CN102924089A - Method for preparing beta-sialon ceramic powders through using coal ash and kaolin - Google Patents
Method for preparing beta-sialon ceramic powders through using coal ash and kaolin Download PDFInfo
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- CN102924089A CN102924089A CN2012105084216A CN201210508421A CN102924089A CN 102924089 A CN102924089 A CN 102924089A CN 2012105084216 A CN2012105084216 A CN 2012105084216A CN 201210508421 A CN201210508421 A CN 201210508421A CN 102924089 A CN102924089 A CN 102924089A
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- kaolin
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- sialon
- flyash
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Abstract
The invention discloses a method for preparing beta-sialon ceramic powders with different Z values through using coal ash and kaolin. The coal ash and the kaolin are mixed according to the molar ratio of the raw materials that Si to Al equals to (1.08-1.85):1; the mixture is then mixed with activated carbon according to the mass ratio of 100: (25-45); the raw materials after ball milling and drying are thermally insulated for 2-8hours at the temperature of 1400-1550 DEG C under the condition of flowing nitrogen atmosphere; and then, the raw materials are thermally insulated for 3 hours in a muffle furnace of 750 DEG C so as to remove the residual carbon, so that the beta-sialon ceramic powders with different Z values is obtained. Through applying industrial solid waste and natural minerals, the costs of the raw materials are lowered, the production technology is simplified, the environmental pollution is relieved, and an effective method is provided for comprehensively utilizing the industrial solid waste and natural minerals in the advanced ceramic material field; and the Z value of beta-sialon is regulated through regulating the ratio of the two raw materials of the coal ash and the kaolin, so that the beta-sialon ceramic powder with high purity (96-98wt%) and the Z value being between 1.9 and 3.1 can be obtained.
Description
Technical field
The present invention relates to a kind of is the method that raw material prepares pottery, particularly a kind of method for preparing different Z value beta-Sialon ceramic powders with flyash and kaolin with industrial solid castoff.
Background technology
(general general formula is Si to beta-Sialon
6-zAl
zO
zN
8-z0＜Z≤4.2 wherein) be the most excellent a kind of of Sialon pottery family performance, have good erosion resistance, resistance to sudden heating, hot strength and chemical stability etc., and with molten metal extraordinary blending is arranged, be difficult for being corroded, be a kind of high performance ceramic material of excellence, be widely used in fields such as fire-resistant, corrosion-resistant, machinofacture.
The industrial preparative method commonly used of beta-Sialon material is with high-purity SiO
2, Al
2O
3, AlN, Si
3N
4Deng to be raw material synthetic by high temperature solid state reaction, expensive cost of material causes too high preparation cost, has limited the widespread use of beta-Sialon material; On the other hand, as the solid waste coal ash that firepower electrical plant is discharged, the annual total amount of discharging of China is greater than 100,000,000 tons, if reasonably do not develop, not only contaminate environment also causes the wasting of resources, although in the existing Application and Development of building material field, added value of product is not high; Kaolin is a kind of resourceful clay mineral resource and cheap; The main ingredient of flyash and natural kaolin is SiO
2And Al
2O
3Be in close proximity to the chemical constitution of beta-Sialon, be suitable for synthetic beta-Sialon stupalith, therefore, employing industrial solid castoff flyash and low-cost raw mineral materials kaolin are that the beta-Sialon material of raw material processability excellence has broad application prospects.
In forefathers' research work, publication number provides " method of the synthetic high-purity sialon material of a kind of Coaseries kaolin " for the Chinese invention patent of CN1594216A, publication number provides " utilizing the method for aluminium ash and the standby Sialon ceramic powder of coal ash for manufacturing " for the Chinese invention patent of CN101325256A, these two kinds of methods take flyash or kaolin as raw material, can not be regulated the beta-Sialon powder that raw material forms to obtain to have different Z values merely.
Summary of the invention
The objective of the invention is based on to industrial solid castoff flyash and the kaolinic comprehensive utilization of natural matter, provide a kind of take flyash and kaolin as compound material, by the method for the standby different Z value beta-Sialon ceramic powders of carbothermal reduction-nitridation legal system.
Concrete steps are:
(1) with levigate rear 0.074 mm sieve of crossing respectively of flyash and kaolin, be that 1.08 ~ 1.85:1 joins and gets flyash and the kaolin that sieves according to the Si:Al mol ratio again, then with agate mortar with join flyash and the kaolin pre-mixing of getting, make mixture.
(2) mixture that step (1) is made mixes according to mass ratio 100:25 ~ 45 with the reductive agent gac, makes mixture.
