CN114318519B - Fixing method of silicon carbide seed crystal and graphite cover, graphite cover and growth process method - Google Patents
Fixing method of silicon carbide seed crystal and graphite cover, graphite cover and growth process method Download PDFInfo
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- CN114318519B CN114318519B CN202111674812.0A CN202111674812A CN114318519B CN 114318519 B CN114318519 B CN 114318519B CN 202111674812 A CN202111674812 A CN 202111674812A CN 114318519 B CN114318519 B CN 114318519B
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Abstract
The invention discloses a method for fixing silicon carbide seed crystals and a graphite cover, the graphite cover and a growth process method, comprising the following steps: forming a diamond film layer on the fixed surface of the silicon carbide seed crystal; forming an organic adhesive layer on the bonding surface of the graphite cover; the back surface of the silicon carbide seed crystal is opposite to the bonding surface of the graphite cover, so that the diamond film layer and the organic adhesive layer are bonded together; and applying a first set pressure to the graphite cover bonded with the silicon carbide seed crystal and heating to a first set temperature to solidify the organic glue layer into a bonded graphite layer, wherein the first set temperature is lower than the graphite phase transition temperature of the diamond. The sublimation of the back surface of the seed crystal in the growth process of the silicon carbide single crystal is reduced, and the yield of the silicon carbide crystal is improved.
Description
Technical Field
The invention belongs to the technical field of semiconductor processing, and particularly relates to a method for fixing silicon carbide seed crystals and a graphite cover, the graphite cover and a growth process method.
Background
The silicon carbide single crystal material is generally grown by adopting a PVT (physical vapor transport) method, in the PVT method, silicon carbide powder is adopted as a raw material for growing single crystals, a silicon carbide seed crystal is adhered to the top (graphite cover) of a graphite crucible to be used as a seed crystal, the graphite crucible is heated by an electromagnetic induction coil, the silicon carbide raw material is heated to sublimate by the heat conduction of the graphite crucible, and the vapor silicon carbide is conveyed to the seed crystal position to start growing under the action of an axial temperature gradient, so that the single crystal silicon carbide can be grown at a specific temperature.
At present, the seed crystal is bonded by adopting a high-temperature curing method of the organic adhesive and the graphite cover, but due to the factors of uneven coating of the adhesive on the back surface of the seed crystal, higher roughness of the processed surface of the bonding surface of the graphite cover and the like, bonding air holes exist between the bonded seed crystal and the graphite cover, and the bonding quality of the organic layer is difficult to control to reduce the void ratio of the bonding layer. With the demand for growing silicon carbide crystals becoming higher and higher, the seed crystals used are larger and larger (currently, 6 inch seed crystals are the main stream in the market, 8 inch silicon carbide crystal growth is started to be developed by individual manufacturers), the porosity of an adhesive organic layer is controlled to be harder and harder, the yield and consistency of the silicon carbide grown crystal are greatly affected, and due to poor heat conduction at the adhesive air holes, local hot spots exist on the back surface of the seed crystals in the crystal growth process, the back surface of the seed crystals are promoted to be locally decomposed and sublimated (sublimated on the back surface) and form tiny cavities, one part of the cavities stay in the seed crystals or the inside of the crystal (form hexagonal cavities) in the crystal growth process, and microtubes are generated in the crystal, so that the yield of the silicon carbide crystal is greatly affected.
Disclosure of Invention
The invention aims to provide a fixing method of a silicon carbide seed crystal and a graphite cover, the graphite cover and a growth process method, so that the bonding quality between the silicon carbide seed crystal and the graphite cover is improved, and the bonding of the silicon carbide seed crystal and the graphite cover is firmer and more stable.
In a first aspect, the present invention provides a method for fixing a silicon carbide seed crystal and a graphite cover, comprising:
forming a diamond film layer on a fixed surface of a silicon carbide seed crystal;
forming an organic adhesive layer on the bonding surface of the graphite cover;
the fixing surface of the silicon carbide seed crystal is opposite to the bonding surface of the graphite cover, so that the diamond film layer and the organic adhesive layer are bonded together;
and applying a first set pressure to the graphite cover adhered with the silicon carbide seed crystal and heating to a first set temperature to enable the organic adhesive layer to be solidified into an adhered graphite layer, wherein the first set temperature is lower than the graphite phase transition temperature of diamond.
