CN102874809A - Silicon carbide composite powder and preparation process thereof - Google Patents
Silicon carbide composite powder and preparation process thereof Download PDFInfo
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- CN102874809A CN102874809A CN2012104028153A CN201210402815A CN102874809A CN 102874809 A CN102874809 A CN 102874809A CN 2012104028153 A CN2012104028153 A CN 2012104028153A CN 201210402815 A CN201210402815 A CN 201210402815A CN 102874809 A CN102874809 A CN 102874809A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 239000000843 powder Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 32
- 239000010703 silicon Substances 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 24
- 239000008187 granular material Substances 0.000 claims description 22
- 238000005516 engineering process Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 235000013312 flour Nutrition 0.000 claims description 11
- 239000002699 waste material Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 5
- 239000003245 coal Substances 0.000 claims description 5
- 239000002802 bituminous coal Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 24
- 230000008569 process Effects 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 7
- 239000000919 ceramic Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000011159 matrix material Substances 0.000 description 10
- 229910052786 argon Inorganic materials 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 230000003014 reinforcing effect Effects 0.000 description 9
- 229910003978 SiClx Inorganic materials 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000012010 growth Effects 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 238000010010 raising Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- -1 pottery Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
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- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 239000011236 particulate material Substances 0.000 description 1
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Abstract
The invention relates to a silicon carbide composite powder and a preparation process thereof, the powder is a mixture of silicon carbide whiskers and silicon carbide micro-nano particles, and is prepared by uniformly mixing silicon and carbon raw materials and heating the mixture to 1100-1700 ℃ in vacuum or protective atmosphere, and the composition and the form of the silicon carbide composite powder are controlled by the property parameters of the carbon raw materials. The process is convenient to operate and suitable for industrial production. The prepared silicon carbide composite powder has good dispersibility, can be added into ceramics, metals and polymers to play a role in toughening and wear resistance, and can also be used as a high-quality raw material for preparing silicon carbide devices.
Description
Technical field
The present invention relates to a kind of silicon carbide composite powder body and preparation technology thereof, this powder can be used as the reinforcing and toughening agent of other matrix material, also can be used as starting material for the production of extraordinary silicon carbide device.
Background technology
Composition of material is the important means of novel material exploitation, that is by physics or chemical process two or more materials are combined and to form the better novel material of performance, its principle is to utilize the complementarity on performance between the material, improves targetedly intensity, toughness, stability of material etc.Matrix material has been used as the structure and function material and has been widely used in field (Liu Congcong, New Chemical Materials, 2012,40 (1): 1-4.) such as aerospace, national defence, the energy, traffic, electronics.
At present, toughness reinforcing and enhancement method comparatively commonly used is to add special fibre and hard particles (Huang Yong etc. in body material, the Jiangsu pottery, 2007,40 (2): 11-15.), wherein filamentary material has glass, pottery, asbestos, carbon, polymkeric substance, metal etc., and particulate material has oxide compound, carbide, alloy etc.Whisker is a kind of fabulous toughner, it be grow with the monocrystalline form formed a kind of than staple fibre, diameter be the micron or nano level.Because crystalline orientation structure of its height, the intensity of whisker is far above other fibers, by in a large number for the manufacture of high strength composite.In hundreds of crystal whisker materials that people have found so far, silicon carbide whisker intensity is high, high temperature resistant, corrosion-resistant, be most widely used, the toughness reinforcing application of matrix material in fields such as aviation, military affairs, metallurgy, chemical industry, automobile, sports equipment, cutting tool, nozzles of silicon carbide whisker gets more and more.The silicon-carbide particle of micro-or nano size, because particle is tiny, and have high strength, the characteristic such as high temperature resistant, it then is a kind of extraordinary matrix material toughener, such as Cui Yan (Cui Yan, material engineering, 2002,6:3-6.) introduced the application of silicon carbide ceramics reinforced aluminum matrix composites in aerospace.
The adding of whisker is obvious to the toughening effect of matrix material, but strengthening action is limited, even on the contrary may be because of density problem material strength reduction.On the other hand, hard particles (particularly tiny micro-or nano size particle) is remarkable to the matrix material strengthening action, but lacks toughening effect.In view of this, the collaborative enhancing of whisker and particle, the toughness reinforcing concern that causes people, its working method mainly is to be matrix material with reshaping in whisker and the particle adding base material respectively.At present, the enhancing toughner and the preparation method that had not only contained whisker but also contained micro-nano granules rarely have report, to the morphology Control of the two and the especially technical barrier that evenly distributes.
