CN114261966B - Method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption - Google Patents
Method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 94
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 73
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000005265 energy consumption Methods 0.000 title claims abstract description 18
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 239000006230 acetylene black Substances 0.000 claims abstract description 6
- 238000011068 loading method Methods 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 30
- 239000000377 silicon dioxide Substances 0.000 claims description 28
- 235000012239 silicon dioxide Nutrition 0.000 claims description 23
- 238000004062 sedimentation Methods 0.000 claims description 21
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- 238000005201 scrubbing Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 239000004927 clay Substances 0.000 claims description 10
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004021 humic acid Substances 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 6
- 238000007885 magnetic separation Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- VSTOHTVURMFCGL-UHFFFAOYSA-N [C].O=[Si]=O Chemical compound [C].O=[Si]=O VSTOHTVURMFCGL-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000009837 dry grinding Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 239000006148 magnetic separator Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 241000209504 Poaceae Species 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 239000011707 mineral Substances 0.000 description 1
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- 239000003208 petroleum Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption, which comprises the following steps: step one, batching: firstly, 50% -70% of carbon-containing silicon dioxide powder and 45% -25% of acetylene black are uniformly mixed, and then 3% -6% of binder is added and uniformly stirred to obtain a mixed material for later use; step two, pressing the mixed material obtained in the step one into blocks and drying; and thirdly, loading the block-shaped mixed materials in the second step into a graphite boat, and sending the graphite boat into a molybdenum wire electric furnace for firing to obtain submicron silicon carbide balls. The invention adopts a large-scale primary synthesis method, overcomes the defects of complex secondary synthesis procedure, long time consumption, artificial introduction of impurities and the like, and the obtained silicon carbide is spherical, has the granularity of 100-200nm and the purity of more than 99.5 percent; the invention realizes a one-step synthesis process based on the raw materials of the carbon-containing silicon dioxide powder, and the acquisition mode of the raw materials of the carbon-containing silicon dioxide powder is based on the existing machine conditions, thus being completely applicable to industrial mass production practice.
Description
Technical Field
The invention relates to the field of inorganic nonmetallic materials, in particular to a method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption.
Background
The silicon carbide has the unique characteristics of large forbidden band width, high breakdown electric field, high thermal conductivity, high electron saturation drift velocity, small dielectric constant, strong radiation resistance, good chemical stability and the like, has obvious superiority compared with the first-generation semiconductor material and the second-generation semiconductor material, is considered to be ideal semiconductor material for manufacturing optoelectronic devices, high-frequency high-power devices and power electronic devices, and has wide application in the aspects of white light illumination, optical storage, screen display, aerospace, high-temperature radiation environment, petroleum exploration, automation, radar and communication, automobile electronization and the like. The quality of submicron silicon carbide powder plays an important role in growing silicon carbide single crystals by a sublimation method, and directly influences the crystallization quality, the growth thickness and the cost of the single crystals. With the wide-scale application of silicon carbide single crystal substrate power devices and power electronic devices, the demand for large diameter single crystals is becoming more and more urgent, extending from 4 inches to 6 inches and even 8 inches, which are currently widely used. The current synthesis method has high cost and can not meet the requirement of industrialized production, so the cost is reduced by improving the technology of synthesis raw materials, the granularity of source materials is controllable, and the method becomes a difficult problem to be solved in the prior art for growing large single crystals.
At present, the SiC is synthesized to be used as a silicon source, and the simple substance Si is also used as the silicon source, so that the granularity is required to be sufficiently fine, the cost is greatly increased due to the crushing process, and the silicon source is also used as SiO2 powder, and the silicon source becomes the bottleneck of mass production of SiC materials. The invention seeks to a special silicon dioxide powder-carbon-containing silicon dioxide powder which is SiO in plants 2 In particular, the annual grasses in the lake phase aggregate, die and deposit together, the granularity is extremely fine, and three types of carbon aggregate together: the inside of the particles is rich in carbon (the carbon content is 1-6% as proved by related detection), the carbon isolation is also carried out between the particles, and the herbaceous plant carbon which is deposited together with the particles is also arranged outside the particles. And adding carbon in an equal ratio chemical form to perform excessive reaction during synthesis.
