CN102992776B - Preparation method of h-BN/VC machinable ceramic - Google Patents

Preparation method of h-BN/VC machinable ceramic Download PDF

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CN102992776B
CN102992776B CN2012105355523A CN201210535552A CN102992776B CN 102992776 B CN102992776 B CN 102992776B CN 2012105355523 A CN2012105355523 A CN 2012105355523A CN 201210535552 A CN201210535552 A CN 201210535552A CN 102992776 B CN102992776 B CN 102992776B
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ceramic
powder
coated
processable
coating
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CN102992776A (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 an h-BN/VC machinable ceramic. The method is characterized in that the h-BN/VC machinable ceramic is obtained via hot-pressing and sintering after a cold isostatic pressing process by using h-BN coated VC ceramic powder. The method comprises the steps of mixing boric acid, urea and ethanol in a sealed container according to a proportion to form an esterification solution; adding VC ceramic powder in the esterification solution to form ceramic slurry; making the ceramic slurry into coated VC powder by using a spray granulator; nitriding the coated VC powder to obtain the h-BN coated VC ceramic powder; pressing the h-BN coated VC ceramic powder into sheet green bodies via an isostatic pressing process; hot-pressing the sheet green bodies under a nitrogen atmosphere; and sintering into the h-BN/VC machinable ceramic. The machinable ceramic obtained by the method has uniform h-BN phase distribution, controllable content, good machinable property, good mechanical properties and excellent thermal properties.

Description

A kind of preparation method of h-BN/VC processable ceramic
Technical field
The present invention relates to a kind of h-BN/VC processable ceramic, belong to the ceramics processing field.
Background technology
Stupalith has many good performances, still, because stupalith hardness is large, while preparing the precise measure ceramic component, only has by the diamond abrasive wheel grinding, and manufacturing cost is very high.So people are finding a kind of method always, can meet 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 3With mol ratio 1:4, mix, after fully grinding in mortar, with high-purity Al 2O 3Powder (median size 03 μ m) is put into together plastic tank and be take dehydrated alcohol as medium, uses the aluminum oxide abrading-ball, and then the wet-milling batch mixing dries (stirring) simultaneously, then ball milling, under hydrogen atmosphere, makes Al 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 by TiB 2, BN and the weighing by a certain percentage of Ni powder, respectively with different mixing method batch mixings, by the mixed slurry dried and screened, and uniform compound is packed into and is scribbled in the graphite jig of BN, be placed in the plasma discharge hot pressing furnace and 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 under nitrogen atmosphere to fire and makes the AlN-h-BN processable ceramic in " low-dielectric loss AIN pottery and the research of BN-AIN base ceramic material ".In above-mentioned system except Si 3N 4The bending strength of-h-BN processable ceramic can reach beyond 950MPa., as TiB 2-h-BN, the anti-intensity of the processable ceramics such as AlN-h-BN also only has 154 MPa. left and right.The bending strength of the processable ceramics material that therefore adopts common mixing, chemical method h-BN coating technology to prepare is lower.
Summary of the invention
The object of the present invention is to provide and a kind ofly can overcome above-mentioned defect, realize preparing the more preparation method of high strength h-BN/VC processable ceramic.Its technical scheme is:
A kind of preparation method of h-BN/VC processable ceramic, adopt h-BN to coat the hot pressing after cold isostatic compaction of VC ceramic powder and burn till the h-BN/VC processable ceramic, and concrete grammar comprises the following steps:
The first step: by boric acid: urea be take the ratio that weight ratio is 2:1 and is evenly mixed, and additional 30 ~ 60% ethanol 50 ~ 90 ℃ of heat treated in encloses container stir after 10 ~ 24 hours again makes esterification solution in 10 ~ 30 minutes;
Second step: the VC ceramic powder 40 ~ 70% that is 0.1 ~ 2 μ m by granularity joins ball milling in 30 ~ 60% above-mentioned esterification solution and makes ceramic size, then by sponging granulator, above-mentioned ceramic size is made to the coating VC powder that diameter is 0.01 ~ 0.5mm, by above-mentioned coating VC powder, in temperature, be that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ * 30 ~ 60 minutes obtains h-BN coating VC ceramic powder, h-BN is coated to the VC ceramic powder and under the pressure of 100 ~ 200MPa., through isostatic cool pressing, make 60 * 10 ~ 20mm flake shaped base substrate, then under 1700 ~ 1850 ℃ * 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into the h-BN/VC processable ceramic.
Compared with prior art, its advantage is in the present invention:
1, the present invention produces h-BN/VC processable ceramic uniform microstructure, and intensity is high, and global reliability is high;
2, can form at the VC grain surface h-BN layer of even thickness by this cladding process, and the thickness of h-BN layer is controlled, the bending strength of prepared h-BN/VC processable ceramic is compared with mixing, chemical method and is improved 1.5 times;
3, the h-BN/VC processable ceramic has good antioxidant property, mechanical property and thermal property.
Embodiment
Embodiment 1
The first step: by boric acid: urea be take the ratio that weight ratio is 2:1 and is evenly mixed, and additional 30% ethanol 50 ℃ of heat treated in encloses container stir after 24 hours again makes esterification solution in 30 minutes;
Second step: the VC ceramic powder 70% that is 0.1 μ m by granularity joins in 30% esterification solution and makes ceramic size; then by sponging granulator, above-mentioned ceramic size is made to the coating VC powder that diameter is 0.5mm; by above-mentioned coating VC powder, in temperature, be that nitrogen atmosphere nitrogenize in 600 ℃ * 30 minutes obtains h-BN coating VC ceramic powder; h-BN is coated to the VC ceramic powder and at the inferior static pressure of the pressure of 100MPa., be pressed into 60 * 10 ~ 20mm flake shaped base substrate, then under 1700 ℃ * 30 minutes nitrogen atmospheres, hot pressing 5MPa. is fired into the h-BN/VC processable ceramic.
The purity of testing proportion material used is technical pure, and the bending strength of the h-BN/ VC processable ceramic obtained is 491MPa..
Embodiment 2
The first step: by boric acid: urea be take ratio that weight ratio is 2:1 and is evenly mixed additional 45% ethanol 70 ℃ of heat treated in encloses container and stir after 16 hours again and within 20 minutes, make esterification solution;
Second step: the VC ceramic powder 55% that is 1 μ m by granularity joins in 45% esterification solution and makes ceramic size; then by sponging granulator, above-mentioned ceramic size is made to the coating VC powder that diameter is 0.2mm; by above-mentioned coating VC powder, in temperature, be that nitrogen atmosphere nitrogenize in 800 ℃ * 45 minutes obtains h-BN coating VC ceramic powder; h-BN is coated to the VC ceramic powder and at the inferior static pressure of the pressure of 150MPa., be pressed into 60 * 10 ~ 20mm flake shaped base substrate, then under 1800 ℃ * 105 minutes nitrogen atmospheres, hot pressing 50MPa. is fired into the h-BN/VC processable ceramic.
The purity of testing proportion material used is technical pure, and the bending strength of the h-BN/ VC processable ceramic obtained is 426MPa..
Embodiment 3
The first step: by boric acid: urea be take the ratio that weight ratio is 2:1 and is evenly mixed, and additional 60% ethanol 90 ℃ of heat treated in encloses container stir after 10 hours again makes esterification solution in 10 minutes;
Second step: the VC ceramic powder 40% that is 2 μ m by granularity joins in 60% esterification solution and makes ceramic size; then by sponging granulator, above-mentioned ceramic size is made to the coating VC powder that diameter is 0.01mm; by above-mentioned coating VC powder, in temperature, be that nitrogen atmosphere nitrogenize in 1000 ℃ * 60 minutes obtains h-BN coating VC ceramic powder; h-BN is coated to the VC ceramic powder and at the inferior static pressure of the pressure of 200MPa., be pressed into 60 * 10 ~ 20mm flake shaped base substrate, then under 1850 ℃ * 180 minutes nitrogen atmospheres, hot pressing 100MPa. is fired into the h-BN/VC processable ceramic.
The purity of testing proportion material used is technical pure, and the bending strength of the h-BN/ VC processable ceramic obtained is 386MPa..

