CN102019153A - Method for compounding fine-particle cubic boron nitride single crystal - Google Patents
Method for compounding fine-particle cubic boron nitride single crystal Download PDFInfo
- Publication number
- CN102019153A CN102019153A CN2010106169513A CN201010616951A CN102019153A CN 102019153 A CN102019153 A CN 102019153A CN 2010106169513 A CN2010106169513 A CN 2010106169513A CN 201010616951 A CN201010616951 A CN 201010616951A CN 102019153 A CN102019153 A CN 102019153A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- cubic boron
- compounding
- fine
- fine grained
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Ceramic Products (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for compounding a fine-particle cubic boron nitride single crystal. In the method, hexagonal boron nitride is used as raw material, lithium nitride is used as catalytic agent and the fine-particle cubic boron nitride product is compounded under the condition of high temperature and high pressure, wherein the weight ratio of the hexagonal boron nitride to the lithium nitride is 1:0.1 to 0.3, the compounding time is 2 to 5 minutes, the compounding temperature is 1300 to 1600 DEG C, and the compounding pressure is 4.5 to 5.5 GPa. After finishing the compounding, the compounded material containing fine-particle cubic boron nitride single crystal is acquired. Compared with the prior art, the invention solves the problems that the traditional compounding method of the fine-particle cubic boron nitride single crystal has many steps, long compounding time and complex post processing and obtains incomplete single crystal shape of majority acquired fine-particle cubic boron nitride. Besides, the method of the invention is short in compounding time, has proper compounding pressure and is beneficial to save instrument loss and industrialized volume production.
Description
Technical field
The present invention relates to superhard material manufacturing technology field, particularly a kind of is the method for raw material synthesizing cubic boron nitride monocrystalline with the cubic boron nitride.
Background technology
Cubic boron nitride (cBN) has extremely strong hardness, is used as a kind of grinding-material and is widely used in the middle of the industry.Though the hardness of cubic boron nitride less than diamond, because it has extremely strong chemical inertness to iron family element and alloy thereof, therefore, is specially adapted to process iron family element.Usually cubic boron nitride is 2000
oBe directly transformed by hexagonal boron nitride under the high temperature of C and the high pressure of 10GPa, having under the situation of catalyst, the condition of synthesizing cubic boron nitride reduces significantly.The catalyst of synthesizing cubic boron nitride commonly used has alkali metal, alkaline-earth metal, and its nitride and boron nitride.In the transition process of cubic boron nitride, these catalyst and hexagonal boron nitride have the relation of congruent melting under HTHP, have reduced the temperature and pressure that cubic boron nitride is separated out greatly.In the process of synthesizing cubic boron nitride, the granularity of cubic boron nitride is an important index, and varigrained cubic boron nitride has different effects industrial.Wherein, 400 orders generally are used for the synthesizing cubic boron nitride condensate at present with thin fine grained cubic boron nitride, but synthetic technology is ripe not enough, and kind is few.
The prior art close with the present invention is that name is called the Chinese patent application (patent No. 200610017867.3, Granted publication CN 1888148A) of " production method of fine granularity cubic boron nitride monocrystal ".The production method of this fine granularity cubic boron nitride monocrystal is to be that 40-85, granularity are 200 orders-250 purpose hexagonal boron nitride by weight portion, weight portion is that the catalyst of 5-15 and purification hexagonal boron nitride powder that weight portion is 40-50 are prepared from according to following method step: 1. be pressed into synthetic rod after hexagonal boron nitride, the catalyst of above-mentioned weight portion being mixed and put into mould and place the intensification of pressurizeing of hexahedron hydraulic press, temperature is 230 ℃-240 ℃; Pressurization suspends 1-2 minute after being forced into for the first time 80MPa; Be forced into for the second time 96-98MPa then, heat-insulation pressure keeping is the release cooling after 8 minutes; 2. the material after the first step release cooling is taken out brokenly, carry out alkali treatment after placing acid soak to stir; To second material of step behind the acid soak carry out ball milling, shaping promptly get content more than 80%, the cubic boron nitride monocrystal of granularity between 270 orders-800 order.Though the method has improved the combined coefficient of cubic boron nitride greatly, significantly reduced synthetic cost, have favorable economic benefit and social benefit, but this method step complexity, generated time is long, and the post-processed complexity, the fine grained cubic boron nitride overwhelming majority who obtains by ball milling is a broken material, does not possess the complete crystalline form and the characteristic of monocrystalline.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of synthetic method of fine grained cubic boron nitride monocrystal, the synthetic method step that the present invention can solve existing fine grained cubic boron nitride monocrystal is many, generated time is long, post-processed complexity, the fine grained cubic boron nitride great majority that obtain are not the problems of complete monocrystalline crystalline form.
