CN1234643C - Liquid-sintered boron-carbide ceramic material and its products making method - Google Patents
Liquid-sintered boron-carbide ceramic material and its products making method Download PDFInfo
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- CN1234643C CN1234643C CN 03111187 CN03111187A CN1234643C CN 1234643 C CN1234643 C CN 1234643C CN 03111187 CN03111187 CN 03111187 CN 03111187 A CN03111187 A CN 03111187A CN 1234643 C CN1234643 C CN 1234643C
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- boron carbide
- powder
- carbide ceramics
- additive
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Abstract
The present invention relates to a method for manufacturing a liquid-phase sintered boron carbide ceramic material and products thereof, which aims to solve the problems that the production cost of hot pressing sintered boron carbide is high, products with complex shapes can not be produced, etc. The material comprises 72 to 99 wt% of boron carbide powder raw material, 0.5 to 25 wt% of Al-Y series additive and 0.5 to 3.0 wt% of either CeO2 or La2O3. In the method of the liquid-phase sintered boron carbide ceramic material and products thereof, boron carbide ceramic materials are mixed, milled and moulded according to the conventional method; then the compact is put in a vacuum sintering furnace, vacuum pumping and three times of argon purging are carried out, the temperature is raised at the speed of 5 to 25 DEG C /min for sintering, and when reaching 1700 to 2000 DEG C, the temperature is preserved for 200 to 500 minutes. The present invention has the advantages of reducing the production cost and increasing the production efficiency, and can be widely applied to the manufacturing field of boron carbide ceramics.
Description
Technical field: the present invention relates to a kind of boron carbide ceramics material and manufacture method thereof.
Background technology: the manufacturing technology of norbide stupalith and goods thereof has two kinds at present: hot pressed sintering and pressureless sintering technology, the subject matter that these two kinds of technology exist is: 1, and hot pressed sintering norbide productive expense height, graphite jig is low work-ing life, thermosteresis is bigger, and the electricity charge are higher; 2, the norbide hot pressing and sintering technique can only be made the goods of simple shape, can not satisfy the demand of market to the complicated shape goods; 3, hot pressed sintering norbide production efficiency is low, can not satisfy the demand of production in enormous quantities; 4, hot pressed sintering norbide blank size precision is poor, and the following process expense is higher; 5, pressureless sintering norbide technical performance index is low, can not satisfy the demand of market to the high quality goods; 6, pure norbide content is lower in the pressureless sintering boron carbide product, and work-ing life is low, can not meet the need of market.
Summary of the invention: the present invention mainly solves hot pressed sintering norbide productive expense height, can not produce the complicated shape goods, production efficiency is low, blank size precision difference and the low problem of pressureless sintering norbide technical performance index, thereby provide a kind of Liquid Sintering Ceramic Boron Carbide And Its Preparation Method, its objective is such realization: liquid phase sintering boron carbide ceramics material, it comprises the boron carbide powder powder stock, comprises that also Al-Y is additive and the CeO that chooses any one kind of them
2Or La
2O
3Composition, each composition quality percentage ratio is respectively: boron carbide powder powder stock 72-99, Al-Y are additive 0.5-25, CeO
2Or La
2O
3Account for 0.5-3.0; Described Al-Y is that additive is AlN or Al
2O
3Powder and Y
2O
3Powder.The manufacture method of liquid phase sintering boron carbide ceramics material: at first, according to a conventional method the boron carbide ceramics material is carried out batch mixing, powder process and moulding, the composition of described boron carbide ceramics material is for by mass percentage: boron carbide powder powder stock 72-99, Al-Y are additive 0.5-25, CeO
2Or La
2O
3Account for 0.5-3.0, Al-Y wherein is that additive is A1N or Al
2O
3Powder and Y
2O
3Powder; Then, pressed compact is placed vacuum sintering furnace, vacuumizes earlier, use argon cleaning again three times, the intensification sintering, heat-up rate is 5-25 ℃/min, be warmed up to 1700-2000 ℃ after, be incubated 200-500 minute, sintering carries out in a vacuum.The present invention compared with prior art has following advantage: 1, and it compares the 30-70% that reduces production costs with the hot pressed sintering norbide, compares the 20-50% that reduces production costs with the pressureless sintering norbide; 2, it can be made such as complex-shaped boron carbide products such as the mouth that sandblasts, wear ring, bearing housings; 3, than the hot pressing sintering boron carbide manufacturing technology 25-160% that enhances productivity; 4, improved the dimensional precision of sintering blank, reduced follow-up accurately machined expense; 5, the comprehensive technical performance index is compared with the pressureless sintering norbide and has been improved 30-65%, has enlarged the product application scope.
