CN103121673A - Method for preparing diamond sintered body by using discharge plasmas in sintering mode - Google Patents
Method for preparing diamond sintered body by using discharge plasmas in sintering mode Download PDFInfo
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- CN103121673A CN103121673A CN2013100465841A CN201310046584A CN103121673A CN 103121673 A CN103121673 A CN 103121673A CN 2013100465841 A CN2013100465841 A CN 2013100465841A CN 201310046584 A CN201310046584 A CN 201310046584A CN 103121673 A CN103121673 A CN 103121673A
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Abstract
The invention discloses a method for preparing a diamond sintered body by using discharge plasmas in a sintering mode. The mass ratio of the total mass of silicon powder and titanium powder to the diamond is (1-1.5):1; the mass ratio of the silicon powder to the titanium powder is (0.9-3.5):1; the method comprises the following steps of: putting the raw materials into a steel ball-milling tank; further putting a corundum milling ball of 18mm in diameter into the steel ball-milling tank, wherein the ratio of the ball material to the raw materials is 2:1; sealing up the steel ball-milling tank and opening a vacuum valve so as to vacuum the steel ball-milling tank; putting the ball-milling tank into a planet type ball mill, wherein the rotation speed of the planet type ball mill is 300r/min and the inverse frequency is 30Hz; continuously ball-milling for 30minutes, subsequently taking down the ball-milling tank and cooling down; and carrying out SPS sintering on the mixture under 10-100MPa at 1,100-1,650 DEF C for 5-20minutes so as to obtain the diamond sintered body. The method is simple in process, short in sintering time and low in energy consumption; the sintered diamond sintered body is fine in crystal grain and uniform in structure, the bending strength is improved to 200-440MPa, and the compactness is increased to 80-98%.
Description
Technical field
The present invention relates to a kind of material preparation method, particularly adamantine preparation method.
Background technology
Diamond is divided into natural diamond and the large class of man-made diamond two.Natural diamond is the mineral that are comprised of carbon that form under field conditions (factors), and man-made diamond makes the graphite of non-diamond structure or gas-phase carbon atom undergo phase transition the diamond that is transformed by artificial means.Usually diamond is the hardest material of occurring in nature, Mohs' hardness is 10, Vickers' hardness is higher than 98GPa, its mill capacity and wear resistance have surpassed all removing materials, therefore also just had many important industrial uses, as fine grinding material, high hard parting tool, all kinds of drill bit, wortle, also be used as the parts of a lot of precision instruments.
What usually, the making dimond synneusis adopted is to carry out sintering under high-temperature and high-pressure conditions.Under non-high-pressure sinter condition, diamond can be converted into graphite, makes the bonding force of diamond interface become Van der Waals force between graphite linings, has had a strong impact on intensity and the grinding performance of matrix material.High temperature and high pressure environment can effectively suppress adamantine graphite transition.It is long that but the high temperature and high pressure method shortcoming is sintering time, and energy consumption is high, and production cost is high, and be subjected to the cavity body of mould limitation of size, and the sintered compact size that institute's sintering goes out is little.This just makes the dimond synneusis sintered compact that under high-temperature and high-pressure conditions, sintering goes out be subject to a lot of restrictions in application facet.Discharge plasma sintering (SPS) method has that equipment is simple, and sintering process is simple, and heat-up rate is fast, and heat-up time is short, and energy consumption is low, and cavity body of mould can not be subjected to the advantages such as size and shape restriction, has solved the problems that the High Temperature High Pressure sintering exists.
But the SPS method is the sintering under normal pressure, has the graphited problem of diamond.
Summary of the invention
The object of the invention is to propose a kind of simple to operate, can not produce that graphite is residual, method that sintered compact density and the high discharge plasma sintering of hardness prepare diamond sinter.The present invention adds graphite to absorb element in sintering process, and not have graphite in sintered compact residual by controlling temperature, pressure and the time of sintering, making.