(3) mixture that step (2) is made 12 hours mixings of planetary ball mill ball milling, wherein drum's speed of rotation is 400 rev/mins, abrading-ball is zirconia ball, ball-milling medium is dehydrated alcohol, abrading-ball: material: the dehydrated alcohol mass ratio is 20:1:1.5, places slip common loft drier lower dry 24 hours in 80 ℃ after the ball milling end.
(4) powder after step (3) oven dry is put into the corundum porcelain boat mid-in the electron tubes type atmosphere furnace, be that 0.5 liter/min of clock, purity are under 99.9% the flowing nitrogen atmosphere at flow, first be warmed up to 1000 ℃ take temperature rise rate as 8 ℃/minute from room temperature, rise to 1400 ~ 1550 ℃ with 5 ℃/minute of temperature rise rates again, be incubated 4 ~ 8 hours, naturally cool to 500 ℃ and stop to pass into nitrogen, continue to be cooled to room temperature.
(5) powder that step (4) is made is heated to 750 ℃ in retort furnace, be incubated 3 hours and remove remaining charcoal, namely makes the beta-Sialon ceramic powder of high-purity different z values after the cooling.
The present invention is by the application to industrial solid castoff and natural mineral, reduce raw materials cost, simplify production technique, alleviate environmental pollution, comprehensive utilization in the advanced ceramics material field provides an effective way for industrial solid castoff and natural mineral raw, and regulate and control the Z value of beta-Sialon by the proportioning of regulating flyash and two kinds of raw materials of kaolin, can obtain high purity (96 ~ 98wt%), the Z value is 1.9 ~ 3.1 beta-Sialon ceramic powder.
Embodiment
In the following example, used flyash is from the power station, Guilin, and kaolin is from Beihai Fisheries Base Guangxi Province, and its chief component is (mass percent):
| Composition | SiO 2 | Al 2O 3 | Fe 2O 3 | TiO 2 | CaO | MgO | K 2O | Na 2O | Loss on ignition |
| Flyash | 55.95 | 25.71 | 1.31 | 2.77 | 3.73 | 1.48 | 2.84 | 1.16 | 4.61 |
| Kaolin | 46.86 | 36.85 | 0.69 | 0.17 | 0.050 | 0.18 | 0.74 | 0.059 | 13.51 |
Embodiment 1:
(1) with flyash and levigate rear 0.074 mm sieve of crossing respectively of kaolin, be that 1.72:1 (the Si:Al mol ratio is 1.5:1) joins and gets flyash and the kaolin that sieves according to flyash and kaolinic mass ratio again, then with agate mortar with join flyash and the kaolin pre-mixing of getting, make mixture.
(2) mixture that step (1) is made mixes according to mass ratio 100:30 with the reductive agent gac, makes mixture.
(3) mixture that step (2) is made 12 hours mixings of planetary ball mill ball milling, wherein drum's speed of rotation is 400 rev/mins, abrading-ball is zirconia ball, ball-milling medium is dehydrated alcohol, abrading-ball: material: the dehydrated alcohol mass ratio is 20:1:1.5, after ball milling finishes slip place common loft drier in 80 ℃ lower dry 24 hours, obtain the mixture powder.
(4) it is mid-in the electron tubes type atmosphere furnace that the mixture powder that step (3) is made is put into the corundum porcelain boat, be that 0.5 liter/min of clock, purity are under 99.9% the flowing nitrogen atmosphere at flow, first be warmed up to 1000 ℃ take temperature rise rate as 8 ℃/minute from room temperature, rise to 1450 ℃ with 5 ℃/minute of temperature rise rates again, be incubated 6 hours, naturally cool to 500 ℃ and stop to pass into nitrogen, continue to be cooled to room temperature.
(5) powder that step (4) is made is heated to 750 ℃ in retort furnace, be incubated 3 hours and remove remaining charcoal, namely makes high-purity beta-Sialon ceramic powder after the cooling.
The beta-Sialon ceramic powder that makes is through X-ray diffraction analysis, wherein Si
3Al
3O
3N
5(z=3) beta-Sialon content 98%, the microstructure of Sialon powder presents fibrous.
Embodiment 2:
(1) with flyash and levigate rear 0.074 mm sieve of crossing respectively of kaolin, be that 5.92:1 (the Si:Al mol ratio is 1.7:1) joins and gets flyash and the kaolin that sieves according to flyash and kaolinic mass ratio again, then with agate mortar with join flyash and the kaolin pre-mixing of getting, make mixture.
(2) mixture that step (1) is made mixes according to mass ratio 100:38 with the reductive agent gac, makes mixture.
(3) mixture that step (2) is made 12 hours mixings of planetary ball mill ball milling, wherein drum's speed of rotation is 400 rev/mins, abrading-ball is zirconia ball, ball-milling medium is dehydrated alcohol, abrading-ball: material: the dehydrated alcohol mass ratio is 20:1:1.5, after ball milling finishes slip place common loft drier in 80 ℃ lower dry 24 hours, obtain the mixture powder.
