CN113548666A - Iron removal process for submicron silicon carbide powder - Google Patents
Iron removal process for submicron silicon carbide powder Download PDFInfo
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- CN113548666A CN113548666A CN202110940019.4A CN202110940019A CN113548666A CN 113548666 A CN113548666 A CN 113548666A CN 202110940019 A CN202110940019 A CN 202110940019A CN 113548666 A CN113548666 A CN 113548666A
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Abstract
The invention discloses a process for removing iron from submicron silicon carbide powder, which belongs to the technical field of silicon carbide iron removal and comprises the following steps: pouring weighed SiC powder needing acid cleaning into an acid cleaning agent solution with the concentration of 0.05-0.2 mol/L, and carrying out ultrasonic-assisted stirring acid cleaning with the ultrasonic power of 180-270W to obtain acid cleaning slurry; repeatedly washing the acid-washed slurry with deionized water to obtain washed SiC powder; and (4) after washing, drying the SiC powder, and then detecting the content of Fe impurities. According to the invention, an ultrasonic-assisted stirring and pickling mode is utilized, and the introduction of ultrasonic waves can induce a large amount of air bubbles to generate, and the collapse of the air bubbles can generate local high-temperature and high-pressure air flow in acid liquor, so that the diffusivity and the dispersibility of the powder in the acid liquor are improved, the technical problems that the submicron SiC powder is easy to agglomerate and is difficult to disperse in water are solved, the chemical reaction rate is further improved, and the removal rate of iron in the powder is greatly improved.
Description
The technical field is as follows:
the invention belongs to the technical field of silicon carbide iron removal, and particularly relates to an iron removal process for submicron silicon carbide powder.
Background art:
SiC is known as a high temperature structural material, and has properties such as high strength, high elastic modulus, high thermal expansion coefficient, good thermal shock resistance, and acid and alkali corrosion resistance. Due to these excellent properties, SiC materials are often used in microelectronics, mechanical sealing, aerospace, and heat exchange industries. While the SiC fine powder, which is a raw material for preparing SiC ceramics, has a significant influence on various properties of the sintered SiC ceramics, manufacturers have made strict demands on the particle size, particle type, purity, fluidity, and the like of SiC powder in order to obtain SiC ceramics having excellent properties.
Currently, SiC is produced industrially in a relatively economic Acheson mode, and quartz sand, petroleum coke, coal, industrial salt and other raw materials used as base materials are inevitably brought into other impurities in the high-temperature smelting process, so that the purity of the SiC block after smelting is not high, and the SiC block comprises common Fe, free C, free Si and SiO2O and other common metal and metal oxide impurities. In addition, SiC smelting blocks can lead to different impurities to be introduced into the powder in the processes of gradual crushing and later storage. In contrast, the most common impurities with the highest occurrence content in the SiC powder are Fe impurities, and the presence of a large amount of Fe impurities seriously affects various properties and application ranges of SiC. Therefore, how to rapidly and effectively perform Fe removal treatment on the SiC fine powder is important.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provide the acid cleaning and purifying method of the submicron silicon carbide powder, which has the advantages of good impurity removal effect, controllable acid amount, simple process and short operation period, and particularly has good removal effect on iron impurities affecting the sintering quality in the silicon carbide micro powder, so that the silicon carbide powder which is suitable for the use requirement of pressureless sintering silicon carbide ceramics is obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for removing iron from submicron silicon carbide powder comprises the following steps:
step 1, acid washing and purification:
pouring weighed SiC powder needing acid washing into an acid washing agent solution, and carrying out ultrasonic-assisted stirring acid washing to obtain acid washing slurry; wherein the concentration of the pickling agent solution is 0.05-0.2 mol/L, and the ultrasonic power is 180-270W;
step 2, washing:
repeatedly washing the acid-washed slurry with deionized water to obtain washed SiC powder;
and (4) after washing, drying the SiC powder, and then detecting the content of Fe impurities.
