CN101357763A - Method for preparing high pure superfine powder - Google Patents
Method for preparing high pure superfine powder Download PDFInfo
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- CN101357763A CN101357763A CNA200710012329XA CN200710012329A CN101357763A CN 101357763 A CN101357763 A CN 101357763A CN A200710012329X A CNA200710012329X A CN A200710012329XA CN 200710012329 A CN200710012329 A CN 200710012329A CN 101357763 A CN101357763 A CN 101357763A
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Abstract
The invention relates to a preparation method for high-purity superfine SiC powder, which comprises the following steps: (1) burdening; (2) preparing La2O3 slurry; (3) preparing the mixed slurry formed by SiO2 and C; (4) preparing the mixed slurry formed by SiO2, C and micro La2O3; (5) preparing the mixed powder formed by SiO2, C and micro La2O3; (6) synthesizing SiC; (7) decarbonization. The method which is suitable for industrialized scale production has the advantages of low cost, simple process and high yield.
Description
Technical field: the present invention relates to a kind of preparation method of technical field of inorganic nonmetallic materials SiC ceramic powder, particularly relate to the preparation method of high pure superfine ceramic powder.
Background technology: the preparation method of high pure superfine powder mainly comprises methods such as colloidal sol-gel, induced with laser gas-phase chemical reaction, plasma body.Sol-gel processing is a kind of wet chemistry method of preparation nanoparticle, its 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, can be converted into gel through long-time placement or drying treatment colloidal sol.In gel, usually also contain a large amount of liquid phases, need to remove liquid medium by extraction or evaporation, and heat treatment under far below traditional sintering temperature, form at last the particulate of respective substance compound.Though colloidal sol-coacervation can synthesize the SiC powder of high pure and ultra-fine, becoming gel by colloidal sol needs the very long production cycle, thereby sol-gel processing is not suitable for the commercial scale production high pure superfine powder.Induced with laser gas-phase chemical reaction method is to utilize the laser beam irradiation of high power laser in reactant gases, reactant gases is by the strong absorption to incident laser, gas molecule or atom obtain heating, activation in moment, after utmost point short period of time reaction gases molecule or the needed temperature of atom acquisition chemical reaction, finish processes such as reaction, nucleation, cohesion, growth rapidly, thereby make the nanoparticle of respective substance.Plasma body is the 4th kind of state that material exists, and it is made up of ionized conducting gas, comprising six kinds of typical particles, the i.e. atom of the atom of electronics, positive ion, negative ion, excited state or molecule, ground state or molecule and photon.Being in corpuscle under the plasmoid can very fast acquisition high temperature by interacting, Gao Han, high activity.Therefore utilize plasma space as heating, evaporation and reaction compartment, can prepare the SiC nanoparticle.Though plasma body and induced with laser gas-phase chemical reaction method all can be prepared the SiC nano-powder of high pure and ultra-fine, but equipment used costliness, complex manufacturing, yield poorly and reason such as expensive raw material price, cause costing an arm and a leg of high pure superfine powder, seriously limited the promotion and application of SiC nano ceramics matrix material.The method of commercial scale production SiC powder remains the carbothermic reduction method at present, but the SiC powder granule that this method is produced is thick, only reaches micron or sub-micrometer scale, is not suitable for the commercial scale production of high pure superfine powder.
Summary of the invention: the invention provides a kind of preparation method of high pure superfine powder, this method suitability for industrialized scale production and cost is low, technology is simple, output is high.
The preparation method of high pure superfine powder is:
(1) batching: raw material is amorphous silica nano-powder SiO
2, carbon nano powder C and micro-high-purity La
2O
3Nano-powder.Wherein, SiO
2Mass percent be 59.7wt.%, the mass percent of C is 40wt.%, La
2O
3Mass percent be 0.3wt.%.Utilize the precise electronic balance to take by weighing respectively an amount of amorphous silica nano-powder SiO according to the mentioned component proportioning
2, carbon nano powder C and micro-high-purity La
2O
3Nano-powder, stand-by.An amount of acetone soln of weighing is stand-by again.
