CN102616781A - Method for preparing SiC ultrafine powder - Google Patents
Method for preparing SiC ultrafine powder Download PDFInfo
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- CN102616781A CN102616781A CN2012100951559A CN201210095155A CN102616781A CN 102616781 A CN102616781 A CN 102616781A CN 2012100951559 A CN2012100951559 A CN 2012100951559A CN 201210095155 A CN201210095155 A CN 201210095155A CN 102616781 A CN102616781 A CN 102616781A
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- ultrafine powder
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims 2
- 235000021355 Stearic acid Nutrition 0.000 claims 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims 2
- 229920001223 polyethylene glycol Polymers 0.000 claims 2
- 230000001681 protective effect Effects 0.000 claims 2
- 239000008117 stearic acid Substances 0.000 claims 2
- 238000004886 process control Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000000713 high-energy ball milling Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000007769 metal material Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- -1 polyoxyethylene Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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- Crushing And Grinding (AREA)
Abstract
本发明涉及一种制备SiC超细粉体的方法，属于无机非金属材料制备技术领域。是采用高能球磨的方法，通过高能球磨工艺的控制，最终获得粒度达到亚微米级，甚至粒度能达到纳米级的SiC粉体。本方法解决了现有制备方法存在的工艺复杂、成本高、效率低以及粉体粒度分布不均匀等缺点，可大批量生产。The invention relates to a method for preparing SiC ultrafine powder, which belongs to the technical field of preparation of inorganic non-metallic materials. It adopts the method of high-energy ball milling, and through the control of high-energy ball milling process, finally obtains SiC powder whose particle size reaches submicron level, and even the particle size can reach nanometer level. The method solves the disadvantages of complex process, high cost, low efficiency, uneven particle size distribution of powder and the like existing in the existing preparation method, and can be mass-produced.
Description
Technical field
The present invention relates to a kind of method of using high-energy ball milling to prepare the SiC superfine powder, belong to the ceramic preparing technical field.
Background technology
Silit is a kind of strong covalent bond compound; Compare with other material; Silit has excellent mechanical property (high firmness, HS, high-wearing feature, strong creep resistance etc.) and chemicalstability (high temperature resistant, corrosion-resistant, radiation hardness etc.), and thermal conductivity height, the coefficient of expansion are little, also have the excellent photoelectric performance; Therefore, obtained using widely in aerospace, machinery, metallurgy, the energy, environmental protection, chemical industry, medical science, electronics and field such as sophisticated technology such as height such as military project grade.
At present, preparation SiC powder method has a lot, like microwave method, carbon reduction method, polymkeric substance thermal decomposition method, sol-gel method, gas-phase reaction sedimentation, plasma method and mechanical crushing method etc.Sol-gel method is a kind of wet chemistry method for preparing nanoparticle; Ultimate principle is that the chemical reagent with liquid is mixed with metal inorganic salt or metal alkoxide precursor; Precursor is dissolved in and forms uniform solution in the solvent; Solute and solvent form colloidal sol after producing hydrolysis or alcoholysis, and colloidal sol can transfer gel to after long-time placement or drying.Generally contain a large amount of liquid phases in the gel, need remove liquid medium, and thermal treatment forms the particulate of respective substance compound under far below the conventional sintering temperature through extraction or evaporation.Colloidal sol transfers gel to and needs long time in this method, and the production cycle is oversize, unsuitable large-scale industrial production.Mechanical crushing method is to pulverize through stirrer or vibration mill etc., because the extreme hardness of SiC material, the minimum limit of size that makes ball milling SiC material is 0.6～0.7 μ m normally.The ball milling grain diameter more hour, the agglomeration between the particle will be serious more, thereby reduced the ball milling effect.Yet the SiC powder that chemical relatively legal system is equipped with, the SiC powder footpath distribution range of existing mechanical comminuting method preparation is wide, is difficult for guaranteeing the stability and the consistence of quality product.Therefore how using mechanical process to prepare the SiC superfine powder becomes a difficult problem that needs to be resolved hurrily, needs badly and develop grinding process efficiently.