Optionally, forming the diamond film layer on the fixing surface of the silicon carbide seed crystal includes:
placing the silicon carbide seed crystal in an epitaxial process chamber;
and heating the silicon carbide seed crystal to a second set temperature, and introducing hydrogen with a first set flow rate and methane with a second set flow rate into the epitaxial process chamber to form the diamond film layer on the fixing surface of the silicon carbide seed crystal.
Optionally, the applying a first set pressure to the graphite cap to which the silicon carbide seed crystal is bonded and heating to a first set temperature comprises:
placing the graphite cover bonded with the silicon carbide seed crystal into a vacuum hot-pressing furnace;
the pressure applied to the graphite cover by the pressure applying mechanism of the vacuum hot pressing furnace is the first set pressure, the graphite cover is heated to the first set temperature, and the hot pressing time of the graphite cover is the first set duration.
Optionally, the first set pressure is 3000N-10000N, and the first set temperature is 700 ℃ to 1000 ℃.
Optionally, the second set temperature is 900-1000 ℃, the first set flow is 100-500 sccm, and the second set flow is 1-10 sccm; the purities of the hydrogen and the methane are 5N-9N.
Optionally, the first set duration is 1 h-10 h.
Optionally, the thickness of the diamond film layer is less than 100um.
In a second aspect, the present invention provides a graphite cap for silicon carbide crystal growth, the graphite cap having the silicon carbide seed crystal bonded thereto obtained by the fixing method of the first aspect.
In a third aspect, the present invention provides a process for growing silicon carbide crystals, the process employing the graphite cap of the second aspect bonded with the silicon carbide seed crystal;
and setting the process temperature of the silicon carbide crystal growth to be a third set temperature, wherein the third set temperature is higher than the first set temperature, so that the diamond film layer is solidified into a graphite filling layer.
Optionally, the third set temperature is equal to or higher than 1900 ℃.
The invention has the beneficial effects that:
according to the method for fixing the silicon carbide seed crystal and the graphite cover, the diamond film layer is firstly formed on the fixing surface of the silicon carbide seed crystal, then the organic adhesive layer is formed on the bonding surface of the graphite cover, the fixing surface of the silicon carbide seed crystal and the bonding surface of the graphite cover are opposite to each other, so that the diamond film layer is bonded with the organic adhesive layer, the graphite cover bonded with the silicon carbide seed crystal is subjected to hot pressing to enable the organic adhesive layer to be thermally pressed and solidified into the bonded graphite layer, the bonding strength between the seed crystal and the graphite cover is increased, the subsequent high-temperature growth process is prevented from falling off, wherein the diamond film layer and the fixing surface of the seed crystal formed at first can form SP3 bond tightly in a C-Si or C-C chemical bond mode, the back surface (fixing surface) of the seed crystal is protected, and the temperature of the hot pressing process is lower than the temperature at which graphite phase transition occurs to diamond is lower than that of the organic adhesive layer can only be carbonized into the graphite phase bonding graphite layer at high temperature through the hot pressing process, and graphite phase transition does not occur to the diamond film layer can provide sublimation protection for the fixing surface of the seed crystal, good seed crystal in the subsequent growth process can be effectively avoided, and the back surface of the silicon carbide crystal can be improved.
According to the process method of the silicon carbide crystal, the graphite cover adhered with the silicon carbide seed crystal is adopted to carry out the growth process of the silicon carbide crystal, and the diamond film layer on the graphite cover can be automatically converted from compact SP3 phase to the same compact graphite SP2 phase under the high-temperature condition of silicon carbide growth, so that the tight combination between the seed crystal fixing surface and the graphite cover is effectively ensured, the protection is formed, the generation of hexagonal cavities due to sublimation on the back surface of the seed crystal can be reduced, and the growth quality of the silicon carbide single crystal is improved.
The system of the present invention has other features and advantages which will be apparent from or are set forth in detail in the accompanying drawings and the following detailed description, which are incorporated herein, and which together serve to explain certain principles of the invention.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 illustrates a step diagram of a method of securing a silicon carbide seed crystal to a graphite cap, in accordance with one embodiment of the present invention.
Detailed Description
In the first prior art, a silicon carbide seed crystal bonding method is provided, a first organic layer is formed on a bonding surface of a seed crystal support, and the first organic layer is used for reducing the porosity of the seed crystal support; forming a second organic layer on the bonding surface of the silicon carbide seed crystal to protect the silicon carbide seed crystal; bonding two surfaces of a flexible barrier sheet (graphite paper) with the first organic layer on the seed crystal support and the second organic layer on the silicon carbide seed crystal respectively; and solidifying the bonded silicon carbide seed crystal by adopting a heating mode.
