CN103121673B - A kind of discharge plasma sintering prepares the method for diamond sinter - Google Patents
A kind of discharge plasma sintering prepares the method for diamond sinter Download PDFInfo
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- CN103121673B CN103121673B CN201310046584.1A CN201310046584A CN103121673B CN 103121673 B CN103121673 B CN 103121673B CN 201310046584 A CN201310046584 A CN 201310046584A CN 103121673 B CN103121673 B CN 103121673B
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- silica flour
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Abstract
Discharge plasma sintering prepares the method for diamond sinter, and its silica flour and titanium valve total mass and adamantine mass ratio are 1 ~ 1.5:1, and the mass ratio of silica flour and titanium valve is 0.9 ~ 3.5:1; Above-mentioned raw materials is put into steel ball grinder, put into the corundum abrading-ball that diameter is 18mm again, ball material and raw material ratio are 2:1, open vacuum valve after sealing to vacuumize, ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling, after 30 minutes, takes off ball grinder, cooling; By said mixture at 10-100MPa, 1100-1650 DEG C, SPS sinters 5-20min.Present invention process is simple, sintering time is short, energy consumption is low, and the diamond sinter crystal grain of sintering is tiny, even structure, and folding strength brings up to 200-440MPa, and density brings up to 80%-98%.
Description
Technical field
The present invention relates to a kind of preparation method of material, 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 be made up of carbon formed 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 be transformed by artificial means.Usual 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 exceeded all removing materials, therefore many important industrial uses are also just provided with, as fine grinding material, high hard parting tool, all kinds of drill bit, wortle, also by the parts as a lot of precision instrument.
Usually, what make dimond synneusis employing is sinter under high-temperature and high-pressure conditions.Under non-pressure sintering conditions, 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.But it is long that high temperature and high pressure method shortcoming is sintering time, and energy consumption is high, and production cost is high, and by cavity body of mould limitation of size, the sintered compact size that sinters out little.The dimond synneusis sintered compact that this sinters out under just making high-temperature and high-pressure conditions is subject to a lot of restrictions in application aspect.It is simple that discharge plasma sintering (SPS) method has equipment, 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 subject to the advantage such as size and shape restriction, solves the problems that High Temperature High Pressure sintering exists.
But SPS method is sintering at ambient pressure, there is the problem of diamond graphitization.
Summary of the invention
The object of the invention is to propose a kind of simple to operate, can not produce that graphite remains, method that sintered compact density and the high discharge plasma sintering of hardness prepare diamond sinter.The present invention mainly adds graphite and absorbs element in sintering process, and by the temperature that controls sintering, pressure and time, makes not have graphite in sintered compact and remain.
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, and the mass ratio of silica flour and titanium valve is 0.9 ~ 3.5:1; Above-mentioned diamond is W10 ~ W40(grain diameter 10 ~ 40 microns) particle, silica flour and titanium valve are for being less than 200 object particles.
2, ball milling:
Above-mentioned raw materials is put into steel ball grinder, put into the corundum abrading-ball that diameter is 18mm again, ball material and raw material ratio are 2:1, open vacuum valve and vacuumize 0.5 hour, then ball grinder is put into planetary ball mill after sealing, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling, after 30 minutes, takes off ball grinder, cooling, takes out mixture;
3, sinter:
Said mixture is put into the mould of SPS sintering, at 10-100Mpa, 1100-1650 DEG C, SPS sinters 5-20min.
The silica flour added 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 speed of diamond graphitization, makes finally not have graphite in sintered compact and remains; The silica flour added and titanium valve have at least one melting phenomenon can occur at a sintering temperature, are beneficial to the infiltration in sintered compact hole, obtain the sintered compact that density is higher, and generate hardness relatively high SiC, TiC etc.
The present invention compared with prior art tool has the following advantages:
1, simple to operate, device simple, sintering time are short, energy consumption is low.
2, the diamond sinter crystal grain prepared is tiny, even structure.
