CN101182191B - Method for preparing rear-earth modified zirconium diboride/aluminum oxide composite powder - Google Patents

Method for preparing rear-earth modified zirconium diboride/aluminum oxide composite powder Download PDF

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CN101182191B
CN101182191B CN2007101704469A CN200710170446A CN101182191B CN 101182191 B CN101182191 B CN 101182191B CN 2007101704469 A CN2007101704469 A CN 2007101704469A CN 200710170446 A CN200710170446 A CN 200710170446A CN 101182191 B CN101182191 B CN 101182191B
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rare earth
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CN101182191A (en
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于志强
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Fudan University
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Abstract

The invention relates to a preparation method of zirconium/aluminum trioxide compound powder which has anti-oxidant property and easily-sintered surface which is coated by nanometer rare earth oxide. The method is characterized in that the method includes the steps as follows: 1), balling-milling zirconium dioxide ZrO2, diboron trioxide B2O3 and metal Aluminum Al powder uniformly and molding and shaping, placing in a self-propagating high temperature synthesizer at room temperature under the protection of argon, igniting and burning, and obtaining high pure ZrB2/Al2O3 ceramic compound powder after combustion products are grinded; 2) adding the ZrB2/Al2O3 ceramic compound powder in rare earth salt solution, mixing into uniform slurry, drying and obtaining the compound powder of precursor ZrB2/Al2O3 compound powder with the rare earth oxide coating layer; 3) sintering the compound powder at high temperature to obtain a final product. The invention has the advantages of simple operation, convenience and little energy and time consumption. The synthesized powder has the advantages of high purity, small grain, sintering easiness and good high temperature oxidation resistance.

