CN102658061B - Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device - Google Patents

Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device Download PDF

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CN102658061B
CN102658061B CN201210115199.3A CN201210115199A CN102658061B CN 102658061 B CN102658061 B CN 102658061B CN 201210115199 A CN201210115199 A CN 201210115199A CN 102658061 B CN102658061 B CN 102658061B
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synthetic
raw material
pyrophillite
spherical
alms bowl
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CN102658061A (en
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陈涛
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SHANDONG RINENG ULTRAHARD MATERIAL CO Ltd
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SHANDONG RINENG ULTRAHARD MATERIAL CO Ltd
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Abstract

The invention discloses a pressure-equalizing type diamond synthesis device and a diamond synthesis method based on the device. The pressure-equalizing type diamond synthesis device comprises a cubic apparatus, wherein the concave arc-shaped top pressing surface of each top hammer forms a spherical top pressing cavity; a pair of opposite top hammers is provided with a conductive electrode respectively; and the conductive electrode is isolated from the corresponding top hammer. The pressure-equalizing type diamond synthesis device further comprises a spherical raw material synthesis block made of graphite and a catalyst, wherein a spherical pyrophyllite synthesis bowl matched with the spherical top pressing cavity is arranged on the raw material synthesis block; a conductive communicating device corresponding to the conductive electrode and the raw material synthesis block are arranged on the pyrophyllite synthesis bowl; the raw material synthesis block and the pyrophyllite synthesis bowl are spherical and matched with each other; the top pressing surface of the top hammer has a concave arc shape matched with the top hammer; the top hammers apply pressure to the raw material synthesis block from six directions; the pressure in the spherical top pressing cavity is uniform; any angle of the raw material synthesis block is extruded uniformly; when the raw material synthesis block are electrified and heated, the raw material synthesis block has high resistance value and is heated quickly and uniformly; and the synthesis efficiency of the diamond is improved.

