Pvt-method and device for producing single crystals in a safe manner with regard to the process
US-2024376633-A1 · Nov 14, 2024 · US
US9856582B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9856582-B2 |
| Application number | US-201213428395-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 23, 2012 |
| Priority date | Sep 29, 2009 |
| Publication date | Jan 2, 2018 |
| Grant date | Jan 2, 2018 |
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A method is disclosed with provides stable growth of SiC single crystals, particularly 4H—SiC single crystals, with an effective crystal growth rate for a prolonged time even at a low temperature range of 2000° C. or lower. A raw material containing Si, Ti and Ni is charged into a crucible made of graphite and heat-melted to obtain a solvent. At the same time, C is dissolved out from the crucible into the solvent to obtain a melt. A SiC seed crystal substrate is then brought into contact with the melt such that SiC is supersaturated in the melt in the vicinity of the surface of the SiC seed crystal substrate, thereby allowing growth and production of an SiC single crystal on the SiC seed crystal substrate.
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What is claimed is: 1. A method for production of a SiC single crystal, comprising: dissolving C in a solvent in which a raw material containing Si, Ti and Ni has been heat-melted, thereby preparing a melt; and bringing a SiC seed crystal into contact with the melt such that SiC is supersaturated in the melt in the vicinity of the surface of the SiC seed crystal, to thereby allow growth of the SiC single crystal on the SiC seed crystal, wherein an atomic ratio of Ti relative to Si satisfies the relation 0.05≦[Ti]/([Si]+[Ti])≦0.3, and wherein an atomic ratio of a total of Ti and Ni relative to Si satisfies the relation 0.1≦([Ti]+[Ni])/([Si]+[Ti]+[Ni])≦0.45. 2. The method according to claim 1 , wherein an atomic ratio of Ti relative to Si satisfies the relation 0.1≦[Ti]/([Si]+[Ti])≦0.3. 3. The method according to claim 1 , wherein an atomic ratio of Ni relative to Ti satisfies the relation 0.05≦[Ni]/[([Ti]+[Ni])≦0.70. 4. The method according to claim 1 , wherein an atomic ratio of Ni relative to Ti satisfies the relation 0.05≦[Ni]/[([Ti]+[Ni])≦0.54. 5. The method according to claim 1 , wherein an atomic ratio of Ni relative to Ti satisfies the relation 0.05≦[Ni]/[([Ti]+[Ni])≦0.70. 6. The method according to claim 1 , wherein an atomic ratio of Ni relative to Ti satisfies the relation 0.05≦[Ni]/[([Ti]+[Ni])≦0.54. 7. The method according to claim 1 , which is carried out at atmospheric pressure or under pressure. 8. The method according to claim 1 , wherein the raw material is charged into a crucible. 9. The method according to claim 8 wherein the crucible is made of impurity-free graphite. 10. The method according to claim 8 , wherein a gas containing C is fed into the crucible and is dissolved in the solvent by gas-liquid interface reaction. 11. The method according to claim 10 , wherein the gas containing C is a carbohydrate gas or a carbohydrate gas diluted with hydrogen. 12. The method according to claim 10 , wherein the gas containing C is fed together with a gas containing Si. 13. The method according to claim 12 , wherein the gas continuing Si is silane, disilane, or SiH n Cl 4−n , wherein n is 1, 2 or 3. 14. The method according to claim 12 , wherein composition of the melt is maintained by feeding the gas containing Si. 15. The method according to claim 1 , wherein temperature of the melt is 2000° C. or lower. 16. The method according to claim 15 , wherein the seed crystal is cooled such that the melt at the side of the seed crystal has a lower temperature, wherein a temperature gradient ΔT is about 40° C./cm. 17. The method according to claim 16 , wherein SiC is supersaturated in the vicinity of the surface of seed crystal. 18. The method according to claim 1 , wherein temperature of the melt is 1700° C. or lower.
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