CN104445202A - High-purity aluminum-doped silicon carbide powder and synthetic method thereof - Google Patents

High-purity aluminum-doped silicon carbide powder and synthetic method thereof Download PDF

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CN104445202A
CN104445202A CN201410688166.7A CN201410688166A CN104445202A CN 104445202 A CN104445202 A CN 104445202A CN 201410688166 A CN201410688166 A CN 201410688166A CN 104445202 A CN104445202 A CN 104445202A
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silicon carbide
induction heating
heating furnace
frequency induction
medium frequency
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CN104445202B (en
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陈启生
高升吉
朱钢
李汉亮
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DEQING ZHOUJING NEW MATERIALS TECHNOLOGY Co Ltd
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Abstract

The invention discloses high-purity aluminum-doped silicon carbide powder and a synthetic method thereof, and relates to the field of silicon carbide semiconductor materials. The silicon carbide powder is high in purity which reaches 99.999%; the one-time synthetic method is adopted, few processes are required, production equipment is simple, the operation is easy and feasible, and the large-scale production is easy to realize; if the raw material silicon powder adopts aluminum-doped monocrystalline silicon or solar polycrystalline silicon in the method, the recycling of the waste monocrystalline silicon or solar polycrystalline silicon can be facilitated, the environmental pollution can be prevented, and the obtained silicon carbide powder is the aluminum-doped silicon carbide powder and can serve as a raw material for producing colorless transparent silicon carbide crystals or p-type doped silicon carbide crystals.

Description

A kind of high-purity, aluminium doped silicon carbide powder and synthetic method thereof
Technical field
The present invention relates to manufacturing silicon carbide semiconductor Material Field, particularly relate to a kind of high-purity, aluminium doped silicon carbide powder and synthetic method thereof.
Background technology
Carborundum crystals has broad application prospects in field at the opto-electronic devices such as display, storage, detection and high temperature, high frequency, high-power electronic device.Carborundum powder is as the growth raw material of crystal, and its purity has important effect when growing semiconductor carborundum crystals, directly can affect crystalline quality and the electrical properties of grow silicon carbide crystals.
At present, preparation method's mainly Acheson method of carborundum powder, the method is that E.G.Acheson proposed (U.S.Patent 492 in 1893,767), by electrically heated carbonaceous material and silicon-dioxide (Silica) (or pure aluminium silicate, Aluminum Silicate) mixture, obtained silicon carbide artificial lens.In process of production, salt is added as solvent.When electric current is by graphite core, salt thawing makes carbon and silicon-dioxide (or pure aluminium silicate) close contact, thus produces chemosynthesis Sum decomposition, and produces a large amount of gas and volatile matter.
Wherein, the coke (Coke) that carbonaceous material can be made for bituminous coal, or gas coke (Gas CokeCarbon).If employing silicon-dioxide, the molar ratio of carbon and silicon-dioxide is up to 10:1, and in the silicon carbide product obtained, aluminum oxide, ferric oxide, calcium oxide and content of magnesia are 0.63%; As adopted pure aluminium silicate, carbon and pure aluminium silicate molar ratio are up to 27:1, and in product, aluminum oxide, ferric oxide, calcium oxide and content of magnesia are 5.13%.
Visible, utilize Acheson method to prepare carborundum powder, the carbon raw material not only needed is many, and the carborundum powder purity obtained is lower, can only be widely used in abrasive material, and can not be used for the production of manufacturing silicon carbide semiconductor material.
A kind of method (Chinese patent ZL200810016665.6) of synthesizing high-pure SiC power that the people such as Hu little Bo propose is secondary synthesis method.Namely first at 1500 DEG C of synthesizing silicon carbide powder, then single sintering powder is mixed, at 1600 DEG C to 2000 DEG C secondary synthesis silicon carbide powders.Although this secondary synthesis method improves the purity of carborundum powder, carborundum powder is made to can be used in the production of semiconductor material, but owing to adopting secondary synthesis, so complex process, production efficiency is lower, expend the energy more, and purity can't meet the requirement of semiconductor material production well.
