CN101838147A - Method for synthesizing ZrB2-SiC-based ultra-high temperature ceramic powder by vacuum auto-combustion method - Google Patents
Method for synthesizing ZrB2-SiC-based ultra-high temperature ceramic powder by vacuum auto-combustion method Download PDFInfo
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- CN101838147A CN101838147A CN 201010179478 CN201010179478A CN101838147A CN 101838147 A CN101838147 A CN 101838147A CN 201010179478 CN201010179478 CN 201010179478 CN 201010179478 A CN201010179478 A CN 201010179478A CN 101838147 A CN101838147 A CN 101838147A
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Abstract
The invention relates to preparation of ZrB2-SiC-based compound ceramic powder, in particular to ZrB2-SiC-based ultra-high temperature ceramic powder synthesized by a vacuum auto-combustion method and a method for synthesizing the same by a vacuum auto-combustion method. The method comprises the following technical steps of: weighing experimental raw materials in a molar ratio of Zr:Si:B4C of 2-2.3:1:1-2, mixing the raw materials in a ball-to-material ratio of 4:1 by a planetary ball-milling method, and pressing the mixed powder into a compact blank under the pressure of 5 to 30MPa; and placing the pressed blank in a vacuum environment, firing the blank by using a tungsten filament, stopping the ignition so as to make the reaction spontaneously continue, and collecting a sample when the blank is cooled, wherein alloy balls are used as stirring balls in the ball-milling process, the ball-to-material ratio is 4:1, and the grain size of the ZrB2-SiC-ZrC mixed powder obtained by drying is 1 to 10 mu m. Because three kinds of particles of ZrB2, SiC and ZrC in the ZrB2-SiC-based ultra-high temperature ceramic powder are generated by a reaction in situ, the size distribution and the mixing uniformity of the ZrB2-SiC-based ultra-high temperature ceramic powder are obviously better than those of the common mixed powder, and the sintering temperature is also 100 to 200 DEG C lower than that of the common mixed powder.
Description
Technical field
The present invention relates to prepare ZrB
2-SiC base composite ceramic powder, the particularly synthetic ZrB of vacuum self-propagating combustion
2-SiC based ultra-high temperature ceramic powder.
Background technology
At space flight and aviation and weaponry field, ZrB
2-SiC based ultra-high temperature ceramic composite have high-melting-point, high heat conductance, mechanical property strong, than the performance of a series of excellences such as the better oxidation-resistance of C/C matrix material, be expected to be widely used.Conventional method is in proportion directly with ZrB
2Carry out forming and sintering again after mixing by physical method with the SiC powder.These class methods are difficult to obtain mixture highly uniformly, and the powder sintering activity is low, and the sintering temperature that needs is higher.The vacuum self-propagating combustion is to utilize the chemical reaction liberated heat to make spontaneous the going on of combustion reactions, to obtain to have the high-temperature synthesis of the products of combustion of specifying composition and structure.It has rapidly save time, energy-conservation, characteristics such as product purity is high, activity is high, cost is low and be produced on a large scale.Utilize the vacuum self-propagating combustion to prepare high-purity high reactivity ZrB
2-SiC base composite ceramic powder is for the development of ultrahigh-temperature pottery provides a brand-new approach.
Summary of the invention
Technical problem to be solved
Utilize the vacuum self-propagating combustion to prepare high-purity high reactivity ZrB
2-SiC base composite ceramic powder is for the development of ultrahigh-temperature pottery provides a brand-new approach
Technical scheme
Vacuum self-propagating combustion of the present invention synthesizes ZrB
2The preparation method of-SiC based ultra-high temperature ceramic powder is characterized in that being realized by following steps:
1, weighing: take by weighing Zr, Si and B
4C, described Zr, Si and B
4The mol ratio of C is 2-2.3: 1: 1-2 raw materials usedly is commercial powder raw material.
