CN111235633A - Method for preparing self-supporting silicon carbide wafer on surface of silicon melt through CVD - Google Patents
Method for preparing self-supporting silicon carbide wafer on surface of silicon melt through CVD Download PDFInfo
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- CN111235633A CN111235633A CN202010050175.9A CN202010050175A CN111235633A CN 111235633 A CN111235633 A CN 111235633A CN 202010050175 A CN202010050175 A CN 202010050175A CN 111235633 A CN111235633 A CN 111235633A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02381—Silicon, silicon germanium, germanium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02529—Silicon carbide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
Abstract
A method for preparing a self-supporting silicon carbide wafer on the surface of a silicon melt by CVD, comprising preparing a silicon film on a patterned substrate; raising the temperature in a growth furnace to melt the silicon film to form a silicon melt; keeping the temperature unchanged, introducing hydrocarbon gas into the growth furnace, and forming a silicon carbide seed crystal layer suspended on the surface layer of the silicon melt after a period of time; introducing hydrocarbon gas and hydrosulfide gas into the growth furnace, and performing homoepitaxial growth on the silicon carbide seed crystal layer to form a silicon carbide self-supporting layer; and cooling the pattern substrate containing the silicon carbide self-supporting layer, removing the silicon film to obtain a stripped silicon carbide self-supporting layer, and grinding, polishing and shaping the stripped silicon carbide self-supporting layer to obtain the silicon carbide wafer. The method avoids the disadvantages of the traditional method, and has the advantages of simplicity, convenience, easy implementation, easy popularization and the like; the invention can use the sapphire substrate with low price, and the substrate can be reused, thereby further reducing the cost.
Description
Technical Field
The invention belongs to the field of silicon carbide semiconductor materials, and particularly relates to a method for preparing a self-supporting silicon carbide wafer on the surface of silicon melt through CVD.
Background
The silicon carbide semiconductor material (4H-SiC) is a novel third-generation semiconductor material and has very important application in the field of high-power electronics. The method comprises the following steps of carrying out homogeneous epitaxial growth on a silicon carbide substrate to obtain a silicon carbide thick film, wherein the key step of realizing the silicon carbide power device is to carry out the homogeneous epitaxial growth on the silicon carbide substrate to obtain the silicon carbide thick film. The currently used preparation scheme has two disadvantages: firstly, a silicon carbide substrate is needed, and the difficulty of manufacturing a silicon carbide power device is increased because the substrate is extremely difficult to prepare; secondly, the substrate needs to be thinned to greatly reduce the resistance of the device. The defects not only increase the preparation cost of the device, but also cause the waste of raw materials.
Disclosure of Invention
In view of the above, it is a primary object of the present invention to provide a method for preparing a self-supporting sic wafer by CVD on a surface of a silicon melt, which is intended to at least partially solve at least one of the above technical problems.
In order to achieve the above object, as one aspect of the present invention, there is provided a method for producing a self-supporting silicon carbide wafer by CVD on a surface of a silicon melt, comprising:
(1) preparing a silicon film on a pattern substrate;
(2) raising the temperature in a growth furnace to melt the silicon film to form a silicon melt;
(3) keeping the temperature unchanged, introducing hydrocarbon gas into the growth furnace, and forming a silicon carbide seed crystal layer suspended on the surface layer of the silicon melt after a period of time;
(4) introducing hydrocarbon gas and hydrosulfide gas into the growth furnace, and performing homoepitaxial growth on the silicon carbide seed crystal layer formed in the step (3) to form a silicon carbide self-supporting layer;
(5) and (4) cooling the patterned substrate containing the silicon carbide self-supporting layer obtained in the step (4), removing the silicon film to obtain a stripped silicon carbide self-supporting layer, and grinding, polishing and shaping the stripped silicon carbide self-supporting layer to obtain the silicon carbide wafer.
Based on the above technical solutions, the method for preparing a self-supporting sic wafer by CVD on the surface of a silicon melt according to the present invention has at least one of the following advantages over the prior art:
1. the method avoids the disadvantages of the traditional method, and has the advantages of simplicity, convenience, easy implementation, easy popularization and the like;
2. the invention does not need to use expensive and rare silicon carbide substrate, but can use cheap sapphire substrate to only play the role of supporting, silicon melt is used as a conversion bed, growth gas of silicon and carbon is introduced into the conversion bed, a silicon carbide crystal layer is generated on the conversion bed through chemical combination reaction, a self-supporting silicon carbide thick film material with certain thickness can be grown after a certain time, and then the thick film silicon carbide layer can be stripped by a method of corroding a residual silicon layer by a wet method to form a starting material for manufacturing the silicon carbide power device. In addition, the substrate can be reused, and the cost is further reduced.