Description

The method for preparing rare earth modified zirconium diboride/aluminium oxide composite powder
Technical field
The present invention relates to a kind of preparation method, relate in particular to a kind of method for preparing rare earth modified zirconium diboride/aluminium oxide composite powder with surface of excellent high temperature oxidation resistance and sintering character through the ceramic composite powder of rare earth parcel modification.
Background technology
Composite granule, especially the composite granule of surface parcel modification can improve material property significantly, is widely used in the hot coating field [1]Powder surface parcel one deck ultrafine powder in hard-to-sinter, easy oxidation can increase densification speed and density, and the high-temperature oxidation resistance that also can improve powder simultaneously is by extensive confirmation [2]
ZrB 2/ Al 2O 3Pottery is as the high temperature complex phase ceramic, has characteristics such as high fusing point, high intensity, high hardness and excellent erosion resistance, wear resistance because of it and in fields such as matrix material, refractory materials, high temperature resistant structure ceramics, obtains certain application.But ZrB under such ceramic post sintering difficulty, the high temperature 2The surface is prone to oxidation, thereby has limited the range of application of material.
ZrB 2/ Al 2O 3Powder is as ZrB 2/ Al 2O 3The stupalith raw material, its performance directly influences ZrB 2/ Al 2O 3The performance of stupalith.
Powder surface modification can reduce the reunion of powder, improves the sintering character of powder [3]At single-phase ZrB 2Powder surface wraps up the existing report of research of modification.As utilize the precipitator method at ZrB 2Powder surface parcel one deck ZrO 2, the sintering character of its coated powder is much better than pure ZrB 2Powder [4]ZrB at high temperature in addition 2The surface is prone to oxidation and generates B 2O 3, this will reduce the performance of material.At ZrB 2Powder surface is introduced a ceramic layer, when improving the powder sintering performance, also can improve ZrB 2The high-temperature oxidation resistance of powder surface.But at ZrB 2The complex phase ceramic surface is wrapped up the research of modification and is also seldom reported.Rare earth is owing to it has the character that the particular chemical structure demonstrates many uniquenesses.The existence of a small amount of rare earth can greatly influence the tissue and the performance of stupalith [5]Rare earth oxide is stablized the phase structure of stupalith with used as stabilizers, suppresses the growth of ceramic crystalline grain [6]As the sintering temperature of sintering aid reduction stupalith, improve the existing certain research of density of stupalith [7]But with the research also rarely seen report of rare earth oxide parcel modification complex phase ceramic powder with the performance of improving powder.Especially utilize rare earth oxide to ZrB 2/ Al 2O 3The research that modification is wrapped up on the composite granule surface does not appear in the newspapers so far.
Reference:
[1] Wu Qide, Wang Hao, Wang Ping. the application [J] of surface coating modification technology in ceramic technology. modern technologies pottery, 2000,4:18-21
[2] Zhang Ning eats red strong value such as the .PH of grade to Al (OH) 3And Y (OH) 3Co-precipitation parcel SiC particulate influence [J]. material and metallurgical journal, 2002,1 (1): 57-60
[3] Zhang Juxian, Yang Jingyi .Al such as high Long Qiao 2O 3And Y 2O 3Coated SiC composite particles preparation [J]. Journal of Inorganic Materials, 1999,14 (3): 380～384
[4] Song Jianrong, Liu Beibei .ZrB such as Li Junguo 2/ ZrO 2The discharge plasma sintering behavior [J] of composite granule. artificial lens journal, 2007,36 (3): 592～595
[5] Mu Baichun, Li Ming is by Xiang Qun etc. and rare earth is to Si 3N 4The influence [J] of pottery mechanical property and microstructure. Chinese rare-earth journal, 2000,18 (1): 38
[6] Zhao Xiaowei, Dong Lirong, Li Haibo etc. doping Y 2O 3To ZrO 2Powder effects of phase transition [J]. Jilin Normal University's journal, 2003,2:30～31
[7] Mu Baichun, Sun Xudong. rare earth is to Al 2O 3The influence of ceramic sintering temperature, microstructure and mechanical property [J]. Chinese rare-earth journal, 2002,20:104～107
Summary of the invention
The objective of the invention is to solve ZrB 2/ Al 2O 3Composite ceramic material is ZrB at high temperature 2The surface is prone to oxidation, and the deficiency of hard-to-sinter proposes that a kind of high-temperature oxidation resistance is good, the surface of easy-sintering is through the ZrB of rare earth oxide parcel modification 2/ Al 2O 3The preparation method of composite granule.
The method of the rare earth modified zirconium diboride/aluminium oxide composite powder of preparation that the present invention proposes is characterized in that it comprises the steps:
