CN101092305A - Method for preparing Sialon hollow ball - Google Patents
Method for preparing Sialon hollow ball Download PDFInfo
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- CN101092305A CN101092305A CN 200610017975 CN200610017975A CN101092305A CN 101092305 A CN101092305 A CN 101092305A CN 200610017975 CN200610017975 CN 200610017975 CN 200610017975 A CN200610017975 A CN 200610017975A CN 101092305 A CN101092305 A CN 101092305A
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Abstract
This invention relates to a method for preparing hollow sialon spheres. The method comprises: (1) uniformly mixing hollow fly ash microbeads and carbon powder at a wt. ratio of (68-74):(32-36), and sieving; (2) heating at a rate of 0-300 deg.C/h in high-purity nitrogen atmosphere (flow rate = 0.05-0.2 L/min), 5 deg.C/min within 300-1000 deg.C, 3 deg.C/min within 1000-1300 deg.C, and 2 deg.C/min within 1300-1500 deg.C, keeping the temperature for 4-6 h, and cooling to obtain powder; (3) keeping the powder in a 750-850 deg.C oxidation furnace for 4-5 to remove residual carbon and obtain hollow sialon spheres. The hollow sialon spheres have purity of 90 plus and minus 5%, and particle sizes larger than 43 mu.m. The method has such advantages as no need for auxiliary materials, no need for acid washing, simple process, abundant raw materials, and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of Sialon hollow ball, belong to the material technology field.
Background technology
At present, match is grand as a kind of new engineering material, all shows up prominently at industrial sectors such as metallurgy, aviation, chemical industry, machineries: as make motor car engine element, metal-cutting machine tool, various wear-resisting high-temperature component and overflow mould, elevated-temperature seal part and bearing etc.
In synthetic Sialon powder research with industrial residue, wherein more is to utilize coal gangue or the synthetic beta-Sialon of flyash, basic skills and principle are: coal gangue is mixed according to a certain percentage with reductive agent, make it reach tight admixture, add certain catalyzer,, in the nitrogen atmosphere High Temperature Furnaces Heating Apparatus of certain flow rate, carry out reduction nitridation through granulation, moulding, synthetic required product, its reaction process are comparatively complicated.
Chinese invention patent discloses a kind of name and has been called: a kind of method for preparing beta-sialon, the patent No. is: 02146408.1 patent of invention, proposition is made raw material with coal gangue, coal dust, nitrogen, and synthesis technique is: the sintering of raw material fine grinding → batching → mixing on request → adding wedding agent mixing → mechanical pressing → drying → under reduction nitridation atmosphere synthesize → cools off → comes out of the stove → and chemically examines; All raw materials are all through being finely ground to granularity≤0.08mm, proportioning raw materials: join carbon by the required carbon amount of chemical reaction excessive 5%; Wedding agent: syrup; Atmosphere: nitrogen; The sintering synthesis temperature: 1400 ℃ were burnt 8 hours, rose to 1600 ℃ of insulations 2 hours again.Finished product thing phase: be mainly the grand phase (about 95%) of match, chemical formula is Si
3Al
3O
3N
5All the other are about 4% SiC and a small amount of glassy phase.
Flyash can be used as a kind of synthetic Sialon starting material of cheapness, yet a large amount of in the flyash spherical granular material with multiple function---microballon is not utilized effectively.
Summary of the invention:
The object of the present invention is to provide a kind ofly to prepare the method for Sialon hollow ball,, simplify production technique to reduce raw materials cost with fly ash micro-sphere.
To achieve these goals, technical program of the present invention lies in adopting a kind of preparation method of Sialon hollow ball, may further comprise the steps:
(1) selecting coal fly ash hollow micro bead for use is raw material, is that the mixed of 68-74: 32-26 is even by weight ratio with coal fly ash hollow micro bead and carbon dust, sieves;
(2) be under the high pure nitrogen atmosphere of 0.05-0.2L/min at flow, freely heat up when being 0-300 ℃ with the heat-up rate, in the time of 300-1000 ℃ with 5 ℃/min, in the time of 1000-1300 ℃ with 3 ℃/min, speed with 2 ℃/min in the time of 1300-1500 ℃ is warming up to 1300-1500 ℃, be incubated 4-6 hour, furnace cooling gets powder;
(3) powder with preparation is incubated 4-5 hour in 750-850 ℃ oxidized still, removes remaining carbon, can obtain Sialon hollow ball.
Described coal fly ash hollow micro bead comprises that weight percent is the SiO of 40-65%
2, weight percent is the Al of 20-40%
2O
3And weight percent is the oxide compound of the iron of 1.0-5.0%.