Summary of the invention
The present invention is directed to the existing problem of reinforcing and toughening material in the prior art, propose a kind of silicon carbide composite powder body and preparation technology thereof.This powder not only contains silicon carbide whisker but also contain the micro-nano carbon silicon carbide particle, and this powder strengthens and toughening functions having simultaneously as meterial additive.Preparation technology of the present invention can obtain silicon carbide whisker and particle simultaneously, and controls the two composition and form.
The present invention solves the problems of the technologies described above and is achieved through the following technical solutions:
A kind of silicon carbide composite powder body, i.e. the mixture of silicon carbide whisker and silicon carbide micro-nano granules, wherein Whisker Content is 1～80wt%, preferred 10～50wt%; Micro-nano granules content is 20～99wt%, preferred 50～90wt%.
Described silicon carbide micro-nano granules refers to particle diameter less than the granular carbonization silicon of 200um, can be one or more mixtures in nanometer, submicron or the micron-scale silicon carbide.
Described silicon carbide whisker and silicon carbide micro-nano granules composite granule, has advantages of cooperative reinforcing and toughening crystal whisker toughened and that particle strengthens, can be used as the strongthener that has the cooperative reinforcing and toughening effect in preparation metal, pottery and the polymer-based carbon composite diphase material, also can be used as the starting material of preparation high-performance silicon carbide ceramic component.
The preparation technology of silicon carbide composite powder body of the present invention is that silicon and carbon raw material are mixed, and the compound that mixes under vacuum or protective atmosphere, is heated to 1100～1700 ℃, and silicon and carbon reaction make described silicon carbide composite powder body.
The preparation method of this technique is silicon-carbon direct reaction method, and silicon and carbon raw material are heated to certain temperature after mixing under nonoxidizing atmosphere, and silicon and the carbon Formed SiClx that namely reacts comprises silicon carbide whisker and silicon carbide micro-nano granules.The reaction equation of its preparation method is: Si+C=SiC.
Employed carbon raw material comprises gac, carbon black, bituminous coal, hard coal or graphite among the preparation technology, perhaps two or more mixture wherein.Use the above-mentioned carbon raw material of unlike material or granular size in the preparation process, can regulate content and the quality of silicon carbide whisker in the prepared composite granule, thereby make the silicon carbide composite powder body of different compositions and form.Unlike material carbon raw material, Whisker Content is the highest in the composite granule of gac preparation, and other carbon raw material is followed successively by hard coal and bituminous coal, graphite, carbon black from high to low; The carbon raw material of identical material, particle is larger, and Whisker Content is higher in the composite granule of preparation, and whisker is more even, and straight brilliant rate is higher.Its reason is that the silicon-carbon direct reaction prepares silicon carbide composite powder body, and silicon and carbon reaction can generate crystal whisker-shaped or granular silicon carbide; The space that the growth needs of silicon carbide whisker is certain, the growing space of whisker is provided by the gap of stock yard in the inventive method.The carbon of unlike material is made the carbon raw material, and each is different for the volume density of mixing raw material, and volume density is less, and the gap in the raw material is just more, and for the growth of silicon carbide whisker provides more spaces, Whisker Content is just higher in the powder of preparation; Loose porous such as gac, relative minimum with the volume density of the compound of silicon, Whisker Content is just higher in the powder of preparation.Simultaneously, the silicon carbide whisker growth shaping is relevant with the size in stock yard gap, and the particle of carbon raw material is too thin, and the stock yard gap is too little, and the whisker growth moulding is limited, and quality (whisker length and homogeneity) is just relatively poor, and content is also low; And particle is larger, the demand of the enough whisker growths in stock yard gap, and prepared whisker quality is high, and good uniformity, content are also high.
Employed silicon can be silica flour or various material among the silicon carbide composite powder body preparation technology of the present invention, the silica flour that reclaims in the waste mortar that preferred sun power or the cutting of semi-conductor silicon chip line produce or the waste mortar.The composition of the silica flour that reclaims in waste mortar or the waste mortar is mainly silicon carbide micro-powder and silica flour; as the silicon source prepare the process of silicon carbide composite powder body and pure silicon powder and carbon reacting phase with; silica flour wherein and carbon react under certain condition and generate crystal whisker-shaped and granular carbonization silicon; and wherein original silicon carbide micro-powder does not change in preparation process, and mixing with the silicon carbide whisker that generates and silicon carbide micro-nano granules becomes silicon carbide composite powder body.
In described silicon and the carbon raw material compound, the mol ratio of silicon and carbon between 1:0.6～1:5, preferred 1:1.2～1:2.
More abundant for silicon is contacted with carbon, thus make reaction more complete, must mix fully raw material, the method for mixing can be ball milling or mechanically mixing.
Reaction can be carried out the purification process such as silica removal, de-carbon to going out furnace charge after finishing, and obtains the high silicon carbide composite powder body of purity.
