CN100460357C - Method for synthesizing zirconium diboride/aluminium oxide composite powder - Google Patents
Method for synthesizing zirconium diboride/aluminium oxide composite powder Download PDFInfo
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- CN100460357C CN100460357C CNB200610117280XA CN200610117280A CN100460357C CN 100460357 C CN100460357 C CN 100460357C CN B200610117280X A CNB200610117280X A CN B200610117280XA CN 200610117280 A CN200610117280 A CN 200610117280A CN 100460357 C CN100460357 C CN 100460357C
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- Prior art keywords
- aluminium oxide
- composite powder
- zirconium diboride
- oxide composite
- ball
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Abstract
The invention is a zirconium diboride/dialuminum trioxide composite powder synthesizing method, belonging to the technical field of ceramics and fireproof materials, comprising the steps of: a) batching Al, ZrO2 and B2O3 powders as raw materials in the molar ratio of 10 to 3 to 3; b) premixing and taking and loading the mixture into the ball-milling tank of a high-energy ball mill, vacuumizing and charging argon gas, and ball- milling with bearing balls, where the ratio of balls to material is 10:(1-1.5); c) ball-milling at 500-600r/min for 2-5 h, and making it. And the invention has characters of simple process, low equipment investment, cheap raw materials, low synthesis cost, fine powder particles, etc. and it can be applied to ceramic and fireproof industries.
Description
Technical field
What the present invention relates to is the synthetic method of a kind of pottery, technical field of refractory materials, specifically is a kind of synthetic method of zirconium diboride/aluminium oxide composite powder.
Background technology
Zirconium diboride (ZrB
2) pottery has the performance of high fusing point, high hardness, fabulous specific conductivity and thermal conductivity, splendid anti-fusion non-ferrous metal, cryolite and heat-resistant impact ability etc.As ultrahigh-temperature structured material, noble electrode, high temperature electrical material, hard tool material, abrasive material, Wimet additive and wear parts etc.ZrB
2Be covalent linkage, sintering character is relatively poor, and conventional sintering method is difficult to densified sintering product.For this reason, material supplier author has attempted a lot of methods and has improved sintering character, and adding other component formation compound system is modal method.Aluminium sesquioxide (Al
2O
3) ceramic applications is extensive, but that shortcoming is a thermal shock resistance is relatively poor, is easy to cracking, damage under the thermal shocking effect.And ZrB
2Have fabulous thermal conductivity, thereby thermal shock resistance is better.For this reason, Al
2O
3Add ZrB to
2The middle compound system of forming had both improved ZrB
2The sintering character of pottery is improved Al again
2O
3The poor shortcoming of self thermal shock resistance.
Find through literature search, in the strong " ZrB that delivers in " silicate journal " (2005, the fourth phase, the 407-410 page) that waits of will prior art
2/ Al
2O
3Synthetic and the sign of self propagating high temperature reduction of composite granule ", propose in this article to adopt from spreading method, synthesize ZrB
2/ Al
2O
3Composite granule, concrete grammar is: with boron trioxide (B
2O
3), zirconium dioxide (ZrO
2) and metallic reducing agent aluminium (Al) be raw material, ball milling, briquetting, at the argon shield down-firing from spreading the ZrB that generates 1-5 microns of particle diameters
2/ Al
2O
3Composite granule.Its deficiency is: processing step complexity, powder granule micron order, and fine not enough, become to produce the cost height.
Summary of the invention
The objective of the invention is at the problems referred to above, proposed a kind of synthetic method of zirconium diboride/aluminium oxide composite powder, promptly adopt high-energy ball milling technology to synthesize ZrB
2/ Al
2O
3The method of composite granule, high-energy ball milling method equipment and technology are simple, and production cost is low, can prepare nanometer grade powder, is easy to sintering.
The present invention is achieved by the following technical solutions, and concrete steps are:
A) raw material adopts metal A l, ZrO
2And B
2O
3Powder, press the following formula batching:
10Al+3B
2O
3+3ZrO
2＝3ZrB
2+5Al
2O
3
Al, ZrO
2And B
2O
3The mol ratio of powder is 10:3:3.Metallic aluminium purity is greater than 99%, and particle diameter is less than 50 microns; ZrO
2Purity is greater than 99%, and particle diameter is less than 15 microns; B
2O
3Purity is greater than 98%, and particle diameter is less than 50 microns.
