CN116924409A - Preparation method of nano silicon carbide abrasive - Google Patents
Preparation method of nano silicon carbide abrasive Download PDFInfo
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- CN116924409A CN116924409A CN202310948202.8A CN202310948202A CN116924409A CN 116924409 A CN116924409 A CN 116924409A CN 202310948202 A CN202310948202 A CN 202310948202A CN 116924409 A CN116924409 A CN 116924409A
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- silicon carbide
- nano silicon
- carbide abrasive
- ferric nitrate
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 51
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 239000002028 Biomass Substances 0.000 claims abstract description 25
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 238000010000 carbonizing Methods 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 238000005496 tempering Methods 0.000 claims abstract description 9
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 37
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 229920000742 Cotton Polymers 0.000 claims description 12
- 235000006408 oxalic acid Nutrition 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 8
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 5
- 244000198134 Agave sisalana Species 0.000 claims description 4
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 4
- 244000105624 Arachis hypogaea Species 0.000 claims description 4
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 4
- 235000018262 Arachis monticola Nutrition 0.000 claims description 4
- 235000020232 peanut Nutrition 0.000 claims description 4
- 235000011624 Agave sisalana Nutrition 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 241000219146 Gossypium Species 0.000 claims description 2
- 238000005498 polishing Methods 0.000 abstract description 27
- 238000000227 grinding Methods 0.000 abstract description 14
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000007517 polishing process Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000004108 freeze drying Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 230000003746 surface roughness Effects 0.000 description 6
- 230000015271 coagulation Effects 0.000 description 5
- 238000005345 coagulation Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- PUSKHXMZPOMNTQ-UHFFFAOYSA-N ethyl 2,1,3-benzoselenadiazole-5-carboxylate Chemical compound CCOC(=O)C1=CC=C2N=[Se]=NC2=C1 PUSKHXMZPOMNTQ-UHFFFAOYSA-N 0.000 description 4
- 239000003082 abrasive agent Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/977—Preparation from organic compounds containing silicon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a nano silicon carbide abrasive, which comprises the steps of taking biomass carbon as a carbon source, tetraethoxysilane as a silicon source, ferric nitrate as a catalyst, preparing silicon carbide nano particles through carbothermic reduction, carrying out acid washing on the silicon carbide nano particles, and tempering at 1000-1200 ℃ to prepare the nano silicon carbide abrasive, wherein the biomass carbon is obtained by carbonizing a dried biomass raw material at a high temperature. The nano silicon carbide abrasive prepared by the invention has good grinding performance, can reach higher polishing rate, is suitable for the mechanical grinding and polishing process of semiconductors, and has low energy consumption and low cost in the preparation process.
Description
Technical Field
The invention relates to a preparation method of silicon carbide, in particular to a preparation method of a nano silicon carbide abrasive.
Background
The current mainstream semiconductor surface finishing method is a mechanical grinding polishing method, and the grinding materials used mainly comprise corundum, zirconia, silicon oxide and the like. However, this mechanical lapping method has a technical bottleneck, and the electronic information industry of high development requires semiconductors with higher surface finish, lower warpage and smaller residual stress, which results in finer abrasive grain size and better grinding performance. Compared with the abrasive, the silicon carbide has certain application in the field of semiconductor surface processing due to the advantages of good heat conductivity, strong corrosion resistance, high mechanical strength, large hardness and the like.
The traditional method for preparing the silicon carbide is to mix quartz sand with coke, add salt and wood dust, and obtain silicon carbide micro powder after heat treatment at a high temperature of about 2000 ℃, and the preparation method has high energy consumption, is difficult to control the granularity of the silicon carbide, and is not beneficial to the preparation of the high-efficiency silicon carbide abrasive. The silicon carbide particles prepared by the DC plasma technology have the particle size of 10-30 nm, but the preparation method has lower yield and is not beneficial to large-scale production. The silicon carbide particles prepared by using fossil fuel coal and sodium silicate as raw materials and ferric nitrate as a catalyst under the argon atmosphere at 1300 ℃ have the particle size of 20-60 nm, but the preparation method uses primary energy coal with limited reserves, which is not beneficial to sustainable development.