2, batch mixing: adopt the planetary ball mill method, use alloy ball as the batch mixing ball, it is to mix at 4: 1 that above-mentioned raw materials and alloy are asked by ratio of grinding media to material, and dehydrated alcohol is done dispersion medium, and drum's speed of rotation mixed 4-16 hour at 100-300rpm; Mix after drying and obtain mixed powder;
3, pressed compact: will be pressed into closely knit base substrate under the effect of mixed powder 5～30MPa pressure;
4, spread certainly synthetic: institute's pressed compact body is placed vacuum environment, and vacuum tightness is 1 * 10
-3Pa-5 * 10
-3Pa, attemperation 150-250 ℃, with the tungsten filament igniting, base substrate is lighted, end igniting, make spontaneous the going on of reaction, collect sample after cooling.From spreading when synthetic (2+3X) Zr+Si+ (1+X) B4C=(2+2X) ZrB
2Reaction is thermopositive reaction in the+SiC+XZrC reaction, and ZrC need not remove in the product, is retained in the powder;
5, ball mill pulverizing:, obtain trickle powder by the wet method planetary ball mill at last because there is hard aggregation in the powder of burning preparation.Ball milling uses alloy ball as stirring ball, and ratio of grinding media to material is 4: 1, and ethanol is done dispersion medium, and rotating speed is at 300-500rpm, and the time is 8-16 hour; Mix after drying and obtain ZrB
2-SiC-ZrC mixed powder, granularity is at 1-10 μ m.
Drying in the step (5) can water-bath distillation or oven drying.
Beneficial effect
1, the present invention utilizes the vacuum self-propagating combustion to prepare high-purity high reactivity ZrB
2The novel method of-SiC base composite ceramic powder.ZrB in its powder
23 kinds of particles of-SiC-ZrC are owing to all be that reaction in generates, and size-grade distribution and mixing uniformity obviously are better than conventional blended powder, and sintering temperature is than low 100-200 ℃ of conventional blended powder.
2, the vacuum self-propagating combustion have rapidly save time, energy-conservation, characteristics such as cost is low and be produced on a large scale.
3, the present invention is according to reaction (2+3X) Zr+Si+ (1+X) B
4C=(2+2X) ZrB
2+ SiC+XZrC takes by weighing required experimental raw, and the X value is adjustable between 0-0.3, according to ZrB
2(6.1g/cm
3), SiC (6.1g/cm
3) and ZrC (6.3g/cm
3) density data calculates and can make the long-pending ratio control of total SiC powder at 20vol%-27vol%, SiC powder volume ratio is in 20vol%-27vol%, and its oxidation-resistance is best.
Embodiment
Embodiment 1
1, weighing: press Zr: Si: B
4The C mol ratio takes by weighing experimental raw at 2: 1: 1, and used experimental raw is commercial powder raw material.
2, batch mixing: adopt the planetary ball mill method, use alloy ball as the batch mixing ball, it is to mix at 4: 1 that above-mentioned experimental raw and alloy are asked by ratio of grinding media to material, and dehydrated alcohol is done dispersion medium, and drum's speed of rotation mixed 4-16 hour at 100-300rpm; Mix after drying and obtain mixed powder;
3, pressed compact: will be pressed into closely knit base substrate under the effect of mixed powder 5～30MPa pressure;
4, spread certainly synthetic: institute's pressed compact body is placed vacuum environment, and vacuum tightness is 1 * 10
-3Pa-5 * 10
-3Pa, attemperation 150-250 ℃, with the tungsten filament igniting, base substrate is lighted, end igniting, make spontaneous the going on of reaction, collect sample after cooling.From spreading when synthetic (2+3X) Zr+Si+ (1+X) B
4C=(2+2X) ZrB
2Reaction is thermopositive reaction in the+SiC+XZrC reaction, and ZrC need not remove in the product, is retained in the powder;
5, ball mill pulverizing:, obtain trickle powder by the wet method planetary ball mill at last because there is hard aggregation in the powder of burning preparation.Ball milling uses alloy ball as stirring ball, and ratio of grinding media to material is 4: 1, and ethanol is done dispersion medium, and rotating speed is at 300-500rpm, and the time is 8-16 hour.Mix back water-bath distillation drying and obtain ZrB
2-SiC-ZrC mixed powder, granularity obtain the ZrB2-SiC based ultra-high temperature ceramic powder at 1-10 μ m.
ZrB in the ZrB2-SiC based ultra-high temperature ceramic powder
23 kinds of particles of-SiC-ZrC are owing to all be that reaction in generates, and size-grade distribution and mixing uniformity obviously are better than conventional blended powder, and sintering temperature is than low 100-200 ℃ of conventional blended powder.
Embodiment 2
1, weighing: press Zr: Si: B
4The C mol ratio takes by weighing experimental raw at 2.3: 1: 2, and used experimental raw is commercial powder raw material.
