process comprising:
a) evacuation of the gaseous precursor out of the vacuum chamber, said evacuation comprising:
heating the at least first cryogenic panel, producing a desorption of the gaseous precursor initially adsorbed on said first cryogenic panel, and
trapping a part of said desorbed gaseous precursor by the first trap, a portion of said part of the desorbed gaseous precursor being trapped on a second cryogenic panel of said first trap, and
b) regeneration of the second cryogenic panel of said first trap, said regeneration comprising:
isolating said first trap from the vacuum chamber,
heating said second cryogenic panel, producing a desorption of the trapped gaseous precursor from the second cryogenic panel, and
pumping said desorbed gaseous precursor by one or more pumps to produce a vacuum,
the process further comprising, during the trapping of the part of said desorbed gaseous precursor by the first trap in step a),
conducting a complementary trapping operation, by the second trap, of an other part of said gaseous precursor released by said first cryogenic panel,
said second trap having a variable pumping capacity S2 configured to be regulated in function of the gaseous precursor partial pressure,
said trapping operations by the first and second traps providing a total pumping capacity S=S1+S2 sufficient to maintain the gaseous precursor partial pressure in the vacuum chamber under a determined pressure PL.

### Claim 10 (depends on 9)

The process according to claim 9, wherein the complementary trapping operation comprises:
measuring the gaseous precursor pressure inside said vacuum chamber, generating a measured pressure PM,
comparing the measured pressure PM to the determined pressure PL, and
if the measured pressure PM is different from the determined pressure PL, then adjusting the pumping capacity S2 of a regulating cryogenic element located inside said vacuum chamber, such that the measured pressure PM reaches the determined pressure PL.

### Claim 11 (depends on 10)

The process according to claim 10, wherein the pumping capacity S2 of said regulating cryogenic element is adjusted by varying the flow of cryogenic fluid in said regulating cryogenic element.

### Claim 12 (depends on 9)

The process according to claim 9, wherein the gaseous precursor is gaseous ammonia, the determined pressure PL being between 10−2 and 10−1 Pascal.

### Claim 13 (depends on 2)

The apparatus according to claim 2, wherein said first trap comprises a pumping duct having a wall, said pumping duct being connected to a pumping device by a first ends and emerging into the vacuum chamber by a second ends, the wall inner surface of said pumping duct being covered by a cryogenic panel.

### Claim 14 (depends on 3)

The apparatus according to claim 3, wherein said first trap comprises a pumping duct having a wall, said pumping duct being connected to a pumping device by a first ends and emerging into the vacuum chamber by a second ends, the wall inner surface of said pumping duct being covered by a cryogenic panel.

### Claim 15 (depends on 4)

The apparatus according to claim 4, wherein said first trap comprises a pumping duct having a wall, said pumping duct being connected to a pumping device by a first ends and emerging into the vacuum chamber by a second ends, the wall inner surface of said pumping duct being covered by a cryogenic panel.

### Claim 16 (depends on 5)

The apparatus according to claim 5, wherein said first trap comprises a pumping duct having a wall, said pumping duct being connected to a pumping device by a first ends and emerging into the vacuum chamber by a second ends, the wall inner surface of said pumping duct being covered by a cryogenic panel.

### Claim 17 (depends on 2)

The apparatus according to claim 2, further comprising a molecular beam epitaxy system for producing wafers of semiconductor material comprising a substrate,
said vacuum chamber being a growth chamber including further a lateral wall having an inner surface, a cryogenic panel covering the inner surface of said lateral wall,
said apparatus comprising at least one effusion cell configured to evaporate atoms or molecules of elements or compounds, a part of said gaseous precursor being configured to react with the evaporated atoms or molecules of elements or compounds on the surface of the substrate to form a layer of semiconductor or insulating compound.

### Claim 18 (depends on 3)

The apparatus according to claim 3, further comprising a molecular beam epitaxy system for producing wafers of semiconductor material comprising a substrate,
said vacuum chamber being a growth chamber including further a lateral wall having an inner surface, a cryogenic panel covering the inner surface of said lateral wall,
said apparatus comprising at least one effusion cell configured to evaporate atoms or molecules of elements or compounds, a part of said gaseous precursor being configured to react with the evaporated atoms or molecules of elements or compounds on the surface of the substrate to form a layer of semiconductor or insulating compound.

### Claim 19 (depends on 4)

The apparatus according to claim 4, further comprising a molecular beam epitaxy system for producing wafers of semiconductor material comprising a substrate,
said vacuum chamber being a growth chamber including further a lateral wall having an inner surface, a cryogenic panel covering the inner surface of said lateral wall,
said apparatus comprising at least one effusion cell configured to evaporate atoms or molecules of elements or compounds, a part of said gaseous precursor being configured to react with the evaporated atoms or molecules of elements or compounds on the surface of the substrate to form a layer of semiconductor or insulating compound.

### Claim 20 (depends on 5)

The apparatus according to claim 5, further comprising a molecular beam epitaxy system for producing wafers of semiconductor material comprising a substrate,
said vacuum chamber being a growth chamber including further a lateral wall having an inner surface, a cryogenic panel covering the inner surface of said lateral wall,
said apparatus comprising at least one effusion cell configured to evaporate atoms or molecules of elements or compounds, a part of said gaseous precursor being configured to react with the evaporated atoms or molecules of elements or compounds on the surface of the substrate to form a layer of semiconductor or insulating compound.