Described microballon density p is 1.9-2.3g/cm
3, particle diameter＞43 μ m.
Described carbon dust can be activated carbon or carbon black.
The median size of described carbon dust＜5 μ m.
The purity of described nitrogen＞99.999%.
Because method of the present invention is to be raw material with the fly ash micro-sphere, carbon (activated carbon or carbon black) is as reductive agent, directly prepare the Sialon hollow ball body with carbothermic method, use fly ash micro-sphere as raw material, not only raw materials cost is low, production technique is simple, and the Sai Long for preparing is hollow ball, can be used as packing materials such as fire-resistant, heat insulation, protection, enhancing.
Utilize method of the present invention can obtain the grand spheroid of hollow matches purity 90 ± 5%, granularity＞43 μ m, need not add any auxiliary adjustment material, need not the pickling deironing, preparation technology is simple, and raw material sources are extensive, and are cheap.Present method can be prepared purity at 90 ± 5% Sialon hollow ball; be expected to become automobile industry and the war industry fine is high-strength, the strongthener of the high filler loading capacity of low density, high temperature resistant friction; this both can reduce cost; given play to its abundant raw material, turned waste into wealth, cheap advantage, help environment protection.If the present invention carries out suitable top layer nitrogenize, reinforcement and keeps its spheroidal particle constant microballon, can become the spherical Sialon functional materials of high-strength, high hard, high temperature resistant friction and high filler loading capacity.Sialon hollow ball body of the present invention is because its distinctive hollow structure, not only has the performances such as wear-resisting, high temperature resistant, stable performance of the grand powder of match, also has characteristics such as low density, light weight, can be used as inertia sprayed protection material, or high temperature resistant protective material etc.
Description of drawings
Fig. 1 is the shape appearance figure of microballon after the nitrogenize in first kind of embodiment of the present invention;
Fig. 2 is the sectional view of microballon after the nitrogenize among Fig. 1;
Fig. 3 is a microballon shape appearance figure after the nitrogenize in second kind of embodiment of the present invention.
Embodiment
Present embodiment is to adopt Henan Feng Yuan Industrial Co., Ltd.＞77 μ m fly ash micro-spheres, and its main chemical compositions is as follows:
| Al 2O 3 | SiO 2 | Fe 2O 3 | CaO | MgO | |
| Duck river microballon | 28.76％ | 60.80％ | 2.30％ | 2.20％ | 0.91％ |
(1) selecting Feng Yuan industry coal fly ash hollow micro bead (particle diameter＞77 μ m) for use is raw material, and coal fly ash hollow micro bead and carbon dust (activated carbon or carbon black) are mixed by 74: 26 weight proportions, sieves;
(2) at flow be the high pure nitrogen (N of 0.05-0.2L/min
2＞99.999%) under the atmosphere, be warming up to 1500 ℃, be incubated 6 hours, furnace cooling gets powder;
(3) powder with preparation is incubated 4-5 hour in 800 ℃ of oxidized stills, removes remaining carbon, can obtain β-Sialon hollow ball.
Embodiment 2
Adopt Yuzhou of Henan power plant＞43 μ m fly ash micro-spheres, its main chemical compositions is as follows:
| Al 2O 3 | SiO 2 | Fe 2O 3 | CaO | MgO | |
| The Yuzhou microballon | 26.61％ | 58.47％ | 4.45％ | 4.40％ | 1.28％ |
(1) selecting Yuzhou of Henan power plant＞43 μ m for use is raw material, and coal fly ash hollow micro bead and carbon dust (activated carbon or carbon black) is even by the mixed of 74: 26 (totally 100 parts), sieves;
(2) at flow be the high pure nitrogen (N of 0.05-0.2L/min
2＞99.999%) under the atmosphere, be warming up to 1450 ℃, be incubated 6 hours, furnace cooling gets powder;
(3) powder with preparation is incubated 4～5 hours in 800 ℃ of oxidized stills, removes remaining carbon, can obtain main component and be 0 '-hollow ball of Sai Long and β-Sai Long.
