CN103011826A - Preparation method of h-BN/ZrB2 machinable ceramics - Google Patents

Preparation method of h-BN/ZrB2 machinable ceramics Download PDF

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CN103011826A
CN103011826A CN2012105359488A CN201210535948A CN103011826A CN 103011826 A CN103011826 A CN 103011826A CN 2012105359488 A CN2012105359488 A CN 2012105359488A CN 201210535948 A CN201210535948 A CN 201210535948A CN 103011826 A CN103011826 A CN 103011826A
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zrb
ceramic
zrb2
powder
ceramic powder
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CN103011826B (en
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唐竹兴
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Shandong University of Technology
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Shandong University of Technology
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Abstract

The invention relates to a preparation method of h-BN/ZrB2 machinable ceramics, which is characterized by performing cold isostatic compaction on an h-BN coated ZrB2 ceramic powder body, then performing hot compaction, and firing to obtain the h-BN/ZrB2 machinable ceramics. The preparation method comprises the following steps: proportionally mixing boric acid and urea with ethanol in a closed container, thus preparing an esterification solution; then, adding a ZrB2 ceramic powder body into the esterification solution, thus preparing ceramic slurry; preparing the ceramic slurry into a coated ZrB2 powder body through a spray granulator; nitridizing the coated ZrB2 powder body to obtain the h-BN coated ZrB2 ceramic powder body; performing isostatic compaction on the h-BN coated ZrB2 ceramic powder body to obtain a lamellar green body; and performing hot compaction under nitrogen atmosphere, and firing to obtain the h-BN/ZrB2 machinable ceramics. The machinable ceramics prepared by the invention are uniform in h-BN phase distribution, controllable in content and fine in machinability, mechanical properties and thermal properties.

