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US4512825A Expired / Lapsed US ⏱️ 0.0 years remaining

Recovery of fragile layers produced on substrates by chemical vapor deposition

Assignee: United States Department of the Navy
•
Filing: 1983-04-12
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Granted: 1985-04-23
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Expires: 2003-04-12
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Abstract

Abstract A method of recovering intact at room temperature a layer of a first material, such as silicon carbide, produced by depositing it from the gas phase at a deposition temperature above room temperature on a substrate of a second material, such as silicon, having a different coefficient of thermal expansion than that of the first material. The substrate is separated from the layer prior to cooling, and then the separated layer is cooled to room temperature free of stresses otherwise present as a result of the different thermal expansions of the substrate and layer.

Inventors

  • 👤 Arrigo Addamiano
  • 👤 Philipp H. Klein

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 12:51
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/01; Y; Y10; Y10S; Y10S117/00; Y10S117/915; Y10S148/00; Y10S148/054; Y10S148/135; Y10S148/148; Y10S438/00; Y10S438/977

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 183 words
A method of recovering intact at room temperature a layer of a first material produced by depositing it from the gas phase at a deposition temperature above room temperature on a substrate of a second material having a lower melting point and a different coefficient of thermal expansion than that of the first material, the uncoated side of the substrate being the underside of the substrate and the side of the layer adjacent to the substrate being the underside of the layer, comprising the steps of: supporting the substrate underside around its perimeter along a support plane at a non-orthogonal incline from horizontal; separating the substrate from the layer by heating the substrate to melt the substrate from the layer; receiving the freed layer underside around its perimeter along a plane parallel to the support plane after it displaces in the range of the thickness of the substrate; and cooling the separated layer to room temperature, whereby the separated layer is not subjected to stresses caused by the different thermal expansion of the substrate and layer when they are cooled to room temperature.
Claim 2
Independent Claim 183 words
A method of recovering intact at room temperature a layer of a first material produced by depositing it from the gas phase at a deposition temperature above room temperature on a substrate of a second material having a lower melting point and a different coefficient of thermal expansion than that of the first material, the uncoated side of the substrate being the underside of the substrate and the side of the layer adjacent to the substrate being the underside of the layer, comprising the steps of: supporting the substrate underside around its perimeter along a support plane at a non-orthogonal incline from horizontal; separating the substrate from the layer by heating the substrate to melt the substrate from the layer; receiving the freed layer underside around its perimeter along a plane parallel to the support plane after it displaces in the range of the thickness of the substrate; and cooling the separated layer to room temperature, whereby the separated layer is not subjected to stresses caused by the different thermal expansion of the substrate and layer when they are cooled to room temperature.
Claim 3
Dependent Claim 37 words
The method recited in claim 1 wherein the melting step includes: heating the substrate to a temperature sufficiently above its melting point to reduce the viscosity of the molten substrate and favor its separation from the layer.
Claim 4
Dependent Claim 29 words
The process recited in claim 2 wherein: the substrate is heated to the temperature above its melting point for a short enough time that the layer is not dissociated.
Claim 5
Dependent Claim 22 words
The process recited in claim 3 wherein: the substrate is heated at a low enough temperature that the layer is not dissociated.
Claim 6
Dependent Claim 32 words
The method recited in claim 4, wherein the step of supporting the substrate includes supporting the substrate along the support plane at an incline in the range of 20 degrees from horizontal.
Claim 7
Independent Claim 208 words
A method of recovering intact at room temperature a layer of a material produced by depositing it from the gas phase at a deposition temperature on a silicon substrate having a lower melting point and a different coefficient of thermal expansion than that of the material, the uncoated side of the substrate being the underside of the substrate and the side of the layer adjacent to the substrate being the underside of the layer, comprising the steps of: supporting the substrate underside around its perimeter along a support plane at an incline from horizontal in the range of 20 degrees; separating the substrate from the layer by heating the substrate to a temperature sufficiently above its melting point to melt the substrate and reduce the viscosity of the melted substrate to favor its separation from the layer, and for a short enough time so that the layer is not dissociated; receiving the freed layer underside around its perimeter along a plane parallel to the support plane after it displaces in the range of the thickness of the substrate; and cooling the separated layer to room temperature, whereby the separated layer is not subjected to stresses caused by the different thermal expansions of the substrate and layer when cooled.