Embodiment one: present embodiment comprises the boron carbide powder powder stock, and it comprises that also Al-Y is additive and the CeO that chooses any one kind of them
2Or La
2O
3Composition, each composition quality percentage ratio is respectively: boron carbide powder powder stock 72-99, Al-Y are additive 0.5-25, CeO
2Or La
2O
3Account for 0.5-3.0.Described Al-Y is in the additive, and the ratio of Al and Y is 2.0-5.5: 5.5-2.0, and Al-Y is that additive is AlN or Al
2O
3Powder and Y
2O
3Powder, their median size is the 0.6-3.0 micron, and purity is 94-99.99%, and the purity of boron carbide powder powder stock is 91-99%, and median size is the 0.6-3.5 micron.The manufacture method of liquid phase sintering boron carbide ceramics material and goods thereof is: at first, according to a conventional method the boron carbide ceramics material is carried out batch mixing, powder process and moulding; Then, pressed compact is placed vacuum sintering furnace, vacuumize earlier, use argon cleaning again three times, the intensification sintering, heat-up rate is 5-25C/min, after being warmed up to 1700-2000 ℃, be incubated 200-500 minute, sintering carries out in vacuum or mobile argon gas, the flow of argon gas is 5-15L/min, and the step of batch mixing, powder process and moulding is:
A. place the nylon jar to mix the boron carbide ceramics material powder, the alcohol that adds conventional quantity is as mixed aid, and the pellet that ball mill is used is the boron carbide ceramics ball;
B. after ball milling mixing 6-24 hour, in 70-100 ℃ flowing nitrogen oven dry broken, the polyvinyl alcohol water solution that adds concentration and be 1-10% is as tackiness agent;
C. mix and carry out the drying fragmentation after 2-8 hour;
D. cross the 60-120 mesh sieve;
E. carry out cold isostatic compaction then, pressure is 100-250Mpa.
Embodiment two: what present embodiment and embodiment one were different is that each composition quality percentage ratio is respectively: boron carbide powder powder stock 72-76.9, Al-Y are additive 21-25, CeO
2Or La
2O
3Account for 2.1-3.0.The manufacture method of liquid phase sintering boron carbide ceramics material and goods thereof is characterized in that the step of described batch mixing, powder process and moulding is:
A. place the polyimide jar to mix the boron carbide ceramics material powder, the alcohol that adds conventional quantity is as mixed aid, and the pellet that ball mill is used is the boron carbide ceramics section;
B. after ball milling mixing 6-24 hour, in 70-100 ℃ flowing nitrogen oven dry broken, the polyvinyl alcohol water solution that adds concentration and be 1-10% is as tackiness agent;
C. mix and carry out the drying fragmentation after 2-8 hour;
D. carry out mist projection granulating then;
E. coldmoulding in punching block, pressure are 100-250Mpa.
Embodiment three: what present embodiment and embodiment one, two were different is that each composition quality percentage ratio is respectively: boron carbide powder powder stock 89-99, Al-Y are additive 0.5-10, CeO
2Or La
2O
3Account for 0.5-1.