Summary of the invention
The object of the present invention is to provide a kind of high-purity, aluminium doped silicon carbide powder and synthetic method thereof, thus solve the foregoing problems existed in prior art.
To achieve these goals, the technical solution used in the present invention is as follows:
Embodiments provide a kind of high-pure SiC power, the purity of described carborundum powder is 99.999%.
Embodiment of the present invention second aspect provides a kind of rafifinal doped silicon carbide powder, and the purity of described aluminium doped silicon carbide powder is 99.999%.
The embodiment of the present invention third aspect provides a kind of synthetic method of high-pure SiC power, comprises the steps:
S1, chooses that purity is 99.999%, granularity is all less than carbon dust and the silica flour of 50 μm, carbon dust and silica flour to be mixed and pours in crucible, with carbon lagging material parcel after sealed crucible, then will be placed in Medium Frequency Induction Heating Furnace according to the ratio of mol ratio 1:1;
S2, is down to below 0.1Pa by the air pressure in the growth room of described Medium Frequency Induction Heating Furnace;
S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1300-1350 DEG C and stop heating, when temperature reaches 1100-1200 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10kPa to 1 normal atmosphere;
S4, repeats S3, continues 1-3 hour;
S5, passes into argon gas and makes the air pressure in the growth room of described Medium Frequency Induction Heating Furnace reach 40kPa to 1 normal atmosphere;
S6, connects the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, heats graphite susceptor, makes the point for measuring temperature of graphite susceptor lower surface reach 2100-2300 DEG C, and keeps the temperature 5-10 hour of 2100-2300 DEG C;
S7, closes intermediate frequency power supply and stops heating, be cooled to after below 1000 DEG C and close argon gas, be cooled to room temperature, obtain the carborundum powder that purity is 99.999%.
Preferably, in S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1300 DEG C and stop heating, when temperature reaches 1200 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10kPa to 1 normal atmosphere; In S4, repeat S3, continue 2 hours.
Preferably, in S6, keep the temperature 5 hours of 2100-2300 DEG C.
Embodiment of the present invention fourth aspect provides a kind of synthetic method of rafifinal doped silicon carbide powder, adopts the synthetic method of above-mentioned high-pure SiC power, and described silica flour adopts silicon single crystal or the solar energy polycrystalline silicon of adulterated al.
The invention has the beneficial effects as follows: the one that the embodiment of the present invention provides is high-purity, aluminium doped silicon carbide powder and synthetic method thereof, and carborundum powder purity is high, reaches 99.999%; In building-up process, raw materials cost is low, and production unit is simple, and technical process is few, operates easy, easily accomplishes scale production; If the method raw material silica flour adopts silicon single crystal or the solar energy polycrystalline silicon of adulterated al, be not only conducive to the recycling to the silicon single crystal discarded or solar energy polycrystalline silicon, prevent environment; And the carborundum powder obtained is aluminium doped silicon carbide powder, can as the raw material producing water white transparency carborundum crystals or p-type doped silicon carbide crystal.
Accompanying drawing explanation
Fig. 1 is the Diffraction fringe distribution figure of 6H many types of aluminium doped silicon carbide powder.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with accompanying drawing, the present invention is further elaborated.Should be appreciated that embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide a kind of high-pure SiC power, its purity is 99.999%.Can be used for the production of semiconductor material.
As will be understood by the skilled person in the art, in the embodiment of the present invention, high-pure SiC power purity can adopt ordinary skill in the art means to detect and analyze.
The embodiment of the present invention additionally provides a kind of aluminium doped silicon carbide powder, and its purity is 99.999%.Aluminium doped silicon carbide powder is used in the process of crystal growth, and high-purity argon gas easily introduces N doping in carborundum crystals, and N doped crystal presents light green; The aluminium doped silicon carbide powder that the present invention obtains can in and the growing silicon carbice crystals process N impact of adulterating, thus prepare water white carborundum crystals; Meanwhile, the carborundum crystals of preparation p-type doping, needs the aluminium of doping greater concn, so the aluminium doped silicon carbide powder that the present invention obtains is useful for preparation p-type doped silicon carbide crystal; Therefore, the aluminium doped silicon carbide powder that the present invention obtains can as the raw material producing water white transparency carborundum crystals or p-type doped silicon carbide crystal.