Method of the present invention is as follows:
1, raw material:
Silica flour, titanium valve and diadust, silica flour and titanium valve total mass and adamantine mass ratio are 1 ~ 1.5:1, the mass ratio of silica flour and titanium valve is 0.9 ~ 3.5:1; Above-mentioned diamond is W10 ~ 10 ~ 40 microns of W40(grain diameters) particle, silica flour and titanium valve are less than 200 purpose particles.
2, ball milling:
Above-mentioned raw materials is put into the steel ball grinder, putting into diameter is the corundum abrading-ball of 18mm again, ball material and raw material ratio are 2:1, open vacuum valve after sealing and vacuumize 0.5 hour, then ball grinder are put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling took off ball grinder after 30 minutes, cooling, take out mixture;
3, sintering:
Said mixture is put into the mould of SPS sintering, at 10-100Mpa, 1100-1650 ℃, SPS sintering 5-20min gets final product.
The silica flour that adds and titanium valve and graphite generation chemical reaction absorb the graphite that in sintering process, diamond transforms, and speed of response is higher than the graphited speed of diamond, make that finally not have graphite in sintered compact residual; The silica flour that adds and titanium valve have at least a kind ofly under sintering temperature, melting phenomenon can occur, and is beneficial to the infiltration in the sintered compact hole, obtains the higher sintered compact of density, and generates relatively high SiC, the TiC etc. of hardness.
The present invention compared with prior art has following advantage:
1, simple to operate, device simple, sintering time is short, energy consumption is low.
2, the diamond sinter crystal grain for preparing is tiny, even structure.
2, obviously restrain the greying phenomenon of diamond in the SPS sintering, made sintered compact performance is good, sintered compact hardness can reach 5000-7000HV, compare with the sintered compact that does not add silica flour and titanium valve, folding strength is brought up to 200-440MPa from 5-20MPa, and density is brought up to 80%-98% from 50%-70%.
Embodiment
Embodiment 1
Get 500 order silica flour 0.58g, 500 order titanium valve 0.58g, W30 diamond 0.78g, put into the steel ball grinder, putting into diameter is the corundum abrading-ball 3.88g of 18mm again, opens vacuum valve after sealing and vacuumizes 0.5 hour, then ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling took off ball grinder after 30 minutes, cooling, take out mixture; Said mixture is put into the mould of SPS sintering, at 50MPa, 1650 ℃, SPS sintering 10min.Exist without graphite in sintered compact, intensity is 440MPa.
Embodiment 2
Get 1000 order silica flour 0.71g, 1000 order titanium valve 0.79g, W10 diamond 1g, put into the steel ball grinder, putting into diameter is the corundum abrading-ball 5g of 18mm again, opens vacuum valve after sealing and vacuumizes 0.5 hour, then ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling took off ball grinder after 30 minutes, cooling, take out mixture; Said mixture is put into the mould of SPS sintering, at 10MPa, 1350 ℃, SPS sintering 5min.Exist without graphite in sintered compact, intensity is 275MPa.
Embodiment 3
Get 400 order silica flour 0.78g, 400 order titanium valve 0.22g, W40 diamond 1g, put into the steel ball grinder, putting into diameter is the corundum abrading-ball 4g of 18mm again, opens vacuum valve after sealing and vacuumizes 0.5 hour, then ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling took off ball grinder after 30 minutes, cooling, take out mixture; Said mixture is put into the mould of SPS sintering, at 100MPa, 1100 ℃, SPS sintering 20min.Exist without graphite in sintered compact, intensity is 200MPa.
Claims (2)
1. a discharge plasma sintering prepares the method for diamond sinter, it is characterized in that:
(1) main raw material comprises silica flour, titanium valve and diadust, and the mass ratio of silica flour and titanium valve total mass and diadust is 1 ~ 1.5:1, and the mass ratio of silica flour and titanium valve is 0.9 ~ 3.5:1;
(2) above-mentioned raw materials is put into the steel ball grinder, putting into diameter is the corundum abrading-ball of 18mm again, ball material and raw material ratio are 2:1, open vacuum valve after sealing and vacuumize 0.5 hour, and ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling took off ball grinder after 30 minutes, cooling, take out mixture;
(3) said mixture is put into the mould of SPS sintering, at 10 ~ 100MPa, 1100 ~ 1650 ℃, sintering 5 ~ 20min.