In the step 1, the average particle size of the SiC powder is 0.5 μm, the pickling agent is one or more of hydrochloric acid (AR, 36-38%), sulfuric acid (AR, 95-98%), nitric acid (AR, 65-68%) or hydrofluoric acid (AR, not less than 40%) which does not react with SiC, and the pickling agent is prepared into a pickling agent solution with the concentration of 0.05-0.2 mol/L.
In the step 1, the SiC powder contains main impurities and mass contents of 0.98-1.85% of O, 0.52-1.68% of free-Si, 0.22-0.67% of free-C, 0.084-0.159% of Fe, 0.0185-0.051% of Ti, 0.0081-0.0174% of Al, 0.0085-0.0194% of Ni and 0.0025-0.0082% of V.
In the step 1, the conditions of ultrasonic-assisted stirring and pickling are as follows: pouring SiC powder to be pickled into a pickling agent solution according to the liquid-solid ratio of (4-6): 1, wherein the pickling temperature is 50-80 ℃, the ultrasonic frequency is 40-150 kHz, the stirring speed is 100-400 rpm, and the pickling time is 30-180 min.
In the step 1, the conditions of ultrasonic-assisted stirring and pickling are preferably as follows: pouring SiC powder to be pickled into a beaker filled with a pickling agent solution according to the liquid-solid ratio of 5:1, wherein the acid concentration is 0.15mol/L, the pickling temperature is 80 ℃, the ultrasonic frequency is 45kHz, the stirring speed is 400rpm, the ultrasonic power is 270W, and the pickling time is 180 min.
In the step 2, the water washing process comprises the following specific steps: injecting the acid-washing slurry into a clean beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
In the step 2, 50ml of the acid-washed slurry was taken out by a syringe every 30min and poured into a clean beaker, and washed with water by a sedimentation method, and the pH value was measured at any time using pH paper.
In the step 3, the drying detection specifically comprises the following steps:
and after washing, transferring the SiC powder into a culture dish cleaned by deionized water, putting the culture dish into an oven for drying, and collecting part of dried powder for Fe impurity content detection.
In the step 3, the powder is dried in an oven at 110 ℃ for 6h and then sealed for later use.
And in the step 3, taking out 2g of acid-washed and dried SiC powder, and analyzing the content of the Fe element by utilizing ICP-OES.
In the step 3, the removal rate of iron impurities is 92.6-96.1%, the impurity content is respectively reduced to less than 1.10% of O, less than 0.72% of free-Si, less than 0.20% of free-C, less than 0.004% of Fe, less than 0.015% of Ti, less than 0.0067% of Al, less than 0.0003% of Ni and less than 0.0014% of V.
The invention has the beneficial effects that:
the invention utilizes an ultrasonic-assisted stirring and pickling mode, and because the introduction of ultrasonic waves can induce a large amount of air bubbles to generate, and the collapse of the air bubbles can generate local high-temperature and high-pressure air flow in acid liquor, the diffusivity and the dispersibility of powder in the acid liquor are improved, so that the technical problems that submicron SiC powder is easy to agglomerate and is not easy to disperse in water are solved, and further the chemical reaction rate is improved. After acid washing and water washing, the Fe removing rate of the SiC powder can reach more than 96 percent, and the impurity content in the powder can be respectively reduced to less than 1.10 percent of O, less than 0.72 percent of free-Si, less than 0.20 percent of free-C, less than 0.004 percent of Fe, less than 0.015 percent of Ti, less than 0.0067 percent of Al, less than 0.0003 percent of Ni and less than 0.0014 percent of V; controllable acid amount and environmental protection: aiming at the different occurrence contents of Fe impurities required by SiC powder, the acid consumption is reduced and unnecessary production waste and environmental pollution are avoided on the premise of ensuring the high-efficiency Fe impurity removal rate by adjusting other pickling process parameters.
Description of the drawings:
FIG. 1 is a graph showing the influence of acid species on the Fe removal rate in example 1 of the present invention.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The weight purity of the SiC powder adopted in the embodiment of the invention is more than 96%, and the particle size range is 0.3-1.5 μm.
The BS224S model electronic balance used in the examples of the present invention was weighed.