The embodiment of the present invention additionally provides a kind of synthetic method of high-pure SiC power, comprises the steps:
S1, chooses that purity is 99.999%, granularity is all less than carbon dust and the silica flour of 50 μm, carbon dust and silica flour to be mixed and pours in crucible, with carbon lagging material parcel after sealed crucible, then will be placed in Medium Frequency Induction Heating Furnace according to the ratio of mol ratio 1:1;
S2, is down to below 0.1Pa by the air pressure in the growth room of described Medium Frequency Induction Heating Furnace;
S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1300-1350 DEG C and stop heating, when temperature reaches 1100-1200 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10kPa to 1 normal atmosphere;
S4, repeats S3, continues 1-3 hour;
S5, passes into argon gas and makes the air pressure in the growth room of described Medium Frequency Induction Heating Furnace reach 40kPa to 1 normal atmosphere;
S6, connects the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, heats graphite susceptor, makes the point for measuring temperature of graphite susceptor lower surface reach 2100-2300 DEG C, and keeps the temperature 5-10 hour of 2100-2300 DEG C;
S7, closes intermediate frequency power supply and stops heating, be cooled to after below 1000 DEG C and close argon gas, be cooled to room temperature, obtain the carborundum powder that purity is 99.999%.
The present invention adopts single sintering method, at 2100-2300 DEG C, maintain synthesizing silicon carbide powder under the environment of 5-10 hour, because β-SiC (3C polytype of silicon carbide) substantially changes α-SiC (6H polytype of silicon carbide) into more than 2100 DEG C, and most of impurity wherein all can volatilize.Therefore, the purity of the carborundum powder obtained is high, can reach 99.999%, makes carborundum powder be well positioned to meet the requirement of semiconductor material production.
In the embodiment of the present invention, after carbon dust and silica flour being mixed, put into crucible, and by after sealed crucible, with carbon lagging material, crucible is wrapped up, enable the synthesis temperature of carbon dust and silica flour reach more than 2100 DEG C.Make β-SiC (3C type) crystal substantially be converted into α-SiC (6H type), thus obtain highly purified silicon carbide.Compared with secondary synthesis method of the prior art, simplify carborundum craft flow process, improve production efficiency, save the energy.
The embodiment of the present invention additionally provides a kind of synthetic method of aluminium doped silicon carbide powder, identical with the synthetic method of above-mentioned carborundum powder, difference is, raw material silica flour can adopt silicon single crystal or the solar energy polycrystalline silicon of adulterated al, obtain aluminium doped silicon carbide powder, and the purity of this aluminium doped silicon carbide powder can reach 99.999%.This method, can realize the recycling of silicon single crystal to adulterated al or solar energy polycrystalline silicon, prevents the silicon single crystal discarded or solar energy polycrystalline silicon to environment.
Embodiment 1
Embodiments provide a kind of synthetic method of high-pure SiC power, comprise the steps:
S1, chooses that purity is 99.999%, granularity is all less than carbon dust and the silica flour of 50 μm, carbon dust and silica flour to be mixed and pours in crucible, with carbon lagging material parcel after sealed crucible, then will be placed in Medium Frequency Induction Heating Furnace according to the ratio of mol ratio 1:1;
S2, is down to below 0.1Pa by the air pressure in the growth room of described Medium Frequency Induction Heating Furnace;
S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1300 DEG C and stop heating, when temperature reaches 1200 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10kPa to 1 normal atmosphere;
S4, repeats S3, continues 2 hours;
S5, passes into argon gas and makes the air pressure in the growth room of described Medium Frequency Induction Heating Furnace reach 40kPa to 1 normal atmosphere;
S6, connects the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, heats graphite susceptor, makes the point for measuring temperature of graphite susceptor lower surface reach 2100 DEG C, and keeps the temperature 5 hours of 2100 DEG C;
S7, closes intermediate frequency power supply and stops heating, be cooled to after below 1000 DEG C and close argon gas, be cooled to room temperature, obtain the carborundum powder that purity is 99.999%.