Drawings
FIG. 1 is a schematic view of a step surface and a cross-sectional shape of a patterned substrate according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the corrugated shape and distribution of the patterned substrate surface in an embodiment of the present invention;
FIG. 3 is a schematic view of the whole process for preparing a silicon carbide epitaxial thick film in the embodiment of the present invention;
fig. 4 is a schematic view of a silicon film melting and silicon carbide growth process in an embodiment of the present invention.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention discloses a method for preparing a self-supporting silicon carbide wafer on the surface of a silicon melt by CVD, which comprises the following steps:
(1) preparing a silicon film on a pattern substrate;
(2) raising the temperature in a growth furnace to melt the silicon film to form a silicon melt;
(3) keeping the temperature unchanged, introducing hydrocarbon gas into the growth furnace, and forming a silicon carbide seed crystal layer suspended on the surface layer of the silicon melt after a period of time;
(4) introducing hydrocarbon gas and hydrosulfide gas into the growth furnace, and performing homoepitaxial growth on the silicon carbide seed crystal layer formed in the step (3) to form a silicon carbide self-supporting layer;
(5) and (4) cooling the patterned substrate containing the silicon carbide self-supporting layer obtained in the step (4), removing the silicon film to obtain a stripped silicon carbide self-supporting layer, and grinding, polishing and shaping the stripped silicon carbide self-supporting layer to obtain the silicon carbide wafer.
In some embodiments of the invention, the temperature is increased to 1500 to 1800 degrees celsius in the increasing temperature step in step (2).
In some embodiments of the present invention, the silicon melt in step (2) is a silicon melt having a surface with steps or ripples.
In some embodiments of the present invention, the silicon carbide seed layer in step (3) is grown for a period of time ranging from 1 to 2 hours.
In some embodiments of the invention, the pressure in the growth furnace in step (3) is 600 to 760 torr.
In some embodiments of the invention, the molar mass ratio of the silicon element to the carbon element in the hydrocarbon gas and the silicon hydride gas in the step (4) is 1: (0.8 to 1.5);
in some embodiments of the invention, the silicon carbide layer is grown in step (4) for a period of 3 to 8 hours.
In some embodiments of the invention, the hydrocarbon gas in step (4) comprises propane and the hydrosilane gas comprises silane.
In some embodiments of the present invention, the pattern on the patterned substrate described in step (1) comprises a step;
in some embodiments of the invention, the shape of the step comprises a micro-nano step, a continuous corrugated step or an intermittent corrugated step;
in some embodiments of the invention, the step is formed due to a substrate tilt angle or by pattern etching.
In some embodiments of the invention, the silicon film in step (1) has a thickness of 200 to 1000 nm.
In some embodiments of the present invention, the method of removing the silicon film in step (5) comprises wet etching;
in some embodiments of the present invention, the wet etching specifically includes:
placing the prepared pattern substrate of the silicon carbide film into an alkaline solution, keeping the temperature at 80-100 ℃, and removing the silicon film after 2-4 hours;
in some embodiments of the invention, the alkali solution comprises an aqueous KOH solution having a concentration of 40 wt% to 60 wt%.
In one exemplary embodiment, the method of making a self-supporting silicon carbide wafer of the present invention comprises the steps of:
taking a pattern substrate as a supporting base plate;
step two, preparing a silicon film on the pattern substrate by adopting a sputtering or electron beam evaporation method, wherein the thickness of the silicon film is 200 nanometers to 1 micron, then raising the temperature in a growth furnace to 1500-1800 ℃ to melt the silicon film to form a melt, and taking the liquid phase as a parent phase and a fluidized bed for the subsequent silicon carbide growth; under high temperature, the surface of the silicon melt is affected by the pattern substrate and has fine steps or forms fine ripples, silicon molecules at the steps of the pattern substrate move to the surface more easily, so that the corresponding positions of the surface of the melt form the fine steps or ripples, the surface area of the silicon melt is increased, and the tips of the steps or ripples and the adjacent facets are more easily contacted with a carbon source.