Description

All die mould diamond synthesizer and diamond synthetic methods based on this device
Technical field
The present invention relates to a kind of diamond synthesizer, also relate to a kind of diamond synthetic method based on this synthesizer.
Background technology
Diamond is the firmest a kind of carbon structure, carbon atom is wherein arranged with the form of crystal structure, each carbon atom and the other tight bonding of four carbon atom, it between diamond atom, is three-dimensional positive tetrahedron structure, be pyramid structure, become space network structure, finally formed that a kind of hardness is large, the solid of poor activity; In graphite, carbon atom is combined with plane stratiform structural bond, and bonding is more fragile between layers, therefore easily slides between layers and by separately.Under high-temperature high-pressure state, between carbon atom between graphite different layers, can form covalent bond, reach certain time limit when this high-temperature high-pressure state duration, between the carbon atom of a large amount of graphite different layers, form mutually covalent bond, the layer structure of graphite gradates as network structure, and graphite is converted into diamond.So, at high-temperature high-pressure state, under the effect of catalyst, can utilize graphite diamond synthesis.
The capital equipment of diamond synthesis monocrystalline has two kinds now: the one, and external top, two sides; The 2nd, domestic cubic apparatus.Principle is all under HTHP, to make graphite catalyst be transformed into diamond.
All to adopt square pyrophyllite block (insulation, pressure transmission, heat insulation, insulation function), conducting steel ring (being commonly called as " plug "), synthetic post (producing adamantine catalyst post) at present.After assembling, through heat treated, be then placed in cubic apparatus and synthesize.Because whole assembly is all square or planar rondure, this structure influence the temperature equalization of inside cavity and the equilibrium of pressure, so some characteristics of diamond grit of producing, form, hardness etc. are unbalanced.Equally, because traditional press top hammer is square, and the inside cavity of pyrophillite assembled block is cylinder, therefore the transmission of internal pressure and electric current move towards unbalanced, therefore the temperature and pressure of the synthetic post of pyrophillite assembled block inside is also unbalanced, affects adamantine combined coefficient.
Summary of the invention
First technical problem to be solved by this invention is to provide one and can guarantees the synthetic piece pressurized of raw material and be heated evenly, thereby improves the equal die mould diamond synthesizer of diamond combined coefficient.
For solving the problems of the technologies described above, technical scheme of the present invention is: all die mould diamond synthesizers, comprise cubic apparatus, the top hammer of described cubic apparatus has indent arched top pressure surface, described indent arched top pressure surface forms pressure chamber, spherical top, wherein in a pair of relative described top hammer, be respectively equipped with conductive electrode, between described conductive electrode and corresponding described top hammer, insulate;
Also comprise the synthetic piece of the spherical raw material of being made by graphite and catalyst, the synthetic alms bowl of the spherical pyrophillite mating with pressure chamber, described spherical top is installed on the synthetic piece of described raw material, the conductive communication device corresponding with described conductive electrode and the synthetic piece of described raw material is installed on the synthetic alms bowl of described pyrophillite;
Described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate.
As the preferred technical scheme of one, six described indent arched top pressure surface shapes are identical.
As the preferred technical scheme of one, described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate.
As the preferred technical scheme of one, the synthetic alms bowl of described spherical pyrophillite comprises two synthetic alms bowls of hemispherical pyrophillite of coupling mutually.
Owing to having adopted technique scheme, all die mould diamond synthesizers, comprise cubic apparatus, the top hammer of described cubic apparatus has indent arched top pressure surface, described indent arched top pressure surface forms pressure chamber, spherical top, wherein in a pair of relative described top hammer, be respectively equipped with conductive electrode, between described conductive electrode and corresponding described top hammer, insulate; Also comprise the synthetic piece of the spherical raw material of being made by graphite and catalyst, the synthetic alms bowl of the spherical pyrophillite mating with pressure chamber, described spherical top is installed on the synthetic piece of described raw material, the conductive communication device corresponding with described conductive electrode and the synthetic piece of described raw material is installed on the synthetic alms bowl of described pyrophillite; Described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate; The synthetic piece of raw material and the synthetic alms bowl of pyrophillite are the spherical of coupling mutually, the top pressure surface of top hammer is the indent arc matching with it, top hammer is exerted pressure to the synthetic piece of raw material from six direction, and spherical top presses cavity pressure even, and any angle of the synthetic piece of raw material can be subject to even extruding; To the synthetic piece energising of raw material heating, because the synthetic piece resistance of raw material is higher, heat up rapidly evenly simultaneously; Improve adamantine combined coefficient.
Second technical problem to be solved by this invention is to provide a kind of diamond synthetic method based on equal die mould diamond synthesizer.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of diamond synthetic method based on equal die mould diamond synthesizer, comprises the steps:
(1) graphite powder and catalyst are mixed, be made into the synthetic piece of spherical raw material;
(2) make the synthetic alms bowl of spherical pyrophillite, the synthetic alms bowl of described spherical pyrophillite has the cavity that holds the synthetic piece of described spherical raw material, and synthetic described raw material piece is installed in the synthetic alms bowl of described spherical pyrophillite; The conductive communication device corresponding with described conductive electrode and the synthetic piece of described raw material is installed on the synthetic alms bowl of described pyrophillite; Described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate;
(3) then the assembly of synthetic pyrophillite alms bowl and the synthetic piece of raw material is placed on the workbench of cubic apparatus, the top hammer of described cubic apparatus has indent arched top pressure surface, described indent arched top pressure surface forms pressure chamber, spherical top, the assembly of the synthetic alms bowl of described pyrophillite and the synthetic piece of raw material is positioned at described shape top and presses chamber, wherein in a pair of relative described top hammer, be respectively equipped with conductive electrode, between described conductive electrode and corresponding described top hammer, insulate; Make the described conductive communication device on the synthetic alms bowl of described pyrophillite corresponding with described conductive electrode;