Chinese patent publication No. CN105016342a discloses a method for preparing silicon carbide micro-tube, which is prepared by carbothermal reduction of silicon solution gel, and the prepared silicon carbide particles are micro-sized, which is difficult to be applied to the grinding and polishing process of semiconductor.
Disclosure of Invention
Aiming at the technical requirements, the invention provides a preparation method of a nano silicon carbide abrasive, which mainly solves the problem of large-scale production of the silicon carbide abrasive meeting the requirements of grinding and polishing processing of the semiconductor surface.
The technical scheme of the invention is as follows: a preparation method of nano silicon carbide abrasive material uses biomass carbon as a carbon source, ethyl orthosilicate as a silicon source and ferric nitrate as a catalyst, silicon carbide nano particles are prepared through carbothermal reduction, the silicon carbide nano particles are pickled and tempered at 1000-1200 ℃ to prepare the nano silicon carbide abrasive material, and the biomass carbon is obtained by carbonizing dried biomass raw materials at high temperature.
Further, the method comprises the steps of: dissolving ferric nitrate in ethanol solution, uniformly stirring, adding biomass carbon, stirring and dispersing, adding tetraethoxysilane and oxalic acid solution for hydrolysis, adding hexamethylenetetramine solution into the hydrolyzed sol to obtain gel, drying the gel, heating to 1200-1500 ℃ under the protection of nitrogen, preserving heat, cooling to room temperature, heating to 600-900 ℃ and preserving heat to remove unreacted carbon, and finally obtaining the silicon carbide nano particles.
Further, the tempering temperature rising rate is 5-15 ℃/min, and the heat preservation time is 1-3 h.
Further, the biomass raw material is one of cotton, sisal hemp and peanut shells.
Further, the temperature of the biomass raw material is 600-800 ℃ and the time is 2-5 h after high-temperature carbonization.
Further, the mass ratio of the ethanol in the ethanol solution to the ferric nitrate is 80-120:1, and the mass ratio of the biomass carbon to the ferric nitrate is 10-15:1.
Further, the mass ratio of the tetraethoxysilane to the ferric nitrate is 40-60:1, the mass ratio of the oxalic acid solution to the ferric nitrate is 6-10:1, and the mass fraction of the concentrated acid in the oxalic acid solution is 3-4%.
Further, the gel is heated to 1200-1500 ℃ under the protection of nitrogen after being dried, and then is cooled to room temperature, wherein the heating rate is 5-15 ℃/min, and the heat preservation time is 6-10 h.
Further, in the process of heating to 600-900 ℃ and preserving heat to remove unreacted carbon, the heating rate is 5-15 ℃/min, and the preserving heat time is 2-5 h.
Further, the acid washing is performed by using mixed acid of hydrochloric acid and hydrofluoric acid, and the concentration ratio of the hydrochloric acid to the hydrofluoric acid is 0.5-1.5:1.
Compared with the prior art, the invention has the advantages that:
(1) The biomass carbon is used as a reaction raw material after being cleaned and carbonized, so that moisture, ash and impurities in the biomass carbon are removed, and the controllability of the raw material is ensured; in addition, a large number of micropore structures can be generated in the pre-carbonized biomass carbon, raw materials in subsequent reactions enter the micropores to increase the reaction rate and improve the reaction efficiency, and meanwhile, the tempering post-treatment is combined to achieve the effects of eliminating the internal stress of the abrasive and refining grains, so that the hardness, the cutting property and the crushing resistance of the nano silicon carbide abrasive are greatly improved, and the requirements of increasingly severe surface finish machining of semiconductors can be met.
(2) Biomass is adopted as a raw material for carbonization and is used as a carbon source, the heat treatment temperature in the preparation process is low, the raw material is environment-friendly, the source is wide, the price is low, the preparation cost of the abrasive is reduced, and the energy consumption is reduced.
Drawings
FIG. 1 is a scanning electron microscope image of the nano silicon carbide abrasive obtained in example 1.