In addition, many utilize SiO 2 When the material is used as a silicon source, compactness is not considered when the material is mixed with carbon, and the organic silicone oil is used as a binder to press the carbon-containing silicon dioxide powder and the acetylene black into blocks, so that gaseous SiO formed by high-temperature reaction can be prevented from escaping, and the SiO can be continuously reacted with C in time to form elemental Si and subsequent SiC. After pyrolysis of the binder silicone oil, si therein is beneficial to triggering SiC reaction. Because the particles of the carbon-containing silicon dioxide powder are smaller, the SiC reaction can be carried out at a lower temperature. The invention has simple process, can realize industrial production, has low energy consumption, accords with the national 'double carbon' target, and has great specificity and innovation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption so as to solve the problems in the technical background.
In order to achieve the above object, the present invention is realized by the following technical scheme:
in one aspect, the invention provides a method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption, comprising the following steps:
step one, batching: firstly, 50% -70% of carbon-containing silicon dioxide powder and 45% -25% of acetylene black are uniformly mixed, and then 3% -6% of binder is added and uniformly stirred to obtain a mixed material for later use;
step two, pressing the mixed material obtained in the step one into blocks and drying;
and thirdly, loading the block-shaped mixed materials in the second step into a graphite boat, and sending the graphite boat into a molybdenum wire electric furnace for firing to obtain submicron silicon carbide balls.
In the technical scheme, in the third step, the specific firing process of the blocky mixed material in the molybdenum wire electric furnace is as follows: heating to 1300-1500 deg.c at 100 deg.c each hr, maintaining for 2-4 hr, and cooling to room temperature.
In the technical scheme, the whole firing process is carried out in a mixed gas of argon and hydrogen, wherein the argon accounts for 85% -85%, and the hydrogen accounts for 5% -15%.
In the technical scheme, the binder is silicone oil.
In the technical scheme, the carbon-containing silicon dioxide powder is obtained by treating the silicon plant body deposited in the Poyang lake ancient way and containing humic acid silicon ore, and the specific treatment method comprises the following steps:
(1) And (3) adding water and gyratory crushing: adding water into the newly mined silicon plant containing humic acid silicon ore, mixing with the mixture, and then putting the mixture into a gyratory crusher for crushing;
(2) Primary mesh screen separation: separating the gravel sieve with the size larger than 5mm by adopting a vibrating screen;
(3) Primary scrubbing and stripping: placing the silicon-implanted body ore with the gravel of 5mm into a scrubbing machine for preliminary scrubbing and stripping, wherein the preliminary scrubbing time is 10-30min;
(4) Secondary mesh screen separation: sieving substances larger than 1mm by a vibrating screen;
(5) Primary superfine ball milling: sieving the material of 1mm from the step (4), and carrying out superfine ball milling for 30-300min; wherein, zirconia ball milling medium is adopted for primary superfine ball milling, and the diameter of the zirconia ball milling medium is 1mm-5mm
(6) Secondary scrubbing and stripping: screening out impurities larger than 0.1mm from the superfine ball-milled material in the step (5), and removing the impurities;
(7) Primary sedimentation: pulping the product of the impurity screened by 0.1mm in the step (6), then feeding the obtained mixed pulp into a primary sedimentation tank for sedimentation for 1-4h, and separating a bottom sediment;
(8) Secondary superfine ball milling: performing secondary superfine ball milling on the slurry separated from the bottom sediment in the step (7), and performing superfine ball milling for 30-300min to enable clay and SiO to be obtained 2 Separating particles; wherein, the secondary superfine ball milling adopts zirconia ball milling medium with the diameter of 0.1mm-1 mm;
(9) Secondary sedimentation: clay and SiO in the step (8) 2 The particles enter a secondary sedimentation tank, after sedimentation for 2-3 hours in the secondary sedimentation tank, the suspended upper part is mixed with clay substances to be discharged, and SiO is obtained 2 Crude products;
(10) Magnetic separation and iron removal: siO obtained in the step (9) 2 Removing iron from the crude product by adopting a high-gradient magnetic separator to obtain feed liquid containing carbon silicon dioxide; wherein the magnetic field intensity of the magnetic separation is more than 6000 gauss;
(11) And (3) separating water: the feed liquid containing the carbon-containing silicon dioxide is sent into a solid-liquid separation process for solid-liquid separation, so that the water-containing carbon-containing silicon dioxide is obtained, and the water content of the water-containing carbon-containing silicon dioxide is less than 5%;
(12) And (3) drying: drying at 120 ℃ to obtain dried carbon-containing silicon dioxide, wherein the carbon-containing silicon dioxide is in a hardened or agglomerated shape;
(13) Dry grinding: and (3) crushing and separating the dried carbon-containing silicon dioxide by a dry method to obtain carbon-containing silicon dioxide powder.