Embodiment four: get raw material powder in following mass percent ratio: median size be 0.7 μ m, purity be 97.4% boron carbide powder powder stock 95.2, median size 1.71 μ m, purity are 98.0% La
2O
30.8 median size 2.7 μ m, purity are 95.5 AlN1.7, median size 1.2 μ m, purity are 99.7% Y
2O
32.3, carrying out batch mixing and powder process, punching block die mould, pressure are 170Mpa, carry out sintering, heat-up rate is 17 ℃/min, is warming up to 1920 ℃, insulation 270min.The salient features that obtains sintered compact is: density 2.53g/cm
3, hardness HV2950,4 bending strength 520Mpa, fracture toughness property K
IC5.4MPam
1/2
Embodiment five: what present embodiment and embodiment four were different is, it gets raw material powder in following mass percent ratio: median size be 3.5 μ m, purity be 94.2% boron carbide powder powder stock 97.7, median size 2.5 μ m, purity are 99.0% CeO
20.5 median size 0.6 μ m, purity are 95.8% Al
2O
31.3 median size 0.7 μ m, purity are 98.0% Y
2O
30.5, carrying out batch mixing and powder process, the cold hydrostatic profile of leading, pressure are 150Mpa, carry out sintering, heat-up rate is 7 ℃/min, is warming up to 1870 ℃, insulation 430min.The salient features that obtains sintered compact is: density 2.50g/cm
3, hardness HV3080,4 bending strength 485Mpa, fracture toughness property K
1C4.9MPam
1/2
Claims (9)
1, a kind of liquid phase sintering boron carbide ceramics material is characterized in that raw material comprises that boron carbide powder, Al-Y are additive and the CeO that chooses any one kind of them
2Or La
2O
3Composition, each composition quality percentage ratio is respectively: boron carbide powder 72-99, Al-Y are additive 0.5-25, CeO
2Or La
2O
3Account for 0.5-3.0; Described Al-Y is that additive is AlN or Al
2O
3Powder and Y
2O
3Powder;
Its manufacture method is: at first, be additive and the CeO that chooses any one kind of them with boron carbide powder and Al-Y according to a conventional method
2Or La
2O
3Composition carries out batch mixing, powder process and moulding in described ratio; Then, pressed compact is placed vacuum sintering furnace, vacuumizes earlier, use argon cleaning again three times, the intensification sintering, heat-up rate is 5-25 ℃/min, be warmed up to 1700-2000 ℃ after, be incubated 200-500 minute, sintering carries out in a vacuum.
2, liquid phase sintering boron carbide ceramics material according to claim 1, it is characterized in that the mass percent of material composition is respectively: boron carbide powder 72-76.9, Al-Y are additive 21-25, CeO
2Or La
2O
3Account for 2.1-3.0.
3, liquid phase sintering boron carbide ceramics material according to claim 1, it is characterized in that the mass percent of material composition is respectively: boron carbide powder 89-99, Al-Y are additive 0.5-10, CeO
2Or La
2O
3Account for 0.5-1.
4, according to claim 1 or 2 or 3 described liquid phase sintering boron carbide ceramics materials, it is characterized in that at described Al-Y be in the additive, the ratio of Al and Y is 2.0-5.5: 5.5-2.0.
5, according to claim 1 or 2 or 3 described liquid phase sintering boron carbide ceramics materials, it is characterized in that described Al-Y is that the median size of additive is the 0.6-3.0 micron, purity is 94-99.99%.
6, according to claim 1 or 2 or 3 described liquid phase sintering boron carbide ceramics materials, the purity that it is characterized in that described boron carbide powder is 91-99%, and median size is the 0.6-3.5 micron.
7, a kind of manufacture method of liquid phase sintering boron carbide ceramics material, it is characterized in that: at first, according to a conventional method the boron carbide ceramics material is carried out batch mixing, powder process and moulding, the composition of described boron carbide ceramics material is for by mass percentage: boron carbide powder 72-99, Al-Y is additive 0.5-25, CeO
2Or La
2O
3Account for 0.5-3.0, Al-Y wherein is that additive is AlN or Al
2O
3Powder and Y
2O
3Powder; Then, pressed compact is placed vacuum sintering furnace, vacuumizes earlier, use argon cleaning again three times, the intensification sintering, heat-up rate is 5-25 ℃/min, be warmed up to 1700-2000 ℃ after, be incubated 200-500 minute, sintering carries out in a vacuum.
