CN102964126A - Preparation method of h-BN/VB2 processable ceramic - Google Patents

Preparation method of h-BN/VB2 processable ceramic Download PDF

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CN102964126A
CN102964126A CN2012105360786A CN201210536078A CN102964126A CN 102964126 A CN102964126 A CN 102964126A CN 2012105360786 A CN2012105360786 A CN 2012105360786A CN 201210536078 A CN201210536078 A CN 201210536078A CN 102964126 A CN102964126 A CN 102964126A
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ceramic
powder
processable
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coated
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CN102964126B (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/VB2 processable ceramic, which is characterized in that h-BN-coated VB2 ceramic powder is subjected to cold isostatic compaction, and fired by hot pressing to obtain the h-BN/VB2 processable ceramic. The preparation method comprises the following steps: proportionally and evenly mixing boric acid and urea in a weight ratio of 2:1, adding 30-60% ethanol, heating the mixture in a closed container at 50-90 DEG C for 10-24 hours, and mixing for 10-30 minutes to obtain an esterification solution; adding 40-70% VB2 ceramic powder into the 30-60% esterification solution to obtain a ceramic slurry; preparing the ceramic slurry into coated VB2 powder with the diameter of 0.01-0.5mm by using a spray granulator; nitridizing the coated VB2 powder at 600-1000 DEG C for 30-60 minutes in a nitrogen atmosphere to obtain h-BN-coated VB2 ceramic powder; carrying out isostatic compaction on the h-BN-coated VB2 ceramic powder under the pressure of 100-200MPa to obtain the 60*(10-20)mm laminar blank; and carrying out hot pressing at 1700-1850 DEG C for 30-180 minutes in a nitrogen atmosphere under the pressure of 5-100MPa to fire the h-BN/VB2 processable ceramic. The processable ceramic prepared by the method provided by the invention has the advantages of even h-BN phase distribution, controllable content, favorable processability, favorable mechanical properties and favorable thermal properties.

Description

A kind of h-BN/VB 2The preparation method of processable ceramic
Technical field
The present invention relates to a kind of h-BN/VB 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/VB 2The preparation method of processable ceramic.Its technical scheme is:
A kind of h-BN/VB 2The preparation method of processable ceramic adopts h-BN to coat the hot pressing behind cold isostatic compaction of VB2 ceramic powder and burns till h-BN/VB 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 VB 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 VB that diameter is 0.01 ~ 0.5mm 2Powder is with above-mentioned coating VB 2Powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ * 30 ~ 60 minutes obtains h-BN coating VB in temperature 2Ceramic powder coats VB 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/VB 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/VB2 processable ceramic uniform microstructure, and intensity is high, and global reliability is high;
2, can be at VB by this cladding process 2Grain surface forms the h-BN layer of even thickness, and the thickness of h-BN layer is controlled, prepared h-BN/VB 2The bending strength of processable ceramic is compared with mixing, chemical method and is improved 1.5 times;
3, h-BN/VB 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 VB 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 VB that diameter is 0.5mm 2Powder is with above-mentioned coating VB 2Powder is that nitrogen atmosphere nitrogenize in 600 ℃ * 30 minutes obtains h-BN coating VB in temperature 2Ceramic powder coats VB 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/VB under 1700 ℃ * 30 minutes nitrogen atmospheres 2Processable ceramic.
The purity of testing used proportion material is technical pure, and the bending strength of the h-BN/ VB2 processable ceramic that obtains is 587MPa..
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 VB 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 VB that diameter is 0.2mm 2Powder is with above-mentioned coating VB 2Powder is that nitrogen atmosphere nitrogenize in 800 ℃ * 45 minutes obtains h-BN coating VB in temperature 2Ceramic powder coats VB 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/VB under 1800 ℃ * 105 minutes nitrogen atmospheres 2Processable ceramic.
The purity of testing used proportion material is technical pure, the h-BN/ VB that obtains 2The bending strength of processable ceramic is 524MPa..
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 VB 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 VB that diameter is 0.01mm 2Powder is with above-mentioned coating VB 2Powder is that nitrogen atmosphere nitrogenize in 1000 ℃ * 60 minutes obtains h-BN coating VB2 ceramic powder in temperature, and h-BN is coated VB 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/VB under 1850 ℃ * 180 minutes nitrogen atmospheres 2Processable ceramic.
The purity of testing used proportion material is technical pure, the h-BN/ VB that obtains 2The bending strength of processable ceramic is 490MPa..

Claims (1)

1. h-BN/VB 2The preparation method of processable ceramic is characterized in that: adopt h-BN to coat VB 2H-BN/ VB 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 VB 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 VB that diameter is 0.01 ~ 0.5mm 2Powder is with above-mentioned coating VB 2Powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ * 30 ~ 60 minutes obtains h-BN coating VB in temperature 2Ceramic powder coats VB 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/ VB under 1700 ~ 1850 ℃ * 30 ~ 180 minutes nitrogen atmospheres 2Processable ceramic.
CN201210536078.6A 2012-12-13 2012-12-13 Preparation method of h-BN/VB2 processable ceramic Expired - Fee Related CN102964126B (en)

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Cited By (1)

* 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

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 (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
CN103864430B (en) * 2012-12-13 2015-03-18 山东理工大学 h-BN/Cr3C2 machinable ceramic preparation method

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