The equipment used in the ultrasonic-assisted stirring and pickling process in the embodiment of the invention is a KQ-300VDE type three-frequency numerical control ultrasonic cleaner and a JB300-SH type digital display constant-speed powerful stirrer.
In the embodiment of the invention, the content of the Fe element in the SiC powder is detected by adopting an Optima 8300DV type inductive plasma generation spectrum.
The SiC powder treated in the examples of the present invention contains main impurities and mass contents of 1.34% O, 1.04% free-Si, 0.34% free-C, 0.102% Fe, 0.0221% Ti, 0.0128% Al, 0.0112% Ni, and 0.0054% V.
Example 1
The iron removal process based on the submicron silicon carbide powder comprises the following steps:
step 1, preparing: washing the experimental article with deionized water; and (4) preparing an acid solution with the concentration required by the experiment by using a volumetric flask and sealing for later use.
Step 2, acid washing and purification: firstly, a certain amount of clear water is filled in an ultrasonic cleaner, and the working temperature of the ultrasonic cleaner is set and heated; selecting hydrochloric acid, sulfuric acid, nitric acid and hydrofluoric acid as pickling agents, controlling pickling parameters, wherein the liquid-solid ratio is 5:1, the acid concentration is 0.15mol/L, the pickling temperature is 70 ℃, the stirring speed is 300rpm, the ultrasonic power is 240W, the ultrasonic frequency is 45kHz, and the pickling time is 180 min; after the water temperature in the ultrasonic cleaner reaches the set temperature and is stable, 70g of SiC powder to be pickled is poured into a beaker filled with 350ml of acid solution (the liquid-solid ratio is 5:1), the stirring speed of the stirrer is adjusted, and the ultrasonic cleaner and the stirrer are started to carry out pickling simultaneously.
And 3, sampling and washing: taking out 50ml of acid-washing slurry by using a plastic syringe every 30min, injecting the acid-washing slurry into a cleaned beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
And 4, drying: and transferring the washed SiC powder into a culture dish washed by deionized water, drying in an oven at 110 ℃ for 6h, and sealing for later use.
And 5, detecting: 2g of the SiC powder after acid washing and drying is taken out and is subjected to Fe element content analysis by utilizing ICP-OES, and the influence curve of acid species on the Fe removal rate is shown in figure 1 after detection.
In the embodiment, under the condition of hydrofluoric acid as a pickling agent, the Fe impurity removal rate of the silicon carbide powder can reach 92.6%, and the impurity content is respectively reduced to less than 1.10% of O, less than 0.72% of free-Si, less than 0.20% of free-C, less than 0.004% of Fe, less than 0.015% of Ti, less than 0.0067% of Al, less than 0.0003% of Ni and less than 0.0014% of V.
Example 2
The iron removal process based on the submicron silicon carbide powder comprises the following steps:
step 1, preparing: washing the experimental article with deionized water; and (4) preparing an acid solution with the concentration required by the experiment by using a volumetric flask and sealing for later use.
Step 2, acid washing and purification: firstly, a certain amount of clear water is filled in an ultrasonic cleaner, and the working temperature of the ultrasonic cleaner is set and heated; selecting hydrofluoric acid as a pickling agent, and controlling pickling parameters, wherein the liquid-solid ratio is 5:1, the acid concentration is 0.20mol/L, the pickling temperature is 70 ℃, the stirring speed is 300rpm, the ultrasonic power is 240W, the ultrasonic frequency is 45kHz, and the pickling time is 180 min; after the water temperature in the ultrasonic cleaner reaches the set temperature and is stable, 70g of SiC powder to be pickled is poured into a beaker filled with 350ml of acid solution (the liquid-solid ratio is 5:1), the stirring speed of the stirrer is adjusted, and the ultrasonic cleaner and the stirrer are started to carry out pickling simultaneously.
And 3, sampling and washing: taking out 50ml of acid-washing slurry by using a plastic syringe every 30min, injecting the acid-washing slurry into a cleaned beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
And 4, drying: and transferring the washed SiC powder into a culture dish washed by deionized water, drying in an oven at 110 ℃ for 6h, and sealing for later use.