(2) preparation La
2O
3Slurry: with the high-purity La of above-mentioned load weighted trace
2O
3Nano-powder is put into the beaker of certain capacity, pours a small amount of acetone soln into again, constantly carry out magnetic agitation, and the minimum 60min of mixing time can make by micro-La
2O
3The slurry that nano-powder consists of, stand-by.
(3) preparation SiO
2Mixed slurry with the C formation: with above-mentioned load weighted amorphous silica nano-powder SiO
2Pour in the ball grinder, in this ball grinder, pour load weighted carbon nano powder C again into, stir, pour proper amount of acetone solution again into, after stirring with glass stick, put into ZrO again with glass stick
2Abrading-ball, ZrO
2The total mass of abrading-ball and raw material mixed powder (SiO
2With the C powder) the ratio of total mass be 5: 1, capping, ball milling can obtain by SiO after 24 hours
2With the mixed slurry that C constitutes, stand-by.
(4) preparation SiO
2, C and micro-La
2O
3The mixed slurry that consists of: with the above-mentioned SiO that is equipped with
2The ball grinder of the mixed slurry that consists of with C is opened, then with the La that has prepared in the above-mentioned beaker
2O
3Slurry is poured in this ball grinder, does not run into the ball grinder wall, uses a small amount of acetone soln cleaning glass rod and beaker again, cleaning solution is together poured in the ball grinder into capping, ball milling 24 hours.Namely obtain by SiO behind the ball mill mixing
2, C and micro-La
2O
3The mixed slurry that consists of, stand-by.
(5) preparation SiO
2, C and micro-La
2O
3The mixed powder that consists of: with above-mentioned ball milling good by SiO
2, C and micro-La
2O
3The mixed slurry that consists of is together with ZrO
2Abrading-ball is together poured in the pallet, and puts into drying baker and dry, and bake out temperature is 65～75 ℃, takes out abrading-ball after the oven dry, can obtain by SiO
2, C and micro-La
2O
3The mixed powder that consists of.
(6) synthetic SiC: with above-mentioned drying good by SiO
2, C and micro-La
2O
3The mixed powder that consists of is put into graphite and is pushed away boat, and the graphite that above-mentioned mixed powder will be housed again pushes away boat and puts into carbon shirt-circuiting furnace and heat; Must extract the air in the carbon shirt-circuiting furnace burner hearth out with vavuum pump earlier when adding thermal synthesis, pass into again argon gas; Argon flow amount is 1.5ml/min, and the heating synthesis temperature is 1450-1600 ℃, and synthetic temperature retention time is 60-90min; Programming rate is 10 ℃/min.
(7) carbonization treatment: behind the end of synthesis, the product S iC powder that obtains is put into chamber type electric resistance furnace, insulation 60-90min just can remove residual carbon under 650 ℃.
Raw material of the present invention mainly is amorphous silica nano-powder SiO
2, carbon nano powder C and micro-high-purity La
2O
3Nano-powder., plasma preparation method synthetic with colloidal sol-gel, induced with laser gas phase compared, these invention raw material sources are extensive, cheap, simultaneously by the production of ball milling machinery mixing method, do not need expensive equipment, the generation cycle is short, output is big, thereby cost is low, technology is simple, output is high, the suitability for industrialized scale production.The chemical reaction of synthesizing high pure superfine SiC powder is the chemical reaction between gas phase SiO and the solid phase C.Utilize carbon nano powder C as the forming core core of SiC, add armorphous nano SiO
2Increase reactivity, reduce reaction temperature, and add micro-high-purity La
2O
3Nano-powder further reduces reaction temperature as catalyst, Reaction time shorten, thereby this invention can obtain high pure superfine powder.
Embodiment:
Embodiment 1
(1) batching: difference weighing amorphous silica nano-powder SiO
259.7g, carbon nano powder 40g and micro-high-purity La
2O
3Nano-powder 0.3g, stand-by; Weighing 400ml acetone soln is stand-by again.
(2) preparation La
2O
3Slurry: with above-mentioned load weighted micro-La
2O
3Nano-powder is put into the beaker of 50ml, pours the 20ml acetone soln into again, and magnetic agitation 60min can make by micro-La
2O
3The slurry that nano-powder consists of, stand-by.
