CN1817434A - Method for sintering polycrystal cubic boron nitride by plasma discharge - Google Patents
Method for sintering polycrystal cubic boron nitride by plasma discharge Download PDFInfo
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- CN1817434A CN1817434A CN 200610012330 CN200610012330A CN1817434A CN 1817434 A CN1817434 A CN 1817434A CN 200610012330 CN200610012330 CN 200610012330 CN 200610012330 A CN200610012330 A CN 200610012330A CN 1817434 A CN1817434 A CN 1817434A
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- boron nitride
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Abstract
A plasma discharge method for sintering the polycrystalline cubic boron nitride with high density (more than 98%) and hardness (20-50 GPa) includes such steps as proportionally mixing binder with cubic boron nitride crystals, loading the mixture in graphite mould, putting the mould between upper and lower electrically conducting plates, plasma discharging in N2 or A2 under 10-100 MPa for sintering at 1100-1450 deg.C for 1-15 min, cooling and demoulding.
Description
Technical field
The present invention relates to a kind of a kind of manufacture method of ultra-hard material poly-crystal sintered body, particularly relate to a kind of method of sintering polycrystal cubic boron nitride by plasma discharge.
Background technology
The manufacture method of traditional polycrystalline cubic boron nitride sintered body is the manufacture method because of polycrystalline diamond sintered body, makes under high temperature-ultra-high pressure condition.In " PDC ultra-hard composite cutter material and application thereof " (Chemical Industry Press 2003) works that this writes at Wang Guangzu " cubic boron nitride synthetic with use " (Henan science tech publishing house 1995) and Deng Fuming etc. write detailed introduction is arranged all.Then disclosed this patented technology abroad, for example: the production method of polycrystalline diamond (patent No. USP 4049783,1967) as far back as 1967.In traditional polycrystalline cubic boron nitride sintered body manufacture process, general work pressure is 4-7GPa, and temperature is 1300～1500 ℃, and keeps under this temperature 2～20 minutes.In the manufacture process relatively the problem of difficulty be: the high-pressure chamber and the desired high temperature that dependence equipment form certain size, high-pressure chamber is made (see figure 1) by carbide alloy usually, the raw material of polycrystalline cubic boron nitride sintered body are filled in the crystal vessel, and the crystal vessel with certain wall thickness forms resistance heated with the low-voltage, high-current that adds.In order to make mechanical pressure be uniformly applied to crystal vessel, and then be uniformly applied to polycrystalline cubic boron nitride sintered body raw material, also will install transmission medium additional at the crystal vessel skin.Because the raw material of above-mentioned transmission medium, crystal vessel and polycrystalline cubic boron nitride sintered body all place high-pressure chamber inside, have taken the space of limited high-pressure chamber.The high-tension apparatus that adopts has two kinds, and a kind of is belt type press, and another kind is a cubic hinge press.The high-pressure chamber that belt type press forms is by (as Fig. 1) of forming relative to the carbide alloy cylinder pressure that moves hydraulic plunger drive carbide alloy pressure head and fix of exerting pressure up and down.Cubic hinge press then drives the carbide alloy pressure head by six hydraulic plungers that relatively move and forms (see figure 2), be that 10～90% cubic boron nitride crystal crystal evenly mixes with metal or metallic compound with ratio, pack in the crystal vessel, the outside suit is as the pyrophillite piece of transmission medium, place between the top hammer of extra-high tension unit, impose static pressure, and kept 〉=2 minutes in the temperature more than 〉=1300 ℃ greater than 4GPa, manufacture process is finished in release then, post processing.Adopt this traditional polycrystalline cubic boron nitride sintered body manufacture method, main cause is that the structure that will prevent cubic boron nitride crystal is damaged under atmosphere, normal pressure and conventional heating condition.Under atmospheric conditions,, temperature will destroy owing to oxidation makes the cubic boron nitride crystal structure when surpassing certain hour above 1300 ℃.And can generally all surpass 1300 ℃ with the bond normal sintering temperature that cubic boron nitride good combination and hardness are complementary, conventional heating means rely on the conduction heating to make this process slow.Realization is a very complicated technology greater than the high pressure of 4GPa, comprises the high pressure sealing technology, the technology that pressure evenly transmits, and need be heated to high temperature more than 1200 ℃ etc. under this high pressure.This high pressure, hot conditions require very high to equipment, exacting terms is restricted the size of high-pressure chamber, so far belt type press can't solve high pressure mould problem well, and the high-pressure chamber structure of cubic hinge press has limited the size of polycrystalline cubic boron nitride sintered body; Simultaneously, the high pressure extreme environment is very difficult again for the manufacture process of research polycrystalline cubic boron nitride sintered body.In a word, tradition is made the device structure complexity of the method employing of polycrystalline cubic boron nitride sintered body, cause that easily the top hammer or the mould consumption that constitute high-pressure chamber increase, limited the size of high-pressure chamber, product size increase, alteration of form etc. are all increased certain difficulty.