1) with particle diameter respectively less than 70 μ m, 150 μ m, the ZIRCONIUM DIOXIDE 99.5 ZrO of 150 μ m 2, boron trioxide B 2O 3Pressed 1: 1 with metallic aluminium Al powder: the 3-5 mass ratio mixes, and puts into the ball mill ball milling and does dark sparing, and ball-to-powder weight ratio is 2～3: 1～2, ball milling time 8～12h; Then compound is pressed down at the pressure of 5～20MPa and process 40～60% the base substrate that density is equivalent to theoretical density; Base substrate is positioned in the self propagating high temperature reduction synthetic reaction device with argon gas atmosphere protection carries out building-up reactions; Ignition source adopts the tungsten filament heating circle that is parallel to specimen surface; Reaction product can obtain high-purity ZrB through pulverizing, sieving 2/ Al 2O 3Ceramic composite powder;
2) with ZrB 2/ Al 2O 3Composite granule joins in the rare earths salt, presses ZrB 2/ Al 2O 3Composite granule: rare earths salt=1 gram: 10～50 milliliters ratio adds, and constant temperature stirs in 20～60 ℃, and the concentration of rare earths salt is 0.5～5mol/L; Then uniform slip is obtained the presoma ZrB of rare earth oxide integument through 100～120 ℃ of dryings 2/ Al 2O 3The composite granule of powder;
3) with step 2) composite granule that obtains is 400 ℃～850 ℃ calcinings, product.
Described rare-earth salts is with cerous nitrate (Ce (NO 3) 36H 2O), Yttrium trinitrate (Y (NO 3) 36H 2O), Lanthanum trinitrate (La (NO 3) 36H 2O) and neodymium nitrate (Nd (NO 3) 36H 2O) be best.
The present invention is with ZrB 2/ Al 2O 3Composite granule carries out the modification of surface rare earth oxide compound parcel to be handled, and preparation has the excellent high-temperature oxidation resistance and the rare earth modified ZrB of sintering character 2/ Al 2O 3Composite granule.This composite granule is because the rare earth oxide (fusing point of cerium oxide, yttrium oxide, lanthanum trioxide, Neodymium trioxide is respectively 1950 ℃, 2680 ℃, 2315 ℃, 2270 ℃) that parcel fusing point in surface is high, antioxidant property is good, makes ZrB 2/ Al 2O 3ZrB in the composite granule 2At high temperature not oxidized.The introducing of rare earth oxide simultaneously can also promote the sintering of composite granule, improves the density of sintered compact.
It is raw material that the present invention has adopted cheap and facile natural mineral, has guaranteed ZrB 2/ Al 2O 3The low cost of composite granule is synthetic.ZrB 2/ Al 2O 3Rare earth nitrate aqueous solution liquid phase packing technology is adopted in the modification of composite granule surface rare earth oxide compound parcel.This preparing method's technology is simple, easy to operate, less energy consumption, and low cost of manufacture is suitable for large-scale industrial production.
Embodiment
Below through specific embodiment the present invention is described further, but the present invention is not constituted any limitation.
Embodiment 1
Get the ZrO that particle diameter is 60～70 μ m 210g, the B of 140～150 μ m 2O 3The Al powder 40g of 10g and 100～150 μ m places ball mill to carry out mechanical dry and mixes 8h, and ball-to-powder weight ratio is 2: 1.Compound pressed down at 5MPa pressure process 40% the base substrate that density is equivalent to theoretical density.Place the self propagating high temperature reduction synthesizer of argon gas atmosphere protection to burn synthetic base substrate then.After the building-up reactions product ground and sieve, obtaining particle diameter is 6～10 μ mZrB 2/ Al 2O 3Ceramic composite powder.With 5g ZrB 2/ Al 2O 3Composite granule joins 50ml, and in the cerous nitrate of 0.5mol/L (Yttrium trinitrate, Lanthanum trinitrate, the neodymium nitrate) aqueous solution, temperature is 25 ℃, stirs.With uniform slip drying under 100 ℃, obtain the ZrB of the presoma parcel of integument then 2/ Al 2O 3The composite granule of powder.Through 450 ℃ (480 ℃, 780 ℃, 830 ℃) calcining, just obtained cerium oxide (yttrium oxide, lanthanum trioxide, Neodymium trioxide) parcel ZrB 2/ Al 2O 3The ZrB of the packaging type of composite particles 2/ Al 2O 3Composite granule.This wraps up composite granule, and cerium oxide (yttrium oxide, lanthanum trioxide, Neodymium trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.
Embodiment 2
Get the ZrO that particle diameter is 60～70 μ m 210g, the B of 140～150 μ m 2O 3The Al powder 50g of 10g and 100～150 μ m places ball mill to carry out mechanical dry and mixes 12h, and ball-to-powder weight ratio is 3: 1.Other conditions obtain this parcel composite granule equally with embodiment 1, and yttrium oxide (cerium oxide, lanthanum trioxide, Neodymium trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.
Embodiment 3
