CN108585855A - A kind of grain polycrystalline diamond compact and preparation method thereof of selenium catalyst - Google Patents
A kind of grain polycrystalline diamond compact and preparation method thereof of selenium catalyst Download PDFInfo
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Abstract
A kind of grain polycrystalline diamond compact and preparation method thereof of selenium catalyst, is related to technical field of superhard material.A kind of preparation method of the grain polycrystalline diamond compact of selenium catalyst, including：The mixed-powder of 31.59~34.047 parts by weight of micron-sized bortz powder and 1.473~4.79 parts by weight of micron-sized selenium powder composition is ground until selenium powder becomes amorphous selenium powder；Mixed-powder is placed in mold, blank is shaped under conditions of room temperature, pressure 5MPa~20MPa；By blank under the pressure of 6.5GPa~12.5GPa sintering curing, wherein sintering temperature be 1500 DEG C~1900 DEG C.The preparation method is simple for process, and the grain polycrystalline diamond compact of high rigidity can be made.
Description
Technical field
The present invention relates to technical field of superhard material, and the grain polycrystalline diamond compact of more particularly to a kind of selenium catalyst and its
Preparation method.
Background technology
Grain polycrystalline diamond compact due to the good mechanical performance such as high hardness, wearability and impact resistance,
The main material of manufacture cutting element, reshaper, wire drawing die and excavating bur is had become at present.
Traditional grain polycrystalline diamond compact is mostly sintered at high temperature under high pressure with metal solvent by diamond particles,
But the technological process of existing grain polycrystalline diamond compact is complicated so that cost increases.
Invention content
The purpose of the present invention is to provide a kind of grain polycrystalline diamond compacts of selenium catalyst, with higher hardness.
Another object of the present invention is to provide a kind of preparation method of the grain polycrystalline diamond compact of selenium catalyst, techniques
Simply, the higher grain polycrystalline diamond compact of hardness can be made.
The present invention is solved its technical problem and is realized using following technical scheme.
The present invention proposes a kind of grain polycrystalline diamond compact of selenium catalyst, and grain polycrystalline diamond compact is by bortz powder and selenium
Powder sintering is made, and the carbide of selenium and selenium is filled between the gap of diamond particles, and D-D keys are formed between diamond particles.
The present invention also proposes a kind of preparation method of the grain polycrystalline diamond compact of selenium catalyst, including：
By 31.59~34.047 parts by weight of micron-sized bortz powder and 1.473~4.79 parts by weight of micron-sized selenium powder
The mixed-powder of composition is ground until selenium powder becomes amorphous selenium powder；
Mixed-powder is placed in mold, blank is shaped under conditions of room temperature, pressure 5MPa~20MPa；
By blank under the pressure of 6.5GPa~12.5GPa sintering curing, wherein sintering temperature be 1500 DEG C~1900
℃。
The advantageous effect of the embodiment of the present invention is：Selenium catalyst grain polycrystalline diamond compact disclosed by the invention and its preparation side
Using selenium powder as catalyst grain polycrystalline diamond compact has successfully been prepared in selenium powder and bortz powder mixed sintering by method,
Selenium at ambient temperature have good inoxidizability, thus using selenium as impurity in the grain polycrystalline diamond compact of catalyst compared with
It is few, the hardness of grain polycrystalline diamond compact is improved, hardness is up to 68GPa or more.And traditional gold is eliminated in preparation process
Belong to the flow that media reductive processing and vacuum in catalyst grain polycrystalline diamond compact production process are pre-sintered.Greatly simplify production
Technological process.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the scanning electron microscope diagram of selenium-polycrystalline diamond of the embodiment of the present invention 2；
Fig. 2 is the result figure of the Vickers hardness of selenium-polycrystalline diamond of the embodiment of the present invention 2.
Icon：1- diamond particles；2-D-D keys；The carbide of 3- selenium and selenium.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Grain polycrystalline diamond compact of a kind of selenium catalyst of the embodiment of the present invention and preparation method thereof is carried out below specific
Explanation.