And 5, detecting: 2g of the acid-washed and dried SiC powder was taken out and subjected to Fe content analysis by ICP-OES.
In this example, the removal rate of Fe impurity in silicon carbide powder at 0.20mol/L acid concentration can reach 93.6%, and the impurity content is reduced to O < 1.10%, free-Si < 0.72%, free-C < 0.20%, Fe < 0.004%, Ti < 0.015%, Al < 0.0067%, Ni < 0.0003%, and V < 0.0014%, respectively.
Example 3
The iron removal process based on the submicron silicon carbide powder comprises the following steps:
step 1, preparing: washing the experimental article with deionized water; and (4) preparing an acid solution with the concentration required by the experiment by using a volumetric flask and sealing for later use.
Step 2, acid washing and purification: firstly, a certain amount of clear water is filled in an ultrasonic cleaner, and the working temperature of the ultrasonic cleaner is set and heated; selecting hydrofluoric acid as a pickling agent, and controlling pickling parameters, wherein the liquid-solid ratio is 5:1, the pickling temperature is 80 ℃, the acid concentration is 0.15mol/L, the pickling time is 180min, the stirring speed is 300rpm, the ultrasonic power is 240W, and the ultrasonic frequency is 45 kHz; after the water temperature in the ultrasonic cleaner reaches the set temperature and is stable, 70g of SiC powder to be pickled is poured into a beaker filled with 350ml of acid solution (the liquid-solid ratio is 5:1), the stirring speed of the stirrer is adjusted, and the ultrasonic cleaner and the stirrer are started to carry out pickling simultaneously.
And 3, sampling and washing: taking out 50ml of acid-washing slurry by using a plastic syringe every 30min, injecting the acid-washing slurry into a cleaned beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
And 4, drying: and transferring the washed SiC powder into a culture dish washed by deionized water, drying in an oven at 110 ℃ for 6h, and sealing for later use.
And 5, detecting: 2g of the acid-washed and dried SiC powder was taken out and subjected to Fe content analysis by ICP-OES.
In the embodiment, the removal rate of Fe impurities in the silicon carbide powder can reach 95.3% at the pickling temperature of 80 ℃, and the impurity content is respectively reduced to less than 1.10% of O, less than 0.72% of free-Si, less than 0.20% of free-C, less than 0.004% of Fe, less than 0.015% of Ti, less than 0.0067% of Al, less than 0.0003% of Ni and less than 0.0014% of V.
Example 4
The iron removal process based on the submicron silicon carbide powder comprises the following steps:
step 1, preparing: washing the experimental article with deionized water; and (4) preparing an acid solution with the concentration required by the experiment by using a volumetric flask and sealing for later use.
Step 2, acid washing and purification: firstly, a certain amount of clear water is filled in an ultrasonic cleaner, and the working temperature of the ultrasonic cleaner is set and heated; selecting hydrofluoric acid as a pickling agent, and controlling pickling parameters, wherein the liquid-solid ratio is 5:1, the ultrasonic frequency is 100kHz, the acid concentration is 0.15mol/L, the pickling temperature is 80 ℃, the stirring speed is 300rpm, the ultrasonic power is 240W, and the pickling time is 180 min; after the water temperature in the ultrasonic cleaner reaches the set temperature and is stable, 70g of SiC powder to be pickled is poured into a beaker filled with 350ml of acid solution (the liquid-solid ratio is 5:1), the stirring speed of the stirrer is adjusted, and the ultrasonic cleaner and the stirrer are started to carry out pickling simultaneously.
And 3, sampling and washing: taking out 50ml of acid-washing slurry by using a plastic syringe every 30min, injecting the acid-washing slurry into a cleaned beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
And 4, drying: and transferring the washed SiC powder into a culture dish washed by deionized water, drying in an oven at 110 ℃ for 6h, and sealing for later use.
And 5, detecting: 2g of the acid-washed and dried SiC powder was taken out and subjected to Fe content analysis by ICP-OES.