2. a kind of discharge plasma sintering according to claim 1 prepares the method for diamond sinter, it is characterized in that: described diadust is that W10 ~ W40 particle diameter is the particle of 10 ~ 40 microns, and described silica flour and titanium valve are less than 200 purpose particles.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310046584.1A CN103121673B (en) | 2013-02-06 | 2013-02-06 | A kind of discharge plasma sintering prepares the method for diamond sinter |
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| CN201310046584.1A CN103121673B (en) | 2013-02-06 | 2013-02-06 | A kind of discharge plasma sintering prepares the method for diamond sinter |
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| CN103121673A true CN103121673A (en) | 2013-05-29 |
| CN103121673B CN103121673B (en) | 2015-11-18 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104588634A (en) * | 2014-05-27 | 2015-05-06 | 天长市天屹模具科技发展有限公司 | Spark plasma sintering manufacturing technology for high-rigidity polycrystalline diamond drawing die |
| CN111843165A (en) * | 2020-08-10 | 2020-10-30 | 中国电子科技集团公司第三十八研究所 | Diffusion connection method for diamond micro-channel |
| CN114315354A (en) * | 2021-12-29 | 2022-04-12 | 武汉理工大学 | Diamond-B4Two-step sintering method of C-SiC three-phase composite ceramic |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101453A (en) * | 1987-11-28 | 1988-06-15 | 国家建筑材料工业局人工晶体研究所 | Welding-type polycrystal composite with synthetic diamond and method for making thereof |
-
2013
- 2013-02-06 CN CN201310046584.1A patent/CN103121673B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101453A (en) * | 1987-11-28 | 1988-06-15 | 国家建筑材料工业局人工晶体研究所 | Welding-type polycrystal composite with synthetic diamond and method for making thereof |
Non-Patent Citations (6)
| Title |
|---|
| X.H. ZHANG ET AL.: "Improvement of thermal stability of diamond by adding Ti powder during sintering of diamond/borosilicate glass composites", 《JOURNAL OF EUROPEAN CERAMIC SOCIETY》 * |
| X.H. ZHANG ET AL.: "Improving oxidation resistance of diamond by adding silicon into diamond–borosilicate glass composites", 《INT. JOURNAL OF REFRACTORY METALS AND HARD MATERIALS》 * |
| 张久兴等: "放电等离子体烧结的发展和应用", 《功能材料增刊》 * |
| 殷声: "《现代陶瓷及其应用》", 31 October 1990 * |
| 芶立等: "微波等离子体烧结金刚石烧结体的研究", 《功能材料增刊》 * |
| 陈文革等: "《粉末冶金工艺及材料》", 31 July 2011 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104588634A (en) * | 2014-05-27 | 2015-05-06 | 天长市天屹模具科技发展有限公司 | Spark plasma sintering manufacturing technology for high-rigidity polycrystalline diamond drawing die |
| CN104588634B (en) * | 2014-05-27 | 2018-03-27 | 天长市天屹模具科技发展有限公司 | A kind of discharge plasma sintering manufacture craft of high rigidity polycrystalline diamond wire drawing die |
| CN111843165A (en) * | 2020-08-10 | 2020-10-30 | 中国电子科技集团公司第三十八研究所 | Diffusion connection method for diamond micro-channel |
| CN111843165B (en) * | 2020-08-10 | 2021-07-09 | 中国电子科技集团公司第三十八研究所 | Diffusion connection method for diamond micro-channel |
| CN114315354A (en) * | 2021-12-29 | 2022-04-12 | 武汉理工大学 | Diamond-B4Two-step sintering method of C-SiC three-phase composite ceramic |
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| CN103121673B (en) | 2015-11-18 |
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