Traditional grain polycrystalline diamond compact is mostly by diamond particles and metal solvent (such as iron, cobalt, nickel) in high temperature height
Made of being sintered under the conditions of pressure.Oxidation is the main problem that metal solvent faces.Generation, packing, transport and with gold
During hard rock powder batch mixing, the oxidizable generation metal oxide of metal solvent brings impurity into grain polycrystalline diamond compact
In, to reduce the performance of grain polycrystalline diamond compact.To reduce the influence of catalyst oxidation, existing metal solvent polycrystalline diamond
In the production process of sintered body, need to carry out the powder of metal solvent into hydrogen reducing processing a few hours more than 700 DEG C of temperature,
And the assembly of pre-molding is placed again into the vacuum sintering furnace of hydrogen reduction atmosphere before high temperature and pressure sintering, 900
More than DEG C temperature it is vacuum-treated a few hours.This makes the technological process for producing grain polycrystalline diamond compact become complicated and increases life
Produce cost.
Based on this, present embodiment provides a kind of grain polycrystalline diamond compact of selenium catalyst, grain polycrystalline diamond compact by
Bortz powder is made with selenium powder sintering, and the carbide of selenium and selenium, and shape between diamond particles are filled between the gap of diamond particles
At D-D keys.
The present invention is using selenium powder as catalyst, and by selenium powder and bortz powder mixed sintering, polycrystalline gold has successfully been prepared
Hard rock sintered body, selenium belong to oxygen group elements, have good inoxidizability under room temperature, thus using selenium as the polycrystalline of catalyst
Impurity is less in diamond sinter, to improve the performance of grain polycrystalline diamond compact.
A kind of preparation method of the grain polycrystalline diamond compact of selenium catalyst, including：
By 31.59~34.047 parts by weight of micron-sized bortz powder and 1.473~4.79 parts by weight of micron-sized selenium powder
The mixed-powder of composition is ground until selenium powder becomes amorphous selenium powder.
In the present embodiment, mainly bortz powder is mixed with selenium powder in the way of ball milling, it is mixed after ball milling
It closes powder and carries out X-ray diffraction analysis, to confirm selenium powder whether all by ball milling for amorphous amorphous selenium.
Further, in some embodiments, the weight percent of selenium powder is 4.2%~13.2%.In some implementations
In mode, the weight percent of selenium powder is 4.2%~6.7%.Herein it should be noted that the weight percent of selenium powder referred to
It is that the weight of selenium powder accounts for the percentage of selenium powder and bortz powder total amount.
In some embodiments, the crystallite dimension of bortz powder is 0.2~7 μm, and the crystallite dimension of selenium powder is 10~30 μ
m.In some embodiments, the crystallite dimension of bortz powder is 2~5 μm.
Mixed-powder after ball milling is placed in mold, base is shaped under conditions of room temperature, pressure 5MPa~20MPa
Part；By blank under the pressure of 6.5GPa~12.5GPa sintering curing, wherein sintering temperature be 1500 DEG C~1900 DEG C.
Selenium element as catalyst belongs to oxygen group elements, has good inoxidizability at room temperature, is carried out with bortz powder
Batch mixing, during precompressed, assembling, selenium will not aoxidize.Present embodiment has successfully been prepared more using selenium powder as catalyst
Diamond sintered body, and save the processing of the media reductive in conventional metals catalyst grain polycrystalline diamond compact production process and true
The flow that sky is pre-sintered.In addition, under relatively high high-temperature and high-pressure conditions, i.e., in the sintering temperature of present embodiment and pressure
Under, selenium is present between the gap of diamond particles in liquid form, increases the contact area of selenium catalyst and diamond, is conducive to
The D-D bonds formed between more diamond particles are closed, and are increased the density of D-D keys in diamond sinter, are improved polycrystalline diamond
The mechanical property of stone sintered body.
It should be noted that D-D keys refer in the sintered body of polycrystalline diamond, effect of the diamond particles in catalyst
Under, together with granular grows, the carbon atom between diamond particles and particle can be connected to particle with the chemical bond of diamond
Together, which is D-D keys.
In addition, room temperature here refers to room temperature or general temperature, in the present embodiment, room temperature is 20~28 DEG C.
In some embodiments, sintering temperature is 1600~1850 DEG C.Sintering time is 30~3600s.In some realities
It applies in mode, sintering time is 100~1800s.In some embodiments, sintering time is 600~1000s.
