# US 4,392,453 A · Molecular beam converters for vacuum coating systems

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- Number: US 4,392,453 A
- Document ID: US4392453A
- Status: Granted
- Kind: A
- Application number: 06/296,288
- Filed: 1981-08-26
- Granted: 1983-07-12
- Earliest claimed: 1981-08-26
- Assignees: Varian Associates, Inc.
- Inventors: Paul E. Luscher
- Web page: https://patentgrep.com/patent/US4392453A

## CPC

- C30B 25/14: Feed and outlet means for the gases; Modifying the flow of the reactive gases
- C23C 14/24: Vacuum evaporation
- C30B 23/002: {Controlling or regulating}
- Y10S 148/169: Vacuum deposition, e.g. including molecular beam epitaxy
- Y10S 438/961: Ion beam source and generation
- 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)
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

This invention relates to coating of substrates in a vacuum system. A beam of molecules incident upon a molecular beam converter is transformed into a molecular beam flowing from the converter toward a substrate to be coated, or on which a layer is to be grown epitaxially. The incident beam is directed onto a heated impingement surface. In most embodiments the impingement surface generally faces the substrate to be coated, and the incident beam strikes the surface from the substrate side. A heating means maintains the impingement surface at a designated temperature. The heating means is separated and shielded from the impingement surface to avoid introducing contaminants from the heating means into the converted molecular beam, and also to avoid adverse physical and chemical effects on the heating means caused by the incident beam and its dissociation products. The incident beam may consist of gaseous compounds of normally solid materials which are at least partially dissociated at the heated impingement surface; the converted beam will then differ from the incident beam in direction, angular distribution, and molecular species. Alternatively, the incident beam may consist of atoms or molecules of elemental solids, in which case reflection and angular redistribution, with or without further dissociation, may occur at the heated impingement surface. Coating uniformity and step coverage can be improved by controlling the size and shape of the incident beam.

## Claims

### Claim 1

A molecular beam converter for use in a vacuum system for coating a substrate, said molecular beam converter comprising:
a body having an impingement surface generally facing said substrate;
a heating means to enable said impingement surface to be maintained at a designated temperature;
a molecular source for forming and directing an incident molecular beam onto said impingement surface;
impingement of said incident molecular beam on said impingement surface maintained at said designated temperature causing a converted molecular beam to flow from said surface;
said impingement surface and said molecular source in combination being configured to largely avoid impingement on said surface by molecular species in said converted molecular beam;
said impingement surface and said molecular source in combination being configured and positioned to direct said converted molecular beam generally toward said substrate.

### Claim 2 (depends on 1)

A molecular beam converter as in claim 1 in which said coating of said substrate is a layer grown epitaxially on said substrate.

### Claim 3 (depends on 1)

A molecular beam converter as in claim 1 in which said heating means is separated and shielded from said impingement surface, whereby introduction of contaminants from said heating means into said converted molecular beam is avoided, and also whereby damage to said heating means through interaction with said incident and converted molecular beams is avoided.

### Claim 4 (depends on 1)

A molecular beam converter as in claim 1 in which said incident molecular beam consists of a gaseous compound of a normally solid material, and in which said impingement on said impingement surface causes said gasous compound to be at least partially dissociated, whereby said converted molecular beam contains molecular species of said normally solid material.

### Claim 5 (depends on 4)

A molecular beam converter as in claim 4 in which said gaseous compound of a normally solid material is arsine and in which said converted molecular beam contains molecular species of arsenic.

### Claim 6 (depends on 4)

A molecular beam converter as in claim 4 in which said gaseous compound of a normally solid material is phosphine and in which said converted molecular beam contains molecular species of phosphorus.

### Claim 7 (depends on 4)

A molecular beam converter as in claim 4 in which said gaseous compound of a normally solid material is silane and in which said converted molecular beam contains molecular species of silicon.

### Claim 8 (depends on 1)

A molecular beam converter as in claim 1 in which said incident molecular beam consists of polymeric molecular species of a normally solid material, and in which said impingement on said impingement surface causes at least partial dissociation of said polymeric molecular species into molecular species of lower polymeric order.