2, the greying phenomenon of diamond in SPS sintering is obviously restrained, made sintered compact performance is good, sintered compact hardness can reach 5000-7000HV, compared with not adding the sintered compact of silica flour and titanium valve, folding strength brings up to 200-440MPa from 5-20MPa, and density brings 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 steel ball grinder, put into the corundum abrading-ball 3.88g that diameter is 18mm again, open vacuum valve after sealing and vacuumize 0.5 hour, then ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling, after 30 minutes, takes off ball grinder, cooling, takes out mixture; Said mixture is put into the mould of SPS sintering, at 50MPa, 1650 DEG C, SPS sinters 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 steel ball grinder, put into the corundum abrading-ball 5g that diameter is 18mm again, open vacuum valve after sealing and vacuumize 0.5 hour, then ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling, after 30 minutes, takes off ball grinder, cooling, takes out mixture; Said mixture is put into the mould of SPS sintering, at 10MPa, 1350 DEG C, SPS sinters 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 steel ball grinder, put into the corundum abrading-ball 4g that diameter is 18mm again, open vacuum valve after sealing and vacuumize 0.5 hour, then ball grinder is put into planetary ball mill, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling, after 30 minutes, takes off ball grinder, cooling, takes out mixture; Said mixture is put into the mould of SPS sintering, at 100MPa, 1100 DEG C, SPS sinters 20min.Exist without graphite in sintered compact, intensity is 200MPa.
Claims (2)
1. discharge plasma sintering prepares a 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 steel ball grinder, put into the corundum abrading-ball that diameter is 18mm again, ball material and raw material ratio are 2:1, open vacuum valve and vacuumize 0.5 hour, ball grinder is put into planetary ball mill after sealing, rotating speed is 300r/min, swing to frequency 30Hz, continuous ball milling, after 30 minutes, takes off ball grinder, cooling, takes out mixture;
(3) said mixture is put into the mould of SPS sintering, at 10 ~ 100MPa, 1100 ~ 1650 DEG C, sintering 5 ~ 20min.
2. a kind of discharge plasma sintering according to claim 1 prepares the method for diamond sinter, and it is characterized in that: described diadust is the particle of 10 ~ 40 microns, described silica flour and titanium valve are for being less than 200 object particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310046584.1A CN103121673B (en) | 2013-02-06 | 2013-02-06 | A kind of discharge plasma sintering prepares the method for diamond sinter |
Applications Claiming Priority (1)
| 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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| Publication Number | Publication Date |
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| CN103121673A CN103121673A (en) | 2013-05-29 |
| CN103121673B true CN103121673B (en) | 2015-11-18 |
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| CN201310046584.1A Expired - Fee Related CN103121673B (en) | 2013-02-06 | 2013-02-06 | A kind of discharge plasma sintering prepares the method for diamond sinter |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN114315354B (en) * | 2021-12-29 | 2023-02-07 | 武汉理工大学 | Diamond-B 4 Two-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 |
|---|
| Improvement of thermal stability of diamond by adding Ti powder during sintering of diamond/borosilicate glass composites;X.H. Zhang et al.;《Journal of European Ceramic Society》;20110427;第31卷;第1897-1903页 * |
| Improving oxidation resistance of diamond by adding silicon into diamond–borosilicate glass composites;X.H. Zhang et al.;《Int. Journal of Refractory Metals and Hard Materials》;20111231;第29卷;第495－498页 * |
| 微波等离子体烧结金刚石烧结体的研究;芶立等;《功能材料增刊》;19981031;第1022-1024页 * |
| 放电等离子体烧结的发展和应用;张久兴等;《功能材料增刊》;20011031;第1593-1598页 * |
| 殷声.现代陶瓷及其应用.《现代陶瓷及其应用》.1990,202-203. * |
| 陈文革等.粉末冶金工艺及材料.《粉末冶金工艺及材料》.2011,第161-164页. * |
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Granted publication date: 20151118 Termination date: 20180206 |