Embodiment 2
Embodiments provide a kind of synthetic method of high-pure SiC power, comprise the steps:
S1, chooses that purity is 99.999%, granularity is 300 object carbon dust and silica flours, carbon dust and silica flour to be mixed and pours in crucible, with carbon lagging material parcel after sealed crucible, then will be placed in Medium Frequency Induction Heating Furnace according to the ratio of mol ratio 1:1;
S2, is down to 0.1Pa by the air pressure in the growth room of described Medium Frequency Induction Heating Furnace;
S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1321 DEG C and stop heating, when temperature reaches 1114 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 1 normal atmosphere;
S4, repeats S3, continues 1 hour;
S5, passes into argon gas and makes the air pressure in the growth room of described Medium Frequency Induction Heating Furnace reach 45kPa;
S6, connects the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, heats graphite susceptor, makes the point for measuring temperature of graphite susceptor lower surface reach 2300 DEG C, and is incubated 8 hours;
S7, closes intermediate frequency power supply and stops heating, closes argon gas, be cooled to room temperature, obtain the carborundum powder that purity is 99.999% when being cooled to 787 DEG C.
Embodiment 3
Embodiments provide a kind of synthetic method of high-pure SiC power, comprise the steps:
S1, chooses that purity is 99.999%, granularity is 300 object carbon dust and silica flours, carbon dust and silica flour to be mixed pour in crucible according to the ratio of mol ratio 1:1, just after sealed crucible with carbon lagging material parcel, then be placed in Medium Frequency Induction Heating Furnace;
S2, is down to 0.01Pa by the air pressure in the growth room of described Medium Frequency Induction Heating Furnace;
S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1338 DEG C and stop heating, when temperature reaches 1195 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10.3kPa;
S4, repeats S3, continues 3 hours;
S5, passes into argon gas and makes the air pressure in the growth room of described Medium Frequency Induction Heating Furnace reach 1 normal atmosphere;
S6, connects the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, heats graphite susceptor, makes the point for measuring temperature of graphite susceptor lower surface reach 2300 DEG C, and is incubated 8 hours;
S7, closes intermediate frequency power supply and stops heating, closes argon gas, be cooled to room temperature, obtain the carborundum powder that purity is 99.999% when being cooled to 500 DEG C.
Embodiment 4
Embodiments provide a kind of synthetic method of high-pure SiC power, step is with any one of embodiment 1-3, and difference is, silica flour is the monocrystalline silica flour mixing aluminium.
Embodiment 5
Embodiments provide a kind of synthetic method of high-pure SiC power, step is with any one of embodiment 1-3, and difference is, silica flour is the polysilicon mixing aluminium.
In the carborundum powder adopting glow discharge mass spectroscopy GDMS to synthesize above-described embodiment 5, the content of impurity measures, and result is as shown in table 1.As can be seen from Table 1, adopt the synthetic method that the embodiment of the present invention provides, in the carborundum powder obtained, the content of iron, calcium and magnesium all reduces compared with the content of respective element in raw silicon.Wherein, in the carborundum powder of synthesis, the total content of iron, calcium and magnesium is 0.64ppm, and aluminium content is 130ppm.
Table 1 foreign matter content analysis (quality/ppm).
Al Fe Ca Mg
Raw silicon - 3 1 1
Material carbon 0.9 0.2 0.7 0.1
Synthesizing silicon carbide 130 0.19 0.38 0.07
Adopt powder diffraction method (XRD), utilize the X-ray diffractometer D/Max-2400 of Rigaku company to synthesize to the embodiment of the present invention 1-5 carborundum powder obtained and carry out x-ray diffraction experiment, carry out material phase analysis to product, the Diffraction fringe distribution of carborundum powder as shown in Figure 1.In figure, X-coordinate: diffraction angle 2 θ, unit: °; Ordinate zou: intensity (integrated intensity) unit cps (numeration/second).
