CN102992768B - Preparation method of h-BN / HfC machinable ceramic - Google Patents
Preparation method of h-BN / HfC machinable ceramic Download PDFInfo
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- CN102992768B CN102992768B CN201210535545.3A CN201210535545A CN102992768B CN 102992768 B CN102992768 B CN 102992768B CN 201210535545 A CN201210535545 A CN 201210535545A CN 102992768 B CN102992768 B CN 102992768B
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Abstract
A preparation method of an h-BN / HfC machinable ceramic. The method is characterized by subjecting an h-BN coated HfC ceramic powder to a cold isostatic pressing for forming, and sintering the ceramic by hot pressing to obtain an h-BN / HfC 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 HfC ceramic powder into the esterification solution to prepare a ceramic slurry; preparing the ceramic slurry into a coated HfC powder by a spray granulation machine; nitridizing the coated HfC powder to obtain the h-BN coated HfC ceramic powder; pressing the h-BN coated HfC 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 / HfC machinable ceramic. The h-BN / HfC 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/HfC processable ceramic, belong 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 and a kind ofly can overcome above-mentioned defect, realize and prepare the more preparation method of high strength h-BN/HfC processable ceramic.Its technical scheme is:
A preparation method for h-BN/HfC processable ceramic, is characterized in that: adopt the coated HfC ceramic powder hot pressing after cold isostatic compaction of h-BN to burn till h-BN/HfC processable 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: the HfC 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 coated HfC powder that diameter is 0.01 ~ 0.5mm, be that nitrogen atmosphere nitrogenize in 600 ~ 1000 DEG C × 30 ~ 60 minutes obtains the coated HfC ceramic powder of h-BN by above-mentioned coated HfC powder in temperature, coated h-BN HfC ceramic powder is made to 60 × 10 ~ 20mm flake shaped base substrate through isostatic cool pressing under the pressure of 100 ~ 200MPa., then under 1700 ~ 1850 DEG C × 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into h-BN/HfC processable ceramic.
Compared with prior art, its advantage is in the present invention:
1, the present invention produces h-BN/HfC processable ceramic uniform microstructure, and intensity is high, and global reliability is high;
2, can form at HfC grain surface the 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/HfC processable ceramic improves 1.5 times compared with mixing, chemical method;
3, h-BN/HfC processable 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: the HfC 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 coated HfC powder that diameter is 0.5mm; be that nitrogen atmosphere nitrogenize in 600 DEG C × 30 minutes obtains the coated HfC ceramic powder of h-BN by above-mentioned coated HfC powder in temperature; coated h-BN HfC ceramic 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/HfC processable ceramic.
The purity of testing proportion material used is technical pure, and the bending strength of the h-BN/ HfC processable ceramic obtaining is 412MPa..
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: the HfC 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 coated HfC powder that diameter is 0.2mm; be that nitrogen atmosphere nitrogenize in 800 DEG C × 45 minutes obtains the coated HfC ceramic powder of h-BN by above-mentioned coated HfC powder in temperature; coated h-BN HfC ceramic 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/HfC processable ceramic.
The purity of testing proportion material used is technical pure, and the bending strength of the h-BN/ HfC processable ceramic obtaining is 357MPa..
embodiment 3
The first step: by boric acid: the ratio of urea taking weight ratio as 2:1 evenly mixed additional 60% ethanol 90 DEG C of heat treated in encloses container and stirred after 10 hours again and makes esterification solution for 10 minutes;
Second step: the HfC 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 coated HfC powder that diameter is 0.01mm; be that nitrogen atmosphere nitrogenize in 1000 DEG C × 60 minutes obtains the coated HfC ceramic powder of h-BN by above-mentioned coated HfC powder in temperature; coated h-BN HfC ceramic 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/HfC processable ceramic.
The purity of testing proportion material used is technical pure, and the bending strength of the h-BN/ HfC processable ceramic obtaining is 299MPa..
Claims (1)
1. a preparation method for h-BN/HfC processable ceramic, is characterized in that: adopt the coated HfC ceramic powder hot pressing after cold isostatic compaction of h-BN to burn till h-BN/HfC processable 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: the HfC 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 coated HfC powder that diameter is 0.01 ~ 0.5mm, be that nitrogen atmosphere nitrogenize in 600 ~ 1000 DEG C × 30 ~ 60 minutes obtains the coated HfC ceramic powder of h-BN by above-mentioned coated HfC powder in temperature, coated h-BN HfC ceramic powder is made to 60 × 10 ~ 20mm flake shaped base substrate through isostatic cool pressing under the pressure of 100 ~ 200MPa., then under 1700 ~ 1850 DEG C × 30 ~ 180 minutes nitrogen atmospheres, hot pressing 5 ~ 100MPa. is fired into h-BN/HfC processable ceramic.
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Citations (1)
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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 |
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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 (8)
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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 * |
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