Description

A kind of h-BN/ZrB 2The preparation method of processable ceramic
Technical field
The present invention relates to a kind of h-BN/ZrB 2Processable ceramic belongs to the ceramics processing field.
Background technology
Stupalith has many good performances, still, because stupalith hardness is large, during preparation precise measure ceramic component, only has by the diamond abrasive wheel grinding, and manufacturing cost is very high.So people are seeking a kind of method always, namely can satisfy the basic mechanical performance requirement and can carry out again the method that mechanical workout obtains the precise measure ceramic component.The nineties in 20th century, the people such as Japanese scholars Niihara adopt Si 3N 4Particle coats h-BN and prepares the high processable ceramic parts of intensity, for a new way has been opened up in the preparation of high-performance processable ceramic parts; 2002, Li Yongli etc. were at " the Al that nanometer BN coats 2O 3The preparation of composite powder and sintering character research thereof " the middle analytical reagent CO (N that adopts 2) 2And H 3BO 3Mix with mol ratio 1:4, after in mortar, fully grinding, with high-purity Al 2O 3Powder (median size 03 μ m) is put into plastic tank together take dehydrated alcohol as medium, uses the aluminum oxide abrading-ball, the wet-milling batch mixing, and then oven dry (stirring simultaneously), ball milling is made Al under hydrogen atmosphere again 2O 3-h-BN processable ceramic; The Dong Yan tinkling of pieces of jade in 2004 etc. are at " TiB 2The preparation technology of one BN complex phase ceramic and performance study " in TiB 2, BN and the by a certain percentage weighing of Ni powder, respectively with different mixing method batch mixings, with the mixed slurry dried and screened, and uniform compound packed into scribble in the graphite jig of BN, place the plasma discharge hot pressing furnace to carry out sintering in the protection of Ar gas and prepare TiB 2-h-BN processable ceramic parts; 2009, Zhang Juxian adopted boric acid and urea and AlN powder to be blended in to fire under the nitrogen atmosphere in " low-dielectric loss AIN pottery and the research of BN-AIN base ceramic material " and makes the AlN-h-BN processable ceramic.In above-mentioned system except Si 3N 4The bending strength of-h-BN processable ceramic can reach beyond the 950MPa., such as TiB 2-h-BN, the anti-intensity of the processable ceramics such as AlN-h-BN also only has about 154 MPa..Therefore adopt the bending strength of processable ceramics material of common mixing, the preparation of chemical method h-BN coating technology lower.
Summary of the invention
The object of the present invention is to provide and a kind ofly can overcome defects, realize preparing more high strength h-BN/ZrB 2The preparation method of processable ceramic.Its technical scheme is:
A kind of h-BN/ZrB 2The preparation method of processable ceramic adopts h-BN to coat ZrB 2H-BN/ZrB is burnt till in ceramic powder hot pressing behind cold isostatic compaction 2Processable ceramic, concrete grammar may further comprise the steps:
The first step: with boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, add 30 ~ 60% ethanol in encloses container 50 ~ 90 ℃ of heat treated after 10 ~ 24 hours restir made esterification solution in 10 ~ 30 minutes;
Second step: be the ZrB of 0.1 ~ 2 μ m with granularity 2Ceramic powder 40 ~ 70% joins in 30 ~ 60% the above-mentioned esterification solution ball milling and makes ceramic size, then by sponging granulator above-mentioned ceramic size is made the coating ZrB that diameter is 0.01 ~ 0.5mm 2Powder is with above-mentioned coating ZrB 2Powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ * 30 ~ 60 minutes obtains h-BN coating ZrB in temperature 2Ceramic powder coats ZrB with h-BN 2Ceramic powder is made 60 * 10 ~ 20mm flake shaped base substrate through isostatic cool pressing under the pressure of 100 ~ 200MPa., then hot pressing 5 ~ 100MPa. is fired into h-BN/ZrB under 1700 ~ 1850 ℃ * 30 ~ 180 minutes nitrogen atmospheres 2Processable ceramic.
The present invention compared with prior art, its advantage is:
1, the present invention produces h-BN/ZrB 2The processable ceramic uniform microstructure, intensity is high, and global reliability is high;
2, can form at the ZrB2 grain surface h-BN layer of even thickness by this cladding process, and the thickness of h-BN layer is controlled, prepared h-BN/ZrB 2The bending strength of processable ceramic is compared with mixing, chemical method and is improved 1 times;
3, h-BN/ZrB 2Processable ceramic has good antioxidant property, mechanical property and thermal property.
Embodiment
Embodiment 1
The first step: with boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, add 30% ethanol in encloses container 50 ℃ of heat treated after 24 hours restir made esterification solution in 30 minutes;
Second step: be the ZrB of 0.1 μ m with granularity 2Ceramic powder 70% joins in 30% the esterification solution and makes ceramic size, then by sponging granulator above-mentioned ceramic size is made the coating ZrB that diameter is 0.5mm 2Powder is with above-mentioned coating ZrB 2Powder is that nitrogen atmosphere nitrogenize in 600 ℃ * 30 minutes obtains h-BN coating ZrB in temperature 2Ceramic powder coats ZrB with h-BN 2Ceramic powder is pressed into 60 * 10mm flake shaped base substrate at the inferior static pressure of the pressure of 100MPa., and then hot pressing 5MPa. is fired into h-BN/ZrB under 1700 ℃ * 30 minutes nitrogen atmospheres 2Processable ceramic.
The purity of testing used proportion material is technical pure, the h-BN/ ZrB that obtains 2The bending strength of processable ceramic is 476MPa..
Embodiment 2
The first step: with boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, add 45% ethanol in encloses container 70 ℃ of heat treated after 16 hours restir made esterification solution in 20 minutes;
Second step: be the ZrB of 1 μ m with granularity 2Ceramic powder 55% joins in 45% the esterification solution and makes ceramic size, then by sponging granulator above-mentioned ceramic size is made the coating ZrB that diameter is 0.2mm 2Powder is with above-mentioned coating ZrB 2Powder is that nitrogen atmosphere nitrogenize in 800 ℃ * 45 minutes obtains h-BN coating ZrB in temperature 2Ceramic powder coats ZrB with h-BN 2Ceramic powder is pressed into 60 * 15mm flake shaped base substrate at the inferior static pressure of the pressure of 150MPa., and then hot pressing 50MPa. is fired into h-BN/ZrB under 1800 ℃ * 105 minutes nitrogen atmospheres 2Processable ceramic.
The purity of testing used proportion material is technical pure, the h-BN/ ZrB that obtains 2The bending strength of processable ceramic is 423MPa..
Embodiment 3
The first step: with boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, add 60% ethanol in encloses container 90 ℃ of heat treated after 10 hours restir made esterification solution in 10 minutes;
Second step: be the ZrB of 2 μ m with granularity 2Ceramic powder 40% joins in 60% the esterification solution and makes ceramic size, then by sponging granulator above-mentioned ceramic size is made the coating ZrB that diameter is 0.01mm 2Powder is with above-mentioned coating ZrB 2Powder is that nitrogen atmosphere nitrogenize in 1000 ℃ * 60 minutes obtains h-BN coating ZrB in temperature 2Ceramic powder coats ZrB with h-BN 2Ceramic powder is pressed into 60 * 20mm flake shaped base substrate at the inferior static pressure of the pressure of 200MPa., and then hot pressing 100MPa. is fired into h-BN/ZrB under 1850 ℃ * 180 minutes nitrogen atmospheres 2Processable ceramic.
The purity of testing used proportion material is technical pure, the h-BN/ ZrB that obtains 2The bending strength of processable ceramic is 439MPa..