Claim 8
Independent Claim 208 words
A method of recovering intact at room temperature a layer of a material produced by depositing it from the gas phase at a deposition temperature on a silicon substrate having a lower melting point and a different coefficient of thermal expansion than that of the material, the uncoated side of the substrate being the underside of the substrate and the side of the layer adjacent to the substrate being the underside of the layer, comprising the steps of: supporting the substrate underside around its perimeter along a support plane at an incline from horizontal in the range of 20 degrees; separating the substrate from the layer by heating the substrate to a temperature sufficiently above its melting point to melt the substrate and reduce the viscosity of the melted substrate to favor its separation from the layer, and for a short enough time so that the layer is not dissociated; receiving the freed layer underside around its perimeter along a plane parallel to the support plane after it displaces in the range of the thickness of the substrate; and cooling the separated layer to room temperature, whereby the separated layer is not subjected to stresses caused by the different thermal expansions of the substrate and layer when cooled.
Claim 9
Dependent Claim 15 words
The method recited in claim 6 wherein: the material of the layer is silicon carbide.
Claim 10
Dependent Claim 24 words
The method recited in claim 7 wherein: the silicon substrate is heated to a temperature in the range of 1500° C. to 1550° C.
Claim 11
Dependent Claim 29 words
The method recited in claim 8 wherein: the silicon substrate is heated to the temperature in the range of 1500° C. to 1550° C. for less than a minute.
Claim 12
Dependent Claim 13 words
The method recited in claim 9 wherein: the deposition temperature is 1400° C.
Claim 13
Independent Claim 176 words
A method of recovering intact at room temperature a layer of silicon carbide produced by depositing it from the gas phase at 1400° C. on a silicon substrate, the uncoated side of the substrate being the underside of the substrate and the side of the layer adjacent to the substrate being the underside of the layer, comprising the steps of: supporting the substrate underside around its perimeter in a hemispherical cavity formed in the upper face of a susceptor positioned with an incline from horizontal in the range of 20° degrees; separating the substrate by heating it to a temperature in the range of 1500° C. to 1550° C. for less than a minute to melt the substrate from the layer; receiving the freed layer underside along its permimeter in the hemispherical cavity after the layer displaces in the range of the thickness of the substrate; and cooling the separated layer to room temperature; whereby the separated layer is not subjected to stresses caused by the different thermal expansions of the substrate and layer when cooled.
Claim 14
Independent Claim 176 words
A method of recovering intact at room temperature a layer of silicon carbide produced by depositing it from the gas phase at 1400° C. on a silicon substrate, the uncoated side of the substrate being the underside of the substrate and the side of the layer adjacent to the substrate being the underside of the layer, comprising the steps of: supporting the substrate underside around its perimeter in a hemispherical cavity formed in the upper face of a susceptor positioned with an incline from horizontal in the range of 20° degrees; separating the substrate by heating it to a temperature in the range of 1500° C. to 1550° C. for less than a minute to melt the substrate from the layer; receiving the freed layer underside along its permimeter in the hemispherical cavity after the layer displaces in the range of the thickness of the substrate; and cooling the separated layer to room temperature; whereby the separated layer is not subjected to stresses caused by the different thermal expansions of the substrate and layer when cooled.
Claim 15
Dependent Claim 31 words
The method recited in claim 11 including the step of: etching the separated layer after it is cooled to room temperature in order to eliminate any residual traces of free silicon.
Claim 16
Dependent Claim 26 words
The method recited in claim 12 wherein: the separated layer is etched with a mixture of one part-by-volume hydrofluoric acid to three parts-by-volume of nitric acid.
Claim 17
Dependent Claim 17 words
The method recited in claim 13 wherein: the separated layer is etched for one to two minutes.

References Cited (Backward Citations)

US3436255A Cited
US3520740A Cited
US3960619A Cited
US3993533A Cited
US4116751A Cited
US4308078A Cited
US4303463A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1988-04-22 1988-10-22 1989-04-23 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1992-04-22 1992-10-22 1993-04-23 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1996-04-22 1996-10-22 1997-04-23 $7700.00 Window Closed / Lapsed

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