CN100569644C - A kind of preparation method of high purity ultra fine zirconium biboride powder - Google Patents
A kind of preparation method of high purity ultra fine zirconium biboride powder Download PDFInfo
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- CN100569644C CN100569644C CNB200610114427XA CN200610114427A CN100569644C CN 100569644 C CN100569644 C CN 100569644C CN B200610114427X A CNB200610114427X A CN B200610114427XA CN 200610114427 A CN200610114427 A CN 200610114427A CN 100569644 C CN100569644 C CN 100569644C
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- zirconium
- zirconium oxychloride
- biboride
- ultra fine
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- 239000000843 powder Substances 0.000 title claims abstract description 56
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 241001672694 Citrus reticulata Species 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 229910052580 B4C Inorganic materials 0.000 abstract description 3
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- JQLZABHNCZQFNR-UHFFFAOYSA-J O.[Cl-].[Cl-].[Cl-].[Cl-].Cl.Cl.[Zr+4] Chemical compound O.[Cl-].[Cl-].[Cl-].[Cl-].Cl.Cl.[Zr+4] JQLZABHNCZQFNR-UHFFFAOYSA-J 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 229910052786 argon Inorganic materials 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010219 correlation analysis Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 241000209456 Plumbago Species 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910007948 ZrB2 Inorganic materials 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical class B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002101 lytic effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000000803 paradoxical effect Effects 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- RCKBMGHMPOIFND-UHFFFAOYSA-N sulfanylidene(sulfanylidenegallanylsulfanyl)gallane Chemical compound S=[Ga]S[Ga]=S RCKBMGHMPOIFND-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention relates to a kind of high purity ultra fine zirconium biboride powder and method thereof, belong to the stupalith field.It is characterized in that: described powder contains zirconium oxychloride, boron carbide powder, activated carbon powder, and its mol ratio proportioning is: ZrOCl
2: B
4C: C=1: 0.4～0.8: 1.4～1.8.Its preparation method be earlier by proportioning with B
4C, C powder and H
2O mixes, and regulates the pH value, obtains B
4C and C powder mixing suspension; Zirconium oxychloride is dissolved in the deionized water, makes zirconyl chloride solution; Mixing suspension and zirconyl chloride solution is mixed, add ammoniacal liquor, make the abundant hydrolytic precipitation of zirconium oxychloride; With the suspensoid solid-liquid separation, NH is removed in washing
4 +And Cl
-, sieve after the oven dry; Powder is put into vacuum oven again and reacted synthetic, 1500～1600 ℃ of synthesis temperatures are incubated 0.5～4 hour; Powder is levigate, sieves.The present invention can synthesize high-purity, ultra fine zirconium biboride powder in enormous quantities with cheap feed oxygen zirconium chloride and simple production unit.Detect through XRD, main component is ZrB in the powder
2, particle such as is at axle shape shape.
Description
Technical field
The present invention relates to a kind of low-cost preparation high purity ultra fine zirconium biboride (ZrB
2) powder and method thereof, belong to the stupalith field.
Background technology
Zirconium diboride (ZrB
2) having characteristics such as high-melting-point, high rigidity, electrical and thermal conductivity are good, excellent flame-retardant performance, thermotolerance, oxidation-resistance, erosion resistance, there is very wide application prospect in a lot of fields such as electrode materials of crucible that uses at aerospace ultrahigh-temperature structure unit, casting industry and refractory materials, metal smelting.
The method of this zirconium diboride powder of preparation mainly contains four kinds at present: first method is self propagating high temperature synthesis method (SHS) (document 1: Chinese invention patent: 200510010014); Second method is zirconium dioxide boronation reduction method (document 2:J.Am.Ceram.Soc., 78[9] 2534-36 (1995)); The third method is that electrolysis contains metal oxide and B
20
3Molten salt bath method (document 3: ceramic-metal composite material: 53 (2004)); The 4th kind of method is direct synthesis by solid state reaction.Method one process is simple, and the time is short, and energy consumption is little, and synthetic powder is active high, but because its speed of response is too fast, reaction is carried out not exclusively sometimes, and impurity accordingly also can be many, and its reaction process, product structure and performance are not easy control.Method two relatively is fit to industrial mass production, but its shortcoming is than being easier to introduce impurity, and the product purity for preparing is not high.Method threeway paradoxical reaction is not easy to carry out fully, and the product particle is bigger, and activity is not high, is unfavorable for the post-treatment processing.Method four is subjected to the expensive restriction of raw material, and often its lytic activity is not high.