(3) preparation SiO
2Mixed slurry with the C formation: with above-mentioned load weighted amorphous silica nano-powder SiO
2Pour in the ball grinder, in this ball grinder, pour load weighted carbon nano powder C again into, stir, pour the 350ml acetone soln again into, after stirring with glass stick, put into the ZrO of 500g again with glass stick
2Abrading-ball, capping, ball milling 24 hours can obtain by SiO
2With the mixed slurry that C constitutes, stand-by.
(4) preparation SiO
2, C and micro-La
2O
3The mixed slurry that consists of: with the above-mentioned SiO that is equipped with
2The ball grinder of the mixed slurry that consists of with C is opened, then with the La that has prepared in the above-mentioned beaker
2O
3Slurry is poured in this ball grinder, notes not running into the ball grinder wall, uses 30ml acetone soln cleaning glass rod and beaker again, together pours in the ball grinder capping, ball milling 24 hours into together with cleaning solution.Namely obtain by SiO behind the ball mill mixing
2, C and micro-La
2O
3The mixed slurry that consists of, stand-by.
(5) preparation SiO
2, C and micro-La
2O
3The mixed powder that consists of: the SiO that above-mentioned ball milling is good
2, C and micro-La
2O
3The mixed slurry that consists of is together with ZrO
2Abrading-ball is together poured in the pallet, and puts into drying baker and dry, and bake out temperature is 70 ℃, takes out abrading-ball after the oven dry, can obtain by SiO
2, C and micro-La
2O
3The mixed powder that consists of.
(6) synthetic SiC: with above-mentioned drying good by SiO
2, C and micro-La
2O
3The mixed powder that consists of is put into graphite and is pushed away boat, and the graphite that above-mentioned mixed powder will be housed again pushes away boat and puts into carbon shirt-circuiting furnace and heat; With vavuum pump the air in the carbon shirt-circuiting furnace burner hearth is extracted out earlier when adding thermal synthesis, passed into again argon gas; Argon flow amount is 1.5ml/min, and synthetic heating-up temperature is 1500 ℃, and synthetic temperature retention time is 90min; Programming rate is 10 ℃/min.
(7) carbonization treatment: behind the end of synthesis, the SiC powder that obtains is put into chamber type electric resistance furnace, insulation 60min just can remove residual carbon under 650 ℃.
Embodiment 2
(1) batching: difference weighing amorphous silica nano-powder SiO
2298.6g, carbon nano powder 200g and micro-high-purity La
2O
3Nano-powder 1.4g, stand-by; Weighing 2000ml acetone soln is stand-by again.
(2) preparation La
2O
3Slurry: with above-mentioned load weighted micro-La
2O
3Nano-powder is put into the beaker of 200ml, pours the 100ml acetone soln into again, and magnetic agitation 60min can make by micro-La
2O
3The slurry that nano-powder consists of, stand-by.
(3) preparation SiO
2Mixed slurry with the C formation: with above-mentioned load weighted amorphous silica nano-powder SiO
2Pour in the ball grinder, in this ball grinder, pour load weighted carbon nano powder C again into, stir, pour the 1800ml acetone soln again into, after stirring with glass stick, put into the ZrO of 2500g again with glass stick
2Abrading-ball, capping, ball milling 24 hours can obtain by SiO
2With the mixed slurry that C constitutes, stand-by.
(4) preparation SiO
2, C and micro-La
2O
3The mixed slurry that consists of: with the above-mentioned SiO that is equipped with
2The ball grinder of the mixed slurry that consists of with C is opened, then with the La that has prepared in the above-mentioned beaker
2O
3Slurry is poured in this ball grinder, notes not running into the ball grinder wall, uses 100ml acetone soln cleaning glass rod and beaker again, together pours in the ball grinder capping, ball milling 24 hours into together with cleaning solution.Namely obtain by SiO behind the ball mill mixing
2, C and micro-La
2O
3The mixed slurry that consists of, stand-by.