Pack into ball grinder on the high energy ball mill of material is got in pre-mixing 3 hours.
B) vacuumize logical argon gas, abrading-ball adopts bearing steel ball, 5 millimeters of diameters, ratio of grinding media to material 10:1-1.5.
C) ball milling is 2-5 hours, and rotating speed is 500-600 rev/mins.Obtain ZrB
2/ Al
2O
3Composite granule.
High-energy ball milling method is by the synthetic ZrB of mechanical alloying principle
2/ Al
2O
2Composite granule, high rotating speed increases the energy of powder collision.
The present invention has substantive distinguishing features, and by high-energy ball milling technology, metallic aluminium, zirconium dioxide and boron trioxide powder are raw material, synthetic ZrB
2/ Al
2O
3Composite granule.Preparation technology is simple, and equipment drops into little, and raw material is cheap, and synthetic cost is low, and powder granule is fine, Al in the composite granule
2O
3Grain diameter reaches nano level, is easy to sintering.This powder can be applicable to pottery, refractories industry.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
The high-energy ball milling equipment that adopts in the present embodiment is the GN type high energy ball mill that Ke Yuan mechanical ﹠ electrical equipment factory, Shenyang City produces, excitation of direct current generator voltage: 220V/2A, armature voltage: 0--110V/2A, power of motor: 308W.Ball grinder material: GCr15 bearing steel, maximum charging capacity :≤30g.Voltage of alternating current is adjustable from 0-110V, voltage and synchronization increase and decrease.
Embodiment 1:
Raw material: metallic aluminium purity 99.2%, 40-50 microns, ZrO
2Purity 99.5%, 5-10 microns, B
2O
3Purity 99.3%, 40-50 microns.Press Al, ZrO
2And B
2O
3Mol ratio 10:3:3 batching, premix 3 hours is got pack into ball grinder on the high energy ball mill of 15 gram material, ratio of grinding media to material 10:1, rotating speed are 560 rev/mins, 3 hours.
Resulting ZrB
2/ Al
2O
3The composite granule technical indicator is:
Purity 96.5-98.5%, ZrB
2Particle diameter is 850-1000 nanometers, Al
2O
3Particle diameter is 65-85 nanometers.
Embodiment 2:
Raw material: metallic aluminium purity 99.1%, 40-50 microns, ZrO
2Purity 99.3%, 3-5 microns, B
2O
3Purity 98.5%, 15-25 microns.Press Al, ZrO
2And B
2O
3Mol ratio 10:3:3 batching, premix 3 hours is got pack into ball grinder on the high energy ball mill of 18 gram material, ratio of grinding media to material 10:1, rotating speed are 560 rev/mins, 5 hours.
Resulting ZrB
2/ Al
2O
3The composite granule technical indicator is:
Purity is 96-98%, ZrB
2Particle diameter is 600-800 nanometers, Al
2O
3Particle diameter is 35-50 nanometers.
Embodiment 3:
Raw material: metallic aluminium purity 99.1%, 40-50 microns, ZrO
2Purity 99.3%, 5-8 microns, B
2O
3Purity 98.5%, 25-35 microns.Press Al, ZrO
2And B
2O
3Mol ratio 10:3:3 batching, premix 3 hours is got pack into ball grinder on the high energy ball mill of 12 gram material, ratio of grinding media to material 10:1, rotating speed are 560 rev/mins, 2 hours.
Resulting ZrB
2/ Al
2O
3The composite granule technical indicator is:
Purity is 96-98%, ZrB
2Particle diameter is 1500-3000 nanometers, Al
2O
3Particle diameter is 90-125 nanometers.
Claims (4)
1. the synthetic method of a zirconium diboride/aluminium oxide composite powder is characterized in that concrete steps are:
A) raw material adopts metal A l, ZrO
2And B
2O
3Powder is pressed Al, ZrO
2And B
2O
3The mol ratio of powder is the 10:3:3 batching;
B) pre-mixing is 3 hours, gets pack into ball grinder on the high energy ball mill of premix, vacuumizes logical argon gas, and abrading-ball adopts bearing steel ball, and diameter is 5 millimeters, ratio of grinding media to material 10:1-1.5;
C) to b) in premix ball milling 2-5 hours on high energy ball mill, rotating speed is 500-600 rev/mins, obtains zirconium diboride/aluminium oxide composite powder.
