CN102992774B - Preparation method of h-BN / HfB2 machinable ceramic - Google Patents
Preparation method of h-BN / HfB2 machinable ceramic Download PDFInfo
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- CN102992774B CN102992774B CN201210535544.9A CN201210535544A CN102992774B CN 102992774 B CN102992774 B CN 102992774B CN 201210535544 A CN201210535544 A CN 201210535544A CN 102992774 B CN102992774 B CN 102992774B
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Abstract
A preparation method of an h-BN / HfB2 machinable ceramic. The method is characterized by subjecting an h-BN coated HfB2 ceramic powder to a cold isostatic pressing for forming, and sintering the ceramic by hot pressing to obtain an h-BN / HfB2 machinable ceramic. The method comprises steps of: mixing boric acid and urea with ethanol according to a proportion to prepare an esterification solution in a closed container; then adding the HfB2 ceramic powder into the esterification solution to prepare a ceramic slurry; preparing the ceramic slurry into a coated HfB2 powder by a spray granulation machine; nitridizing the coated HfB2 powder to obtain the h-BN coated HfB2 ceramic powder; pressing the h-BN coated HfB2 ceramic powder by isostatic pressure into a plate blank; subjecting the plate blank to hot pressing under nitrogen atmosphere; and sintering the plate blank into the h-BN / HfB2 machinable ceramic. The h-BN / HfB2 machinable ceramic prepared by the method provided by the invention has advantages of uniform h-BN phase distribution, controllable content, and good processing property, mechanical property and thermal property.
Description
Technical field
The present invention relates to a kind of h-BN/HfB
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 taking 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/HfB
2the preparation method of processable ceramic.Its technical scheme is:
A kind of h-BN/HfB
2the preparation method of processable ceramic, is characterized in that: adopt the coated HfB of h-BN
2h-BN/HfB 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 taking weight ratio as 2:1 evenly mixed, and additional 30 ~ 60% ethanol 50 ~ 90 DEG C of heat treated in encloses container stir after 10 ~ 24 hours again makes esterification solution for 10 ~ 30 minutes;
Second step: be the HfB 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 HfB that diameter is 0.01 ~ 0.5mm
2powder, by above-mentioned coated HfB
2powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 DEG C × 30 ~ 60 minutes obtains the coated HfB of h-BN in temperature
2ceramic powder, by coated h-BN HfB
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 DEG C × 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into h-BN/HfB
2processable ceramic.
Compared with prior art, its advantage is in the present invention:
1, the present invention produces h-BN/HfB
2processable ceramic uniform microstructure, intensity is high, and global reliability is high;
2, can be at HfB 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/HfB
2the bending strength of processable ceramic improves 1 times compared with mixing, chemical method;
3, h-BN/HfB
2processable ceramic has good antioxidant property, mechanical property and thermal property.
Embodiment
embodiment 1
The first step: by boric acid: the ratio of urea taking weight ratio as 2:1 evenly mixed, and additional 30% ethanol 50 DEG C of heat treated in encloses container stir after 24 hours again makes esterification solution for 30 minutes;
Second step: be the HfB 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 HfB that diameter is 0.5mm
2powder, by above-mentioned coated HfB
2powder is that nitrogen atmosphere nitrogenize in 600 DEG C × 30 minutes obtains the coated HfB of h-BN in temperature
2ceramic powder, by coated h-BN HfB
2ceramic powder is pressed into 60 × 10mm flake shaped base substrate at the inferior static pressure of pressure of 100MPa., and then under 1700 DEG C × 30 minutes nitrogen atmospheres, hot pressing 5MPa. is fired into h-BN/HfB
2processable ceramic.
The purity of testing proportion material used is technical pure, the h-BN/ HfB obtaining
2the bending strength of processable ceramic is 379MPa..
embodiment 2
The first step: by boric acid: the ratio of urea taking weight ratio as 2:1 evenly mixed, and additional 45% ethanol 70 DEG C of heat treated in encloses container stir after 16 hours again makes esterification solution for 20 minutes;
Second step: be the HfB 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 HfB that diameter is 0.2mm
2powder, by above-mentioned coated HfB
2powder is that nitrogen atmosphere nitrogenize in 800 DEG C × 45 minutes obtains the coated HfB of h-BN in temperature
2ceramic powder, by coated h-BN HfB
2ceramic powder is pressed into 60 × 15mm flake shaped base substrate at the inferior static pressure of pressure of 150MPa., and then under 1800 DEG C × 105 minutes nitrogen atmospheres, hot pressing 50MPa. is fired into h-BN/HfB
2processable ceramic.
