CN103011826B - Preparation method of h-BN/ZrB2 machinable ceramics - Google Patents
Preparation method of h-BN/ZrB2 machinable ceramics Download PDFInfo
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- CN103011826B CN103011826B CN201210535948.8A CN201210535948A CN103011826B CN 103011826 B CN103011826 B CN 103011826B CN 201210535948 A CN201210535948 A CN 201210535948A CN 103011826 B CN103011826 B CN 103011826B
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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
Technical field
The present invention relates to a kind of h-BN/ZrB
2processable ceramic, belongs to ceramics processing field.
Background technology
Stupalith has many good performances, still, because stupalith hardness is large, while preparing precise measure ceramic component, only has by diamond abrasive wheel grinding, and manufacturing cost is very high.So people are finding a kind of method always, can meet basic mechanical performance requirement and can carry out again mechanical workout and obtain the method for precise measure ceramic component.The nineties in 20th century, the people such as Japanese scholars Niihara adopt Si
3n
4the coated h-BN of particle 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 is coated
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 fully grinding in mortar, with high-purity Al
2o
3(median size 03 μ m) puts into plastic tank take dehydrated alcohol as medium to powder together, uses aluminum oxide abrading-ball, and then 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 Ni powder weigh by a certain percentage, respectively with different mixing method batch mixings, by mixed slurry dried and screened, and uniform compound packed in the graphite jig that scribbles BN, be placed in 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 and fires and make 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.Therefore adopt the bending strength of processable ceramics material prepared by common mixing, chemical method h-BN coating technology lower.
Summary of the invention
The object of the present invention is to provide one can overcome above-mentioned defect, realize and prepare 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 the coated ZrB of h-BN
2h-BN/ZrB is burnt till in ceramic powder hot pressing after cold isostatic compaction
2processable ceramic, concrete grammar comprises the following steps:
The first step: by boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, and additional 30 ~ 60% ethanol 50 ~ 90 ℃ of heat treated in encloses container stir after 10 ~ 24 hours again makes esterification solution for 10 ~ 30 minutes;
Second step: be the ZrB of 0.1 ~ 2 μ m by granularity
2ceramic powder 40 ~ 70% 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 coated ZrB that diameter is 0.01 ~ 0.5mm
2powder, by above-mentioned coated ZrB
2powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ × 30 ~ 60 minutes obtains the coated ZrB of h-BN in temperature
2ceramic powder, by coated h-BN ZrB
2ceramic powder is made 60 × 10 ~ 20mm flake shaped base substrate through isostatic cool pressing under the pressure of 100 ~ 200MPa., and then under 1700 ~ 1850 ℃ × 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into h-BN/ZrB
2processable ceramic.
Compared with prior art, its advantage is in the present invention:
1, the present invention produces h-BN/ZrB
2processable ceramic uniform microstructure, intensity is high, and global reliability is high;
2, can form at ZrB2 grain surface the 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 improves 1 times compared with mixing, chemical method;
3, h-BN/ZrB
2processable ceramic has good antioxidant property, mechanical property and thermal property.
Embodiment
embodiment 1
The first step: by boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, and additional 30% ethanol 50 ℃ of heat treated in encloses container stir after 24 hours again makes esterification solution for 30 minutes;
Second step: be the ZrB of 0.1 μ m by granularity
2ceramic powder 70% joins in 30% esterification solution and makes ceramic size, then by sponging granulator, above-mentioned ceramic size is made to the coated ZrB that diameter is 0.5mm
2powder, by above-mentioned coated ZrB
2powder is that nitrogen atmosphere nitrogenize in 600 ℃ × 30 minutes obtains the coated ZrB of h-BN in temperature
2ceramic powder, by coated h-BN ZrB
2ceramic powder is pressed into 60 × 10mm flake shaped base substrate at the inferior static pressure of pressure of 100MPa., and then under 1700 ℃ × 30 minutes nitrogen atmospheres, hot pressing 5MPa. is fired into h-BN/ZrB
2processable ceramic.