Claims (1)

1. the preparation method of a h-BN/VC processable ceramic is characterized in that: adopt h-BN to coat the hot pressing after cold isostatic compaction of VC ceramic powder and burn till the h-BN/VC processable ceramic, concrete grammar comprises the following steps:
The first step: by boric acid: urea be take the ratio that weight ratio is 2:1 and is evenly mixed, and additional 30 ~ 60% weight percent ethanol 50 ~ 90 ℃ of heat treated in encloses container stir after 10 ~ 24 hours again makes esterification solution in 10 ~ 30 minutes;
Second step: VC ceramic powder 40 ~ 70% weight percents that are 0.1 ~ 2 μ m by granularity join ball milling in the above-mentioned esterification solution of 30 ~ 60% weight percents and make ceramic size, then by sponging granulator, above-mentioned ceramic size is made to the coating VC powder that diameter is 0.01 ~ 0.5mm, by above-mentioned coating VC powder, in temperature, be that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ * 30 ~ 60 minutes obtains h-BN coating VC ceramic powder, h-BN is coated to the VC ceramic powder and under the pressure of 100 ~ 200MPa., through isostatic cool pressing, make 60 * 10 ~ 20mm flake shaped base substrate, then under 1700 ~ 1850 ℃ * 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into the h-BN/VC processable ceramic.
CN2012105355523A 2012-12-13 2012-12-13 Preparation method of h-BN/VC machinable ceramic Expired - Fee Related CN102992776B (en)

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CN103964855A (en) * 2014-04-02 2014-08-06 芜湖浙鑫新能源有限公司 Coated zirconium boride based core and preparation method thereof
CN103964857B (en) * 2014-04-02 2016-05-18 芜湖浙鑫新能源有限公司 A kind of cladded type boron nitride-base core and preparation method thereof
CN107382325B (en) * 2017-06-12 2020-04-21 金华中烨超硬材料有限公司 Polycrystalline cubic boron nitride composite sheet for high-end cutter and production method thereof

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CN1240640C (en) * 2004-04-14 2006-02-08 哈尔滨工业大学 Method preparing BN/SiO2 composite ceramics through dipping, and cracking precursor body
CN100387549C (en) * 2004-11-22 2008-05-14 刘书锋 Ultra-pressure sintered dense solid knife from polycrystalline integrated cubic boron nitride and production thereof
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