CN103922360A - Process of preparing rod-like zirconium boride powder at low temperature - Google Patents
Process of preparing rod-like zirconium boride powder at low temperature Download PDFInfo
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Abstract
The invention provides a process of preparing rod-like zirconium boride powder at a low temperature, and belongs to the technical field of powder material preparation. The process is characterized by comprising the steps: (1), preparing rod-like zirconium boride powder: taking rod-like zirconium tetrachloride powder as the material, heating to 900 DEG C-1100 DEG C and preserving heat for 0.2 hour-1 hour to obtain the rod-like zirconium boride powder; (2), preparing carbon powder: taking thermosetting phenol resin as the material, curing at 80 DEG C-120 DEG C, roasting at 900 DEG C-1000 DEG C under an argon-gas atmosphere, preserving the heat for 10 minutes-60 minutes, and cracking to generate carbon powder; and (3), preparing rod-like zirconium boride powder: firstly mixing the rod-like zirconium boride powder, boric acid and carbon powder according to a molar ratio of 1:(2-2.2):5, sintering under the argon-gas atmosphere with a sintering temperature of 1500 DEG C-1700 DEG G and heat-preserving time of 0.5 hour-2 hours to obtain the rod-like zirconium boride powder. The process disclosed by the invention is low in sintering temperature, simple in process, safe to operate, low in cost and easy for industrialization; and the prepared rod-like zirconium boride powder is good in dispersion, and has a slenderness ratio greater than twice.
Description
Technical field
The invention provides a kind of low temperature and prepare the technique of bar-shaped zirconium boride powder, belong to technical field of powdered material preparation.
Background technology
Zirconium diboride superhigh temperature ceramics has high-melting-point (3245 DEG C), (Mohs' hardness is 9 to high rigidity, microhardness is 22.1GPa), the premium properties such as high heat conductance (thermal conductivity is 23～25W/ (mK)), be a kind of high-temperature structural material of excellent performance, be widely used in the fields such as high-temperature structural ceramics, matrix material, electrode materials, thin-film material, refractory materials, nuclear control material.Research shows that ceramic performance is relevant with the pattern of powder used, as replaced particulate state powder can make the intensity of stupalith increase by fibrous powder in the preparation of composite ceramics; In the time preparing one-component ceramic, as can making the density of stupalith, use spherical powder increases.Along with zirconium boride 99.5004323A8ure is in the continuous expansion of high-tech sector application, the zirconium boride powder of preparing different-shape has become the another focus of zirconium boride 99.5004323A8ure research.And bar-shaped zirconium boride powder there is no report.
Summary of the invention
The object of this invention is to provide a kind of sintering temperature low, technique is simple, operational safety, and cost is low, is easy to the technique that industrialization low temperature is prepared bar-shaped zirconium boride powder, and its technical scheme is:
1) prepare bar-shaped Zirconium powder: taking bar-shaped zirconium tetrachloride powder as raw material, bar-shaped zirconium tetrachloride powder diameter is 5～10 μ m, and length is 100～200 μ m, and purity is greater than 99 %, be heated to 900～1100 DEG C of insulation 0.2～1 h, obtain bar-shaped Zirconium powder; 2) prepare carbon dust: taking heat-reactive phenolic resin as raw material, at 80～120 DEG C, solidify, under argon gas atmosphere, 900～1100 DEG C of calcinings, heat-up rate is 5～10 DEG C/min, insulation 10～60 min, cracking generates carbon dust; 3) prepare bar-shaped zirconium boride powder: first by carbon dust fragmentation, make powder granularity reach 1～20 μ m, be 1:(2～2.2 in molar ratio by bar-shaped Zirconium powder, boric acid, carbon dust again): 5 mix, sintering under argon gas atmosphere, sintering temperature is 1500～1700 DEG C, soaking time is 0.5～2h, obtains bar-shaped zirconium boride powder.
compared with prior art, tool has the following advantages in the present invention:
1, the present invention prepares bar-shaped zirconium boride powder, and length-to-diameter ratio is greater than 2 times;
2, to prepare the sintering temperature of bar-shaped zirconium boride powder low in the present invention, good dispersity;
3, the present invention prepares the technique of bar-shaped zirconium boride powder, and technique is simple, operational safety, and cost is low, is easy to industrialization.
Brief description of the drawings
Fig. 1 is the XRD spectrum that the present invention prepares powder;
Fig. 2 is the SEM photo that the present invention prepares powder.
Embodiment
Embodiment 1
1) prepare bar-shaped Zirconium powder: taking bar-shaped zirconium tetrachloride powder as raw material, bar-shaped zirconium tetrachloride powder diameter is 5 μ m, and length is 100 μ m, and purity is greater than 99 %, be heated to 900 DEG C of insulation 1 h, obtain bar-shaped Zirconium powder;
2) prepare carbon dust: taking heat-reactive phenolic resin as raw material, at 80 DEG C, solidify, under argon gas atmosphere, calcining at 900 DEG C, heat-up rate is 5 DEG C/min, insulation 60 min, cracking generates carbon dust;
3) prepare bar-shaped zirconium boride powder: first by carbon dust fragmentation, make powder granularity reach 1 μ m, then be to mix at 1: 2: 5 in molar ratio by bar-shaped Zirconium powder, boric acid, carbon dust, sintering under argon gas atmosphere, sintering temperature is 1500 DEG C, and soaking time is 2h, obtains bar-shaped zirconium boride powder.