In CN 102020471A patent, having reported a kind of method for preparing silit, is that SiC powder and nano SiC granule are prepared burden by mass ratio, places the water ball milling 8～12 hours, at last with mixed slurry 60 ℃～80 ℃ oven dry in baking oven.The raw material that this method is used is complicated, and operation is more, and cost is high, and wet-grinding technology and relative device need be dried, and energy expenditure is bigger.
In CN 1636870A patent, having reported a kind of method for preparing silit, is that Si source, carbon source and alcohol are mixed by mass ratio, carries out high temperature cabonization processing and high temperature sintering then and handles.The raw material that this method is used is complicated, complex process, and need to handle 1～12 hour at 600 ℃～1000 ℃ high temperature cabonizations, to handle 0.5～8 hour at 1200 ℃～2000 ℃ high temperature sinterings, this has increased the input of cost greatly, has prolonged the cycle of experiment simultaneously.
Summary of the invention
The present invention provides a kind of method of the SiC of preparation superfine powder, and this method technology is simple, cost is low, efficient is high and diameter of particle is evenly distributed.
Technical scheme of the present invention is to be raw material with the SiC powder directly, adopts the method for high-energy ball milling to prepare the SiC superfine powder.Concrete grammar passes through as follows: by ball material mass ratio is that 5:1～40:1 takes by weighing Stainless Steel Ball and SiC powder; And take by weighing the technology controlling and process agent of certain mass; Powder, technology controlling and process agent and steel ball are packed in the horizontal agitating ball mill of high energy, feed shielding gas, according to 200 rev/mins～1000 rev/mins of drum'ss speed of rotation; Ball milling 1～10 hour promptly obtains the SiC superfine powder.
The median size D of said SiC powder
50Be 5 μ m～115 μ m.
The diameter of said Stainless Steel Ball is 1mm～5mm.
Said technology controlling and process agent is Triple Pressed Stearic Acid and polyoxyethylene glycol, and the Triple Pressed Stearic Acid add-on is 0.1%～5.0wt% of SiC powder, and the add-on of polyoxyethylene glycol is 0.1～3.0wt% of SiC powder.
The shielding gas that charges in the said mechanical milling process is argon gas or nitrogen.
Advantage of the present invention and positively effect are:
(1) overcome that the traditional mechanical disintegrating process is complicated, efficient is low, the diameter of particle distribution range is wide, classification is difficult, be difficult for guaranteeing the stability and the conforming shortcoming of quality product, prepared the superfine powder of particle diameter at 0.35～0.55 μ m.
(2) the technology controlling and process agent can better disperse and refinement powder in the high-energy ball milling process, can prevent the reunion of powder, and the size-grade distribution of superfine powder is more even, purity is higher.
(3) suitability for industrialized production, technology is simple, efficient is high, constant product quality and with low cost.
Embodiment
Below in conjunction with embodiment the present invention is done to further describe, but the invention is not restricted to the following stated scope.
Embodiment 1: present embodiment prepares the concrete steps of SiC superfine powder to be passed through as follows:
At first taking by weighing SiC powder and the diameter that median size is 5 μ m～115 μ m according to ball material mass ratio 5:1 is the 5mm Stainless Steel Ball; Take by weighing 1.0wt% Triple Pressed Stearic Acid and 0.5wt% polyoxyethylene glycol again; Powder, technology controlling and process agent and steel ball are packed in the horizontal agitating ball mill of high energy, charge into argon shield.It is that 600 rev/mins, ball milling time are 4h that the ball milling parameter of ball mill is set to rotational speed of ball-mill.After ball milling finishes, take by weighing the SiC powder behind a small amount of ball milling, add ethanol and be mixed with dilute suspension, record the median size D of submicron order SiC
50Be 0.50 μ m.