In order to finish the foregoing invention task, the synthetic method of this fine grained cubic boron nitride monocrystal is performed such: be raw material with the hexagonal boron nitride, lithium nitride is a catalyst, by the synthetic fine grained cubic boron nitride product of HTHP, wherein the weight proportion of hexagonal boron nitride and lithium nitride is hexagonal boron nitride: lithium nitride=1:0.1 ~ 0.3, generated time is 2 ~ 5 minutes, and synthesis temperature is 1300 ~ 1600
oC, synthesis pressure are 4.5 ~ 5.5 GPa; Obtain containing the synthesis material of fine grained cubic boron nitride monocrystal after synthetic the finishing.
In the synthetic method of above-mentioned fine grained cubic boron nitride monocrystal, scheme can be more specifically: the purity of used hexagonal boron nitride 〉=95%; The described synthesis material that contains the fine grained cubic boron nitride monocrystal soaks back water cleaning through peracid, alkali respectively and obtains highly purified fine grained cubic boron nitride monocrystal.
Synthetic in the technique scheme under the HTHP can be at belt type press, or carries out on the special-purpose press of superhard material such as cubic hinge press.
Owing to adopted technique scheme, the present invention has following beneficial effect compared with prior art:
1. can obtain synthetic complete cubic boron nitride monocrystal crystal with 111 crystal faces;
2. synthesis technique is simplified greatly, has avoided the loaded down with trivial details setting synthesis pressure and the step of temperature, has saved the synthetic time, has avoided the waste of raw material and catalyst;
3. the conversion ratio of fine grained cubic boron nitride can reach 60%.
The specific embodiment
Embodiment 1:
Hexagonal boron nitride, the lithium nitride powder of purity 〉=95% is respectively 1:0.1 by weight evenly to be mixed and is pressed into cylindric bar in advance and pack in the graphite-pipe, because bar is originally as insulator, therefore, between bar and graphite-pipe, need not to add insulating sleeve, bar is a little less than graphite-pipe, put into the synthetic assembled block of pyrophillite, on homemade cubic hinge press, carry out HTHP and synthesize.At 5.0GPa, 1450
oUnder the condition of C, heat-insulation pressure keeping 5 minutes, stop to heat the back and wait for 2 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal.
Embodiment 2:
Hexagonal boron nitride, lithium nitride with purity 〉=95%
PowderBeing respectively 1:0.15 by weight evenly mixes and is pressed into cylindric bar in advance and pack in the graphite-pipe, because bar is originally as insulator, therefore, between bar and graphite-pipe, need not to add insulating sleeve, bar is a little less than graphite-pipe, put into the synthetic assembled block of pyrophillite, on homemade cubic hinge press, carry out HTHP and synthesize.At 5.0GPa, 1450
oUnder the condition of C, heat-insulation pressure keeping 5 minutes, stop to heat the back and wait for 2 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal
Embodiment 3:
Hexagonal boron nitride, lithium nitride with purity 〉=95%
PowderBeing respectively 1:0.3 by weight evenly mixes and is pressed into cylindric bar in advance and pack in the graphite-pipe, because bar is originally as insulator, therefore, between bar and graphite-pipe, need not to add insulating sleeve, bar is a little less than graphite-pipe, put into the synthetic assembled block of pyrophillite, on homemade cubic hinge press, carry out HTHP and synthesize.At 5.0GPa, 1450
oUnder the condition of C, heat-insulation pressure keeping 5 minutes, stop to heat the back and wait for 2 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal
Embodiment 4
Hexagonal boron nitride, lithium nitride with purity 〉=95%
PowderBe respectively 1:0.1 by weight and evenly mix and be pressed into cylindric bar in advance and pack in the graphite-pipe, bar is put into the synthetic assembled block of pyrophillite a little less than graphite-pipe, and it is synthetic to carry out HTHP on homemade cubic hinge press.Begin to heat during at pressure, when temperature arrives 1000 for 3.5GPa
oDuring C, be incubated 30 seconds, heating is pressurized to 5.0GPa, 1300
oC, be incubated 5 minutes, stop to heat the back and wait for 2 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal
Embodiment 5:
Hexagonal boron nitride, lithium nitride with purity 〉=95%
PowderBe respectively 1:0.1 by weight and evenly mix and be pressed into cylindric bar in advance and pack in the graphite-pipe, bar is put into the synthetic assembled block of pyrophillite a little less than graphite-pipe, and it is synthetic to carry out HTHP on homemade cubic hinge press.Begin to heat during at pressure, when temperature arrives 1000 for 4.0GPa