(5) preparation SiO
2, C and micro-La
2O
3The mixed powder that consists of: the SiO that above-mentioned ball milling is good
2, C and micro-La
2O
3The mixed slurry that consists of is together with ZrO
2Abrading-ball is together poured in the pallet, and puts into drying baker and dry, and bake out temperature is 75 ℃, takes out abrading-ball after the oven dry, can obtain by SiO
2, C and micro-La
2O
3The mixed powder that consists of.
(6) synthetic SiC: with above-mentioned SiO of having dried
2, C and micro-La
2O
3The mixed powder that consists of is put into graphite and is pushed away boat, and the graphite that above-mentioned mixed powder will be housed again pushes away boat and puts into carbon shirt-circuiting furnace and heat; With vavuum pump the air in the carbon shirt-circuiting furnace burner hearth is extracted out earlier when adding thermal synthesis, passed into again argon gas; Argon flow amount is 1.5ml/min, and synthetic heating-up temperature is 1500 ℃, and synthetic temperature retention time is 90min; Programming rate is 10 ℃/min.
(7) carbonization treatment: behind the end of synthesis, the SiC powder that obtains is put into chamber type electric resistance furnace, insulation 90min just can remove residual carbon under 650 ℃.
Claims (1)
1, a kind of preparation method of high pure superfine powder is characterized in that: the preparation method of high pure superfine powder is:
(1) batching: raw material is amorphous silica nano-powder SiO
2, carbon nano powder C and micro-high-purity La
2O
3Nano-powder; Wherein, SiO
2Mass percent be 59.7wt.%, the mass percent of C is 40wt.%, La
2O
3Mass percent be 0.3wt.%; Utilize the precise electronic balance to take by weighing respectively an amount of amorphous silica nano-powder SiO according to the mentioned component proportioning
2, carbon nano powder C and micro-high-purity La
2O
3Nano-powder, stand-by; An amount of acetone soln of weighing is stand-by again;
(2) preparation La
2O
3Slurry: with the high-purity La of above-mentioned load weighted trace
2O
3Nano-powder is put into the beaker of certain capacity, pours a small amount of acetone soln into again, constantly carry out magnetic agitation, and the minimum 60min of mixing time can make by micro-La
2O
3The slurry that nano-powder consists of, stand-by;
(3) preparation SiO
2Mixed slurry with the C formation: with above-mentioned load weighted amorphous silica nano-powder SiO
2Pour in the ball grinder, in this ball grinder, pour load weighted carbon nano powder C again into, stir, pour proper amount of acetone solution again into, after stirring with glass stick, put into ZrO again with glass stick
2Abrading-ball, ZrO
2The total mass of abrading-ball and raw material mixed powder (SiO
2With the C powder) the ratio of total mass be 5: 1, capping, ball milling can obtain by SiO after 24 hours
2With the mixed slurry that C constitutes, stand-by;
(4) preparation SiO
2, C and micro-La
2O
3The mixed slurry that consists of; With the above-mentioned SiO that is equipped with
2The ball grinder of the mixed slurry that consists of with C is opened, then with the La that has prepared in the above-mentioned beaker
2O
3Slurry is poured in this ball grinder, does not run into the ball grinder wall, uses a small amount of acetone soln cleaning glass rod and beaker again, cleaning solution is together poured in the ball grinder into capping, ball milling 24 hours.Namely obtain by SiO behind the ball mill mixing
2, C and micro-La
2O
3The mixed slurry that consists of, stand-by;
(5) preparation SiO
2, C and micro-La
2O
3The mixed powder that consists of: with above-mentioned ball milling good by SiO
2, C and micro-La
2O
3The mixed slurry that consists of is together with ZrO
2Abrading-ball is together poured in the pallet, and puts into drying baker and dry, and bake out temperature is 65～75 ℃, takes out abrading-ball after the oven dry, can obtain by SiO
2, C and micro-La
2O
3The mixed powder that consists of;
(6) synthetic SiC: with above-mentioned drying good by SiO
2, C and micro-La
2O
3The mixed powder that consists of is put into graphite and is pushed away boat, and the graphite that above-mentioned mixed powder will be housed again pushes away boat and puts into carbon shirt-circuiting furnace and heat; Must extract the air in the carbon shirt-circuiting furnace burner hearth out with vavuum pump earlier when adding thermal synthesis, pass into again argon gas; Argon flow amount is 1.5ml/min, and the heating synthesis temperature is 1450-1600 ℃, and synthetic temperature retention time is 60-90min; Programming rate is 10 ℃/min;
(7) carbonization treatment: behind the end of synthesis, the product S iC powder that obtains is put into chamber type electric resistance furnace, insulation 60-90min just can remove residual carbon under 650 ℃.