In the method, organic materials are used as the adhesive, and hydroxyl groups are contained in the organic coating in the carbonization process and expand after being heated, so that the risk of generating bubbles in the bonding layer can be caused, and the problem of generation of bonding air holes can not be fundamentally solved. If the bonding air holes are generated, the fixed surface of the seed crystal is heated unevenly, the back surface of the seed crystal material can still sublimate, and then in the crystal growth process, the seed crystal and the crystal generate hexagonal cavities and micropipe defects, so that the yield is reduced.
According to the invention, the diamond film is extended on the back surface of the seed crystal, and the diamond is tightly combined with the fixing surface (back surface) of the silicon carbide seed crystal, so that the back surface sublimation caused by a gap introduced by the organic bonding layer can be fundamentally avoided, and the silicon carbide crystal growth cannot be polluted by pure carbon material, so that the gas phase substances generated by the back surface sublimation are reduced from continuously escaping from bonding pores, and the defect of hexagonal cavities formed on the seed crystal is further reduced.
The invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention are illustrated in the drawings, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Example 1
Fig. 1 shows a step diagram of a method of securing a silicon carbide seed crystal to a graphite cap in accordance with the present invention.
As shown in fig. 1, a method for fixing a silicon carbide seed crystal and a graphite cover comprises the following steps:
step S101: forming a diamond film layer on the fixed surface of the silicon carbide seed crystal;
the method specifically comprises the following steps:
placing a silicon carbide seed crystal into an epitaxial process chamber;
and heating the silicon carbide seed crystal to a second set temperature, and introducing hydrogen with a first set flow and methane with a second set flow into the epitaxial process chamber to form a diamond film layer on the fixing surface of the silicon carbide seed crystal.
Wherein the second set temperature is 900-1000 ℃, the first set flow is 100-500 sccm, and the second set flow is 1-10 sccm; the purities of the hydrogen and the methane are 5N-9N.
In a specific application scenario, a silicon carbide seed crystal is placed in a microwave plasma CVD process chamber, hydrogen with a first set flow rate and methane with a second set flow rate are introduced into the process chamber, and after the process chamber reaches a second set temperature, a diamond film layer is epitaxially grown on a fixed surface of the silicon carbide seed crystal. Wherein, the purity of the hydrogen and the methane is preferably 9N (the specially-made ultrapure gas with the purity of 99.9999999 percent), and the first set flow is preferably 300sccm; the second set flow rate is preferably 3sccm; the first set temperature is preferably 900 ℃. The thickness of the diamond film layer formed is preferably less than 100um.
According to the method, a diamond film layer is epitaxially grown on the silicon carbide seed crystal fixing surface in a Chemical Vapor Deposition (CVD) mode, the epitaxial diamond film layer can be a monocrystalline diamond film layer, a polycrystalline diamond film layer or a nano diamond film layer, high-purity hydrogen and high-purity methane are introduced into an epitaxial process, an atomic-level and flat diamond film layer can be formed on the silicon carbide seed crystal fixing surface, the surface roughness of the diamond film layer can be less than 100nm, SP3 bonds are tightly combined between the diamond film layer and the seed crystal fixing surface (Si surface) in a C-Si or C-C chemical bond mode, and the SP3 bond structure is denser and firmer than an SP2 bond formed by a carbonization organic coating method adopted in the prior art, the atomic structure is also more stable, and the seed crystal fixing surface (Si surface) can be protected from generating void defects due to high-temperature sublimation.
Step S102: forming an organic adhesive layer on the bonding surface of the graphite cover;
in the above specific application scenario, an organic adhesive layer may be formed by spin-coating a layer of organic adhesive on the bonding surface of the graphite cover. The organic glue may comprise a two-component epoxy adhesive (AB glue) which acts to bond the seed crystal with the epitaxial diamond film.
Step S103: the fixing surface of the silicon carbide seed crystal is opposite to the bonding surface of the graphite cover, so that the diamond film layer and the organic adhesive layer are bonded together;
in the specific application scene, the fixing surface of the silicon carbide seed crystal is opposite to the bonding surface of the graphite cover and bonded together, so that the seed crystal with the epitaxial diamond film layer and the graphite cover are bonded and fixed together.
Step S104: and applying a first set pressure to the graphite cover bonded with the silicon carbide seed crystal and heating to a first set temperature to solidify the organic glue layer into a bonded graphite layer, wherein the first set temperature is lower than the graphite phase transition temperature of the diamond.