In some embodiments, the pressure of blank sintering curing is 9~12.5GPa.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of preparation methods of the grain polycrystalline diamond compact of selenium catalyst, including：
Weigh the bortz powder 3.159g that crystal grain is 2~5 μm and the selenium powder 0.479g that crystal grain is 10~30 μm, wherein gold
The weight percent of emery is 86.8%, and the weight percent of selenium powder is 13.2%；
Above-mentioned bortz powder and selenium powder are mixed to get mixed-powder, mixed-powder, which is put into one, is equipped with tungsten-carbide ball
In tungsten carbide bottle, then by tungsten carbide bottle be put into CERTIPREP SPEX8000-D high energy ball mills (Metuchen, NJ) into
Row processing.Wherein, ball mill is located in the seal box crossed with purification for argon.The ball milling of mixed-powder at least needs 10 small
When, until selenium powder carries out X-ray diffraction analysis, with true all by ball milling at amorphous amorphous selenium to the mixed-powder after ball milling
Selenium powder whole ball milling is determined into amorphous amorphous selenium.
Mixed-powder after ball milling is filled in people's mold, then in room temperature, the condition of pressure 5MPa on belt type press
Lower pressurize 5min is shaped to blank；
Molding blank is put into the press (15MN three pillar types press) of octahedra pressure chamber, is in room temperature, pressure
Then pressurize 10min under the conditions of 6.5GPa slowly increases temperature while keeping the pressure, is warming up within the time of 5min
1500 DEG C, after being sintered 30s under the temperature, pressure conditions, room temperature is cooled the temperature in 10min, drops pressure in 15min
To normal pressure, recycling sample can be obtained selenium-grain polycrystalline diamond compact.
Embodiment 2
The present embodiment provides a kind of preparation methods of the grain polycrystalline diamond compact of selenium catalyst, including：
Weigh the bortz powder 3.404g that crystal grain is 2~5 μm and the selenium powder 0.147g that crystal grain is 10~30 μm, wherein gold
The weight percent of emery is 95.8%, and the weight percent of selenium powder is 4.2%；
Above-mentioned bortz powder and selenium powder are mixed to get mixed-powder, mixed-powder, which is put into one, is equipped with tungsten-carbide ball
In tungsten carbide bottle, then by tungsten carbide bottle be put into CERTIPREP SPEX8000-D high energy ball mills (Metuchen, NJ) into
Row processing.Wherein, ball mill is located in the seal box crossed with purification for argon.The ball milling of mixed-powder at least needs 10 small
When, until selenium powder carries out X-ray diffraction analysis, with true all by ball milling at amorphous amorphous selenium to the mixed-powder after ball milling
Selenium powder whole ball milling is determined into amorphous amorphous selenium.
Mixed-powder after ball milling is filled in people's mold, then in room temperature, the condition of pressure 20MPa on belt type press
Lower pressurize 5min is shaped to blank；
Molding blank is put into the press (15MN three pillar types press) of octahedra pressure chamber, is in room temperature, pressure
Then pressurize 10min under the conditions of 12.5GPa slowly increases temperature while keeping the pressure, heats up within the time of 5min
To 1900 DEG C, after being sintered 3600s under the temperature, pressure conditions, room temperature is cooled the temperature in 15min, by pressure in 6h
It is down to normal pressure, recycling sample can be obtained selenium-grain polycrystalline diamond compact.
Embodiment 3
The present embodiment provides a kind of preparation methods of the grain polycrystalline diamond compact of selenium catalyst, including：
Weigh the bortz powder 3.334g that crystal grain is 0.2~5 μm and the selenium powder 0.239g that crystal grain is 10~30 μm, wherein
The weight percent of bortz powder is 93.3%, and the weight percent of selenium powder is 6.7%；
Above-mentioned bortz powder and selenium powder are mixed to get mixed-powder, mixed-powder, which is put into one, is equipped with tungsten-carbide ball
In tungsten carbide bottle, then by tungsten carbide bottle be put into CERTIPREP SPEX8000-D high energy ball mills (Metuchen, NJ) into
Row processing.Wherein, ball mill is located in the seal box crossed with purification for argon.The ball milling of mixed-powder at least needs 10 small
When, until selenium powder carries out X-ray diffraction analysis, with true all by ball milling at amorphous amorphous selenium to the mixed-powder after ball milling
Selenium powder whole ball milling is determined into amorphous amorphous selenium.