FIG. 2 is a graph showing the particle size distribution of the nano silicon carbide abrasive obtained in example 1.
Detailed Description
The invention is further illustrated, but is not limited, by the following examples.
Example 1
Weighing washed and dried biomass cotton as a raw material, carbonizing in a tube furnace, carbonizing at 700 ℃ under the protection of nitrogen, and preserving heat for 3h to obtain a carbonized product of cotton.
Weighing 1 g ferric nitrate, dissolving in 100 g ethanol solution, and magnetically stirring for a period of time to obtain a uniform solution; the carbonized product of 12 g cotton was then added and magnetically stirred until equally dispersed, then 50 g ethyl orthosilicate and 8 g oxalic acid solution (3.5 wt%) were added to promote hydrolysis of the ethyl orthosilicate. After stirring 20 h thoroughly, the coagulation was promoted by adding 8 g hexamethylenetetramine solution. After solidification, 12 h is dried at 120 ℃.
And (3) fully grinding the dried product, placing the ground product into a tube furnace, heating to 1300 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, preserving heat for 8 h, and cooling to room temperature under the protection of nitrogen atmosphere. Subsequently, the sample was placed in a muffle furnace, heated to 700 ℃ at a heating rate of 10 ℃/min, and incubated for 3h, after which unreacted carbon was removed. Then the mixed acid of hydrochloric acid and hydrofluoric acid with the concentration ratio of 1:1 is used for washing out impurities. And finally, washing with water for several times, filtering, and freeze-drying to obtain the nano silicon carbide abrasive. Finally, the sample is placed in a muffle furnace, and is heated to 1100 ℃ at a heating rate of 10 ℃/min, and is subjected to tempering heat treatment by heat preservation 2 h. The prepared nano silicon carbide abrasive is light green powder; the scanning electron microscope image is shown in figure 1, and the nanometer silicon carbide has good dispersivity, which is beneficial to improving the grinding performance. As can be seen from fig. 2, the particle size of the nano silicon carbide is mainly distributed in the range of 40 to 90 nm. The abrasive and water prepared in example 1 were uniformly mixed at a mass ratio of 1:4, and then a round silicon wafer having a diameter of 10 cm was processed on a 1200-DB polisher (Chang macro-electromechanical), using a subara 600 polishing pad, a pressure of 4 psi, a lower disc rotation speed of 60 rpm, a polishing liquid flow rate of 12L/min, a polishing time of 120 min, a polishing rate of 6.5 μm/h, and a surface roughness of 0.35 nm.
Example 2
Weighing washed and dried biomass sisal hemp as a raw material, carbonizing in a tube furnace, carbonizing at 600 ℃ under the protection of nitrogen, and preserving heat for 2 h to obtain carbonized cotton products.
Weighing 1 g ferric nitrate, dissolving in an 80 g ethanol solution, and magnetically stirring for a period of time to obtain a uniform solution; the carbonized product of 10 g sisal was then added and magnetically stirred until equally dispersed, then 40 g ethyl orthosilicate and 6 g oxalic acid solution (3.0 wt%) were added to promote hydrolysis of ethyl orthosilicate. After stirring 20 h thoroughly, the solidification was promoted by adding 6 g hexamethylenetetramine solution. After solidification, 12 h is dried at 110 ℃.
And (3) fully grinding the dried product, placing the ground product into a tube furnace, heating to 1200 ℃ at a heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 6 h, and cooling to room temperature under the protection of nitrogen atmosphere. Subsequently, the sample was placed in a muffle furnace, heated to 700 ℃ at a heating rate of 5 ℃/min, and incubated for 3h, after which unreacted carbon was removed. Then the mixed acid of hydrochloric acid and hydrofluoric acid with the concentration ratio of 1:1 is used for washing out impurities. And finally, washing with water for several times, filtering, and freeze-drying to obtain the nano silicon carbide abrasive. Finally, the sample is placed in a muffle furnace, heated to 1000 ℃ at a heating rate of 5 ℃/min, and heat-insulated for 1 h for tempering heat treatment. The abrasive and water prepared in example 2 were uniformly mixed at a mass ratio of 1:4, and then a round silicon wafer having a diameter of 10 cm was processed on a 1200-DB polisher (Chang macro-electromechanical), using a subara 600 polishing pad, a pressure of 4 psi, a lower disc rotation speed of 60 rpm, a polishing liquid flow rate of 12L/min, a polishing time of 120 min, a polishing rate of 5.8 μm/h, and a surface roughness of 0.45 nm.