In this step, applying a first set pressure to the graphite cap to which the silicon carbide seed crystal is bonded and heating to a first set temperature includes:
placing the graphite cover bonded with the silicon carbide seed crystal into a vacuum hot-pressing furnace;
the pressure applied to the graphite cover by the pressure applying mechanism of the vacuum hot-pressing furnace is a first set pressure, the graphite cover is heated to a first set temperature, and the hot-pressing time of the graphite cover is a first set duration.
Wherein the first set pressure is 3000N-10000N, the first set temperature is 700-1000 ℃, and the first set time is 1-10 h.
In the specific application scene, placing the graphite cover bonded with the silicon carbide seed crystal into a vacuum hot-pressing furnace; setting the pressure of a vacuum hot-pressing furnace as a first set pressure, setting the temperature as a first set temperature, setting the hot-pressing time as a first set duration, and solidifying and carbonizing the organic adhesive layer into a graphite layer at high temperature and high pressure. The first set pressure is preferably 7000N, the first set temperature is preferably 900 ℃, and the first set duration is preferably 2h.
The organic glue layer is carbonized into a graphite phase at high temperature to form an adhesive graphite layer, the cured adhesive graphite layer can be tightly combined with the diamond film layer, the adhesive strength between the silicon carbide seed crystal and the graphite cover is improved, and the seed crystal and the graphite cover are prevented from falling off when the silicon carbide single crystal grows at the subsequent high temperature. The diamond film layer and the back (Si surface) of the seed crystal form SP3 bond tightly through C-Si or C-C chemical bond, the diamond film layer is more compact, the bonding is firmer, and the atomic structure is also more stable, so that under the protection of the diamond film layer, even if the organic adhesive layer generates bonding air holes in the carbonization process, hexagonal cavity defects generated by high-temperature sublimation can not occur on the back of the seed crystal in the subsequent growth process.
Example 2
This example proposes a graphite cap for silicon carbide crystal growth, which is obtained by the fixing method of example 1, to which silicon carbide seed crystals are bonded.
In the graphite cover of this embodiment, bond through fine and close diamond rete and bonding graphite layer between the bonding face of carborundum seed crystal fixed surface and graphite cover for combine closely between carborundum seed crystal and the graphite cover, bonding strength and stability are all higher, and, because the bonding face of carborundum seed crystal is covered by fine and close diamond rete, can effectively avoid the problem that leads to at the back sublimation of seed crystal material in the growth process owing to bonding gas pocket.
Example 3
The embodiment provides a process method for growing silicon carbide crystals, wherein the process method adopts the graphite cover adhered with the silicon carbide seed crystal in the embodiment 2;
and setting the process temperature of the growth of the silicon carbide crystal to be a third set temperature, wherein the third set temperature is higher than the first set temperature, so that the diamond film layer is solidified into a graphite filling layer.
Wherein the third set temperature is equal to or higher than 1900 ℃.
In a specific application scenario, the graphite cap with silicon carbide seed crystal bonded thereto of example 2 is assembled with a crucible filled with silicon carbide raw material and placed into a PVT growth furnace for a growth process, and when the diamond protection layer temperature approaches 1950 ℃, it will be slowly converted into a dense filled graphite layer.
The diamond film layer is automatically converted from SP3 phase to SP2 phase of graphite under the high temperature condition of silicon carbide single crystal growth, and the diamond film layer is very compact in combination with the silicon carbide seed crystal fixing surface, so that the diamond film layer can be very compact in combination with the silicon carbide seed crystal fixing surface (Si surface) after being converted into the graphite phase, and the silicon carbide seed crystal (Si surface) can be better protected from sublimating in the growth process. Compared with the prior art, the diamond film layer is converted from SP3 bond to graphite phase SP2 bond, and the graphite phase is formed by carbonizing the bonding agent directly to form the SP2 bond more compactly and firmly, and the atomic structure is also more stable.