oDuring C, be incubated 30 seconds, heating is pressurized to 5.0GPa, 1300
oC, be incubated 5 minutes, stop to heat the back and wait for 2 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal
Embodiment 6:
Hexagonal boron nitride, lithium nitride with purity 〉=95%
PowderBe respectively 1:0.1 by weight and evenly mix and be pressed into cylindric bar in advance and pack in the graphite-pipe, bar is put into the synthetic assembled block of pyrophillite a little less than graphite-pipe, and it is synthetic to carry out HTHP on homemade cubic hinge press.Begin to heat during at pressure, when temperature arrives 1000 for 4.5GPa
oDuring C, be incubated 30 seconds, heating is pressurized to 5.0GPa, 1300
oC, be incubated 5 minutes, stop to heat the back and wait for 2 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal
Embodiment 7:
Hexagonal boron nitride, lithium nitride with purity 〉=95%
PowderBe respectively 1:0.1 by weight and evenly mix and be pressed into cylindric bar in advance and pack in the graphite-pipe, bar is put into the synthetic assembled block of pyrophillite a little less than graphite-pipe, and it is synthetic to carry out HTHP on homemade cubic hinge press.Begin to heat during at pressure, when temperature arrives 1000 for 3.5GPa
oDuring C, be incubated 30 seconds, heating then is pressurized to 5.5GPa, 1300
oC, be incubated 3 minutes, slowly be depressurized to normal pressure, take out bar then and carry out the complete cubic boron nitride monocrystal crystal that following chemical treatment obtains having 111 crystal faces: gains are placed sulfuric acid: nitric acid: the acid solution of water=1:3:10 is boiled half an hour, place 30% sodium hydrate aqueous solution to boil half an hour after the cleaning again, clean with pure water then and obtain highly purified fine grained cubic boron nitride monocrystal.
In the middle of the various embodiments described above, about about 60%, granularity is probably at the 200-800 order greatly for conversion ratio, and through screening, 200-400 purpose cubic boron nitride is 10-30%; 400-600 purpose cubic boron nitride is 40-60%; 600-800 purpose cubic boron nitride is 1-10%.
Claims (3)
1. the synthetic method of a fine grained cubic boron nitride monocrystal, it is characterized in that: be raw material with the hexagonal boron nitride, lithium nitride is a catalyst, by the synthetic fine grained cubic boron nitride product of HTHP, wherein the weight proportion of hexagonal boron nitride and lithium nitride is: hexagonal boron nitride: lithium nitride=1:0.1 ~ 0.3, generated time is 2-5 minute, and synthesis temperature is 1300-1600
oC, synthesis pressure are 4.5-5.5 GPa; Obtain to contain the synthesis material of fine grained cubic boron nitride monocrystal after synthetic the finishing.
2. the synthetic method of fine grained cubic boron nitride monocrystal according to claim 1 is characterized in that: the purity of used hexagonal boron nitride 〉=95%.
3. the synthetic method of fine grained cubic boron nitride monocrystal according to claim 1 and 2 is characterized in that: the described synthesis material that contains the fine grained cubic boron nitride monocrystal respectively after peracid, alkali immersion treatment water clean and obtain highly purified fine grained cubic boron nitride monocrystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106169513A CN102019153A (en) | 2010-12-31 | 2010-12-31 | Method for compounding fine-particle cubic boron nitride single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106169513A CN102019153A (en) | 2010-12-31 | 2010-12-31 | Method for compounding fine-particle cubic boron nitride single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102019153A true CN102019153A (en) | 2011-04-20 |
Family
ID=43861181
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106169513A Pending CN102019153A (en) | 2010-12-31 | 2010-12-31 | Method for compounding fine-particle cubic boron nitride single crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102019153A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316612A (en) * | 2013-06-25 | 2013-09-25 | 河南飞孟金刚石工业有限公司 | Continuous growing method for synthesizing large single crystals of cubic boron nitride by using seed crystals |
| CN103521133A (en) * | 2013-10-22 | 2014-01-22 | 许斌 | High-impact-toughness cubic boron nitride, synthetic method and application thereof |
| CN103877914A (en) * | 2014-04-01 | 2014-06-25 | 许斌 | High-strength fine-particle cubic boron nitride monocrystal as well as synthesizing method thereof and application |
| CN105170029A (en) * | 2015-07-16 | 2015-12-23 | 河南飞孟金刚石工业有限公司 | Synthetic method of granularity-centralized cubic boron nitride |