Mixed-powder after ball milling is filled in people's mold, then in room temperature, the condition of pressure 10MPa on belt type press
Lower pressurize 1min is shaped to blank；
Molding blank is put into the press (15MN three pillar types press) of octahedra pressure chamber, in room temperature, pressure 10GPa
Under the conditions of pressurize 10min, then slowly increase temperature while keeping the pressure, 1850 be warming up within the time of 5min
DEG C, after being sintered 1800s under the temperature, pressure conditions, room temperature is cooled the temperature in 10min, is down to pressure often in 6h
Pressure, recycling sample can be obtained selenium-grain polycrystalline diamond compact.
Embodiment 4
The present embodiment provides a kind of preparation methods of the grain polycrystalline diamond compact of selenium catalyst, including：
Weigh the bortz powder 3.231g that crystal grain is 5~10 μm and the selenium powder 0.358g that crystal grain is 10~30 μm, wherein gold
The weight percent of emery is 90%, and the weight percent of selenium powder is 10%；
Above-mentioned bortz powder and selenium powder are mixed to get mixed-powder, mixed-powder, which is put into one, is equipped with tungsten-carbide ball
In tungsten carbide bottle, then by tungsten carbide bottle be put into CERTIPREP SPEX8000-D high energy ball mills (Metuchen, NJ) into
Row processing.Wherein, ball mill is located in the seal box crossed with purification for argon.The ball milling of mixed-powder at least needs 10 small
When, until selenium powder carries out X-ray diffraction analysis, with true all by ball milling at amorphous amorphous selenium to the mixed-powder after ball milling
Selenium powder whole ball milling is determined into amorphous amorphous selenium.
Mixed-powder after ball milling is filled in people's mold, then in room temperature, the condition of pressure 15MPa on belt type press
Lower pressurize 4min is shaped to blank；
Molding blank is put into the press (15MN three pillar types press) of octahedra pressure chamber, in room temperature, pressure 9GPa
Under the conditions of pressurize 10min, then slowly increase temperature while keeping the pressure, 1600 be warming up within the time of 5min
DEG C, after being sintered 600s under the temperature, pressure conditions, room temperature is cooled the temperature in 15min, is down to pressure often in 4h
Pressure, recycling sample can be obtained selenium-grain polycrystalline diamond compact.
Test example
(1) microstructure of selenium-grain polycrystalline diamond compact made from embodiment 2 is carried out using scanning electron microscope
Sweep test, obtained micro-structure diagram are as shown in Figure 1.
Fig. 1 interpretations of result:It will be noted from fig. 1 that in the selenium-grain polycrystalline diamond compact, with D- between diamond particles 1
D keys 2 combine, and the carbide 3 filled with selenium and selenium between diamond particles 1.
(2) selenium-polycrystalline diamond prepared by MICRO4 micro-hardnesses meter (BUEHLER LTD) detection the present embodiment 1 is used
The hardness of sintered body：To sample load 9.8N, simultaneously pressurize 15s, every piece of sample make a call to 12 impressions, measure the average hardness of sample,
Acquired average hardness is 21GPa.
(3) selenium-polycrystalline diamond made from MICRO4 micro-hardnesses meter (BUEHLER LTD) detection embodiment 2 is utilized to burn
The hardness of knot body：2.45N, 4.9N, 9.8N, 19.6N are loaded respectively to sample, load pressurize 15s every time, each loading force uses
Repeated loading, and hardness average value is taken, the asymptote hardness that figure measures sample is done, as shown in Figure 2.
Figure it is seen that the asymptote hardness in Fig. 2 is 68GPa, illustrate that selenium-made from the method for this implementation is more
Diamond sintered body has preferable hardness.