In the technical proposal, siO in the carbon-containing silicon dioxide powder obtained after treatment 2 88.5 to 90.5 percent of carbon content, 9 to 11 percent of carbon content and SiO 2 The particle size is 300nm-5 μm.
In the technical scheme, in the second step, the pressure used for pressing the mixed materials into blocks is more than 10MPa.
On the other hand, the invention also provides submicron silicon carbide balls, which are prepared by adopting the method for synthesizing submicron silicon carbide balls by using the carbon-containing silicon dioxide powder with low energy consumption.
On the other hand, the invention also provides an application of the carbon-containing silicon dioxide powder in preparing submicron silicon carbide balls, wherein the application mode is that the method for synthesizing the submicron silicon carbide balls by using the carbon-containing silicon dioxide powder with low energy consumption is adopted.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts a large-scale primary synthesis method, and overcomes the defects of complex secondary synthesis procedures, long time consumption, artificial impurity introduction and the like.
2. The preparation of submicron SiC in the prior art consumes huge energy, and the cost performance restricts the market development. The invention adopts a brand new process, and particularly has the characteristics that the raw material carbon-containing silicon dioxide powder is a natural SiC raw material; the invention realizes a one-step synthesis process based on the raw materials of the carbon-containing silicon dioxide powder, and the acquisition mode of the raw materials of the carbon-containing silicon dioxide powder is based on the existing machine conditions, thus being completely applicable to industrial mass production practice. The obtained silicon carbide is spherical, the granularity is 100-200nm, and the purity is more than 99.5%.
3. According to the invention, the organic silicone oil is used as a binder to press the carbon-containing silicon dioxide powder and the acetylene black into blocks, so that gaseous SiO formed by high-temperature reaction can be prevented from escaping, and the SiO can be continuously reacted with C in time to form elemental Si and subsequent SiC. Meanwhile, after the binder silicone oil is decomposed at high temperature, si in the binder silicone oil is beneficial to triggering SiC reaction.
Drawings
FIG. 1 is an SEM image of a silicon plant containing humic acid silicon ore;
FIG. 2 is an XRD pattern of a carbon-containing silica powder;
FIG. 3 is an SEM image of a char-containing silica powder;
FIG. 4 is an XRD pattern for submicron silicon carbide spheres;
FIG. 5 is an SEM image of submicron silicon carbide spheres (scale 2 um);
fig. 6 is an SEM image of submicron silicon carbide spheres (200 nm on scale).
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict.
It should be noted that the illustrations provided in the following embodiments merely illustrate the basic concept of the present invention by way of illustration, and only the components related to the present invention are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of the components in actual implementation may be arbitrarily changed, and the layout of the components may be more complicated.