In the embodiment, the removal rate of Fe impurities in the silicon carbide powder under the ultrasonic frequency of 45kHz can reach 93.9 percent, and the impurity content is respectively reduced to less than 1.10 percent of O, less than 0.72 percent of free-Si, less than 0.20 percent of free-C, less than 0.004 percent of Fe, less than 0.015 percent of Ti, less than 0.0067 percent of Al, less than 0.0003 percent of Ni and less than 0.0014 percent of V.
Example 5
The iron removal process based on the submicron silicon carbide powder comprises the following steps:
step 1, preparing: washing the experimental article with deionized water; and (4) preparing an acid solution with the concentration required by the experiment by using a volumetric flask and sealing for later use.
Step 2, acid washing and purification: firstly, a certain amount of clear water is filled in an ultrasonic cleaner, and the working temperature of the ultrasonic cleaner is set and heated; selecting hydrofluoric acid as a pickling agent, and controlling pickling parameters, wherein the liquid-solid ratio is 5:1, the stirring speed is 400rpm, the acid concentration is 0.15mol/L, the pickling time is 180min, the pickling temperature is 80 ℃, the ultrasonic power is 240W, and the ultrasonic frequency is 45 kHz; after the water temperature in the ultrasonic cleaner reaches the set temperature and is stable, 70g of SiC powder to be pickled is poured into a beaker filled with 350ml of acid solution (the liquid-solid ratio is 5:1), the stirring speed of the stirrer is adjusted, and the ultrasonic cleaner and the stirrer are started to carry out pickling simultaneously.
And 3, sampling and washing: taking out 50ml of acid-washing slurry by using a plastic syringe every 30min, injecting the acid-washing slurry into a cleaned beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
And 4, drying: and transferring the washed SiC powder into a culture dish washed by deionized water, drying in an oven at 110 ℃ for 6h, and sealing for later use.
And 5, detecting: 2g of the acid-washed and dried SiC powder was taken out and subjected to Fe content analysis by ICP-OES.
In the embodiment, the Fe impurity removal rate of the silicon carbide powder can reach 95.8% at the ultrasonic stirring speed of 400rpm, and the impurity content is respectively reduced to less than 1.10% of O, less than 0.72% of free-Si, less than 0.20% of free-C, less than 0.004% of Fe, less than 0.015% of Ti, less than 0.0067% of Al, less than 0.0003% of Ni and less than 0.0014% of V.
Example 6
The iron removal process based on the submicron silicon carbide powder comprises the following steps:
step 1, preparing: washing the experimental article with deionized water; and (4) preparing an acid solution with the concentration required by the experiment by using a volumetric flask and sealing for later use.
Step 2, acid washing and purification: firstly, a certain amount of clear water is filled in an ultrasonic cleaner, and the working temperature of the ultrasonic cleaner is set and heated; selecting hydrofluoric acid as a pickling agent, and controlling pickling parameters, wherein the liquid-solid ratio is 5:1, the ultrasonic power is 270W, the acid concentration is 0.15mol/L, the pickling time is 180min, the pickling temperature is 80 ℃, the stirring speed is 400rpm, and the ultrasonic frequency is 45 kHz; after the water temperature in the ultrasonic cleaner reaches the set temperature and is stable, 70g of SiC powder to be pickled is poured into a beaker filled with 350ml of acid solution (the liquid-solid ratio is 5:1), the stirring speed of the stirrer is adjusted, and the ultrasonic cleaner and the stirrer are started to carry out pickling simultaneously.
And 3, sampling and washing: taking out 50ml of acid-washing slurry by using a plastic syringe every 30min, injecting the acid-washing slurry into a cleaned beaker, adding deionized water, and standing; after the powder is fully settled, pouring out supernatant liquor, and adding deionized water again; and repeatedly washing the SiC powder after the acid washing until the pH value is adjusted to 6-7.
And 4, drying: and transferring the washed SiC powder into a culture dish washed by deionized water, drying in an oven at 110 ℃ for 6h, and sealing for later use.
And 5, detecting: 2g of the acid-washed and dried SiC powder was taken out and subjected to Fe content analysis by ICP-OES.