The preparation technology of silicon carbide composite powder body of the present invention, temperature of reaction are 1100～1700 ℃, and the soaking time under this temperature of reaction is 1～30h.For preventing that reactant from oxidation at high temperature occuring, building-up process needs to carry out under vacuum condition or in the protective atmosphere, and protective atmosphere comprises the nonoxidizing atmospheres such as argon gas, hydrogen, nitrogen.
By technique scheme, the present invention has following advantages at least:
Silicon carbide composite powder body of the present invention comprises silicon carbide whisker and silicon carbide micro-nano granules, as strongthener, has advantages of simultaneously whisker and particle cooperative reinforcing and toughening, can improve intensity and the toughness of matrix material.Its preparation method technique is simple, and is easy to operate, is fit to large-scale industrialization production; And pass through in the preparation to use the carbon of unlike material and granular size to be the carbon raw material, can regulate content and the quality of prepared silicon carbide whisker, make the silicon carbide composite powder body of different compositions and form.The good dispersity of the silicon carbide composite powder body of the inventive method preparation, and the ratio of two kinds of constituents is adjustable, for the cooperative reinforcing and toughening of matrix material provides cheaply strongthener, the starting material of high-quality are provided simultaneously for preparation high-performance silicon carbide ceramic component.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Description of drawings
The silicon carbide composite powder body SEM photo of Fig. 1 embodiment 1 preparation.
The silicon carbide composite powder body SEM photo of Fig. 2 embodiment 2 preparations.
The silicon carbide composite powder body SEM photo of Fig. 3 embodiment 3 preparations.
The silicon carbide composite powder body SEM photo of Fig. 4 embodiment 4 preparations.
Embodiment
Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, silicon carbide composite powder body that foundation the present invention is proposed and preparation method thereof by embodiment, and is described with reference to the accompanying drawings as rear.
Embodiment 1
Selecting 200 order silica flours and 8 purpose wood quality gacs is silicon source and carbon raw material, the two is prepared burden according to the mol ratio of Si:C=1:1.2, and mix and become compound.Compound is packed in the corundum crucible, and cover lid is put into and is incubated 3h after electric furnace is heated to 1500 ℃, makes silicon and the carbon Formed SiClx that reacts.In the process of heat temperature raising, insulation and cooling, pass into continuously argon gas in body of heater, argon pressure is 0.1MPa, and flow is 20ml/min.Reaction finishes, after sample is with the furnace temperature cooling, come out of the stove, then the method for using sodium hydroxide solution to clean heated oxide de-carbon in silica removal and the air is carried out purification process to going out furnace charge, and silicon carbide whisker content is about 50wt% in the composite granule of preparation, and the SEM photo as shown in Figure 1.
Embodiment 2
Selecting 200 order silica flours and 200 purpose wood quality gacs is silicon source and carbon raw material, the two is prepared burden according to the mol ratio of Si:C=1:1.2, and mix and become compound.Compound is packed in the corundum crucible, and cover lid is put into and is incubated 3h after electric furnace is heated to 1500 ℃, makes silicon and the carbon Formed SiClx that reacts.In the process of heat temperature raising, insulation and cooling, pass into continuously argon gas in body of heater, argon pressure is 0.1MPa, and flow is 20ml/min.Reaction finishes, after sample is with the furnace temperature cooling, come out of the stove, then the method for using sodium hydroxide solution to clean heated oxide de-carbon in silica removal and the air is carried out purification process to going out furnace charge, and silicon carbide whisker content is about 30wt% in the composite granule of preparation, and the SEM photo as shown in Figure 2.
Embodiment 3
Selecting 200 order silica flours and 200 purpose coal mass active carbons is silicon source and carbon raw material, the two is prepared burden according to the mol ratio of Si:C=1:1.2, and mix and become compound.Compound is packed in the corundum crucible, and cover lid is put into and is incubated 3h after electric furnace is heated to 1500 ℃, makes silicon and the carbon Formed SiClx that reacts.In the process of heat temperature raising, insulation and cooling, pass into continuously argon gas in body of heater, argon pressure is 0.1MPa, and flow is 20ml/min.Reaction finishes, after sample is with the furnace temperature cooling, come out of the stove, then the method for using sodium hydroxide solution to clean heated oxide de-carbon in silica removal and the air is carried out purification process to going out furnace charge, and silicon carbide whisker content is about 10wt% in the composite granule of preparation, and the SEM photo as shown in Figure 3.