Priority Applications (1)
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|---|---|---|---|
| CNA200710012329XA CN101357763A (en) | 2007-07-31 | 2007-07-31 | Method for preparing high pure superfine powder |
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030534A (en) * | 2010-11-09 | 2011-04-27 | 浙江大学 | Method for preparing silicon carbide ceramic |
| CN103360098A (en) * | 2012-04-05 | 2013-10-23 | 深圳光启创新技术有限公司 | Metamaterial substrate and preparation method thereof |
| CN106430212A (en) * | 2016-11-15 | 2017-02-22 | 扬州中天利新材料股份有限公司 | Method for industrialized mass production of silicon carbide powder |
| CN111205071A (en) * | 2018-11-21 | 2020-05-29 | 宝山钢铁股份有限公司 | Low-temperature-sintered aluminum-zirconium-carbon sliding plate containing nano silica fume and preparation method thereof |
| CN111908472A (en) * | 2020-06-30 | 2020-11-10 | 山东天岳先进材料科技有限公司 | Silicon carbide powder doped with rare earth elements and preparation method and application thereof |
| WO2022000997A1 (en) * | 2020-06-30 | 2022-01-06 | 山东天岳先进科技股份有限公司 | Rare earth element-doped silicon carbide powder |
| CN114249594A (en) * | 2020-09-21 | 2022-03-29 | 山东硅纳新材料科技有限公司 | Preparation process of superfine silicon carbide powder |
| CN116023145A (en) * | 2022-12-29 | 2023-04-28 | 湖南福德电气有限公司 | Preparation method of silicon carbide series piezoresistor |
-
2007
- 2007-07-31 CN CNA200710012329XA patent/CN101357763A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030534A (en) * | 2010-11-09 | 2011-04-27 | 浙江大学 | Method for preparing silicon carbide ceramic |
| CN102030534B (en) * | 2010-11-09 | 2013-01-02 | 浙江大学 | Method for preparing silicon carbide ceramic |
| CN103360098A (en) * | 2012-04-05 | 2013-10-23 | 深圳光启创新技术有限公司 | Metamaterial substrate and preparation method thereof |
| CN103360098B (en) * | 2012-04-05 | 2016-03-09 | 深圳光启高等理工研究院 | A kind of metamaterial substrate and preparation method thereof |
| CN106430212A (en) * | 2016-11-15 | 2017-02-22 | 扬州中天利新材料股份有限公司 | Method for industrialized mass production of silicon carbide powder |
| CN106430212B (en) * | 2016-11-15 | 2017-08-22 | 扬州中天利新材料股份有限公司 | A kind of method for industrializing large-scale production silicon carbide powder |
| CN111205071A (en) * | 2018-11-21 | 2020-05-29 | 宝山钢铁股份有限公司 | Low-temperature-sintered aluminum-zirconium-carbon sliding plate containing nano silica fume and preparation method thereof |
| CN111908472A (en) * | 2020-06-30 | 2020-11-10 | 山东天岳先进材料科技有限公司 | Silicon carbide powder doped with rare earth elements and preparation method and application thereof |
| WO2022000997A1 (en) * | 2020-06-30 | 2022-01-06 | 山东天岳先进科技股份有限公司 | Rare earth element-doped silicon carbide powder |
| CN114249594A (en) * | 2020-09-21 | 2022-03-29 | 山东硅纳新材料科技有限公司 | Preparation process of superfine silicon carbide powder |
| CN116023145A (en) * | 2022-12-29 | 2023-04-28 | 湖南福德电气有限公司 | Preparation method of silicon carbide series piezoresistor |
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