(4) it is mid-in the electron tubes type atmosphere furnace that the mixture powder that step (3) is made is put into the corundum porcelain boat, be that 0.5 liter/min of clock, purity are under 99.9% the flowing nitrogen atmosphere at flow, first be warmed up to 1000 ℃ take temperature rise rate as 8 ℃/minute from room temperature, rise to 1450 ℃ with 5 ℃/minute of temperature rise rates again, be incubated 6 hours, naturally cool to 500 ℃ and stop to pass into nitrogen, continue to be cooled to room temperature.
(5) powder that step (4) is made is heated to 750 ℃ in retort furnace, be incubated 3 hours and remove remaining charcoal, namely makes high-purity beta-Sialon ceramic powder after the cooling.
The beta-Sialon ceramic powder that makes is through X-ray diffraction analysis, wherein Si
4Al
2O
2N
6(z=1.9) beta-Sialon content 97%, the microstructure of Sialon powder presents fibrous.
Embodiment 3:
(1) with levigate rear mistake 0.074 mm sieve of flyash, again the flyash that sieves is mixed (the Si:Al mol ratio is 1.85:1 in the raw material) with the reductive agent gac according to mass ratio 100:38, make mixture.
(2) mixture that step (1) is made 12 hours mixings of planetary ball mill ball milling, wherein drum's speed of rotation is 400 rev/mins, abrading-ball is zirconia ball, ball-milling medium is dehydrated alcohol, abrading-ball: material: the dehydrated alcohol mass ratio is 20:1:1.5, after ball milling finishes slip place common loft drier in 80 ℃ lower dry 24 hours, obtain the mixture powder.
(3) it is mid-in the electron tubes type atmosphere furnace that the mixture powder that step (2) is made is put into the corundum porcelain boat, be that 0.5 liter/min of clock, purity are under 99.9% the flowing nitrogen atmosphere at flow, first be warmed up to 1000 ℃ take temperature rise rate as 8 ℃/minute from room temperature, rise to 1450 ℃ with 5 ℃/minute of temperature rise rates again, be incubated 6 hours, naturally cool to 500 ℃ and stop to pass into nitrogen, continue to be cooled to room temperature.
(4) powder that step (3) is made is heated to 750 ℃ in retort furnace, be incubated 3 hours and remove remaining charcoal, namely makes high-purity beta-Sialon ceramic powder after the cooling.
The beta-Sialon ceramic powder that makes is through X-ray diffraction analysis, and its main phase is Si
4.1Al
1.9O
1.9N
6.1Be the beta-Sialon of z=1.9, content 96% also has a small amount of O '-Sialon in addition.
Embodiment 4:
(1) with levigate rear mistake 0.074 mm sieve of kaolin, again the kaolin that sieves is mixed (the Si:Al mol ratio is 1.08:1 in the raw material) with the reductive agent gac according to mass ratio 100:30, make mixture.
(2) mixture that step (1) is made 12 hours mixings of planetary ball mill ball milling, wherein drum's speed of rotation is 400 rev/mins, abrading-ball is zirconia ball, ball-milling medium is dehydrated alcohol, abrading-ball: material: the dehydrated alcohol mass ratio is 20:1:1.5, after ball milling finishes slip place common loft drier in 80 ℃ lower dry 24 hours, obtain the mixture powder.
(3) it is mid-in the electron tubes type atmosphere furnace that the mixture powder that step (2) is made is put into the corundum porcelain boat, be that 0.5 liter/min of clock, purity are under 99.9% the flowing nitrogen atmosphere at flow, first be warmed up to 1000 ℃ take temperature rise rate as 8 ℃/minute from room temperature, rise to 1450 ℃ with 5 ℃/minute of temperature rise rates again, be incubated 6 hours, naturally cool to 500 ℃ and stop to pass into nitrogen, continue to be cooled to room temperature.
(4) powder that step (3) is made is heated to 750 ℃ in retort furnace, be incubated 3 hours and remove remaining charcoal, namely makes high-purity beta-Sialon ceramic powder after the cooling.
The beta-Sialon ceramic powder that makes is through X-ray diffraction analysis, and its main phase is Si
2.9Al
3.1O
3.1N
4.9Be the beta-Sialon ceramic powder of z=3.1, content 96% also has a small amount of corundum and 15R-Sialon mutually.