Claims (1)

1. h-BN/ZrB 2The preparation method of processable ceramic is characterized in that: adopt h-BN to coat ZrB 2H-BN/ ZrB is burnt till in ceramic powder hot pressing behind cold isostatic compaction 2Processable ceramic, concrete grammar may further comprise the steps:
The first step: with boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, add 30 ~ 60% ethanol in encloses container 50 ~ 90 ℃ of heat treated after 10 ~ 24 hours restir made esterification solution in 10 ~ 30 minutes;
Second step: be the ZrB of 0.1 ~ 2 μ m with granularity 2Ceramic powder 40 ~ 70% joins in 30 ~ 60% the above-mentioned esterification solution ball milling and makes ceramic size, then by sponging granulator above-mentioned ceramic size is made the coating ZrB that diameter is 0.01 ~ 0.5mm 2Powder is with above-mentioned coating ZrB 2Powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ * 30 ~ 60 minutes obtains h-BN coating ZrB in temperature 2Ceramic powder coats ZrB with h-BN 2Ceramic powder is made 60 * 10 ~ 20mm flake shaped base substrate through isostatic cool pressing under the pressure of 100 ~ 200MPa., then hot pressing 5 ~ 100MPa. is fired into h-BN/ ZrB under 1700 ~ 1850 ℃ * 30 ~ 180 minutes nitrogen atmospheres 2Processable ceramic.
CN201210535948.8A 2012-12-13 2012-12-13 Preparation method of h-BN/ZrB2 machinable ceramics Expired - Fee Related CN103011826B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864430A (en) * 2012-12-13 2014-06-18 山东理工大学 h-BN/Cr3C2 machinable ceramic preparation method
CN104557050A (en) * 2014-12-20 2015-04-29 北京矿冶研究总院 ZrB with core-shell structure2-SiC/Si composite powder and preparation method thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 20090601 张薇 "热压烧结BN基复合陶瓷的力学与物理性能" , 第S2期 *
《稀有金属材料与工程》 20030730 王向东等 "可加工Si3N4/BN复相陶瓷的制备及性能研究" 第32卷, 第7期 *
张薇: ""热压烧结BN基复合陶瓷的力学与物理性能"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *
王向东等: ""可加工Si3N4/BN复相陶瓷的制备及性能研究"", 《稀有金属材料与工程》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864430A (en) * 2012-12-13 2014-06-18 山东理工大学 h-BN/Cr3C2 machinable ceramic preparation method
CN103864430B (en) * 2012-12-13 2015-03-18 山东理工大学 h-BN/Cr3C2 machinable ceramic preparation method
CN104557050A (en) * 2014-12-20 2015-04-29 北京矿冶研究总院 ZrB with core-shell structure2-SiC/Si composite powder and preparation method thereof

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