Example 3
Weighing washed and dried biomass peanut shells as raw materials, carbonizing in a tube furnace, carbonizing at 800 ℃ under the protection of nitrogen, and preserving heat for 5h to obtain carbonized cotton products.
Weighing 1 g ferric nitrate, dissolving in 120 g ethanol solution, and magnetically stirring for a period of time to obtain a uniform solution; the carbonized product of 15 g peanut hulls was then added and magnetically stirred until evenly dispersed, followed by 00 g ethyl orthosilicate and 10 g oxalic acid solution (4.0 wt%) to promote hydrolysis of the ethyl orthosilicate. After stirring 26, h thoroughly, the coagulation is promoted by adding 10, g hexamethylenetetramine solution. After solidification, 15 h is dried at 130 ℃.
And (3) fully grinding the dried product, placing the ground product into a tube furnace, heating to 1500 ℃ at a heating rate of 15 ℃/min under the protection of nitrogen, preserving heat for 10h, and cooling to room temperature under the protection of nitrogen atmosphere. Subsequently, the sample was placed in a muffle furnace, heated to 900 ℃ at a heating rate of 15 ℃/min, and kept at 5h, after which unreacted carbon was removed. Then the mixed acid of hydrochloric acid and hydrofluoric acid with the concentration ratio of 1:1 is used for washing out impurities. And finally, washing with water for several times, filtering, and freeze-drying to obtain the nano silicon carbide abrasive. Finally, the sample is placed in a muffle furnace, heated to 1200 ℃ at a heating rate of 15 ℃/min, and heat-insulated for 3h for tempering heat treatment. The abrasive and water prepared in example 3 were uniformly mixed at a mass ratio of 1:4, and then a round silicon wafer having a diameter of 10 cm was processed on a 1200-DB polisher (Chang macro-electromechanical), using a subara 600 polishing pad, a pressure of 4 psi, a lower disc rotation speed of 60 rpm, a polishing liquid flow rate of 12L/min, a polishing time of 120 min, a polishing rate of 5.9 μm/h, and a surface roughness of 0.42 nm.
Comparative example 1
Weighing washed and dried biomass cotton as a raw material, carbonizing in a tube furnace, carbonizing at 700 ℃ under the protection of nitrogen, and preserving heat for 3h to obtain a carbonized product of cotton.
Weighing 1 g ferric nitrate, dissolving in 100 g ethanol solution, and magnetically stirring for a period of time to obtain a uniform solution; the carbonized product of 12 g cotton was then added and magnetically stirred until equally dispersed, then 50 g ethyl orthosilicate and 8 g oxalic acid solution (3.5 wt%) were added to promote hydrolysis of the ethyl orthosilicate. After stirring 20 h thoroughly, the coagulation was promoted by adding 8 g hexamethylenetetramine solution. After solidification, 12 h is dried at 120 ℃.
And (3) fully grinding the dried product, placing the ground product into a tube furnace, heating to 1300 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, preserving heat for 8 h, and cooling to room temperature under the protection of nitrogen atmosphere. Subsequently, the sample was placed in a muffle furnace, heated to 700 ℃ at a heating rate of 10 ℃/min, and incubated for 3h, after which unreacted carbon was removed. Then the mixed acid of hydrochloric acid and hydrofluoric acid with the concentration ratio of 1:1 is used for washing out impurities. Finally, the nano silicon carbide abrasive is obtained through washing, filtering and freeze drying for a plurality of times. The abrasive material and water prepared in comparative example 1 were uniformly mixed at a mass ratio of 1:4, and then a round silicon wafer having a diameter of 10 cm was processed on a 1200-DB polisher (Chang macro-electromechanical), using a subar 600 polishing pad, a pressure of 4 psi, a lower disc rotation speed of 60 rpm, a polishing liquid flow rate of 12L/min, a polishing time of 120 min, a polishing rate of 5.4 μm/h, and a surface roughness of 0.39 nm.