Introducing hydrocarbon gas containing carbon element into the growth furnace, dissolving the carbon element in the near-surface layer of the silicon melt at the high temperature of 1500-1800 ℃, combining the carbon element with the silicon element to form silicon carbide seed crystal particle suspension with certain density, growing the seed crystal particles and fusing the seed crystal particles after lasting for 1-2 hours to form a silicon carbide seed crystal layer with the thickness of 100-300 nanometers, suspending the seed crystal layer on the surface layer of the silicon melt and forming a sealing layer of the silicon melt; the vapor pressure of silicon and the pressure of the growing furnace are controlled and balanced, so that the seed crystal is controlled to suspend on the surface of the silicon melt and is not sunk and stirred and split by silicon molecules in the melt. After a certain time, the seed grains grow and fuse with the adjacent seed grains to form a silicon carbide seed crystal film on the silicon fusion surface.
Simultaneously introducing hydrocarbon gas containing carbon elements and simple silicon hydride gas containing silicon elements into the growth furnace, carrying out homoepitaxial growth by taking the silicon carbide seed crystal layer as the substrate at high temperature, and keeping the thickness of the homoepitaxial layer to be 50-200 microns after lasting for 3-8 hours to form the silicon carbide self-supporting thick film material; wherein the molar mass ratio of carbon element to silicon element in the hydrocarbon gas and the silicon hydride gas is 1: 0.8-1.5;
step five, taking out the pattern substrate with the silicon carbide self-supporting thick film material after the growth furnace is cooled to room temperature, and then removing the residual silicon film by wet etching to ensure that the self-supporting thick film material automatically falls off from the surface of the pattern substrate, namely the silicon carbide self-supporting material can be stripped;
and sixthly, carrying out double-side grinding and polishing and circumferential shaping treatment on the obtained silicon carbide self-supporting material to enable the double sides of the silicon carbide self-supporting material to be flat and bright, and thus obtaining the silicon carbide wafer.
The technical solution of the present invention is further illustrated by the following specific embodiments in conjunction with the accompanying drawings. It should be noted that the following specific examples are given by way of illustration only and the scope of the present invention is not limited thereto.
The chemicals and raw materials used in the following examples were either commercially available or self-prepared by a known preparation method.
In the preparation method of the silicon carbide epitaxial film of this embodiment, a nano-patterned substrate is adopted, the material is sapphire (sapphire) or 4H-SiC, the surface crystal orientation is (0001) or (000-1), and a certain included angle is formed between the nano-patterned substrate and the <11-20> or other directions, such as the <1100> direction, so as to form a substrate tilt angle, such as 0 degree, 4 degrees, 8 degrees, and the like, and form a micro-nano strip-shaped step, as shown in fig. 1, a specific included angle or an angle, such as 0 degree, 30 degrees, 45 degrees, 90 degrees, and the like, is formed between the nano-patterned substrate and the reference edge, and the angle is 0 degree in fig.. The surface steps may also be of other shapes, as shown in fig. 2, either continuous or discontinuous corrugations with specific angles or angles between the corrugations, as well as with reference edges, such as 0 degrees, 30 degrees, 45 degrees, 90 degrees, etc. The step height is 50 nm to 1 micron and the mesa width is 100 nm to 2 micron as shown in fig. 1. The surface micro-nano step can be formed by the inclination angle of the substrate or by pattern etching.
And preparing a thin silicon film on the surface of the patterned substrate by adopting an electron beam or magnetron sputtering method. The silicon film thickness is 200 nm to 1 μm. As shown in step 2 of fig. 3.
The silicon film is melted in a silicon carbide epitaxial growth furnace. As shown in step 1 of fig. 4. The furnace temperature is raised to about 1500-1800 ℃ to melt the silicon film and make it have a certain vapor pressure.
The silicon melt surface is influenced by the pattern substrate and has similarity, fine steps or fine ripples are formed, because silicon molecules at the step position of the substrate move towards the surface more easily at high temperature, the fine steps or the ripples are formed at the corresponding position of the melt surface, the silicon melt surface area is increased, the step or the ripple tip position and the adjacent facet position are easy to contact with a carbon source, the seed crystals are generated through chemical combination reaction, a high-density seed crystal area is formed and suspended on the silicon melt surface, the seed crystals grow up and are fused with each other under certain conditions to form a sealing layer, namely, the seed crystal film ultrathin layer also has fine surface steps, and the step flow growth mode is adopted for simultaneous epitaxial silicon carbide growth in subsequent chemical vapor deposition.