Example 1
The invention provides a method for synthesizing submicron silicon carbide balls by using carbon-containing silicon dioxide powder with low energy consumption, which comprises the following steps:
step one, batching: firstly, uniformly mixing 50% -70% of carbon-containing silicon dioxide powder and 45% -25% of acetylene black (purity 99.99%), then adding 3% -6% of binder, and uniformly stirring to obtain a mixed material for later use;
wherein the binder is silicone oil, which is of analytically pure grade.
The carbon-containing silicon dioxide powder is obtained by treating silicon dioxide ore containing humic acid of a silicon plant deposited in the ancient of Poyang lake, and the adopted silicon dioxide ore containing humic acid is shown in the figure 1, and the raw mineral components are about: 8% of gangue, 3% of clay, 0.5% of pyrite, 0.5% of goethite, 10% of carbon content and SiO 2 78%; the raw chemical components are as follows: siO (SiO) 2 77.01-80.54％、Al 2 O 3 3.03-5.35％、Fe 2 O 3 1.08-3.73%, caO 0.07-0.69%, LOI (loss on ignition) 11.96-16.13%, tiO 2 About 0.69%. The specific treatment method comprises the following steps:
(1) And (3) adding water and gyratory crushing: adding water into the newly mined silicon plant containing humic acid silicon ore, mixing with the mixture, and then putting the mixture into a gyratory crusher for crushing;
(2) Primary mesh screen separation: separating the gravel sieve with the size larger than 5mm by adopting a vibrating screen;
(3) Primary scrubbing and stripping: placing the silicon-implanted body ore with the gravel of 5mm into a scrubbing machine for preliminary scrubbing and stripping, wherein the preliminary scrubbing time is 10-30min;
(4) Secondary mesh screen separation: sieving substances larger than 1mm by a vibrating screen;
(5) Primary superfine ball milling: sieving the material of 1mm from the step (4), and carrying out superfine ball milling for 30-300min; wherein, zirconia ball milling medium is adopted for primary superfine ball milling, and the diameter of the zirconia ball milling medium is 1mm-5mm
(6) Secondary scrubbing and stripping: screening out impurities larger than 0.1mm from the superfine ball-milled material in the step (5), and removing the impurities;
(7) Primary sedimentation: pulping the product of the impurity screened by 0.1mm in the step (6), then feeding the obtained mixed pulp into a primary sedimentation tank for sedimentation for 1-4h, and separating a bottom sediment;
(8) Secondary superfine ball milling: performing secondary superfine ball milling on the slurry separated from the bottom sediment in the step (7), and performing superfine ball milling for 30-300min to enable clay and SiO to be obtained 2 Separating particles; wherein, the secondary superfine ball milling adopts zirconia ball milling medium with the diameter of 0.1mm-1 mm;
(9) Secondary sedimentation: clay and SiO in the step (8) 2 The particles enter a secondary sedimentation tank, after sedimentation for 2-3 hours in the secondary sedimentation tank, the suspended upper part is mixed with clay substances to be discharged, and SiO is obtained 2 Crude products;
(10) Magnetic separation and iron removal: siO obtained in the step (9) 2 Removing iron from the crude product by adopting a high-gradient magnetic separator to obtain feed liquid containing carbon silicon dioxide; wherein the magnetic field intensity of the magnetic separation is more than 6000 gauss;
(11) And (3) separating water: the feed liquid containing the carbon-containing silicon dioxide is sent into a solid-liquid separation process for solid-liquid separation, so that the water-containing carbon-containing silicon dioxide is obtained, and the water content of the water-containing carbon-containing silicon dioxide is less than 5%;
(12) And (3) drying: drying at 120 ℃ to obtain dried carbon-containing silicon dioxide, wherein the carbon-containing silicon dioxide is in a hardened or agglomerated shape;
(13) Dry grinding: and (3) crushing and separating the dried carbon-containing silicon dioxide by a dry method to obtain carbon-containing silicon dioxide powder. The chemical composition of the treated carbon-containing silicon dioxide powder is SiO 2 88.5% -90.5%, 9% -11% carbon, and the balance about 1%, possiblyIs Al 2 O 3 、Fe 2 O 3 Substances such as; and SiO 2 The particle size was 300 nm-5. Mu.m, as shown in FIGS. 2 and 3.
