CN103922360B - The technique of the bar-shaped zirconium boride powder of low temperature preparation - Google Patents
The technique of the bar-shaped zirconium boride powder of low temperature preparation Download PDFInfo
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Abstract
The present invention provides a kind of technique of the bar-shaped zirconium boride powder of low temperature preparation, belongs to technical field of powdered material preparation.It is characterized in that：1）Prepare bar-shaped Zirconium powder：Using bar-shaped zirconium chloride powder as raw material, 900~1100 DEG C of 0.2~1 h of insulation are heated to, obtain bar-shaped Zirconium powder；2）Prepare carbon dust：Using thermosetting phenolic resin as raw material, solidify at 80~120 DEG C, under an argon atmosphere, 900~1100 DEG C of calcinings, be incubated 10~60 min, be cracked to form carbon dust；3）Prepare bar-shaped zirconium boride powder：First carbon dust is crushed, then by bar-shaped Zirconium powder, boric acid, carbon dust in molar ratio be 1:(2~2.2):5 mixing, are sintered under an argon atmosphere, and sintering temperature is 1500~1700 DEG C, and soaking time is 0.5~2h, produces bar-shaped zirconium boride powder.Sintering temperature of the present invention is low, and technique is simple, and safe operation, cost is low, is easy to industrialization, prepares bar-shaped zirconium boride powder, good dispersion, and draw ratio is more than 2 times.
Description
Technical field
The present invention provides a kind of technique of the bar-shaped zirconium boride powder of low temperature preparation, belongs to technical field of powdered material preparation.
Background technology
Zirconium diboride superhigh temperature ceramics have high-melting-point（3245℃）, high rigidity（Mohs' hardness is 9, and microhardness is
22.1GPa）, high heat conductance（Thermal conductivity is 23~25W/ (mK)）It is a kind of thermal structure of excellent performance Deng premium properties
Material, it is widely used in high-temperature structural ceramics, composite, electrode material, thin-film material, refractory material, nuclear control material etc.
Field.Research shows that the performance of ceramics is relevant with the pattern of powder used, such as by fibrous powder in the preparation of composite ceramics
The intensity that can make ceramic material instead of graininess powder increases；Such as it can make ceramic material using spherical powder when preparing one-component ceramic
The density increase of material.With the continuous expansion that zirconium boride is applied in high-tech sector, the zirconium boride powder of different-shape has been prepared
Another focus through being studied as zirconium boride.And bar-shaped zirconium boride powder there is no report.
The content of the invention
It is an object of the invention to provide a kind of sintering temperature is low, technique is simple, and safe operation, cost is low, is easy to industrialization
The technique of the bar-shaped zirconium boride powder of low temperature preparation, its technical scheme are：
1）Prepare bar-shaped Zirconium powder：Using bar-shaped zirconium chloride powder as raw material, bar-shaped zirconium chloride powder a diameter of 5
~10 μm, length is 100~200 μm, and purity is more than 99 %, is heated to 900~1100 DEG C of 0.2~1 h of insulation, obtains bar-shaped oxygen
Change zirconium powder body；2）Prepare carbon dust：Using thermosetting phenolic resin as raw material, solidify at 80~120 DEG C, under an argon atmosphere, 900
~1100 DEG C of calcinings, programming rate is 5~10 DEG C/min, is incubated 10~60 min, is cracked to form carbon dust；3）Prepare bar-shaped boronation
Zirconium powder body：First carbon dust is crushed, makes powder granularity up to 1~20 μm, then by bar-shaped Zirconium powder, boric acid, carbon dust in molar ratio
For 1:(2~2.2):5 mixing, are sintered under an argon atmosphere, and sintering temperature is 1500~1700 DEG C, soaking time 0.5
~2h, produce bar-shaped zirconium boride powder.
The present invention compared with prior art, has the following advantages that：
1st, the present invention prepares bar-shaped zirconium boride powder, and draw ratio is more than 2 times；
2nd, the present invention prepare bar-shaped zirconium boride powder sintering temperature it is low, good dispersion；
3rd, the present invention prepares the technique of bar-shaped zirconium boride powder, and technique is simple, and safe operation, cost is low, is easy to industrialization.
Brief description of the drawings
Fig. 1 is the XRD spectrums that the present invention prepares powder；
Fig. 2 is the SEM photograph that the present invention prepares powder.
Embodiment
Embodiment 1
1）Prepare bar-shaped Zirconium powder：Using bar-shaped zirconium chloride powder as raw material, bar-shaped zirconium chloride powder a diameter of 5
μm, length is 100 μm, and purity is more than 99 %, is heated to 900 DEG C of 1 h of insulation, obtains bar-shaped Zirconium powder；
2）Prepare carbon dust：Using thermosetting phenolic resin as raw material, solidify at 80 DEG C, under an argon atmosphere, forged at 900 DEG C
Burn, programming rate is 5 DEG C/min, is incubated 60 min, is cracked to form carbon dust；
3）Prepare bar-shaped zirconium boride powder：First carbon dust is crushed, makes powder granularity up to 1 μm, then by bar-shaped Zirconium powder,
Boric acid, carbon dust are 1 in molar ratio: 2 :5 mixing, are sintered under an argon atmosphere, and sintering temperature is 1500 DEG C, soaking time
For 2h, bar-shaped zirconium boride powder is produced.