Get particle diameter and be respectively 60～65 μ m, 100～120 μ m, the ZrO of 100～150 μ m 2, B 2O 3With Al powder 30g, 30g and 120g place ball mill to carry out ball milling and do mixed 9h, and ball-to-powder weight ratio is 2: 1.Mixed material pressed down at 10MPa pressure process 50% the base substrate that density is equivalent to theoretical density.Place the self propagating high temperature reduction synthesizer of argon gas atmosphere protection to burn synthetic base substrate then.After the building-up reactions product ground and sieve, obtaining particle diameter is 6～8 μ mZrB 2/ Al 2O 3Ceramic composite powder.With 5g ZrB 2/ Al 2O 3Composite granule joins 100ml, and in the Yttrium trinitrate of 1mol/L (cerous nitrate, Lanthanum trinitrate, the neodymium nitrate) aqueous solution, temperature is 30 ℃, stirs.With uniform slip drying under 110 ℃, obtain the ZrB of the presoma parcel of integument then 2/ Al 2O 3The composite granule of powder.Through 500 ℃ (470 ℃, 800 ℃, 850 ℃) calcining, just obtained yttrium oxide (cerium oxide, lanthanum trioxide, Neodymium trioxide) parcel ZrB 2/ Al 2O 3The ZrB of the packaging type of composite particles 2/ Al 2O 3Composite granule.This wraps up composite granule, and yttrium oxide (cerium oxide, lanthanum trioxide, Neodymium trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.
Embodiment 4
Get the ZrO that particle diameter is 55～60 μ m 240g, the B of 85～100 μ m 2O 3The Al powder 160g of 40g and 120～150 μ m places ball mill to carry out mechanical dry and mixes 11h, and ball-to-powder weight ratio is 3: 2.Compound pressed down at 15MPa pressure process 55% the base substrate that density is equivalent to theoretical density.Place the self propagating high temperature reduction synthesizer of argon gas atmosphere protection to burn synthetic base substrate then.After the building-up reactions product ground and sieve, obtain the ZrB that particle diameter is 5～9 μ m 2/ Al 2O 3Ceramic composite powder.With 5g ZrB 2/ Al 2O 3Composite granule joins 150ml, and in the Lanthanum trinitrate of 2mol/L (cerous nitrate, Yttrium trinitrate, the neodymium nitrate) aqueous solution, temperature is 35 ℃, stirs.With uniform slip drying under 120 ℃, obtain the ZrB of the presoma parcel of integument then 2/ Al 2O 3The composite granule of powder.Through 820 ℃ (400 ℃, 550 ℃, 840 ℃) calcining, just obtained lanthanum trioxide (cerium oxide, yttrium oxide, Neodymium trioxide) parcel ZrB 2/ Al 2O 3The ZrB of the packaging type of composite particles 2/ Al 2O 3Composite granule.This wraps up composite granule, and lanthanum trioxide (cerium oxide, yttrium oxide, Neodymium trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.
Embodiment 5
Get particle diameter and be respectively 40～50 μ m, 75～85 μ m, the ZrO of 110～120 μ m 2, B 2O 3With Al powder 50g, 50g and 200g place ball mill to carry out ball milling and do mixed 12h, and ball-to-powder weight ratio is 3: 1.Mixed material pressed down at 20MPa pressure process 60% the base substrate that density is equivalent to theoretical density.Place the self propagating high temperature reduction synthesizer of argon gas atmosphere protection to burn synthetic base substrate then.After the building-up reactions product ground and sieve, obtain the ZrB that particle diameter is 5～7 μ m 2/ Al 2O 3Ceramic composite powder.With 5g ZrB 2/ Al 2O 3Composite granule joins 200ml, and in the neodymium nitrate of 4mol/L (cerous nitrate, Yttrium trinitrate, the Lanthanum trinitrate) aqueous solution, temperature is 40 ℃, stirs.With uniform slip drying under 120 ℃, obtain the ZrB of the presoma parcel of integument then 2/ Al 2O 3The composite granule of powder.Through 850 ℃ (550 ℃, 600 ℃, 820 ℃) calcining, just obtained Neodymium trioxide (cerium oxide, yttrium oxide, lanthanum trioxide) parcel ZrB 2/ Al 2O 3The ZrB of the packaging type of composite particles 2/ Al 2O 3Composite granule.This wraps up composite granule, and Neodymium trioxide (cerium oxide, yttrium oxide, lanthanum trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.
Embodiment 6
Get the ZrO that particle diameter is 30～40 μ m 240g, the B of 50～60 μ m 2O 3The Al powder 160g of 40g and 100～120 μ m places ball mill to carry out mechanical dry and mixes 12h, and ball-to-powder weight ratio is 3: 1.Compound pressed down at 20 MPa pressure process 60% the base substrate that density is equivalent to theoretical density.Place the self propagating high temperature reduction synthesizer of argon gas atmosphere protection to burn synthetic base substrate then.After the building-up reactions product ground and sieve, obtain the ZrB that particle diameter is 5～6 μ m 2/ Al 2O 3Ceramic composite powder.With 5g ZrB 2/ Al 2O 3Composite granule joins 250ml, and in the Yttrium trinitrate of 5mol/L (cerous nitrate, Lanthanum trinitrate, the neodymium nitrate) aqueous solution, temperature is 50 ℃, stirs.With uniform slip drying under 120 ℃, obtain the ZrB of the presoma parcel of integument then 2/ Al 2O 3The composite granule of powder.Through 700 ℃ (750 ℃, 830 ℃, 850 ℃) calcining, just obtained yttrium oxide (cerium oxide, lanthanum trioxide, Neodymium trioxide) parcel ZrB 2/ Al 2O 3The ZrB of the packaging type of composite particles 2/ Al 2O 3Composite granule.This wraps up composite granule, and yttrium oxide (cerium oxide, lanthanum trioxide, Neodymium trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.
Embodiment 7
Get the ZrO that particle diameter is 30～40 μ m 240g, the B of 50～60 μ m 2O 3The Al powder 120g of 40g and 100～120 μ m places ball mill to carry out mechanical dry and mixes 12h, and ball-to-powder weight ratio is 3: 1.Other conditions obtain this parcel composite granule equally with embodiment 6, and yttrium oxide (cerium oxide, lanthanum trioxide, Neodymium trioxide) parcel is even, fine and close, and integument thickness is about 20～30nm.