Step two, pressing the mixed material obtained in the step one into blocks, and drying at 100 ℃; wherein the pressure used for pressing the mixed materials into blocks is more than 10MPa.
And step three, loading the block-shaped mixed material in the step two into a graphite boat, and sending the graphite boat into a molybdenum wire electric furnace for firing to obtain submicron silicon carbide balls, wherein the granularity of the obtained submicron silicon carbide balls is 100-200nm, and the purity is more than 99.5 percent, referring to fig. 4-6. The specific firing process of the blocky mixed materials in the molybdenum wire electric furnace is as follows: heating to 1300-1500 deg.c at 100 deg.c each hr, maintaining for 2-4 hr, and cooling to room temperature. The whole firing process is carried out in a mixed gas of argon and hydrogen, wherein the argon is 85% -85%, the hydrogen is 5% -15%, and the purities of the argon and the hydrogen are both more than 99.9%.
Example 2
This example provides a submicron silicon carbide sphere prepared using the method of low energy consumption synthesis of submicron silicon carbide spheres using carbon-containing silica powder described in example 1.
Example 3
The embodiment also provides an application of the carbon-containing silicon dioxide powder in preparing submicron silicon carbide balls, wherein the application mode is that the method for synthesizing the submicron silicon carbide balls by using the carbon-containing silicon dioxide powder with low energy consumption is adopted in the embodiment 1.
The above examples merely illustrate specific embodiments of the invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (6)
1. The method for synthesizing the submicron silicon carbide balls by using the carbon-containing silicon dioxide powder with low energy consumption is characterized by comprising the following steps:
step one, batching: firstly, 50% -70% of carbon-containing silicon dioxide powder and 45% -25% of acetylene black are uniformly mixed, and then 3% -6% of binder is added and uniformly stirred to obtain a mixed material for later use;
step two, pressing the mixed material obtained in the step one into blocks and drying;
step three, loading the blocky mixed material in the step two into a graphite boat, and sending the graphite boat into a molybdenum wire electric furnace to be fired to obtain submicron silicon carbide balls;
wherein the binder is silicone oil;
the carbon-containing silicon dioxide powder is obtained by treating silicon dioxide ore containing humic acid of a silicon plant body deposited in the ancient way of the Poyang lake, and the specific treatment method comprises the following steps:
(1) And (3) adding water and gyratory crushing: adding water into the newly mined silicon plant containing humic acid silicon ore, mixing with the mixture, and then putting the mixture into a gyratory crusher for crushing;
(2) Primary mesh screen separation: separating the gravel sieve with the size larger than 5mm by adopting a vibrating screen;
(3) Primary scrubbing and stripping: placing the silicon-implanted body ore with the gravel of 5mm into a scrubbing machine for preliminary scrubbing and stripping, wherein the preliminary scrubbing time is 10-30min;
(4) Secondary mesh screen separation: sieving substances larger than 1mm by a vibrating screen;
(5) Primary superfine ball milling: sieving the material of 1mm from the step (4), and carrying out superfine ball milling for 30-300min; wherein, zirconia ball milling medium is adopted for primary superfine ball milling, and the diameter of the zirconia ball milling medium is 1mm-5mm
(6) Secondary scrubbing and stripping: screening out impurities larger than 0.1mm from the superfine ball-milled material in the step (5), and removing the impurities;
(7) Primary sedimentation: pulping the product of the impurity screened by 0.1mm in the step (6), then feeding the obtained mixed pulp into a primary sedimentation tank for sedimentation for 1-4h, and separating a bottom sediment;
(8) Secondary superfine ball milling: performing secondary superfine ball milling on the slurry separated from the bottom sediment in the step (7), and performing superfine ball milling for 30-300min to enable clay and SiO to be obtained 2 Separating particles; wherein, the secondary superfine ball milling adopts zirconia ball milling medium with the diameter of 0.1mm-1 mm;