A kind of high purity ultra fine zirconium biboride (ZrB that the present invention proposes
2) the carbothermic reduction boronation method of powder, filled up the technological gap of low-cost preparation high purity ultra fine zirconium biboride powder aspect just.
Summary of the invention
The purpose of this invention is to provide the method that a kind of low cost prepares high purity ultra fine zirconium biboride powder, utilize carbothermic reduction boronation legal system to be equipped with the zirconium biboride powder of high pure and ultra-fine.The present invention is simple and easy to do, productive rate is high, purity is high, efficient is high, be fit to commercial scale production.
A kind of high purity ultra fine zirconium biboride powder that the present invention proposes, it is characterized in that: described powder contains zirconium oxychloride, boron carbide powder, activated carbon powder, and its mol ratio proportioning is: ZrOCl
2: B
4C: C=1: (0.4～0.8): (1.4～1.8).
The preparation method of a kind of high purity ultra fine zirconium biboride powder that the present invention proposes, it is characterized in that: described method is carried out successively as follows:
(1) proportioning is in molar ratio: ZrOCl
2: B
4C: C=1: (0.4～0.8): (1.4～1.8) weigh batching, at first with B
4C and C powder are put into beaker, press solid: H
2O=1: 50～80 ratio adds deionized water, stirs, and the pH value is adjusted to 2～5, obtains B
4C and C powder mixing suspension;
(2) take by weighing zirconium oxychloride by prescription, and with zirconium oxychloride: deionized water is made zirconyl chloride solution in 1: 50～80 ratio;
(3) B that step 1 is obtained
4The zirconyl chloride solution that C and C powder mixing suspension and step 2 obtain is mixed, and magnetic agitation, and dropping ammonia dropwise make the abundant hydrolytic precipitation of zirconium oxychloride, up to the pH value greater than 9;
(4) use suspensoid solid-liquid separation centrifugal or that method of pumping filtration obtains step 3, and wash with water, remove NH
4 +And Cl
-, put into baking oven afterwards after 80～100 ℃ of oven dry, cross 100 mesh sieves;
(5) powder that step 4 is obtained is put into graphite or alumina crucible, reacts synthetic in vacuum oven, the argon shield of flowing, and 1500～1600 ℃ of synthesis temperatures are incubated 0.5～4 hour;
(6) powder that then step 5 is obtained is further levigate, crosses 300～500 mesh sieves, promptly obtains content greater than 99%, and granularity is the ZrB of micron or submicron order
2Powder.
Utilize the present invention can utilize cheap feed oxygen zirconium chloride and simple production unit, just can synthesize in large quantity high-purity (＞99wt%), the zirconium biboride powder of ultra-fine (micron or submicron).Detect through XRD, main component is ZrB in the powder
2, particle such as is at axle shape shape.
The present invention is simple and easy to do, productive rate is high, purity is high, efficient is high, be fit to commercial scale production.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
(1). raw material:
Zirconium oxychloride (ZrOCl
2,～300 orders, purity＞99%), boron carbide powder (B
4C, 3.5 μ m, purity＞99%), activated carbon powder (analytical pure), ammoniacal liquor (analytical pure).
(2). proportioning (mol ratio, down together):
Proportioning raw materials is: ZrOCl
2: B
4C: C=1: (0.4～0.8): (1.4～1.8)
(3). by prescription weigh batching in (2).At first with B
4C and C powder are put into beaker, press solid: H
2O=1: 50～80 ratio adds deionized water, stirs 0.5～1h, and the pH value is adjusted to 2～5, obtains B
4C and C powder mixing suspension.
(4). takes by weighing zirconium oxychloride by prescription in (2), and with zirconium oxychloride: deionized water is made zirconyl chloride solution in 1: 50～80 ratio.
(5). with the B in (3)
4Zirconyl chloride solution in C and C powder mixing suspension and (4) is mixed, and magnetic agitation, and dropping ammonia dropwise make the abundant hydrolytic precipitation of zirconium oxychloride, up to the pH value greater than 9.
(6). use centrifugal or method of pumping filtration to make suspensoid solid-liquid separation in (5), and wash with water 3 times, remove NH
4 +And Cl
-Put into baking oven afterwards after 80～100 ℃ of thorough oven dry, cross 100 mesh sieves.
(7). the powder in the process (6) is put into graphite or alumina crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1500～1600 ℃ of synthesis temperatures are incubated 0.5～4 hour.