### Claim 9 (depends on 1)

A molecular beam converter as in claim 1 in which said incident molecular beam consists principally of the tetramer molecular specie of arsenic, and in which said impingement on said impingement surface causes at least partial dissociation of said tetramer molecular specie of arsenic into dimer and monomer molecular species of arsenic.

### Claim 10 (depends on 1)

A molecular beam converter as in claim 1 in which said incident molecular beam consists principally of the tetramer molecular specie of phosphorous and in which said impingement on said impingement surface causes at least partial dissociation of said tetramer molecular specie of phosphorous into dimer and monomer molecular species of phosphorus.

### Claim 11 (depends on 1)

A molecular beam converter as in claim 1 in which said converted molecular beam consists of substantially the same molecular species as said incident molecular beam, said converted molecular beam differing generally from said incident molecular beam in direction of flow and in angular distribution.

### Claim 12 (depends on 1)

A molecular beam converter as in claim 1 in which said molecular source is a gallium furnace directing a molecular beam of atomic gallium onto said heated impingement surface, said converted molecular beam consisting of said atomic gallium, said converted molecular beam differing generally from said incident molecular beam in direction of flow and in angular distribution.

### Claim 13 (depends on 1)

A molecular beam converter as in claim 1 in which said substrate is generally planar and circular in shape.

### Claim 14 (depends on 13)

A molecular beam converter as in claim 13 in which said impingement surface is a planar disc, said planar disc being generally parallel with said planar substrate, and in which central axes of said planar disc and said substrate generally coincide.

### Claim 15 (depends on 14)

A molecular beam converter as in claim 14 in which the diameter of said planar disc is approximately the same as the diameter of said substrate, and in which said planar disc and said substrate are spaced axially apart by a distance greater than the diameter of said substrate.

### Claim 16 (depends on 15)

A molecular beam converter as in claim 15 in which said incident molecular beam consists of a gaseous compound of a normally solid material, and in which said impingement on said impingement surface causes said gaseous compound to be at least partially dissociated, whereby said converted molecular beam contains molecular species of said normally solid material.

### Claim 17 (depends on 16)

A molecular beam converter as in claim 16 in which said gaseous compound is supplied to said molecular source from a container external to said vacuum system, said gaseous compound being supplied at a controlled rate to said molecular source by a leak valve means, and said molecular source directing said incident molecular beam onto said impingement surface by a source gas feed means.

### Claim 18 (depends on 17)

A molecular beam converter as in claim 17 in which said source gas feed means is a tubular nozzle having a diameter small in comparison with said diameter of said planar disc, said nozzle positioned to direct said incident molecular beam generally toward the central area of said planar disc, said nozzle positioned generally away from the path of flow of said converted molecular beam to said substrate.

### Claim 19 (depends on 17)

A molecular beam converter as in claim 17 in which said source gas feed means comprises a plurality of tubular nozzles, said incident molecular beam thereby comprising a corresponding plurality of individual incident molecular beams, and said converted molecular beam thereby comprising a corresponding plurality of individual converted molecular beams, individual ones of said tubulr nozzles having diameters small in comparison with said diameter of said planar disc, said plurality of individual nozzles positioned to direct said plurality of individual incident molecular beams onto generally spaced-apart areas adjacent the periphery of said planar disc, whereby said converted molecular beam provides substantially improved step coverage and uniformity in arrival rate at said substrate of molecules from said converted molecular beam, said improved step coverage and uniformity being over the area of said substrate.

### Claim 20 (depends on 17)

A molecular beam converter as in claim 17 in which said source gas feed means is of annular configuration and positioned to direct said incident molecular beam onto an annular region adjacent the periphery of said planar disc, whereby said converted molecular beam provides substantially improved step coverage and uniformity in arrival rate at said substrate of molecules from said converted molecular beam, said improved step coverage and uniformity being over the area of said substrate.

### Claim 21 (depends on 4)

A molecular beam converter as in claim 4 in which said substrate is generally planar and circular in shape.