Embodiment 4
Selecting silica flour and 30nm carbon black is silicon source and carbon raw material, the two is prepared burden according to the mol ratio of Si:C=1:1.2, and the method that adopts mechanically mixing of will preparing burden mixes and becomes compound.Compound is packed in the corundum crucible, and cover lid is put into and is incubated 3h after electric furnace is heated to 1500 ℃, makes silicon and the carbon Formed SiClx that reacts.In the process of heat temperature raising, insulation and cooling, pass into continuously argon gas in body of heater, argon pressure is 0.1MPa, and flow is 20ml/min.Reaction finishes, and comes out of the stove after sample is with the furnace temperature cooling, then uses the method for heated oxide in sodium hydroxide solution cleaning and the air to carry out purification process to going out furnace charge, and silicon carbide whisker content is about 3wt% in the composite granule of preparation, and the SEM photo as shown in Figure 4.
Embodiment 5
The waste silicon powder that produces with silicon chip of solar cell line cutting and 8 purpose wood quality gacs are prepared burden according to the mol ratio of Si:C=1:1.5 as raw materials, and mix and become compound.Compound is packed in the corundum crucible, and cover lid is put into and is incubated 4h after electric furnace is heated to 1400 ℃, makes silicon and the carbon Formed SiClx that reacts.In the process of heat temperature raising, insulation and cooling, keeping in the body of heater is vacuum state, and vacuum tightness is 1Pa.Reaction finishes, and takes out after sample is down to room temperature with furnace temperature, and the method for then using sodium hydroxide solution to clean heated oxide de-carbon in silica removal and the air is carried out purification process to going out furnace charge, makes silicon carbide composite powder body.
Claims (10)
1. a silicon carbide composite powder body is characterized in that, this silicon carbide composite powder body is the mixture of silicon carbide whisker and silicon carbide micro-nano granules.
2. silicon carbide composite powder body according to claim 1 is characterized in that, the content of silicon carbide whisker is 1～80wt% in the described silicon carbide composite powder body, and the content of micro-nano granules is 20～99wt%.
3. silicon carbide composite powder body according to claim 2 is characterized in that, the content of silicon carbide whisker is 10～50wt% in the described silicon carbide composite powder body, and the content of micro-nano granules is 50～90wt%.
4. according to claim 1,2 or 3 described silicon carbide composite powder bodies, it is characterized in that the particle diameter of described silicon carbide micro-nano granules≤200 μ m.
5. the preparation technology of the described silicon carbide composite powder body of claim 1; it is characterized in that, silicon and carbon raw material are mixed, with compound under vacuum or protective atmosphere; be heated to 1100～1700 ℃, silicon and carbon reaction make described silicon carbide composite powder body.
6. the preparation technology of silicon carbide composite powder body according to claim 5 is characterized in that, employed material carbon is one or more in gac, carbon black, bituminous coal, hard coal, the graphite.
7. the preparation technology of silicon carbide composite powder body according to claim 5 is characterized in that, described preparation technology adopts following one or both modes, controls composition and the form of silicon carbide composite powder body by the carbon raw material:
1) be followed successively by by the carbon raw material: gac hard coal or bituminous coal graphite the order of carbon black selects the carbon raw material, improves the content of silicon carbide whisker in the composite granule;
2) increase the carbon raw material particle size, improve content and the straight brilliant rate of silicon carbide whisker in the composite granule.
8. the preparation technology of silicon carbide composite powder body according to claim 5 is characterized in that, employed raw silicon is silica flour or material.
9. the preparation technology of silicon carbide composite powder body according to claim 8 is characterized in that, employed raw silicon is the waste mortar that sun power or the cutting of semi-conductor silicon chip line produce, or the silica flour that reclaims from waste mortar.
10. the preparation technology of silicon carbide composite powder body according to claim 5 is characterized in that, in the compound of described silicon and carbon raw material, the mol ratio of silicon/carbon is between 1: 0.6～5.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104495847A (en) * | 2014-12-17 | 2015-04-08 | 北京科技大学 | Production method of nanometer iron carbide powder |
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| CN106314462B (en) * | 2016-08-30 | 2018-08-07 | 江苏同庆车辆配件有限公司 | A kind of box car composite floor board |
| CN107587187A (en) * | 2017-08-04 | 2018-01-16 | 海南大学 | A kind of method that SiC Nanometer Whiskers are prepared using crystalline silicon cutting waste mortar |
| CN107587187B (en) * | 2017-08-04 | 2020-06-16 | 海南大学 | Method for preparing silicon carbide nano crystal whiskers by using crystalline silicon cutting waste mortar |
| CN115044842A (en) * | 2021-06-24 | 2022-09-13 | 珠海亿特立新材料有限公司 | Production system for preparing high-specific-rigidity aluminum silicon carbide structural part |
| WO2023277711A1 (en) * | 2021-06-30 | 2023-01-05 | Universidad Católica San Pablo | Method for producing an agent for mechanical reinforcement of materials and a reinforced hydraulic cement mortar obtained by means of said method |
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