Tested by XRD, it is seen that powder is zirconium diboride（See Fig. 1）；Tested by SEM, it is seen that Zirconium powder is rod
Shape, a diameter of 2 μm or so, length is 5 μm or so（See Fig. 2）.
Embodiment 2
1）Prepare bar-shaped Zirconium powder：Using bar-shaped zirconium chloride powder as raw material, bar-shaped zirconium chloride powder is a diameter of
10 μm, length is 200 μm, and purity is more than 99 %, is heated to 1100 DEG C of 0.2 h of insulation, obtains bar-shaped Zirconium powder；
2）Prepare carbon dust：Using thermosetting phenolic resin as raw material, solidify at 120 DEG C, under an argon atmosphere, at 1100 DEG C
Calcining, programming rate is 10 DEG C/min, is incubated 10 min, is cracked to form carbon dust；
3）Prepare bar-shaped zirconium boride powder：First carbon dust is crushed, makes powder granularity up to 20 μm, then by bar-shaped zirconia powder
Body, boric acid, carbon dust are 1 in molar ratio: 2.2 :5 mixing, are sintered under an argon atmosphere, and sintering temperature is 1700 DEG C, insulation
Time is 0.5h, produces bar-shaped zirconium boride powder.
Embodiment 3
1）Prepare bar-shaped Zirconium powder：Using bar-shaped zirconium chloride powder as raw material, bar-shaped zirconium chloride powder a diameter of 8
μm, length is 150 μm, and purity is more than 99 %, is heated to 1000 DEG C of 0.5 h of insulation, obtains bar-shaped Zirconium powder；
2）Prepare carbon dust：Using thermosetting phenolic resin as raw material, solidify at 100 DEG C, under an argon atmosphere, at 1000 DEG C
Calcining, programming rate is 7 DEG C/min, is incubated 30 min, is cracked to form carbon dust；
3）Prepare bar-shaped zirconium boride powder：First carbon dust is crushed, makes powder granularity up to 10 μm, then by bar-shaped zirconia powder
Body, boric acid, carbon dust are 1 in molar ratio: 2.1 :5 mixing, are sintered under an argon atmosphere, and sintering temperature is 1600 DEG C, insulation
Time is 1h, produces bar-shaped zirconium boride powder.
Claims (1)
- A kind of 1. technique of the bar-shaped zirconium boride powder of low temperature preparation, it is characterised in that：1）Prepare bar-shaped Zirconium powder：With bar-shaped Zirconium chloride powder is raw material, bar-shaped a diameter of 5~10 μm of zirconium chloride powder, and length is 100~200 μm, and purity is more than 99 %, 900~1100 DEG C of 0.2~1 h of insulation are heated to, obtain bar-shaped Zirconium powder；2）Prepare carbon dust：With thermosetting phenolic tree Fat is raw material, is solidified at 80~120 DEG C, under an argon atmosphere, 900~1100 DEG C calcining, programming rate be 5~10 DEG C/ Min, 10~60 min are incubated, are cracked to form carbon dust；3）Prepare bar-shaped zirconium boride powder：First carbon dust is crushed, makes powder granularity It is 1 in molar ratio up to 1~20 μm, then by bar-shaped Zirconium powder, boric acid, carbon dust:(2~2.2):5 mixing, in argon gas gas Sintered under atmosphere, sintering temperature is 1500~1700 DEG C, and soaking time is 0.5~2h, produces bar-shaped zirconium boride powder.
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Families Citing this family (7)
| 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 |
| CN105084380B (en) * | 2015-08-06 | 2017-05-10 | 电子科技大学 | Method for preparing hollow rodlike zirconium boride powder |
| CN105197953A (en) * | 2015-09-29 | 2015-12-30 | 山东理工大学 | Synthetic process of rod zirconium boride powder |
| CN105197954B (en) * | 2015-09-29 | 2018-03-30 | 山东理工大学 | The synthetic method of bar-shaped zirconium boride powder |
| CN105152180B (en) * | 2015-10-19 | 2017-11-10 | 山东理工大学 | The preparation technology of hollow rod-shape zirconium boride powder |
| WO2017131108A1 (en) * | 2016-01-27 | 2017-08-03 | 第一稀元素化学工業株式会社 | Zirconium boride and method for producing same |
| CN113149676B (en) * | 2021-06-02 | 2022-12-13 | 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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| CN101914810B (en) * | 2010-08-16 | 2012-05-02 | 山东大学 | Zirconium diboride whisker material and preparation method thereof |
| CN102464323A (en) * | 2010-11-04 | 2012-05-23 | 中国科学院过程工程研究所 | Method for preparing high-purity superfine zirconium boride powder by high-frequency plasma |
| CN102139883A (en) * | 2011-05-14 | 2011-08-03 | 长沙云麓粉末材料科技有限公司 | Method for preparing high-purity zirconium diboride |
| CN102249688B (en) * | 2011-05-25 | 2013-02-20 | 山东理工大学 | Method for preparing zirconium boride powder |
| CN102745704A (en) * | 2012-07-25 | 2012-10-24 | 深圳市新星轻合金材料股份有限公司 | Method for producing zirconium boride and synchronously outputting cryolite |
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