The grand spherome surface of formed match is coarse behind carbothermal reduction-nitridation as seen from Figure 1, but spherical morphology can be kept substantially; Fig. 2 shows that it is a hollow structure; Fig. 3 shows, among the embodiment 2 after the fly ash micro-sphere nitrogenize the grand ball spherical morphology of formed match remain intact.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (6)
1, a kind of preparation method of Sialon hollow ball is characterized in that: may further comprise the steps:
(1) selecting coal fly ash hollow micro bead for use is raw material, is that the mixed of 68-74: 32-26 is even by weight ratio with coal fly ash hollow micro bead and carbon dust, sieves;
(2) be under the high pure nitrogen atmosphere of 0.05-0.2L/min at flow, freely heat up when being 0-300 ℃ with the heat-up rate, in the time of 300-1000 ℃ with 5 ℃/min, in the time of 1000-1300 ℃ with 3 ℃/min, speed with 2 ℃/min in the time of 1300-1500 ℃ is warming up to 1300-1500 ℃, be incubated 4-6 hour, furnace cooling gets powder;
(3) powder with preparation is incubated 4-5 hour in 750-850 ℃ oxidized still, removes remaining carbon, can obtain Sialon hollow ball.
2, the preparation method of Sialon hollow ball according to claim 1 is characterized in that: described coal fly ash hollow micro bead comprises that weight percent is the SiO of 40-65%
2And weight percent is the Al of 20-40%
2O
3And weight percent is the oxide compound of the iron of 1.0-5.0%.
3, the preparation method of Sialon hollow ball according to claim 2 is characterized in that: described microballon density p is 1.9-2.3g/cm
3, particle diameter＞43 μ m.
4, the preparation method of Sialon hollow ball according to claim 1 is characterized in that: described carbon dust can be activated carbon or carbon black.
5, the preparation method of Sialon hollow ball according to claim 4 is characterized in that: the median size of described carbon dust＜5 μ m.
6, the preparation method of Sialon hollow ball according to claim 1 is characterized in that: the purity of described nitrogen＞99.999%.
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|---|---|---|---|
| CNB2006100179750A CN100445236C (en) | 2006-06-19 | 2006-06-19 | Method for preparing Sialon hollow ball |
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|---|---|---|---|
| CNB2006100179750A CN100445236C (en) | 2006-06-19 | 2006-06-19 | Method for preparing Sialon hollow ball |
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| CN101092305A true CN101092305A (en) | 2007-12-26 |
| CN100445236C CN100445236C (en) | 2008-12-24 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613206A (en) * | 2009-07-17 | 2009-12-30 | 宁波工程学院 | A kind of preparation method of alumina hollow structure |
| CN103102160A (en) * | 2013-03-13 | 2013-05-15 | 桂林理工大学 | Microwave sintering method for preparing beta-Sialon powder by using coal ash |
| CN106495714A (en) * | 2016-10-31 | 2017-03-15 | 武汉科技大学 | A kind of cellular titanium calcium aluminate hollow ball and preparation method thereof |
| CN110078521A (en) * | 2019-05-13 | 2019-08-02 | 西北工业大学 | A kind of submicron order silicon nitride hollow microsphere and preparation method |
| CN112209739A (en) * | 2020-09-29 | 2021-01-12 | 郑州大学 | Lightweight high-strength magnesium aluminate spinel hollow sphere porous ceramic and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1157347C (en) * | 2001-09-14 | 2004-07-14 | 中国科学院上海硅酸盐研究所 | Low cost process of synthesizing sialon ceramic powder |
| CN1181013C (en) * | 2001-12-24 | 2004-12-22 | 徐利华 | Process for preparing composition 'Sailong' from industrial waste dregs by in-situ synthesis |
-
2006
- 2006-06-19 CN CNB2006100179750A patent/CN100445236C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613206A (en) * | 2009-07-17 | 2009-12-30 | 宁波工程学院 | A kind of preparation method of alumina hollow structure |
| CN103102160A (en) * | 2013-03-13 | 2013-05-15 | 桂林理工大学 | Microwave sintering method for preparing beta-Sialon powder by using coal ash |
| CN106495714A (en) * | 2016-10-31 | 2017-03-15 | 武汉科技大学 | A kind of cellular titanium calcium aluminate hollow ball and preparation method thereof |
| CN106495714B (en) * | 2016-10-31 | 2019-04-26 | 武汉科技大学 | A kind of honeycomb titanium calcium aluminate hollow sphere and preparation method thereof |
| CN110078521A (en) * | 2019-05-13 | 2019-08-02 | 西北工业大学 | A kind of submicron order silicon nitride hollow microsphere and preparation method |
| CN110078521B (en) * | 2019-05-13 | 2021-06-11 | 西北工业大学 | Submicron silicon nitride hollow microsphere and preparation method thereof |
| CN112209739A (en) * | 2020-09-29 | 2021-01-12 | 郑州大学 | Lightweight high-strength magnesium aluminate spinel hollow sphere porous ceramic and preparation method thereof |
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|---|---|
| CN100445236C (en) | 2008-12-24 |
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Granted publication date: 20081224 Termination date: 20100619 |