Summary of the invention
In order to overcome deficiencies such as equipment complexity, mould consumption that traditional polycrystalline cubic boron nitride sintered body manufacture method exists big and product size, shape are restricted, the invention provides a kind of method of sintering polycrystal cubic boron nitride by plasma discharge, this method has not only overcome the problems referred to above that traditional polycrystalline cubic boron nitride sintered body manufacture method exists, and greatly reduce operating pressure and mould consumption, product size and shape are greatly improved.
The method of this sintering polycrystal cubic boron nitride by plasma discharge may further comprise the steps:
A. bond is evenly mixed with 40～90% cubic boron nitride crystal, be loaded in the graphite jig of making by the shape and size of product 11;
B. the graphite jig 11 that filling is finished places between the conductive pressing plate up and down 8 of plasma discharge Fast Sintering machine;
C. plasma discharge Fast Sintering machine is started, in the ambiance of nitrogen or argon gas body, under 10～100MPa pressure, apply the plasma discharge Fast Sintering, sintering temperature is 1100 ℃～1450 ℃, keeps with this understanding 1～15 minute;
D. treating that the retention time reaches at first stops the heating cooling after the requirement, and removal pressure takes out the polycrystalline cubic boron nitride sintered body from graphite jig 11 after a while;
After sintering finishes, form new compound between metal or the compound, and form compact block with the cubic boron nitride crystal secure bond, its density reaches more than 98%, and hardness reaches 20～50GPa.
The component of described bond is: Al, TiN, AlN, Si
3N
4, TiC, Y
2O
3And Al
2O
3One or both or two or more metal and compound form; The chemical composition of metal and compound powder is wt%:Al:0～10% in the bond; TiN:0～60%; AlN:0～35%; Si
3N
4: 0～40%; TiC:0～60%; Y
2O
3: 0～10%; Al
2O
3: 0～45%.
Advantage of the present invention is: because the present invention has adopted the plasma discharge flash sintering method to prepare the polycrystalline cubic boron nitride sintered body, therefore under lower pressure and relative lower temperature, prepare the polycrystalline cubic boron nitride sintered body, overcome the deficiency that conventional method exists, the high-pressure chamber that does not need carbide alloy to constitute.
The plasma discharge flash sintering method is the new material preparation method who grows up nearly decades, and industrial production is used and is less than 20 years.Its main feature is by pulsed discharge, stored charge between the powder body material particle surface, the moment plasma discharge takes place after being accumulated to a certain degree, the point of discharge temperature raises fast, make sintering between particle, it is characteristics of the present invention that the plasma discharge flash sintering method is applied to make the polycrystalline cubic boron nitride sintered body, and this method remains unchanged the crystal structure of manufactured goods cubic boron nitride crystal.
Description of drawings
Fig. 1 is traditional polycrystalline cubic boron nitride belt type press sintering machine structural representation;
Fig. 2 is traditional polycrystalline cubic boron nitride cubic hinge press sintering machine structural representation;
Fig. 3 is a plasma discharge Fast Sintering machine structural representation;
The X-ray material phase analysis curve of Fig. 4 embodiment 1;
The X-ray material phase analysis curve of Fig. 5 embodiment 2.
In Fig. 1, Fig. 2, Fig. 3,1. carbide alloy pressure head, 2,4. strengthen steel loop, 3. carbide alloy cylinder pressure, 5. sample, 6. transmission medium, 7. crystal vessel, 8. conductive pressing plate, 9. graphite pressure head, 10. graphite die sleeve, 11. samples, 12. pulse powers.
The specific embodiment
With mass ratio (wt%) is Si
3N
436.1%, Y
2O
31.8%, Al
2O
35.4%, the powder of AlN 6.7% and average grain diameter be 5 μ m and 10 μ m cubic boron nitride crystal each 25% evenly mix, the (see figure 3) in the graphite jig 11 of packing into, place on the Dr Sinter 3.20-MK-V type plasma discharge flash sintering method sintering machine, kept 3 minutes in 30MPa, 1350 ℃.Obtaining hardness is HV44.6GPa, grey polycrystalline cubic boron nitride sintered body.X-ray thing phase collection of illustrative plates such as Fig. 4 of the polycrystalline cubic boron nitride sintered body of embodiment 1.
With mass ratio (wt%) is Si
3N
432%, Y
2O
34%, Al
2O
310%, the powder of AlN 4% and average grain diameter be 10 μ m and 20 μ m cubic boron nitride crystal each 25% evenly mix, the (see figure 3) in the graphite jig 11 of packing into, place on the Dr Sinter 3.20-MK-V plasma discharge flash sintering method sintering machine, kept 5 minutes in 30MPa, 1430 ℃.Obtaining hardness is HV46.1GPa, grey polycrystalline cubic boron nitride sintered body.X-ray thing phase collection of illustrative plates such as Fig. 5 of the polycrystalline cubic boron nitride sintered body of embodiment 2.