Claims (1)

1. the method for preparing rare earth modified zirconium diboride/aluminium oxide composite powder is characterized in that it comprises the steps:
1) with ZIRCONIUM DIOXIDE 99.5 ZrO 2, boron trioxide B 2O 3Mix by 1: 1: 3～5 mass ratioes with metallic aluminium Al powder; Putting into the ball mill ball milling does dark even; Ball-to-powder weight ratio is 2～3: 1～2, and ball milling time 8～12h presses down compound then and processes 40～60% the base substrate that density is equivalent to theoretical density at the pressure of 5～20MPa; Base substrate is positioned in the self propagating high temperature reduction synthetic reaction device with argon gas atmosphere protection carries out building-up reactions; Ignition source adopts the tungsten filament heating circle that is parallel to specimen surface, and reaction product can obtain high-purity ZrB through pulverizing, sieving 2/ Al 2O 3Ceramic composite powder;
2) with ZrB 2/ Al 2O 3Composite granule joins in the rare earths salt, presses ZrB 2/ Al 2O 3Composite granule: rare earths salt=1 gram: 10～50 milliliters ratio adds, and constant temperature stirs in 20～60 ℃, then uniform slip is obtained the presoma ZrB of rare earth oxide integument through 100～120 ℃ of dryings 2/ Al 2O 3The composite granule of powder;
3) with step 2) composite granule that obtains is 400 ℃～850 ℃ calcinings, the finished product;
Wherein, synthesis material ZrO 2, B 2O 3Be respectively with the Al particle diameter: ZrO 2Powder is less than 70 μ m, B 2O 3Powder is less than 150 μ m, and the Al powder is less than 150 μ m;
Rare-earth salts is the nitrate salt of yttrium, lanthanum, cerium and neodymium;
The concentration of rare earths salt is 0.5～5mol/L.
CN2007101704469A 2007-11-15 2007-11-15 Method for preparing rear-earth modified zirconium diboride/aluminum oxide composite powder Expired - Fee Related CN101182191B (en)

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CN102485690B (en) * 2010-12-03 2013-04-03 兰州理工大学 ZrO2/Al2O3 nano-grade multiphase ceramic material and preparation method thereof
CN102701246B (en) * 2012-05-08 2016-06-15 赣州博晶科技有限公司 A kind of preparation method of the rare earth modified aluminium oxide of high heat stability
CN103160148A (en) * 2013-03-13 2013-06-19 复旦大学 Surface-modified metal boride/Al2O3 multiphase ceramic powder and preparation method thereof
CN103408809A (en) * 2013-07-01 2013-11-27 芜湖市银鸿液压件有限公司 High-abrasion-resistance hydraulic sealing gasket and preparation method thereof
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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

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