The purity of testing proportion material used is technical pure, the h-BN/ ZrB obtaining
2the bending strength of processable ceramic is 476MPa..
embodiment 2
The first step: by boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, and additional 45% ethanol 70 ℃ of heat treated in encloses container stir after 16 hours again makes esterification solution for 20 minutes;
Second step: be the ZrB of 1 μ m by granularity
2ceramic powder 55% joins in 45% esterification solution and makes ceramic size, then by sponging granulator, above-mentioned ceramic size is made to the coated ZrB that diameter is 0.2mm
2powder, by above-mentioned coated ZrB
2powder is that nitrogen atmosphere nitrogenize in 800 ℃ × 45 minutes obtains the coated ZrB of h-BN in temperature
2ceramic powder, by coated h-BN ZrB
2ceramic powder is pressed into 60 × 15mm flake shaped base substrate at the inferior static pressure of pressure of 150MPa., and then under 1800 ℃ × 105 minutes nitrogen atmospheres, hot pressing 50MPa. is fired into h-BN/ZrB
2processable ceramic.
The purity of testing proportion material used is technical pure, the h-BN/ ZrB obtaining
2the bending strength of processable ceramic is 423MPa..
embodiment 3
The first step: by boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, and additional 60% ethanol 90 ℃ of heat treated in encloses container stir after 10 hours again makes esterification solution for 10 minutes;
Second step: be the ZrB of 2 μ m by granularity
2ceramic powder 40% joins in 60% esterification solution and makes ceramic size, then by sponging granulator, above-mentioned ceramic size is made to the coated ZrB that diameter is 0.01mm
2powder, by above-mentioned coated ZrB
2powder is that nitrogen atmosphere nitrogenize in 1000 ℃ × 60 minutes obtains the coated ZrB of h-BN in temperature
2ceramic powder, by coated h-BN ZrB
2ceramic powder is pressed into 60 × 20mm flake shaped base substrate at the inferior static pressure of pressure of 200MPa., and then under 1850 ℃ × 180 minutes nitrogen atmospheres, hot pressing 100MPa. is fired into h-BN/ZrB
2processable ceramic.
The purity of testing proportion material used is technical pure, the h-BN/ ZrB obtaining
2the bending strength of processable ceramic is 439MPa..
Claims (1)
1. a h-BN/ZrB
2the preparation method of processable ceramic, is characterized in that: adopt the coated ZrB of h-BN
2h-BN/ ZrB is burnt till in ceramic powder hot pressing after cold isostatic compaction
2processable ceramic, concrete grammar comprises the following steps:
The first step: by boric acid: the ratio of urea take weight ratio as 2:1 evenly mixed, and additional 30 ~ 60% ethanol 50 ~ 90 ℃ of heat treated in encloses container stir after 10 ~ 24 hours again makes esterification solution for 10 ~ 30 minutes;
Second step: be the ZrB of 0.1 ~ 2 μ m by granularity
2ceramic powder 40 ~ 70% 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 coated ZrB that diameter is 0.01 ~ 0.5mm
2powder, by above-mentioned coated ZrB
2powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 ℃ × 30 ~ 60 minutes obtains the coated ZrB of h-BN in temperature
2ceramic powder, by coated h-BN ZrB
2ceramic powder is made 60 × 10 ~ 20mm flake shaped base substrate through isostatic cool pressing under the pressure of 100 ~ 200MPa., and then under 1700 ~ 1850 ℃ × 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into h-BN/ ZrB
2processable ceramic.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210535948.8A CN103011826B (en) | 2012-12-13 | 2012-12-13 | Preparation method of h-BN/ZrB2 machinable ceramics |
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|---|---|---|---|
| CN201210535948.8A CN103011826B (en) | 2012-12-13 | 2012-12-13 | Preparation method of h-BN/ZrB2 machinable ceramics |
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|---|---|
| CN103011826A CN103011826A (en) | 2013-04-03 |
| CN103011826B true CN103011826B (en) | 2014-06-18 |
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| CN201210535948.8A Expired - Fee Related CN103011826B (en) | 2012-12-13 | 2012-12-13 | Preparation method of h-BN/ZrB2 machinable ceramics |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864430B (en) * | 2012-12-13 | 2015-03-18 | 山东理工大学 | h-BN/Cr3C2 machinable ceramic preparation method |
| CN104557050B (en) * | 2014-12-20 | 2017-02-22 | 北京矿冶研究总院 | ZrB 2-SiC/Si composite powder with core-shell structure and preparation method thereof |
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