2, batch mixing: adopt the planetary ball mill method, use alloy ball as the batch mixing ball, it is to mix at 4: 1 that above-mentioned experimental raw and alloy are asked by ratio of grinding media to material, and dehydrated alcohol is done dispersion medium, and drum's speed of rotation mixed 4-16 hour at 100-300rpm; Mix after drying and obtain mixed powder;
3, pressed compact: will be pressed into closely knit base substrate under the effect of mixed powder 5～30MPa pressure;
4, spread certainly synthetic: institute's pressed compact body is placed vacuum environment, and vacuum tightness is 1 * 10
-3Pa-5 * 10
-3Pa, attemperation 150-250 ℃, with the tungsten filament igniting, base substrate is lighted, end igniting, make spontaneous the going on of reaction, collect sample after cooling.From spreading when synthetic (2+3X) Zr+Si+ (1+X) B
4C=(2+2X) ZrB
2Reaction is thermopositive reaction in the+SiC+XZrC reaction, and ZrC need not remove in the product, is retained in the powder;
5, ball mill pulverizing:, obtain trickle powder by the wet method planetary ball mill at last because there is hard aggregation in the powder of burning preparation.Ball milling uses alloy ball as stirring ball, and ratio of grinding media to material is 4: 1, and ethanol is done dispersion medium, and rotating speed is at 300-500rpm, and the time is 8-16 hour.Mix back water-bath distillation drying and obtain ZrB
2-SiC-ZrC mixed powder, granularity obtain the ZrB2-SiC based ultra-high temperature ceramic powder at 1-10 μ m.
ZrB in the ZrB2-SiC based ultra-high temperature ceramic powder
23 kinds of particles of-SiC-ZrC are owing to all be that reaction in generates, and size-grade distribution and mixing uniformity obviously are better than conventional blended powder, and sintering temperature is than low 100-200 ℃ of conventional blended powder.
Embodiment 3
1, weighing: press Zr: Si: B
4The C mol ratio takes by weighing experimental raw at 2.1: 1: 1.8, and used experimental raw is commercial powder raw material.
2, batch mixing: adopt the planetary ball mill method, use alloy ball as the batch mixing ball, it is to mix at 4: 1 that above-mentioned experimental raw and alloy are asked by ratio of grinding media to material, and dehydrated alcohol is done dispersion medium, and drum's speed of rotation mixed 4-16 hour at 100-300rpm; Mix after drying and obtain mixed powder;
3, pressed compact: will be pressed into closely knit base substrate under the effect of mixed powder 5～30MPa pressure;
4, spread certainly synthetic: institute's pressed compact body is placed vacuum environment, and vacuum tightness is 1 * 10
-3Pa-5 * 10
-3Pa, attemperation 150-250 ℃, with the tungsten filament igniting, base substrate is lighted, end igniting, make spontaneous the going on of reaction, collect sample after cooling.From spreading when synthetic (2+3X) Zr+Si+ (1+X) B
4C=(2+2X) ZrB
2Reaction is thermopositive reaction in the+SiC+XZrC reaction, and ZrC need not remove in the product, is retained in the powder;
5, ball mill pulverizing:, obtain trickle powder by the wet method planetary ball mill at last because there is hard aggregation in the powder of burning preparation.Ball milling uses alloy ball as stirring ball, and ratio of grinding media to material is 4: 1, and ethanol is done dispersion medium, and rotating speed is at 300-500rpm, and the time is 8-16 hour.Mix back water-bath distillation drying and obtain ZrB
2-SiC-ZrC mixed powder, granularity obtain the ZrB2-SiC based ultra-high temperature ceramic powder at 1-10 μ m.
ZrB in the ZrB2-SiC based ultra-high temperature ceramic powder
23 kinds of particles of-SiC-ZrC are owing to all be that reaction in generates, and size-grade distribution and mixing uniformity obviously are better than conventional blended powder, and sintering temperature is than low 100-200 ℃ of conventional blended powder.