Claims (3)
1, a kind of method that adopts sintering polycrystal cubic boron nitride by plasma discharge, it is characterized in that: this method may further comprise the steps:
A. bond is evenly mixed with 40～90% cubic boron nitride crystal, be loaded in the graphite jig of making by the shape and size of product (11);
B. the graphite jig that filling is finished (11) places between the conductive pressing plate up and down (8) of plasma discharge Fast Sintering machine;
C. plasma discharge Fast Sintering machine is started, in the ambiance of nitrogen or argon gas body, under 10～100MPa pressure, apply the plasma discharge Fast Sintering, sintering temperature is 1100 ℃～1450 ℃, keeps with this understanding 1～15 minute;
D. treating that the retention time reaches at first stops the heating cooling after the requirement, removal pressure after a while, taking-up polycrystalline cubic boron nitride sintered body from graphite jig (11);
After sintering finishes, form new compound between metal or the compound, and form compact block with the cubic boron nitride crystal secure bond, its density reaches more than 98%, and hardness reaches 20～50GPa.
2, employing spark plasma sintering according to claim 1 prepares the method for polycrystalline cubic boron nitride sintered body, it is characterized in that: the component of described bond is: Al, TiN, AlN, Si
3N
4, TiC, Y
2O
3And Al
2O
3One or both or two or more metal and compound form.
3, employing spark plasma sintering according to claim 1 and 2 prepares the method for polycrystalline cubic boron nitride sintered body, it is characterized in that: the chemical composition of metal and compound powder is wt%:Al:0～10% in the bond; TiN:0～60%; AlN:0～35%; Si
3N
4: 0～40%; TiC:0～60%; Y
2O
3: 0～10%; Al
2O
3: 0～45%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560624B (en) * | 2009-05-18 | 2010-12-29 | 河南富耐克超硬材料有限公司 | Method for preparing polycrystalline cubic boron nitride |
| CN101676233B (en) * | 2008-09-19 | 2011-12-14 | 中国科学院上海硅酸盐研究所 | Method for preparing block functional glass |
| CN102794448A (en) * | 2012-07-30 | 2012-11-28 | 中南钻石股份有限公司 | Nanometal bonding agent and polycrystal CBN (cubic boron nitride) composite sheet made by using same |
| CN105622106A (en) * | 2015-12-25 | 2016-06-01 | 富耐克超硬材料股份有限公司 | Method for preparing cBN composite by adopting low-melting-point bonding agent |
| CN110423121A (en) * | 2019-08-28 | 2019-11-08 | 郑州中南杰特超硬材料有限公司 | A kind of composite material and preparation method of titanium nitride cladding polycrystalline cubic boron nitride |
| CN111362703A (en) * | 2020-03-30 | 2020-07-03 | 中原工学院 | Polycrystalline cubic boron nitride cutter sintered at low pressure and preparation method |
| CN114133250A (en) * | 2021-11-19 | 2022-03-04 | 武汉理工大学 | Preparation method of BN-containing multiphase ceramic with adjustable components by reactive sintering |
-
2006
- 2006-01-11 CN CNB2006100123308A patent/CN100506367C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676233B (en) * | 2008-09-19 | 2011-12-14 | 中国科学院上海硅酸盐研究所 | Method for preparing block functional glass |
| CN101560624B (en) * | 2009-05-18 | 2010-12-29 | 河南富耐克超硬材料有限公司 | Method for preparing polycrystalline cubic boron nitride |
| CN102794448A (en) * | 2012-07-30 | 2012-11-28 | 中南钻石股份有限公司 | Nanometal bonding agent and polycrystal CBN (cubic boron nitride) composite sheet made by using same |
| CN105622106A (en) * | 2015-12-25 | 2016-06-01 | 富耐克超硬材料股份有限公司 | Method for preparing cBN composite by adopting low-melting-point bonding agent |
| CN105622106B (en) * | 2015-12-25 | 2018-05-29 | 富耐克超硬材料股份有限公司 | A kind of preparation method of low molten bonding mixture cBN composite materials |
| CN110423121A (en) * | 2019-08-28 | 2019-11-08 | 郑州中南杰特超硬材料有限公司 | A kind of composite material and preparation method of titanium nitride cladding polycrystalline cubic boron nitride |
| CN111362703A (en) * | 2020-03-30 | 2020-07-03 | 中原工学院 | Polycrystalline cubic boron nitride cutter sintered at low pressure and preparation method |
| CN111362703B (en) * | 2020-03-30 | 2022-03-25 | 中原工学院 | Polycrystalline cubic boron nitride cutter sintered at low pressure and preparation method |
| CN114133250A (en) * | 2021-11-19 | 2022-03-04 | 武汉理工大学 | Preparation method of BN-containing multiphase ceramic with adjustable components by reactive sintering |
| CN114133250B (en) * | 2021-11-19 | 2022-09-02 | 武汉理工大学 | Preparation method of BN-containing multiphase ceramic with adjustable components by reactive sintering |
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|---|---|
| CN100506367C (en) | 2009-07-01 |
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Granted publication date: 20090701 Termination date: 20120111 |