In the embodiment, under the condition of 270W ultrasonic power, the removal rate of Fe impurities in the silicon carbide powder can reach 96.1%, and the impurity contents are respectively reduced to less than 1.10% of O, less than 0.72% of free-Si, less than 0.20% of free-C, less than 0.004% of Fe, less than 0.015% of Ti, less than 0.0067% of Al, less than 0.0003% of Ni and less than 0.0014% of V.
Claims (8)
1. A process for removing iron from submicron silicon carbide powder is characterized by comprising the following steps:
step 1, acid washing and purification:
pouring the SiC powder into a pickling agent solution, and carrying out ultrasonic-assisted stirring and pickling to obtain pickling slurry; wherein the concentration of the pickling agent solution is 0.05-0.2 mol/L, and the ultrasonic power is 180-270W;
step 2, washing:
repeatedly washing the acid-washed slurry with deionized water to obtain washed SiC powder;
step 3, drying detection:
and (4) after washing, drying the SiC powder, and then detecting the content of Fe impurities.
2. The process for removing iron from submicron-sized silicon carbide powder according to claim 1, wherein in the step 1, the average particle size of the SiC powder is 0.5 μm, the pickling agent is one or more selected from hydrochloric acid, sulfuric acid, nitric acid and hydrofluoric acid, and the pickling agent is prepared into a pickling agent solution with a concentration of 0.05 to 0.2 mol/L.
3. The process for removing iron from submicron silicon carbide powder according to claim 1, wherein in the step 1, the SiC powder contains impurities in an amount of 0.98 to 1.85% by mass, 0.52 to 1.68% by mass of free-Si, 0.22 to 0.67% by mass of free-C, 0.084 to 0.159% by mass of Fe, 0.0185 to 0.051% by mass of Ti, 0.0081 to 0.0174% by mass of Al, 0.0085 to 0.0194% by mass of Ni, and 0.0025 to 0.0082% by mass of V.
4. The process for removing iron from submicron-sized silicon carbide powder according to claim 1, wherein in the step 1, the conditions of ultrasonic-assisted stirring and acid washing are as follows: pouring SiC powder to be pickled into a pickling agent solution according to the liquid-solid ratio of (4-6): 1, wherein the pickling temperature is 50-80 ℃, the ultrasonic frequency is 40-150 kHz, the stirring speed is 100-400 rpm, and the pickling time is 30-180 min.
5. The process for removing iron from submicron-sized silicon carbide powder according to claim 4, wherein in the step 1, the conditions of ultrasonic-assisted stirring and acid washing are as follows: pouring SiC powder to be pickled into a beaker filled with a pickling agent solution according to the liquid-solid ratio of 5:1, wherein the acid concentration is 0.15mol/L, the pickling temperature is 80 ℃, the ultrasonic frequency is 45kHz, the stirring speed is 400rpm, the ultrasonic power is 270W, and the pickling time is 180 min.
6. The process for removing iron from submicron-sized silicon carbide powder according to claim 1, wherein in the step 2, the water washing comprises the following specific steps: injecting the acid-washing slurry into a clean beaker, adding deionized water, and standing; and after the powder is fully settled, pouring out the supernatant, adding deionized water again, and washing the acid-washed SiC powder until the pH value is adjusted to 6-7.
7. The process for removing iron from submicron-sized silicon carbide powder according to claim 1, wherein in the step 3, the content of Fe element in the acid-washed and dried SiC powder is analyzed by ICP-OES.
8. The process for removing iron from submicron-sized silicon carbide powder according to claim 1, wherein in step 3, the removal rate of iron impurities is 92.6-96.1%, and the impurity contents are respectively reduced to O < 1.10%, free-Si < 0.72%, free-C < 0.20%, Fe < 0.004%, Ti < 0.015%, Al < 0.0067%, Ni < 0.0003%, and V < 0.0014%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114409407A (en) * | 2022-02-15 | 2022-04-29 | 陕西固勤材料技术有限公司 | Method for purifying and improving silicon carbide content of semiconductor cantilever paddle product |
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