Claims (1)
1. a vacuum self-propagating combustion synthesizes ZrB
2The preparation method of-SiC based ultra-high temperature ceramic powder is characterized in that following steps:
(1), weighing: take by weighing Zr, Si and B
4C, described Zr, Si and B
4The mol ratio of C is 2-2.3: 1: 1-2;
(2), batch mixing: adopting the planetary ball mill method, use alloy ball as the batch mixing ball, is to mix at 4: 1 the mixture of alloy ball and above-mentioned raw materials by ratio of grinding media to material, dehydrated alcohol is done dispersion medium, drum's speed of rotation mixed 4-16 hour at 100-300rpm, mixed after drying and obtained mixed powder;
(3), pressed compact: will be pressed into closely knit base substrate under the effect of mixed powder 5～30MPa pressure;
(4), certainly spread synthetic: institute's pressed compact body is placed vacuum environment, and vacuum tightness is 1 * 10
-3Pa-5 * 10
-3Pa, attemperation 150-250 ℃, with the tungsten filament igniting, base substrate is lighted, end igniting, make spontaneous the going on of reaction, collect sample after cooling;
(5), ball mill pulverizing: above-mentioned sample obtains trickle powder by planetary ball mill, uses alloy ball as stirring ball, and ratio of grinding media to material is 4: 1, and ethanol is done dispersion medium, and rotating speed is at 300-500rpm, and the time is 8-16 hour, mixes after drying and obtains ZrB
2-SiC-ZrC mixed powder, granularity obtain ZrB at 1-10 μ m
2-SiC based ultra-high temperature ceramics powder.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584240A (en) * | 2012-01-17 | 2012-07-18 | 哈尔滨工业大学 | Sintering method of ZrB2-SiC superhigh temperature ceramics |
| CN102617148A (en) * | 2012-04-06 | 2012-08-01 | 牡丹江金钢钻碳化硼有限公司 | Novel boron carbide ceramic base composite material and preparation method thereof |
| CN103304228A (en) * | 2012-03-16 | 2013-09-18 | 西北师范大学 | Self-propagating combustion synthesis method for palladium-copper ferrite nano-powder |
| CN106747464A (en) * | 2017-01-04 | 2017-05-31 | 广东工业大学 | ZrB2SiC ceramic heater and superhigh temperature firing equipment |
| CN107056334A (en) * | 2017-04-28 | 2017-08-18 | 哈尔滨理工大学 | A kind of ZrC ceramic material surfaces ZrB2The preparation method of SiC composite coatings |
| CN110041091A (en) * | 2019-04-02 | 2019-07-23 | 上海交通大学 | A kind of preparation method of the heat-insulated microballoon filler of the resistance to ablation of high emissivity |
| CN114380602A (en) * | 2020-10-20 | 2022-04-22 | 中国科学院理化技术研究所 | Preparation method of ultrahigh-temperature ceramic composite powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215173A (en) * | 2008-01-04 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | Method for preparing ZrB2-SiC-ZrC diphase ceramic material |
-
2010
- 2010-05-21 CN CN 201010179478 patent/CN101838147A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215173A (en) * | 2008-01-04 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | Method for preparing ZrB2-SiC-ZrC diphase ceramic material |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102584240A (en) * | 2012-01-17 | 2012-07-18 | 哈尔滨工业大学 | Sintering method of ZrB2-SiC superhigh temperature ceramics |
| CN103304228A (en) * | 2012-03-16 | 2013-09-18 | 西北师范大学 | Self-propagating combustion synthesis method for palladium-copper ferrite nano-powder |
| CN102617148A (en) * | 2012-04-06 | 2012-08-01 | 牡丹江金钢钻碳化硼有限公司 | Novel boron carbide ceramic base composite material and preparation method thereof |
| CN106747464A (en) * | 2017-01-04 | 2017-05-31 | 广东工业大学 | ZrB2SiC ceramic heater and superhigh temperature firing equipment |
| CN107056334A (en) * | 2017-04-28 | 2017-08-18 | 哈尔滨理工大学 | A kind of ZrC ceramic material surfaces ZrB2The preparation method of SiC composite coatings |
| CN107056334B (en) * | 2017-04-28 | 2020-04-17 | 哈尔滨理工大学 | ZrB ceramic material surface ZrB2Preparation method of-SiC composite coating |
| CN110041091A (en) * | 2019-04-02 | 2019-07-23 | 上海交通大学 | A kind of preparation method of the heat-insulated microballoon filler of the resistance to ablation of high emissivity |
| CN110041091B (en) * | 2019-04-02 | 2022-08-09 | 上海交通大学 | Preparation method of high-emissivity ablation-resistant heat-insulation microsphere filler |
| CN114380602A (en) * | 2020-10-20 | 2022-04-22 | 中国科学院理化技术研究所 | Preparation method of ultrahigh-temperature ceramic composite powder |
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Application publication date: 20100922 |