Comparative example 2
Weighing 1 g ferric nitrate, dissolving in 100 g ethanol solution, and magnetically stirring for a period of time to obtain a uniform solution; then 60 g is added to clean the crushed powder of the dried cotton, the powder is stirred by magnetic force until the powder is equally dispersed, and then 50 g ethyl orthosilicate and 8 g oxalic acid solution (3.5 wt%) are added to promote the hydrolysis of the ethyl orthosilicate. After stirring 20 h thoroughly, the coagulation was promoted by adding 8 g hexamethylenetetramine solution. After solidification, 12 h is dried at 120 ℃.
And (3) fully grinding the dried product, placing the ground product into a tube furnace, heating to 1300 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, preserving heat for 8 h, and cooling to room temperature under the protection of nitrogen atmosphere. Subsequently, the sample was placed in a muffle furnace, heated to 700 ℃ at a heating rate of 10 ℃/min, and incubated for 3h, after which unreacted carbon was removed. Then the mixed acid of hydrochloric acid and hydrofluoric acid with the concentration ratio of 1:1 is used for washing out impurities. And finally, washing with water for several times, filtering, and freeze-drying to obtain the nano silicon carbide abrasive. Finally, the sample is placed in a muffle furnace, and is heated to 1100 ℃ at a heating rate of 10 ℃/min, and is subjected to tempering heat treatment by heat preservation 2 h. The abrasive and water prepared in comparative example 2 were uniformly mixed at a mass ratio of 1:4, and then a round silicon wafer having a diameter of 10 cm was processed on a 1200-DB polisher (Chang macro-electromechanical), using a subara 600 polishing pad, a pressure of 4 psi, a lower disc rotation speed of 60 rpm, a polishing liquid flow rate of 12L/min, a polishing time of 120 min, a polishing rate of 5.3 μm/h, and a surface roughness of 0.38 nm.
Comparative example 3
Weighing 1 g ferric nitrate, dissolving in 100 g ethanol solution, and magnetically stirring for a period of time to obtain a uniform solution; then 60 g is added to clean the crushed powder of the dried cotton, the powder is stirred by magnetic force until the powder is equally dispersed, and then 50 g ethyl orthosilicate and 8 g oxalic acid solution (3.5 wt%) are added to promote the hydrolysis of the ethyl orthosilicate. After stirring 20 h thoroughly, the coagulation was promoted by adding 8 g hexamethylenetetramine solution. After solidification, 12 h is dried at 120 ℃.
And (3) fully grinding the dried product, placing the ground product into a tube furnace, heating to 1300 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, preserving heat for 8 h, and cooling to room temperature under the protection of nitrogen atmosphere. Subsequently, the sample was placed in a muffle furnace, heated to 700 ℃ at a heating rate of 10 ℃/min, and incubated for 3h, after which unreacted carbon was removed. Then the mixed acid of hydrochloric acid and hydrofluoric acid with the concentration ratio of 1:1 is used for washing out impurities. Finally, the nano silicon carbide abrasive is obtained through washing, filtering and freeze drying for a plurality of times. The abrasive and water prepared in comparative example 3 were uniformly mixed at a mass ratio of 1:4, and then a round silicon wafer having a diameter of 10 cm was processed on a 1200-DB polisher (Chang macro-electromechanical), using a subara 600 polishing pad, a pressure of 4 psi, a lower disc rotation speed of 60 rpm, a polishing liquid flow rate of 12L/min, a polishing time of 120 min, a polishing rate of 4.2 μm/h, and a surface roughness of 0.41 nm.