Test by XRD, visible powder is zirconium diboride (see figure 1); Test by SEM, visible Zirconium powder is bar-shaped, and diameter is 2 μ m left and right, and length is 5 μ m left and right (see figure 2)s.
Embodiment 2
1) prepare bar-shaped Zirconium powder: taking bar-shaped zirconium tetrachloride powder as raw material, bar-shaped zirconium tetrachloride powder diameter is 10 μ m, and length is 200 μ m, and purity is greater than 99 %, be heated to 1100 DEG C of insulation 0.2 h, obtain bar-shaped Zirconium powder;
2) prepare carbon dust: taking heat-reactive phenolic resin as raw material, at 120 DEG C, solidify, under argon gas atmosphere, calcining at 1100 DEG C, heat-up rate is 10 DEG C/min, insulation 10 min, cracking generates carbon dust;
3) prepare bar-shaped zirconium boride powder: first by carbon dust fragmentation, make powder granularity reach 20 μ m, be to mix at 1: 2.2: 5 more in molar ratio by bar-shaped Zirconium powder, boric acid, carbon dust, sintering under argon gas atmosphere, sintering temperature is 1700 DEG C, soaking time is 0.5h, obtains bar-shaped zirconium boride powder.
Embodiment 3
1) prepare bar-shaped Zirconium powder: taking bar-shaped zirconium tetrachloride powder as raw material, bar-shaped zirconium tetrachloride powder diameter is 8 μ m, and length is 150 μ m, and purity is greater than 99 %, be heated to 1000 DEG C of insulation 0.5 h, obtain bar-shaped Zirconium powder;
2) prepare carbon dust: taking heat-reactive phenolic resin as raw material, at 100 DEG C, solidify, under argon gas atmosphere, calcining at 1000 DEG C, heat-up rate is 7 DEG C/min, insulation 30 min, cracking generates carbon dust;
3) prepare bar-shaped zirconium boride powder: first by carbon dust fragmentation, make powder granularity reach 10 μ m, then be to mix at 1: 2.1: 5 in molar ratio by bar-shaped Zirconium powder, boric acid, carbon dust, sintering under argon gas atmosphere, sintering temperature is 1600 DEG C, and soaking time is 1h, obtains bar-shaped zirconium boride powder.
Claims (1)
1. a low temperature is prepared the technique of bar-shaped zirconium boride powder, it is characterized in that: 1) prepare bar-shaped Zirconium powder: taking bar-shaped zirconium tetrachloride powder as raw material, bar-shaped zirconium tetrachloride powder diameter is 5～10 μ m, length is 100～200 μ m, purity is greater than 99 %, be heated to 900～1100 DEG C of insulation 0.2～1 h, obtain bar-shaped Zirconium powder; 2) prepare carbon dust: taking heat-reactive phenolic resin as raw material, at 80～120 DEG C, solidify, under argon gas atmosphere, 900～1100 DEG C of calcinings, heat-up rate is 5～10 DEG C/min, insulation 10～60 min, cracking generates carbon dust; 3) prepare bar-shaped zirconium boride powder: first by carbon dust fragmentation, make powder granularity reach 1～20 μ m, be 1:(2～2.2 in molar ratio by bar-shaped Zirconium powder, boric acid, carbon dust again): 5 mix, sintering under argon gas atmosphere, sintering temperature is 1500～1700 DEG C, soaking time is 0.5～2h, obtains bar-shaped zirconium boride powder.
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Cited By (7)
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|---|---|---|---|---|
| CN104211063A (en) * | 2014-09-17 | 2014-12-17 | 山东理工大学 | Method for preparing rod-like zirconium carbide powder by solid-phase reaction |
| CN105084380A (en) * | 2015-08-06 | 2015-11-25 | 电子科技大学 | Method for preparing hollow rodlike zirconium boride powder |
| CN105152180A (en) * | 2015-10-19 | 2015-12-16 | 山东理工大学 | Preparation process of hollow rod-like zirconium boride powder |
| CN105197954A (en) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | Synthetic method of rod zirconium boride powder |
| CN105197953A (en) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | Synthetic process of rod zirconium boride powder |
| CN108349820A (en) * | 2016-01-27 | 2018-07-31 | 第稀元素化学工业株式会社 | zirconium boride and preparation method thereof |
| CN113149676A (en) * | 2021-06-02 | 2021-07-23 | 哈尔滨工程大学 | Method for sintering in-situ toughened boron carbide-based multiphase ceramic by using two-step method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211063A (en) * | 2014-09-17 | 2014-12-17 | 山东理工大学 | Method for preparing rod-like zirconium carbide powder by solid-phase reaction |
| CN105084380A (en) * | 2015-08-06 | 2015-11-25 | 电子科技大学 | Method for preparing hollow rodlike zirconium boride powder |
| CN105197954A (en) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | Synthetic method of rod zirconium boride powder |
| CN105197953A (en) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | Synthetic process of rod zirconium boride powder |
| CN105152180A (en) * | 2015-10-19 | 2015-12-16 | 山东理工大学 | Preparation process of hollow rod-like zirconium boride powder |
| CN108349820A (en) * | 2016-01-27 | 2018-07-31 | 第稀元素化学工业株式会社 | zirconium boride and preparation method thereof |
| CN108349820B (en) * | 2016-01-27 | 2021-11-30 | 第一稀元素化学工业株式会社 | Zirconium boride and preparation method thereof |
| CN113149676A (en) * | 2021-06-02 | 2021-07-23 | 哈尔滨工程大学 | Method for sintering in-situ toughened boron carbide-based multiphase ceramic by using two-step method |
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