The purity of testing proportion material used is technical pure, the h-BN/ HfB obtaining
2the bending strength of processable ceramic is 336MPa..
embodiment 3
The first step: by boric acid: the ratio of urea taking weight ratio as 2:1 evenly mixed, and additional 60% ethanol 90 DEG C of heat treated in encloses container stir after 10 hours again makes esterification solution for 10 minutes;
Second step: be the HfB 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 HfB that diameter is 0.01mm
2powder, by above-mentioned coated HfB
2powder is that nitrogen atmosphere nitrogenize in 1000 DEG C × 60 minutes obtains the coated HfB of h-BN in temperature
2ceramic powder, by coated h-BN HfB
2ceramic powder is pressed into 60 × 20mm flake shaped base substrate at the inferior static pressure of pressure of 200MPa., and then under 1850 DEG C × 180 minutes nitrogen atmospheres, hot pressing 100MPa. is fired into h-BN/HfB
2processable ceramic.
The purity of testing proportion material used is technical pure, the h-BN/HfB obtaining
2the bending strength of processable ceramic is 283MPa..
Claims (1)
1. a h-BN/HfB
2the preparation method of processable ceramic, is characterized in that: adopt the coated HfB of h-BN
2h-BN/ HfB 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 taking weight ratio as 2:1 evenly mixed, and additional 30 ~ 60% ethanol 50 ~ 90 DEG C of heat treated in encloses container stir after 10 ~ 24 hours again makes esterification solution for 10 ~ 30 minutes;
Second step: be the HfB 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 HfB that diameter is 0.01 ~ 0.5mm
2powder, by above-mentioned coated HfB
2powder is that nitrogen atmosphere nitrogenize in 600 ~ 1000 DEG C × 30 ~ 60 minutes obtains the coated HfB of h-BN in temperature
2ceramic powder, by coated h-BN HfB
2ceramic powder is through make × 10 ~ 20mm of isostatic cool pressing flake shaped base substrate under the pressure of 100 ~ 200MPa., and then under 1700 ~ 1850 DEG C × 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into h-BN/ HfB
2processable ceramic.
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|---|---|---|---|
| CN201210535544.9A CN102992774B (en) | 2012-12-13 | 2012-12-13 | Preparation method of h-BN / HfB2 machinable ceramic |
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| CN201210535544.9A CN102992774B (en) | 2012-12-13 | 2012-12-13 | Preparation method of h-BN / HfB2 machinable ceramic |
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| CN102992774B true CN102992774B (en) | 2014-07-09 |
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| CN104529456B (en) * | 2014-12-03 | 2017-03-22 | 武汉理工大学 | Preparation method for B4C-HfB2 high-temperature eutectic in-situ composite ceramic |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4312293B2 (en) * | 1999-03-16 | 2009-08-12 | 独立行政法人科学技術振興機構 | Silicon carbide ceramic composite material and manufacturing method thereof |
-
2012
- 2012-12-13 CN CN201210535544.9A patent/CN102992774B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4312293B2 (en) * | 1999-03-16 | 2009-08-12 | 独立行政法人科学技術振興機構 | Silicon carbide ceramic composite material and manufacturing method thereof |
Non-Patent Citations (9)
| Title |
|---|
| B_4C/BN纳米复合粉末的制备与显微结构的研究;江涛 等;《稀有金属材料与工程》;20090415;第38卷;第280-283页 * |
| 可加工Si_3N_4/BN复相陶瓷的制备及性能研究;王向东 等;《稀有金属材料与工程》;20030730;第32卷(第07期);第498-501页 * |
| 尿素法制备氮化物陶瓷材料的研究进展;李端 等;《宇航材料工艺》;20110531;第41卷(第05期);第1-5页 * |
| 李端 等.尿素法制备氮化物陶瓷材料的研究进展.《宇航材料工艺》.2011,第41卷(第05期),第1-5页. |
| 杨刚宾等.纳米BN复合SiC材料的抗热震性研究.《耐火材料》.2008,第42卷(第01期),第44页左栏倒数第1段、右栏第1段，第45页右栏第1段，第46页右栏倒数第1段. |
| 江涛 等.B_4C/BN纳米复合粉末的制备与显微结构的研究.《稀有金属材料与工程》.2009,第38卷第280-283页. |
| 王向东 等.可加工Si_3N_4/BN复相陶瓷的制备及性能研究.《稀有金属材料与工程》.2003,第32卷(第07期),第498-501页. |
| 纳米BN复合SiC材料的抗热震性研究;杨刚宾等;《耐火材料》;20080215;第42卷(第01期);第44页左栏倒数第1段、右栏第1段，第45页右栏第1段，第46页右栏倒数第1段 * |
| 龚雪.原位合成BN/TiB_2纳米—微米复合粉末及其烧结性能研究.《中国优秀硕士学位论文全文数据库(工程科技Ⅰ辑)》.2010, * |
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