Claims (10)
1. The preparation method of the nano silicon carbide abrasive is characterized in that biomass carbon is used as a carbon source, ethyl orthosilicate is used as a silicon source, ferric nitrate is used as a catalyst, silicon carbide nano particles are prepared through carbothermal reduction, the silicon carbide nano particles are subjected to acid washing and tempering at 1000-1200 ℃ to prepare the nano silicon carbide abrasive, and the biomass carbon is obtained by carbonizing a dried biomass raw material at a high temperature.
2. The method for preparing nano silicon carbide abrasive according to claim 1, comprising the steps of: dissolving ferric nitrate in ethanol solution, uniformly stirring, adding biomass carbon, stirring and dispersing, adding tetraethoxysilane and oxalic acid solution for hydrolysis, adding hexamethylenetetramine solution into the hydrolyzed sol to obtain gel, drying the gel, heating to 1200-1500 ℃ under the protection of nitrogen, preserving heat, and cooling to room temperature to obtain the silicon carbide nano particles.
3. The method for preparing nano silicon carbide abrasive according to claim 1, wherein the tempering temperature rise rate is 5-15 ℃/min and the heat preservation time is 1-3 h.
4. The method for preparing nano silicon carbide abrasive according to claim 1, wherein the biomass raw material is one of cotton, sisal hemp and peanut shell.
5. The method for preparing nano silicon carbide abrasive according to claim 1, wherein the temperature of the biomass raw material is 600-800 ℃ and the time is 2-5 h after high temperature carbonization.
6. The method for preparing nano silicon carbide abrasive according to claim 2, wherein the mass ratio of ethanol in the ethanol solution to the ferric nitrate is 80-120:1, and the mass ratio of biomass carbon to the ferric nitrate is 10-15:1.
7. The method for preparing nano silicon carbide abrasive according to claim 2, wherein the mass ratio of the ethyl orthosilicate to the ferric nitrate is 40-60:1, the mass ratio of the oxalic acid solution to the ferric nitrate is 6-10:1, and the mass fraction of the concentrated acid in the oxalic acid solution is 3-4%.
8. The method for preparing nano silicon carbide abrasive according to claim 2, wherein the gel is heated to 1200-1500 ℃ under nitrogen protection after drying, and then cooled to room temperature at a heating rate of 5-15 ℃/min for 6-10 h.
9. The method for preparing nano silicon carbide abrasive according to claim 2, wherein in the process of removing unreacted carbon by heating to 600-900 ℃ and maintaining the temperature, the heating rate is 5-15 ℃/min, and the maintaining time is 2-5 h.
10. The method for preparing nano silicon carbide abrasive according to claim 1, wherein the acid washing is performed by using a mixed acid of hydrochloric acid and hydrofluoric acid, and the concentration ratio of hydrochloric acid to hydrofluoric acid is 0.5-1.5:1.
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| EP0193970A2 (en) * | 1985-03-07 | 1986-09-10 | Elektroschmelzwerk Kempten GmbH | Method of producing sinterable powders of silicon carbide and/or boron carbide |
| CN101705076A (en) * | 2009-09-30 | 2010-05-12 | 汉寿金诚研磨材有限公司 | Method for producing green silicon carbide FEPA F P |
| CN104310402A (en) * | 2014-09-28 | 2015-01-28 | 渭南师范学院 | Method for preparing silicon carbide nanoparticles by use of agricultural waste biomass |
| CN109052404A (en) * | 2018-09-19 | 2018-12-21 | 鲁东大学 | A kind of preparation method of biomass carbon material in situ growth silicon carbide nano material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0193970A2 (en) * | 1985-03-07 | 1986-09-10 | Elektroschmelzwerk Kempten GmbH | Method of producing sinterable powders of silicon carbide and/or boron carbide |
| CN101705076A (en) * | 2009-09-30 | 2010-05-12 | 汉寿金诚研磨材有限公司 | Method for producing green silicon carbide FEPA F P |
| CN104310402A (en) * | 2014-09-28 | 2015-01-28 | 渭南师范学院 | Method for preparing silicon carbide nanoparticles by use of agricultural waste biomass |
| CN109052404A (en) * | 2018-09-19 | 2018-12-21 | 鲁东大学 | A kind of preparation method of biomass carbon material in situ growth silicon carbide nano material |
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