In an experimental example, after the silicon carbide seed crystal was treated by the method of example 1, no bubbles were generated on the seed crystal fixing surface in the silicon carbide single crystal obtained by the growth process method of example 3, whereas the number of bubbles generated on the seed crystal fixing surface was usually 5 per cm in the prior art, which uses an organic gel to directly adhere to the graphite paper 2 About 15 pieces/cm 2 Between, bubble diameter<1mm。
In conclusion, the diamond film layer is extended on the seed crystal fixing surface, and the diamond film layer can be automatically converted from the SP3 phase to the graphite SP2 phase under the high-temperature condition of silicon carbide growth. The close combination of the diamond and the silicon carbide seed crystal fixing surface can fundamentally avoid the sublimation of the fixing surface caused by the gap introduced by the organic bonding layer, and the diamond is made of pure carbon material and does not pollute the growth of silicon carbide crystal, so that the gas phase substances generated by the sublimation of the fixing surface are reduced from continuously escaping from the holes of the seed crystal support, and the defect of hexagonal cavity formed by the seed crystal or the crystal is further caused.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (10)
1. A method for fixing a silicon carbide seed crystal and a graphite cover, comprising the steps of:
forming a diamond film layer on a fixed surface of a silicon carbide seed crystal;
forming an organic adhesive layer on the bonding surface of the graphite cover;
the fixing surface of the silicon carbide seed crystal is opposite to the bonding surface of the graphite cover, so that the diamond film layer and the organic adhesive layer are bonded together;
and applying a first set pressure to the graphite cover adhered with the silicon carbide seed crystal and heating to a first set temperature to enable the organic adhesive layer to be solidified into an adhered graphite layer, wherein the first set temperature is lower than the graphite phase transition temperature of diamond.
2. The method of fixing a silicon carbide seed crystal to a graphite cap according to claim 1, wherein forming a diamond film on the fixing surface of the silicon carbide seed crystal comprises:
placing the silicon carbide seed crystal in an epitaxial process chamber;
and heating the silicon carbide seed crystal to a second set temperature, and introducing hydrogen with a first set flow rate and methane with a second set flow rate into the epitaxial process chamber to form the diamond film layer on the fixing surface of the silicon carbide seed crystal.
3. The method of securing a silicon carbide seed crystal to a graphite cap according to claim 1, wherein the applying a first set pressure to the graphite cap to which the silicon carbide seed crystal is bonded and heating to a first set temperature comprises:
placing the graphite cover bonded with the silicon carbide seed crystal into a vacuum hot-pressing furnace;
the pressure applied to the graphite cover by the pressure applying mechanism of the vacuum hot pressing furnace is the first set pressure, the graphite cover is heated to the first set temperature, and the hot pressing time of the graphite cover is the first set duration.
4. The method for fixing a silicon carbide seed crystal and a graphite cover according to claim 1 or 3, wherein the first set pressure is 3000N to 10000N, and the first set temperature is 700 ℃ to 1000 ℃.
5. The method for fixing a silicon carbide seed crystal and a graphite cover according to claim 2, wherein the second set temperature is 900 ℃ to 1000 ℃, the first set flow rate is 100sccm to 500sccm, and the second set flow rate is 1sccm to 10sccm; the purities of the hydrogen and the methane are 5N-9N.
6. The method of fixing a silicon carbide seed crystal to a graphite cap according to claim 3, wherein the first set period of time is 1h to 10h.
7. The method of securing a silicon carbide seed crystal to a graphite cap according to claim 1 or 2, wherein the diamond film has a thickness of less than 100um.
8. A graphite cap for use in the growth of silicon carbide crystals, characterized in that said graphite cap to which said silicon carbide seed crystal is bonded is obtained by the fixing method as claimed in any one of claims 1 to 7.
9. A process for the growth of silicon carbide crystals, characterized in that it uses the graphite cap of claim 8 bonded with the silicon carbide seed crystal;
and setting the process temperature of the silicon carbide crystal growth to be a third set temperature, wherein the third set temperature is higher than the first set temperature, so that the diamond film layer is solidified into a graphite filling layer.
10. The process for producing a silicon carbide crystal according to claim 9, wherein the third set temperature is 1900 ℃ or higher.
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| CN101580964B (en) * | 2008-05-12 | 2012-02-01 | 中国科学院物理研究所 | Seed crystal support for growing silicon carbide crystal with high quality |
| CN101985773B (en) * | 2009-11-05 | 2013-12-18 | 新疆天科合达蓝光半导体有限公司 | Seed crystal treatment method and silicon carbide mono-crystal growing method |
| JP2012250865A (en) * | 2011-06-01 | 2012-12-20 | Sumitomo Electric Ind Ltd | Method for manufacturing single crystal, and seed crystal fixing agent |
| CN105463575B (en) * | 2016-01-15 | 2019-02-19 | 北京天科合达半导体股份有限公司 | A kind of seed crystal processing method for growing silicon carbide crystal with high quality |
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