| CN107523875A (en) * | 2017-10-12 | 2017-12-29 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN107805489A (en) * | 2017-10-12 | 2018-03-16 | 信阳市德隆超硬材料有限公司 | A kind of micro/nano level cubic boron nitride abrasive materials and preparation method thereof |
| CN109455680A (en) * | 2019-01-07 | 2019-03-12 | 郑州中南杰特超硬材料有限公司 | A kind of cubic boron nitride surface roughening treatment method |
-
2010
- 2010-12-31 CN CN2010106169513A patent/CN102019153A/en active Pending
Non-Patent Citations (5)
| Title |
|---|
| 《吉林大学博士学位论文》 20080927 杨大鹏 立方氮化硼、六方硼碳氮化合物的高压合成及应用研究 第三章 1-3 , * |
| 《吉林大学硕士学位论文》 20080912 郭玮 Al对Li基触媒合成cBN影响的研究 第三章 1-3 , * |
| 张铁臣: "大颗粒立方氮化硼单晶的合成", 《高压物理学报》 * |
| 杨大鹏: "立方氮化硼、六方硼碳氮化合物的高压合成及应用研究", 《吉林大学博士学位论文》 * |
| 郭玮: "Al对Li基触媒合成cBN影响的研究", 《吉林大学硕士学位论文》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316612A (en) * | 2013-06-25 | 2013-09-25 | 河南飞孟金刚石工业有限公司 | Continuous growing method for synthesizing large single crystals of cubic boron nitride by using seed crystals |
| CN103521133A (en) * | 2013-10-22 | 2014-01-22 | 许斌 | High-impact-toughness cubic boron nitride, synthetic method and application thereof |
| CN103521133B (en) * | 2013-10-22 | 2015-06-03 | 山东建筑大学 | High-impact-toughness cubic boron nitride, synthetic method and application thereof |
| CN103877914A (en) * | 2014-04-01 | 2014-06-25 | 许斌 | High-strength fine-particle cubic boron nitride monocrystal as well as synthesizing method thereof and application |
| CN103877914B (en) * | 2014-04-01 | 2016-01-27 | 山东建筑大学 | High-intensity fine particle cubic boron nitride monocrystal and synthetic method thereof and application |
| CN105170029A (en) * | 2015-07-16 | 2015-12-23 | 河南飞孟金刚石工业有限公司 | Synthetic method of granularity-centralized cubic boron nitride |
| CN107523875A (en) * | 2017-10-12 | 2017-12-29 | 信阳市德隆超硬材料有限公司 | A kind of cubic boron nitride monocrystal and preparation method thereof |
| CN107805489A (en) * | 2017-10-12 | 2018-03-16 | 信阳市德隆超硬材料有限公司 | A kind of micro/nano level cubic boron nitride abrasive materials and preparation method thereof |
| CN109455680A (en) * | 2019-01-07 | 2019-03-12 | 郑州中南杰特超硬材料有限公司 | A kind of cubic boron nitride surface roughening treatment method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102019153A (en) | Method for compounding fine-particle cubic boron nitride single crystal | |
| CN101323438B (en) | Cubic boron nitride synthetic method | |
| CN100542949C (en) | The synthetic method of coarse-grain degree cubic boron nitride | |
| CN101973552B (en) | Method for separating silicon from impurities | |
| CN106191600B (en) | A kind of polycrystalline diamond wire drawing die blank with carbide ring and preparation method thereof | |
| CN101891481B (en) | Method for producing polycrystal cubic boron nitride abrasive materials | |
| CN103521132A (en) | Synthesis technique of high-grade self-sharpening polycrystalline diamond | |
| CN103272527A (en) | High temperature and high pressure direct synthesis method of cubic boron nitride in titanium nitride plated coating | |
| CN112371148A (en) | Preparation method of novel catalyst for synthesizing diamond at high temperature and high pressure | |
| CN109650355A (en) | A kind of method of low temperature preparation hexagonal boron nitride | |
| CN101181979A (en) | Method for synthesizing cubic boron nitride by residual hexagonal boron nitride in high pressure synthesis of cubic boron nitride | |
| CN103272528A (en) | Method for synthesizing cubic boron nitrides by using alkali metal azide | |
| CN103272529A (en) | Method for synthesizing cubic boron nitride polycrystalline particles | |
| CN101580383A (en) | Magnesia-alumina spinel material prepared by waste activated alumina and preparation method thereof | |
| CN100496696C (en) | Method of synthesizing cubic boron nitride using alkali metal fluoride | |
| CN105080429B (en) | The synthetic method of grade cubic boron nitride large single crystal | |
| CN110205500B (en) | Method for removing impurities in reduced gold powder | |
| CN101869817A (en) | Method for synthesizing cubic boron nitride by using Mg3N2 and CaH2 | |
| CN107523875B (en) | Cubic boron nitride single crystal and preparation method thereof | |
| CN108176329B (en) | Synthesis method of cubic boron nitride | |
| CN103303914B (en) | Diamond purification technology | |
| CN102068943A (en) | Method for synthesizing flaky brown cubic boron nitride single crystal | |
| CN101428861B (en) | Process for producing high-purity manganese dioxide | |
| CN104876196A (en) | Preparation method for producing high purity beta-phase silicon nitride by combustion synthesis method | |
| CN101580382A (en) | Cordierite material prepared by waste activated alumina and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20110420 |