Wherein, in the embodiment of the present invention, XRD diffraction have employed CuK α 1 target, and radiation source wavelength λ is 1.54056nm, and walking wide is 0.02 °, and diffraction angle 2 θ is 20 ° ~ 90 °.
As can be seen from Figure 1, the embodiment of the present invention synthesizes the aluminium doped silicon carbide powder obtained is that 6H is many types of.
For hexagonal system, adjacent two interplanar distance d in following formula determination crystal face (hkl) can be utilized, in formula, h, k, l are crystal face coordinate, and a, c are the lattice parameter of 6H polytype of silicon carbide crystal, wherein, the calculation result of d is as shown in table 2.
In the embodiment of the present invention, incidence angle θ can utilize Bragg equation to determine, 2ds in θ=n λ, n=1,2 ..., wherein, d is adjacent two interplanar distances in crystal face (hkl), and its numerical value is as shown in table 2, θ is input angle, and n is diffraction progression, and λ is radiation source wavelength.
Because in the embodiment of the present invention, synthesize the aluminium doped silicon carbide purity obtained high, the secondary diffracted intensity of its powder is less, so in above-mentioned Bragg equation, n can get 1, then above-mentioned Bragg equation is: 2dsin θ=λ, utilize the numerical value of adjacent two interplanar distance d in crystal face (hkl) in this formula and table 2, the value of the incidence angle θ calculated, the θ value measured with XRD in Fig. 1 is coincide better.
The XRD data of table 2 α-SiC (6H polytype of silicon carbide)
By adopting technique scheme disclosed by the invention, obtain effect useful as follows:
1), the present invention's synthesizing silicon carbide under 2100-2300 DEG C of environment, compared with prior art, in synthesizing silicon carbide powder, the foreign matter content such as iron, calcium and magnesium is lower;
2), present invention process is single sintering method, and technical process simplifies compared with columbite process, and production efficiency obtains larger raising;
3), the present invention's silicon single crystal of directly adopting aluminium to adulterate or solar energy polycrystalline silicon as the silicon raw material producing carborundum powder, and do not need the aluminium to adulterating in silicon raw material to purify, and therefore, greatly reduces the cost producing carborundum powder;
4), the present invention's silicon single crystal of adopting aluminium to adulterate or solar energy polycrystalline silicon are as the silicon raw material producing carborundum powder, so, The inventive method achieves the recycling of silicon single crystal to adulterated al or solar energy polycrystalline silicon, prevent the silicon single crystal discarded or solar energy polycrystalline silicon to environment;
5), equipment required for the present invention is simple, operates easy, easily realizes scale production synthesis;
6), in growing silicon carbice crystals process, high-purity argon gas easily introduces N doping in carborundum crystals, and N doped crystal presents light green; The aluminium doped silicon carbide powder that the present invention obtains can in and the growing silicon carbice crystals process N impact of adulterating, thus prepare water white carborundum crystals; In addition, the carborundum crystals of preparation p-type doping, needs the aluminium of doping greater concn, so the aluminium doped silicon carbide powder that the present invention obtains is useful for preparation p-type doped silicon carbide crystal; Therefore, the aluminium doped silicon carbide powder that the present invention obtains can as the raw material producing water white transparency carborundum crystals or p-type doped silicon carbide crystal.
Each embodiment in this specification sheets all adopts the mode of going forward one by one to describe, and what each embodiment stressed is the difference with other embodiments, between each embodiment identical similar part mutually see.
Those skilled in the art it should be understood that the sequential of the method steps that above-described embodiment provides can carry out accommodation according to practical situation, also can carry out according to practical situation are concurrent.