8, the manufacture method of liquid phase sintering boron carbide ceramics material according to claim 7, it is characterized in that: the step of described batch mixing, powder process and moulding is:
A. place the nylon jar to mix the boron carbide ceramics material powder, the alcohol that adds conventional quantity is as mixed aid, and the pellet that ball mill is used is the boron carbide ceramics ball;
B. after ball milling mixing 6-24 hour, in 70-100 ℃ flowing nitrogen oven dry broken, the polyvinyl alcohol water solution that adds concentration and be 1-10% is as tackiness agent;
C. mix and carry out the drying fragmentation after 2-8 hour;
D. cross the 60-120 mesh sieve;
E. carry out cold isostatic compaction then, pressure is 100-250Mpa.
9, the manufacture method of liquid phase sintering boron carbide ceramics material according to claim 7 is characterized in that the step of described batch mixing, powder process and moulding is:
A. place the polyimide jar to mix the boron carbide ceramics material powder, the alcohol that adds conventional quantity is as mixed aid, and the pellet that ball mill is used is the boron carbide ceramics section;
B. after ball milling mixing 6-24 hour, in 70-100 ℃ flowing nitrogen oven dry broken, the polyvinyl alcohol water solution that adds concentration and be 1-10% is as tackiness agent;
C. mix and carry out the drying fragmentation after 2-8 hour;
D. carry out mist projection granulating then;
E. coldmoulding in punching block, pressure are 100-250Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03111187 CN1234643C (en) | 2003-03-14 | 2003-03-14 | Liquid-sintered boron-carbide ceramic material and its products making method |
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|---|---|---|---|
| CN 03111187 CN1234643C (en) | 2003-03-14 | 2003-03-14 | Liquid-sintered boron-carbide ceramic material and its products making method |
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| Publication Number | Publication Date |
|---|---|
| CN1438201A CN1438201A (en) | 2003-08-27 |
| CN1234643C true CN1234643C (en) | 2006-01-04 |
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| CN 03111187 Expired - Fee Related CN1234643C (en) | 2003-03-14 | 2003-03-14 | Liquid-sintered boron-carbide ceramic material and its products making method |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313419C (en) * | 2003-12-19 | 2007-05-02 | 李文辉 | Producing method for composite carbide ceramic material by liquid-phase sintering and ceramic products |
| CN100430339C (en) * | 2003-12-19 | 2008-11-05 | 李文辉 | Ceramic slide bearing and its producing method |
| CN1830899B (en) * | 2006-03-21 | 2010-04-21 | 东北大学 | Method for preparing composite ceramic material containing boron carbide and rare earth |
| US7419925B1 (en) * | 2006-08-23 | 2008-09-02 | Ut-Battelle, Llc | Lightweight high performance ceramic material |
| CN101337816B (en) * | 2008-08-29 | 2011-04-20 | 牡丹江金刚钻碳化硼有限公司 | Boron carbide-based composite material and preparation method thereof |
| CN104529457B (en) * | 2014-12-03 | 2017-06-13 | 中国兵器工业第五二研究所烟台分所 | Pressureless sintering boron carbide ceramics preparation method based on coarse granule powder |
| CN106380201B (en) * | 2016-08-28 | 2019-06-14 | 大连正兴磨料有限公司 | A method of preparing special-shaped boron carbide ceramics |
| CN111517794A (en) * | 2020-04-24 | 2020-08-11 | 朔州西廊煤炭科技有限公司 | Preparation method for preparing hollow nest-shaped damage-preventing engineering material base material by using coal solid waste or bauxite solid waste through sintering method |
| CN113666750A (en) * | 2021-08-16 | 2021-11-19 | 中硼科技(威海)有限公司 | Light high-performance boron carbide-based bulletproof ceramic and preparation method thereof |
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2003
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Harbin Xinhui Special Ceramic Co.,Ltd. Assignor: Li Wenxin|Li Wenhui Contract fulfillment period: 2008.10.13 to 2020.10.31 contract change Contract record no.: 2008230000141 Denomination of invention: Liquid-sintered boron-carbide ceramic material and its products making method Granted publication date: 20060104 License type: Exclusive license Record date: 20081022 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.13 TO 2020.10.31; CHANGE OF CONTRACT Name of requester: HARBIN XINHUI SPECIAL CERAMICS CO., LTD. Effective date: 20081022 |
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Assignee: Harbin Xinhui Special Ceramic Co.,Ltd. Assignor: Li Wenxin|Li Wenhui Contract record no.: 2008230000141 Date of cancellation: 20100802 |