2. the synthetic method of zirconium diboride/aluminium oxide composite powder according to claim 1 is characterized in that, described metal A l purity is greater than 99%, and particle diameter is less than 50 microns.
3. the synthetic method of zirconium diboride/aluminium oxide composite powder according to claim 1 is characterized in that, described ZrO
2Purity is greater than 99%, and particle diameter is less than 15 microns.
4. the synthetic method of zirconium diboride/aluminium oxide composite powder according to claim 1 is characterized in that, described B
2O
3Purity is greater than 98%, and particle diameter is less than 50 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610117280XA CN100460357C (en) | 2006-10-19 | 2006-10-19 | Method for synthesizing zirconium diboride/aluminium oxide composite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610117280XA CN100460357C (en) | 2006-10-19 | 2006-10-19 | Method for synthesizing zirconium diboride/aluminium oxide composite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1935737A CN1935737A (en) | 2007-03-28 |
| CN100460357C true CN100460357C (en) | 2009-02-11 |
Family
ID=37953510
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|---|---|---|---|
| CNB200610117280XA Expired - Fee Related CN100460357C (en) | 2006-10-19 | 2006-10-19 | Method for synthesizing zirconium diboride/aluminium oxide composite powder |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182212B (en) * | 2007-11-06 | 2010-04-07 | 武汉理工大学 | YAG/ZrB2 series multi-phase ceramics and preparation method thereof |
| CN101423413B (en) * | 2008-11-27 | 2011-09-21 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing ZrB2-Al2O3 composite powder |
| CN105130446A (en) * | 2015-09-01 | 2015-12-09 | 广西南宁智翠科技咨询有限公司 | High-strength zirconium boride ceramic and preparing method thereof |
| CN105236989B (en) * | 2015-09-11 | 2017-07-07 | 洛阳布鲁姆电子科技有限公司 | A kind of high-strength high-temperature zirconium boride ceramic and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587188A (en) * | 2004-07-08 | 2005-03-02 | 复旦大学 | Process for synthesizing high purity zirconium diboride-aluminium oxide Al2O3 ceramic composite powder in one step |
| CN1699168A (en) * | 2005-05-23 | 2005-11-23 | 哈尔滨工业大学 | Combustion synthesis method of zirconium diboride micro-powder |
-
2006
- 2006-10-19 CN CNB200610117280XA patent/CN100460357C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587188A (en) * | 2004-07-08 | 2005-03-02 | 复旦大学 | Process for synthesizing high purity zirconium diboride-aluminium oxide Al2O3 ceramic composite powder in one step |
| CN1699168A (en) * | 2005-05-23 | 2005-11-23 | 哈尔滨工业大学 | Combustion synthesis method of zirconium diboride micro-powder |
Non-Patent Citations (10)
| Title |
|---|
| ZrB2在无机非金属材料中的应用现状. 熊金松.武汉科技大学学报（自然科学版），第29卷第3期. 2006 |
| ZrB2在无机非金属材料中的应用现状. 熊金松.武汉科技大学学报（自然科学版），第29卷第3期. 2006 * |
| 燃烧合成ZrB2/Al2O3复合粉体及其界面分析. 于志强.复合材料学报，第22卷第4期. 2005 |
| 燃烧合成ZrB2/Al2O3复合粉体及其界面分析. 于志强.复合材料学报，第22卷第4期. 2005 * |
| 高能球磨在材料制备领域的工业化应用. 马明亮.热加工工艺（热处理版），第35卷第6期. 2006 |
| 高能球磨在材料制备领域的工业化应用. 马明亮.热加工工艺（热处理版），第35卷第6期. 2006 * |
| 高能球磨法及其在纳米晶磁性材料制备中的应用（一）. 肖军.磁性材料及器件，第36卷第1期. 2005 |
| 高能球磨法及其在纳米晶磁性材料制备中的应用（一）. 肖军.磁性材料及器件，第36卷第1期. 2005 * |
| 高能球磨的机械合金化机理. 陈君平.机械，第31卷第3期. 2004 |
| 高能球磨的机械合金化机理. 陈君平.机械，第31卷第3期. 2004 * |
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| Publication number | Publication date |
|---|---|
| CN1935737A (en) | 2007-03-28 |
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Granted publication date: 20090211 Termination date: 20171019 |