To sum up, the grain polycrystalline diamond compact and preparation method thereof of selenium catalyst disclosed by the invention, using selenium powder as tactile
Grain polycrystalline diamond compact is successfully prepared in selenium powder and bortz powder mixed sintering by matchmaker, and selenium has good at ambient temperature
Good inoxidizability, thus it is less using selenium as impurity in the grain polycrystalline diamond compact of catalyst, improve polycrystalline diamond burning
The hardness of knot body, hardness is up to 68GPa or more.And conventional metals catalyst grain polycrystalline diamond compact is eliminated in preparation process
The flow that media reductive processing and vacuum in production process are pre-sintered.Greatly simplify the technological process of production.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (9)
1. a kind of grain polycrystalline diamond compact of selenium catalyst, which is characterized in that the grain polycrystalline diamond compact is by bortz powder
It is made with selenium powder sintering, the carbide of selenium and selenium is filled between the gap of diamond particles, and D-D is formed between the diamond particles
Key.
2. a kind of preparation method of the grain polycrystalline diamond compact of selenium catalyst, which is characterized in that including：
31.59~34.047 parts by weight of micron-sized bortz powder and 1.473~4.79 parts by weight of micron-sized selenium powder are formed
Mixed-powder be ground until the selenium powder become amorphous selenium powder；
The mixed-powder after grinding is placed in mold, base is shaped under conditions of room temperature, pressure 5MPa~20MPa
Part；
By the blank under the pressure of 6.5GPa~12.5GPa sintering curing, wherein sintering temperature be 1500 DEG C~1900
℃。
3. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 2, which is characterized in that the burning
The knot time is 30~3600s.
4. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 2, which is characterized in that the burning
Junction temperature is 1600~1850 DEG C.
5. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 2, which is characterized in that the base
The pressure of part sintering curing is 9~12.5GPa.
6. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 2, which is characterized in that the selenium
The weight percent of powder is 4.2%~13.2%.
7. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 6, which is characterized in that the selenium
The weight percent of powder is 4.2%~6.7%.
8. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 2, which is characterized in that the gold
The crystallite dimension of emery is 0.2~10 μm；Preferably, the crystallite dimension of the bortz powder is 2~5 μm.
9. the preparation method of the grain polycrystalline diamond compact of selenium catalyst according to claim 2, which is characterized in that the selenium
The crystallite dimension of powder is 10~30 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204765A (en) * | 2020-02-13 | 2020-05-29 | 西南交通大学 | Hexagonal structure carbon selenium compound and preparation method thereof |
| CN111809227A (en) * | 2020-06-09 | 2020-10-23 | 四川大学 | Method for preparing porous monocrystalline diamond |
| CN113968736A (en) * | 2021-12-01 | 2022-01-25 | 西南交通大学 | Polycrystalline diamond sintered body of tellurium catalyst and preparation method thereof |
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| US5001452A (en) * | 1987-06-02 | 1991-03-19 | Sumitomo Electric Industries, Ltd. | Semiconducting diamond and process for producing the same |
| CN105013400A (en) * | 2015-06-24 | 2015-11-04 | 河南科技大学 | Use of nonmetal catalyst in synthetic diamond |
| CN105209649A (en) * | 2013-03-31 | 2015-12-30 | 六号元素磨料股份有限公司 | Superhard constructions & methods of making same |
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2018
- 2018-01-26 CN CN201810082112.4A patent/CN108585855B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5001452A (en) * | 1987-06-02 | 1991-03-19 | Sumitomo Electric Industries, Ltd. | Semiconducting diamond and process for producing the same |
| CN105209649A (en) * | 2013-03-31 | 2015-12-30 | 六号元素磨料股份有限公司 | Superhard constructions & methods of making same |
| CN105013400A (en) * | 2015-06-24 | 2015-11-04 | 河南科技大学 | Use of nonmetal catalyst in synthetic diamond |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204765A (en) * | 2020-02-13 | 2020-05-29 | 西南交通大学 | Hexagonal structure carbon selenium compound and preparation method thereof |
| CN111809227A (en) * | 2020-06-09 | 2020-10-23 | 四川大学 | Method for preparing porous monocrystalline diamond |
| CN113968736A (en) * | 2021-12-01 | 2022-01-25 | 西南交通大学 | Polycrystalline diamond sintered body of tellurium catalyst and preparation method thereof |
Also Published As
| Publication number | Publication date |
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| CN108585855B (en) | 2020-07-28 |
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