(8). then that the powder that obtains in (7) is further levigate, can adopt ball milling method or stir the method for grinding, cross 300～500 mesh sieves, can obtain content greater than 99%, granularity is the ZrB of micron or submicron order
2Powder.
Embodiment one:
Select for use prescription to be: ZrOCl
2: B
4C: C=1: 0.5: 1.5 (mol ratio).At first, according to prescription weighing B
4C and carbon dust are put into beaker, press solid: H
2O=1: 50 ratio adds deionized water, its pH value is adjusted to 2～5, then dispersed with stirring 30min.Other gets a beaker, takes by weighing zirconium oxychloride according to prescription, presses zirconium oxychloride: H
2O=1: 80 ratio adds deionized water, and zirconium oxychloride is fully dissolved, and obtains transparent solution.To disperse back B
4The suspension of C and carbon dust and zirconyl chloride solution are mixed, adopt magnetic agitation, dropwise drip the ammoniacal liquor of 25% concentration while stirring in mixing solutions, make the abundant hydrolytic precipitation of zirconium oxychloride, up to the pH value greater than 9.Then with the suspension suction filtration, and wash repeatedly 3 times.Put into baking oven then, 100 ℃ of fully oven dry.The powder of oven dry is crossed 100 mesh sieves, put into alumina crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1550 ℃ of synthesis temperatures are incubated 1 hour.Taking-up synthetic powder is put into ball grinder, and fully ball milling is levigate, crosses 300 mesh sieves, can obtain ZrB
2Powder.Through correlation analysis as can be known, resulting powder main component is ZrB
2, purity is 99.2wt%, median size is 1.2 μ m.
Embodiment two:
Select for use prescription to be: ZrOCl
2: B
4C: C=1: 0.55: 1.5 (mol ratio).At first, according to prescription weighing B
4C and carbon dust are put into beaker, press solid: H
2O=1: 60 ratio adds deionized water, its pH value is adjusted to 2～5, then dispersed with stirring 1h.Other gets a beaker, takes by weighing zirconium oxychloride according to prescription, presses zirconium oxychloride: H
2O=1: 60 ratio adds deionized water, and zirconium oxychloride is fully dissolved, and obtains transparent solution.To disperse back B
4The suspension of C and carbon dust and zirconyl chloride solution are mixed, adopt magnetic agitation, dropwise drip the ammoniacal liquor of 25% concentration while stirring in mixing solutions, make the abundant hydrolytic precipitation of zirconium oxychloride, up to the pH value greater than 9.Then with the suspension suction filtration, and wash repeatedly 3 times.Put into baking oven then, 100 ℃ of fully oven dry.The powder of oven dry is crossed 100 mesh sieves, put into plumbago crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1500 ℃ of synthesis temperatures are incubated 4 hours.It is fully levigate that taking-up synthetic powder is put into the stirring mill, crosses 300 mesh sieves, can obtain ZrB
2Powder.Through correlation analysis as can be known, resulting powder main component is ZrB
2, purity is 99.0wt%, median size is 0.8 μ m.
Embodiment three:
Select for use prescription to be: ZrOCl
2: B
4C: C=1: 0.6: 1.65 (mol ratio).At first, according to prescription weighing B
4C and carbon dust are put into beaker, press solid: H
2O=1: 80 ratio adds deionized water, its pH value is adjusted to 2～5, then dispersed with stirring 1h.Other gets a beaker, takes by weighing zirconium oxychloride according to prescription, presses zirconium oxychloride: H
2O=1: 50 ratio adds deionized water, and zirconium oxychloride is fully dissolved, and obtains transparent solution.To disperse back B
4The suspension of C and carbon dust and zirconyl chloride solution are mixed, adopt magnetic agitation, dropwise drip the ammoniacal liquor of 25% concentration while stirring in mixing solutions, make the abundant hydrolytic precipitation of zirconium oxychloride, up to the pH value greater than 9.Then with the suspension suction filtration, and wash repeatedly 3 times.Put into baking oven then, 80 ℃ of fully oven dry.The powder of oven dry is crossed 100 mesh sieves, put into plumbago crucible, in vacuum oven, react synthetic, the argon shield of flowing, 1600 ℃ of synthesis temperatures are incubated 1 hour.It is fully levigate that taking-up synthetic powder is put into the stirring mill, crosses 300 mesh sieves, can obtain ZrB
2Powder.Through correlation analysis as can be known, resulting powder main component is ZrB
2, purity is 99.5wt%, median size is 1.5 μ m.