At this time, a carrier gas hydrogen atmosphere is introduced, the flow rate is 1slm to 30slm, and the pressure of the growth chamber is 600-760 Torr. At this time, a reaction source gas (namely hydrocarbon gas) of carbon is introduced into a carrier gas hydrogen atmosphere, such as propane, the pressure of a growth chamber is kept unchanged, the flow rate of the propane is 100sccm-500sccm and is different, a carbon source is dissolved on the surface of silicon melt to form high-density silicon carbide seed crystal grains which can be used as seed crystals for growing silicon carbide, and after 1-2 hours, the seed crystal grains grow and are fused with adjacent seed crystal grains, so that a silicon carbide seed crystal ultrathin film is formed on the surface of a molten silicon film. As shown in step 2 of fig. 4.
At this time, a silicon source (i.e. a silicon hydride gas) such as silane is introduced, the molar mass ratio of carbon to silicon is 1: 0.8-1.5, homoepitaxial growth is carried out, the reaction source gases of silicon and carbon can be closed when the silicon carbide film grows to 50-200 microns after 3-8 hours, and the temperature is reduced to room temperature in a hydrogen atmosphere, so that the growth is finished, as shown in step 3 of fig. 4.
The substrate with the grown silicon carbide film is removed and the remaining silicon layer is carefully removed by wet etching, as shown in step 5 of fig. 3. And (3) placing the substrate with the grown silicon carbide film in 40-60% of KOH aqueous solution by mass, keeping the temperature at about 80-100 ℃, and corroding and removing the residual silicon film between the silicon carbide film and the substrate after 2-4 hours, so that the grown silicon carbide film is stripped from the pattern substrate to form the self-supporting silicon carbide thick film material.
And (3) flattening the two sides of the self-supporting silicon carbide thick film material by adopting a grinding and polishing method, removing burrs on the surface of the silicon carbide material, reducing the surface roughness to be below 1 nanometer, and shaping the self-supporting silicon carbide thick film material to finish the preparation of the self-supporting silicon carbide wafer, as shown in the 6 th step in figure 3.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a self-supporting silicon carbide wafer by CVD on a surface of a silicon melt, comprising:
(1) preparing a silicon film on a pattern substrate;
(2) raising the temperature in a growth furnace to melt the silicon film to form a silicon melt;
(3) keeping the temperature unchanged, introducing hydrocarbon gas into the growth furnace, and forming a silicon carbide seed crystal layer suspended on the surface layer of the silicon melt after a period of time;
(4) introducing hydrocarbon gas and hydrosulfide gas into the growth furnace, and performing homoepitaxial growth on the silicon carbide seed crystal layer formed in the step (3) to form a silicon carbide self-supporting layer;
(5) and (4) cooling the patterned substrate containing the silicon carbide self-supporting layer obtained in the step (4), removing the silicon film to obtain a stripped silicon carbide self-supporting layer, and grinding, polishing and shaping the stripped silicon carbide self-supporting layer to obtain the silicon carbide wafer.
2. The method of claim 1,
and (3) in the temperature increasing step in the step (2), increasing the temperature to 1500-1800 ℃.
3. The method of claim 1,
the silicon melt in the step (2) is a silicon melt with steps or ripples on the surface.
4. The method of claim 1,
in the step (4), the hydrocarbon gas comprises propane, and the hydrosilane gas comprises silane.
5. The method of claim 1,
the pattern on the pattern substrate in the step (1) comprises a step;
the step shape comprises a micro-nano step, a continuous corrugated step or an intermittent corrugated step.
6. The method of claim 5,
the step is formed due to the substrate tilt angle or by pattern etching.
7. The method of claim 1,
the thickness of the silicon film in the step (1) is 200 to 1000 nm.
8. The method of claim 1,
the method for removing the silicon film in the step (5) includes wet etching.
9. The method of claim 8,
the wet etching specifically includes:
and (3) placing the patterned substrate with the prepared silicon carbide film into an alkaline solution, keeping the temperature at 80-100 ℃, and removing the silicon film after 2-4 hours.
10. The method of claim 9,
the alkali solution comprises a KOH aqueous solution, and the concentration of the KOH aqueous solution is 40 to 60 weight percent.
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Cited By (1)
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