The hardware that all or part of step in the method that above-described embodiment relates to can carry out instruction relevant by program has come, described program can be stored in the storage media that computer equipment can read, for performing all or part of step described in the various embodiments described above method.Described computer equipment, such as: Personal Computer, server, the network equipment, intelligent mobile terminal, intelligent home device, wearable intelligent equipment, vehicle intelligent equipment etc.; Described storage media, such as: the storage of RAM, ROM, magnetic disc, tape, CD, flash memory, USB flash disk, portable hard drive, storage card, memory stick, the webserver, network cloud storage etc.
Finally, also it should be noted that, in this article, the such as relational terms of first and second grades and so on is only used for an entity or operation to separate with another entity or operational zone, and not necessarily requires or imply the relation that there is any this reality between these entities or operation or sequentially.And, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, commodity or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, commodity or equipment.When not more restrictions, the key element limited by statement " comprising ... ", and be not precluded within process, method, commodity or the equipment comprising described key element and also there is other identical element.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should look protection scope of the present invention.

Claims (6)

1. a high-pure SiC power, is characterized in that, the purity of described carborundum powder is 99.999%.
2. a rafifinal doped silicon carbide powder, is characterized in that, the purity of described aluminium doped silicon carbide powder is 99.999%.
3. a synthetic method for high-pure SiC power, is characterized in that, comprises the steps:
S1, chooses that purity is 99.999%, granularity is all less than carbon dust and the silica flour of 50 μm, carbon dust and silica flour to be mixed and pours in crucible, with carbon lagging material parcel after sealed crucible, then will be placed in Medium Frequency Induction Heating Furnace according to the ratio of mol ratio 1:1;
S2, is down to below 0.1Pa by the air pressure in the growth room of described Medium Frequency Induction Heating Furnace;
S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1300-1350 DEG C and stop heating, when temperature reaches 1100-1200 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10kPa to 1 normal atmosphere;
S4, repeats S3, continues 1-3 hour;
S5, passes into argon gas and makes the air pressure in the growth room of described Medium Frequency Induction Heating Furnace reach 40kPa to 1 normal atmosphere;
S6, connects the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, heats graphite susceptor, makes the point for measuring temperature of graphite susceptor lower surface reach 2100-2300 DEG C, and keeps the temperature 5-10 hour of 2100-2300 DEG C;
S7, closes intermediate frequency power supply and stops heating, be cooled to after below 1000 DEG C and close argon gas, be cooled to room temperature, obtain the carborundum powder that purity is 99.999%.
4. the synthetic method of high-pure SiC power according to claim 3, it is characterized in that, in S3, connect the intermediate frequency power supply of described Medium Frequency Induction Heating Furnace, graphite susceptor is heated, close intermediate frequency power supply when the point for measuring temperature of graphite susceptor lower surface reaches 1300 DEG C and stop heating, when temperature reaches 1200 DEG C, pass into argon gas and make the air pressure in described Medium Frequency Induction Heating Furnace reach 10kPa to 1 normal atmosphere; In S4, repeat S3, continue 2 hours.
5. the synthetic method of high-pure SiC power according to claim 3, is characterized in that, in S6, keeps the temperature 5 hours of 2100-2300 DEG C.
6. a synthetic method for rafifinal doped silicon carbide powder, is characterized in that, adopts the synthetic method of the high-pure SiC power described in any one of claim 3-5, and described silica flour adopts silicon single crystal or the solar energy polycrystalline silicon of adulterated al.
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CN107974712A (en) * 2017-11-14 2018-05-01 山东天岳先进材料科技有限公司 A kind of preparation method of Semi-insulating silicon carbide mono-crystal
CN111591994A (en) * 2020-06-03 2020-08-28 璨隆科技发展有限公司 Preparation method of high-purity silicon carbide powder for silicon carbide single crystal growth
CN115976625A (en) * 2023-02-14 2023-04-18 中国科学院物理研究所 Method for producing 3C-SiC single crystal
CN115976625B (en) * 2023-02-14 2024-03-05 中国科学院物理研究所 Method for producing 3C-SiC single crystals

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