Claims (1)
1, a kind of preparation method of high purity ultra fine zirconium biboride powder is characterized in that: described method contains following steps:
(1) raw material is: zirconium oxychloride (ZrOCl
28H
2O), norbide (B
4C) and carbon dust (C);
(2) the material molar ratio proportioning is: ZrOCl
2: B
4C: C=1: (0.4～0.8): (1.4～1.8);
(3) set by step prescription weigh batching in (2): at first with B
4C and C powder are put into beaker, press solid: H
2O=1: 50～80 ratio adds deionized water, stirs, and the pH value is adjusted to 2～5, obtains B
4The mixing suspension of C and C powder;
(4) set by step prescription takes by weighing zirconium oxychloride in (2), and in zirconium oxychloride: the ratio of deionized water=1: 50～80, zirconium oxychloride is fully dissolved, make zirconyl chloride solution;
(5) B that step (3) is obtained
4The zirconyl chloride solution that C and C powder mixing suspension and step (4) obtain is mixed, and magnetic agitation, and dropping ammonia dropwise make the abundant hydrolytic precipitation of zirconium oxychloride, up to the pH value greater than 9;
(6) use centrifugal or method of pumping filtration makes the suspensoid solid-liquid separation that obtains in the step (5), and wash with water, remove NH
4+And Cl
-, put into baking oven afterwards after 80～100 ℃ of oven dry, cross 100 mesh sieves;
(7) powder that step (6) is obtained is put into graphite or aluminum oxide mandarin orange pot, reacts synthetic in vacuum oven, the atmosphere gas shiled of flowing, and 1500～1600 ℃ of synthesis temperatures are incubated 0.5～4 hour;
(8) powder that then step (7) is obtained is further levigate, crosses the 300-500 mesh sieve, promptly obtains content greater than 99%, and granularity is the ZrB of micron or submicron order
2Powder.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486577B (en) * | 2009-02-24 | 2012-03-28 | 武汉理工大学 | Preparation of nano zirconium diboride ceramic powder |
| CN101774601B (en) * | 2010-01-29 | 2012-07-04 | 北京航空航天大学 | Method for preparing ZrB2 powder by adopting sol-gel method |
| CN101830478B (en) * | 2010-04-02 | 2011-06-22 | 北京航空航天大学 | Method for synthesizing submicron ZrB2 powder by using boron thermal reduction and carbon thermal reduction coordinate regulation |
| CN101914810B (en) * | 2010-08-16 | 2012-05-02 | 山东大学 | Zirconium diboride whisker material and preparation method thereof |
| CN102557642B (en) * | 2010-12-08 | 2013-03-27 | 中国科学院金属研究所 | Preparation method for synthesizing zirconium boride powder material by zirconium-containing organic matter precursor |
| CN103708485B (en) * | 2013-12-26 | 2017-01-18 | 湖南稀土金属材料研究院 | Preparation method of scandium diboride |
| CN103754891B (en) * | 2014-01-09 | 2016-02-10 | 航天材料及工艺研究所 | The method of a kind of boron/carbothermic method low-temperature growth hafnium boride powder |
| CN104045093B (en) * | 2014-06-18 | 2016-04-06 | 陕西科技大学 | A kind of microwave hydrothermal auxiliary preparation nanometer ZrB 2the method of powder |
| CN106631004B (en) * | 2016-12-26 | 2019-07-12 | 湖南先导电子陶瓷科技产业园发展有限公司 | A kind of technique that improved liquid-phase precipitation method prepares high-purity superfine barium titanate |
| CN109019676B (en) * | 2018-10-10 | 2022-03-11 | 湖北天瓷电子材料有限公司 | Method for preparing high-purity nano-grade barium titanate by precipitation method |
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| CN1317519A (en) * | 2001-03-30 | 2001-10-17 | 中国核动力研究设计院 | Process for preparing superfine powder of ZrB2 or TiB2 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317519A (en) * | 2001-03-30 | 2001-10-17 | 中国核动力研究设计院 | Process for preparing superfine powder of ZrB2 or TiB2 |
| CN1699168A (en) * | 2005-05-23 | 2005-11-23 | 哈尔滨工业大学 | Combustion synthesis method of zirconium diboride micro-powder |
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| Title |
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| Zr-B体系自蔓延高温合成ZrB2陶瓷粉末. 方舟，王皓，傅正义.硅酸盐学报，第32卷第8期. 2004 * |
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