(9) Secondary sedimentation: clay and SiO in the step (8) 2 The particles enter a secondary sedimentation tank, after sedimentation for 2-3 hours in the secondary sedimentation tank, the suspended upper part is mixed with clay substances to be discharged, and SiO is obtained 2 Crude products;
(10) Magnetic separation and iron removal: siO obtained in the step (9) 2 Removing iron from the crude product by adopting a high-gradient magnetic separator to obtain feed liquid containing carbon silicon dioxide; wherein the magnetic field intensity of the magnetic separation is more than 6000 gauss;
(11) And (3) separating water: the feed liquid containing the carbon-containing silicon dioxide is sent into a solid-liquid separation process for solid-liquid separation, so that the water-containing carbon-containing silicon dioxide is obtained, and the water content of the water-containing carbon-containing silicon dioxide is less than 5%;
(12) And (3) drying: drying at 120 ℃ to obtain dried carbon-containing silicon dioxide, wherein the carbon-containing silicon dioxide is in a hardened or agglomerated shape;
(13) Dry grinding: and (3) crushing and separating the dried carbon-containing silicon dioxide by a dry method to obtain carbon-containing silicon dioxide powder.
2. The method for synthesizing submicron silicon carbide balls with low energy consumption by utilizing carbon-containing silicon dioxide powder according to claim 1, wherein in the third step, the specific firing process of the bulk mixed material in a molybdenum wire electric furnace is as follows: heating to 1300-1500 deg.c at 100 deg.c each hr, maintaining for 2-4 hr, and cooling to room temperature.
3. The method for synthesizing submicron silicon carbide balls with low energy consumption using the carbonaceous silica powder according to claim 2, wherein the entire firing process is performed in a mixed gas of argon and hydrogen, wherein the argon is 85% -85% and the hydrogen is 5-15%.
4. The method for synthesizing submicron silicon carbide balls with low energy consumption by utilizing carbon-containing silicon dioxide powder according to claim 1, wherein SiO in the carbon-containing silicon dioxide powder obtained after treatment 2 88.5 to 90.5 percent of carbon content, 9 to 11 percent of carbon content and SiO 2 The particle size is 300nm-5 μm.
5. The method for synthesizing submicron silicon carbide balls with low energy consumption by utilizing carbon-containing silicon dioxide powder according to claim 1, wherein in the second step, the pressure for pressing the mixed materials into blocks is more than 10MPa.
6. Submicron silicon carbide sphere prepared by the method of any one of claims 1-5 using carbon-containing silica powder to synthesize submicron silicon carbide sphere with low energy consumption.
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| CN101704523A (en) * | 2009-11-25 | 2010-05-12 | 杨大锦 | Production technology of high purity silicon carbide |
| CN109790035A (en) * | 2017-05-18 | 2019-05-21 | 株式会社Lg化学 | Silicon carbide powder and preparation method thereof |
| CN111484017A (en) * | 2020-06-22 | 2020-08-04 | 黑龙江冠瓷科技有限公司 | Method for preparing SiC nanoparticles based on silica microspheres @ C |
| CN112923733A (en) * | 2021-02-02 | 2021-06-08 | 北京绿清科技有限公司 | Method for producing silicon carbide by adopting multi-furnace series connection grading melting furnace and special production system |
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| CN101704523A (en) * | 2009-11-25 | 2010-05-12 | 杨大锦 | Production technology of high purity silicon carbide |
| CN109790035A (en) * | 2017-05-18 | 2019-05-21 | 株式会社Lg化学 | Silicon carbide powder and preparation method thereof |
| CN111484017A (en) * | 2020-06-22 | 2020-08-04 | 黑龙江冠瓷科技有限公司 | Method for preparing SiC nanoparticles based on silica microspheres @ C |
| CN112923733A (en) * | 2021-02-02 | 2021-06-08 | 北京绿清科技有限公司 | Method for producing silicon carbide by adopting multi-furnace series connection grading melting furnace and special production system |
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