### Claim 22 (depends on 21)

A molecular beam converter as in claim 21 in which said impingement surface is a flat-bottomed stubby cylinder positioned generally coaxially with said substrate, said cylinder having an inside wall of diameter greater than that of said substrate, said inside wall of said cylinder extending less than the radius of said substrate from said flat bottom toward said substrate, and said flat bottom and said substrate being generally parallel and spaced axially apart by a distance greater than the diameter of said substrate.

### Claim 23 (depends on 21)

A molecular beam converter as in claim 21 in which said impingement surface is a flat-bottomed cone positioned generally coaxially with said substrate, interior conical sidewalls of said cone extending toward said substrate and terminating at a distance from said substrate greater than the radius of said substrate, extensions of said interior conical sidewalls encompassing said substrate.

### Claim 24 (depends on 21)

A molecular beam converter as in claim 21 in which said impingement surface is a truncated conic section positioned generally coaxially with said substrate, spaced axially apart from said substrate by a distance greater than the diameter of said substrate, said truncated conic section having a central opening, thus enabling said molecular source to direct said incident molecular beam onto said impingement surface from an interiorly-located, coaxial position.

### Claim 25 (depends on 21)

A molecular beam converter as in claim 21 in which said impingement surface is a truncated spheric section positioned generally coaxially with said substrate, spaced axially apart from said substrate by a distance greater than the diameter of said substrate, said truncated spheric section having a central opening, thus enabling said molecular source to direct said incident molecular beam onto said impingement surface from an interiorly-located, coaxial position.

### Claim 26

A molecular beam converter for use in a vacuum system for coating a substrate, said molecular beam converter comprising:
a body having an impingement surface generally facing said substrate;
a heating means to enable said impingement surface to be maintained at a designated temperature;
a plurality of molecular sources for forming and directing a plurality of incident molecular beams onto said impingement surface;
impingement of said plurality of incident molecular beams on said impingement surface maintained at said designated temperature causing a plurality of converted molecular beam to flow from said surface;
said impingement surface and said plurality of molecular sources in combination being configured to largely avoid impingement on said surface by molecular species in said plurality of converted molecular beams;
said impingement surface and said plurality of molecular sources in combination being configured and positioned to direct said plurality of converted molecular beams generally toward said substrate.

### Claim 27 (depends on 26)

A molecular beam converter as in claim 26 in which said plurality of incident molecular beams all consist of generally identical molecular species, individual ones of said incident molecular beams being directed onto generally spaced-apart areas on said impingement surface, whereby said plurality of converted molecular beams provides substantially improved step coverage and uniformity in arrival rate at said substrate of molecules from said converted molecular beams, said improved step coverage and uniformity being over the area of said substrate.

### Claim 28 (depends on 26)

A molecular beam converter as in claim 26 in which individual ones of said plurality of incident molecular beams consist of differing molecular species, whereby said plurality of converted molecular beams provides a corresponding multiplicity of molecular species flowing toward said substrate.

### Claim 29 (depends on 1)

A molecular beam converter as in claim 1 in which said molecular source directs said incident molecular beam onto said impingement surface in a ribbon-like area adjacent the periphery of said surface, whereby said converted molecular beam provides substantially improved step coverage and uniformity in arrival rate at said substrate of molecules from said converted molecular beam, said improved step coverage and uniformity being over the area of said substrate.

### Claim 30 (depends on 7)

A molecular beam converter as in claim 7 in which said coating of said substrate is a layer of silicon grown epitaxially on said substrate.

### Claim 31

A molecular beam converter for use in a vacuum system for coating a substrate, said molecular beam converter comprising:
a body having an impingement surface generally facing said substrate;
a heating means to enable said impingement surface to be maintained at a designated temperature;
a molecular source for forming and directing an incident molecular beam onto said impingement surface;
impingement of said incident molecular beam on said impingement surface maintained at said designated temperature causing a converted molecular beam to flow from said surface generally toward said substrate;
said impingement surface and said molecular source in combination being configured such that the axis of said incident molecular beam is directed against a portion of said impingement surface which is non-parallel to the axis of said incident beam.

### Claim 32 (depends on 31)

A molecular beam converter as claimed in claim 31 wherein said portion of said impingement surface is non-parallel to the axis of said converted molecular beam.