Embodiment 2: present embodiment prepares the concrete steps of SiC superfine powder to be passed through as follows:
At first taking by weighing SiC powder and the diameter that median size is 5～115 μ m according to ball material mass ratio 30:1 is the Stainless Steel Ball of 3mm; Take by weighing 5wt% Triple Pressed Stearic Acid and 3wt% polyoxyethylene glycol again; Powder, technology controlling and process agent and steel ball are packed in the horizontal agitating ball mill of high energy, charge into nitrogen protection.It is that 200 rev/mins, ball milling time are 10h that the ball milling parameter of ball mill is set to rotational speed of ball-mill.After ball milling finishes, take by weighing the SiC powder behind a small amount of ball milling, add water and be mixed with dilute suspension, record the median size D of submicron order SiC
50Be 0.39 μ m.
Embodiment 3: present embodiment prepares the concrete steps of SiC superfine powder to be passed through as follows:
At first taking by weighing SiC powder and the diameter that median size is 5～115 μ m according to ball material mass ratio 40:1 is the Stainless Steel Ball of 1mm; Take by weighing 0.1wt% Triple Pressed Stearic Acid and 0.1wt% polyoxyethylene glycol again; Powder, technology controlling and process agent and steel ball are packed in the horizontal agitating ball mill of high energy, charge into nitrogen protection.It is that 1000 rev/mins, ball milling time are 1h that the ball milling parameter of ball mill is set to rotational speed of ball-mill.After ball milling finishes, take by weighing the SiC powder behind a small amount of ball milling, add water and be mixed with dilute suspension, record the median size D of submicron order SiC
50Be 0.42 μ m.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100951559A CN102616781A (en) | 2012-04-01 | 2012-04-01 | Method for preparing SiC ultrafine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100951559A CN102616781A (en) | 2012-04-01 | 2012-04-01 | Method for preparing SiC ultrafine powder |
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| Publication Number | Publication Date |
|---|---|
| CN102616781A true CN102616781A (en) | 2012-08-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012100951559A Pending CN102616781A (en) | 2012-04-01 | 2012-04-01 | Method for preparing SiC ultrafine powder |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111229274A (en) * | 2020-03-13 | 2020-06-05 | 浙江工业大学 | A kind of high-energy mechanical ball milling SiC Lewis acid catalyst and its preparation method and its preparation method and application |
| CN112479716A (en) * | 2020-12-14 | 2021-03-12 | 山田研磨材料有限公司 | Extrusion molding process for pressureless sintering silicon carbide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4571331A (en) * | 1983-12-12 | 1986-02-18 | Shin-Etsu Chemical Co., Ltd. | Ultrafine powder of silicon carbide, a method for the preparation thereof and a sintered body therefrom |
| CN1636870A (en) * | 2004-12-30 | 2005-07-13 | 清华大学 | A kind of preparation method of SiC micron powder |
-
2012
- 2012-04-01 CN CN2012100951559A patent/CN102616781A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4571331A (en) * | 1983-12-12 | 1986-02-18 | Shin-Etsu Chemical Co., Ltd. | Ultrafine powder of silicon carbide, a method for the preparation thereof and a sintered body therefrom |
| US4571331B1 (en) * | 1983-12-12 | 1988-09-27 | ||
| CN1636870A (en) * | 2004-12-30 | 2005-07-13 | 清华大学 | A kind of preparation method of SiC micron powder |
Non-Patent Citations (2)
| Title |
|---|
| 吴清军等: "高能球磨法制备SiC/Al复合材料", 《材料热处理技术》 * |
| 赵麦群等: "《材料化学处理工艺与设备》", 30 September 2011 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111229274A (en) * | 2020-03-13 | 2020-06-05 | 浙江工业大学 | A kind of high-energy mechanical ball milling SiC Lewis acid catalyst and its preparation method and its preparation method and application |
| CN111229274B (en) * | 2020-03-13 | 2022-08-19 | 浙江工业大学 | High-energy mechanical ball-milling SiC Lewis acid catalyst and preparation method and application thereof |
| CN112479716A (en) * | 2020-12-14 | 2021-03-12 | 山田研磨材料有限公司 | Extrusion molding process for pressureless sintering silicon carbide |
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Application publication date: 20120801 |