Claims (1)
1. method for preparing the beta-Sialon ceramic powder with flyash and kaolin, concrete steps are:
(1) with levigate rear 0.074 mm sieve of crossing respectively of flyash and kaolin, be that 1.08 ~ 1.85:1 joins and gets flyash and the kaolin that sieves according to the Si:Al mol ratio again, then with agate mortar with join flyash and the kaolin pre-mixing of getting, make mixture;
(2) mixture that step (1) is made mixes according to mass ratio 100:25 ~ 45 with the reductive agent gac, makes mixture;
(3) mixture that step (2) is made 12 hours mixings of planetary ball mill ball milling, wherein drum's speed of rotation is 400 rev/mins, abrading-ball is zirconia ball, ball-milling medium is dehydrated alcohol, abrading-ball: material: the dehydrated alcohol mass ratio is 20:1:1.5, places slip common loft drier lower dry 24 hours in 80 ℃ after the ball milling end;
(4) powder after step (3) oven dry is put into the corundum porcelain boat mid-in the electron tubes type atmosphere furnace, be that 0.5 liter/min of clock, purity are under 99.9% the flowing nitrogen atmosphere at flow, first be warmed up to 1000 ℃ take temperature rise rate as 8 ℃/minute from room temperature, rise to 1400 ~ 1550 ℃ with 5 ℃/minute of temperature rise rates again, be incubated 4 ~ 8 hours, naturally cool to 500 ℃ and stop to pass into nitrogen, continue to be cooled to room temperature;
(5) powder that step (4) is made is heated to 750 ℃ in retort furnace, be incubated 3 hours and remove remaining charcoal, namely makes the beta-Sialon ceramic powder after the cooling.
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589365A (en) * | 2013-11-05 | 2014-02-19 | 重庆市锦艺硅材料开发有限公司苏州分公司 | Inorganic filler for copper-cladded plate and preparation method thereof |
| CN106634557A (en) * | 2016-12-08 | 2017-05-10 | 长兴天晟能源科技有限公司 | High-temperature-resisting and oxidation-resisting coating for SiAlON-AlN-TiN-based stainless steel |
| CN110203894A (en) * | 2019-06-26 | 2019-09-06 | 西北农林科技大学 | A method of β-SiAlON is prepared using aluminium lime-ash |
| CN114057492A (en) * | 2021-11-26 | 2022-02-18 | 江苏科技大学 | Beta' -Sialon-AlN-TiC composite ceramic material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0023869A1 (en) * | 1979-08-03 | 1981-02-11 | LAFARGE REFRACTAIRES Société Anonyme | Process for producing sialons |
| CN1521142A (en) * | 2003-02-14 | 2004-08-18 | 中国科学院上海硅酸盐研究所 | Process for preparation of self-spread high-temperature synthesizing low-cost diphase alpha/beta-sialon powder |
| CN1594216A (en) * | 2004-07-01 | 2005-03-16 | 北京科技大学 | Process for synthesizing high purity sialon material by coal-series kaolin |
-
2012
- 2012-12-03 CN CN2012105084216A patent/CN102924089A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0023869A1 (en) * | 1979-08-03 | 1981-02-11 | LAFARGE REFRACTAIRES Société Anonyme | Process for producing sialons |
| CN1521142A (en) * | 2003-02-14 | 2004-08-18 | 中国科学院上海硅酸盐研究所 | Process for preparation of self-spread high-temperature synthesizing low-cost diphase alpha/beta-sialon powder |
| CN1594216A (en) * | 2004-07-01 | 2005-03-16 | 北京科技大学 | Process for synthesizing high purity sialon material by coal-series kaolin |
Non-Patent Citations (3)
| Title |
|---|
| 《岩石矿物学杂志》 20051130 李金洪 利用高铝粉煤灰合成beta-Sialon 粉体的实验研究 643-647 1 第24卷, 第6期 * |
| 李金洪: "利用高铝粉煤灰合成β-Sialon 粉体的实验研究", 《岩石矿物学杂志》 * |
| 王体壮: "碳热还原氮化法制备SiAlON陶瓷材料", 《佛山陶瓷》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103589365A (en) * | 2013-11-05 | 2014-02-19 | 重庆市锦艺硅材料开发有限公司苏州分公司 | Inorganic filler for copper-cladded plate and preparation method thereof |
| CN106634557A (en) * | 2016-12-08 | 2017-05-10 | 长兴天晟能源科技有限公司 | High-temperature-resisting and oxidation-resisting coating for SiAlON-AlN-TiN-based stainless steel |
| CN110203894A (en) * | 2019-06-26 | 2019-09-06 | 西北农林科技大学 | A method of β-SiAlON is prepared using aluminium lime-ash |
| CN114057492A (en) * | 2021-11-26 | 2022-02-18 | 江苏科技大学 | Beta' -Sialon-AlN-TiC composite ceramic material and preparation method thereof |
| CN114057492B (en) * | 2021-11-26 | 2022-11-15 | 江苏科技大学 | Beta' -Sialon-AlN-TiC composite ceramic material and preparation method thereof |
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Application publication date: 20130213 |