(4) start cubic apparatus, the synthetic alms bowl of top hammer extruding pyrophillite, the pressure in the synthetic alms bowl of pyrophillite raises, and treats that pressure is increased to 2.1~5.8Gpa, simultaneously by conductive electrode and power connection, the synthetic piece energising of raw material heating, temperature is increased to 1100~1500 ℃, is incubated after 2~5 minutes, slowly cool to below 80 ℃, then slowly removal pressure, to normal pressure, is removed the synthetic alms bowl of pyrophillite, finally takes out and contains adamantine sintered body.
As the preferred technical scheme of one, the synthetic alms bowl of described spherical pyrophillite comprises two synthetic alms bowls of hemispherical pyrophillite of coupling mutually.
As the preferred technical scheme of one, described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate.
As the preferred technical scheme of one, six described indent arched top pressure surface shapes are identical.
Because equal die mould diamond synthesizer can guarantee that raw material synthesizes all even being heated evenly of piece pressurized, i.e. pressure conduction equilibrium, current trend equilibrium; Pyrophillite synthesizes the inside cavity temperature equalization that alms bowl surrounds, and not only can improve the efficiency of diamond synthesis, and the grade of diamond synthesis is higher, form is more complete.
accompanying drawing explanation
The following drawings is only intended to the present invention to schematically illustrate and explain, not delimit the scope of the invention.Wherein,
Fig. 1 is embodiment of the present invention top pressure condition schematic diagram;
Fig. 2 is that the embodiment of the present invention is treated top pressure condition schematic diagram;
Fig. 3 is the assembled state schematic diagram of the synthetic alms bowl of the spherical pyrophillite of the embodiment of the present invention and the synthetic piece of raw material;
Fig. 4 is the synthetic alms bowl of the spherical pyrophillite of the embodiment of the present invention and the synthetic piece disassembled state schematic diagram of raw material;
In figure: 1-top hammer; 11-indent arched top pressure surface; Pressure chamber, the spherical top of 2-; 3-conductive electrode; 4-raw material synthesizes piece; 5-pyrophillite synthesizes alms bowl; 61-conductive cap; 62-insulating barrier; 63-electrode jack.
The specific embodiment
Describe in detail with reference to the accompanying drawings according to exemplary embodiment of the present invention.Here, it should be noted that in the accompanying drawings, give structure and the essentially identical part of function by identical Reference numeral, and in order to make description simpler and clearer, omitted about the redundancy of substantially the same part and described.
As depicted in figs. 1 and 2, all die mould diamond synthesizer, comprises cubic apparatus, comprises six top hammers 1, only shows four top hammer 1 sections of upper and lower and left and right in Fig. 1 and Fig. 2, and two top hammers 1 of vertical section direction are not shown; The top hammer 1 of described cubic apparatus has indent arched top pressure surface 11, six described indent arched top pressure surface 11 shapes are identical, described indent arched top pressure surface 11 forms pressure chamber, spherical top 2, wherein in a pair of relative described top hammer, be respectively equipped with conductive electrode 3, between described conductive electrode 3 and corresponding described top hammer 1, insulate;
As shown in Figure 3 and Figure 4, also comprise the synthetic piece 4 of the spherical raw material of being made by graphite and catalyst, the synthetic alms bowl 5 of the spherical pyrophillite mating with pressure chamber, described spherical top 2 is installed on the synthetic piece 4 of described raw material, and the synthetic alms bowl 5 of described spherical pyrophillite comprises two synthetic alms bowls 5 of hemispherical pyrophillite of coupling mutually, on the synthetic alms bowl 5 of hemispherical pyrophillite of the synthetic alms bowl 5 of described pyrophillite, the conductive communication device corresponding with described conductive electrode 3 and the synthetic piece 4 of described raw material is installed, described conductive communication device comprises the conductive cap 61 corresponding with described conductive electrode 3 and the synthetic piece 4 of described raw material, insulation between described conductive cap 61 and all described top hammers 1, described conductive cap 61 is provided with insulating barrier 62 towards the end face of adjacent described top hammer 1, described insulating barrier 62 is provided with the electrode jack 63 corresponding with described conductive electrode 3, the end of described conductive electrode 3 is inserted described electrode jack 63 and is contacted with described conductive cap 61.The conductive electrode 3 that is positioned at two relative top hammers 1 is communicated with by the synthetic piece 4 of corresponding conductive cap 61 and raw material.
The synthetic piece 4 of raw material is made after being mixed by graphite powder and catalyst powder, and catalyst can adopt the material such as Co, Ni.
The synthetic piece 4 of raw material is spherical, the top pressure surface of top hammer 1 is the indent arc matching with it, start after cubic apparatus, top hammer 1 is exerted pressure to the synthetic piece 4 of raw material from six direction, pressure chamber, spherical top 2 internal pressures are even, the synthetic cavity pressure that the synthetic alms bowl 5 of pyrophillite surrounds is also even, and any angle of the synthetic piece 4 of raw material can be subject to even extruding; Two conductive electrode 3 places in circuit in relative top hammer 1 will be positioned at, conductive cap 61, raw material synthetic piece 4, another conductive cap 61 and another conductive electrode 3 that electric current is answered through a conductive electrode 3, with this electrode pair, to the synthetic piece 4 energising heating of raw material, because synthetic piece 4 resistances of raw material are higher, produce heat very many, heat up rapidly evenly; The pressure of uniform balance and the temperature of uniform balance have improved adamantine combined coefficient.
Based on a diamond synthetic method for equal die mould diamond synthesizer, comprise the steps:
(1) graphite powder and catalyst are mixed, be made into the synthetic piece 4 of spherical raw material;
(2) make the synthetic alms bowl of spherical pyrophillite, the synthetic alms bowl of described spherical pyrophillite comprises two synthetic alms bowls of hemispherical pyrophillite of coupling mutually; The synthetic alms bowl of described spherical pyrophillite has the cavity that holds the synthetic piece 4 of described spherical raw material, and synthetic described raw material piece 4 is installed in the synthetic alms bowl of described spherical pyrophillite; The conductive communication device corresponding with described conductive electrode 3 and the synthetic piece 4 of described raw material is installed on the synthetic alms bowl 5 of described pyrophillite, described conductive communication device comprises the conductive cap 61 corresponding with described conductive electrode 3 and the synthetic piece 4 of described raw material, insulation between described conductive cap 61 and all described top hammers 1;
(3) then the assembly of synthetic pyrophillite alms bowl 5 and the synthetic piece 4 of raw material is placed on the workbench of cubic apparatus, it is identical that the top hammer 1 of described cubic apparatus has 11, six described indent arched top pressure surface 11 shapes of indent arched top pressure surface; Described indent arched top pressure surface 11 forms pressure chamber, spherical top 2, the assembly of the synthetic alms bowl 5 of described pyrophillite and the synthetic piece 4 of raw material is positioned at pressure chamber, described spherical top 2, wherein in a pair of relative described top hammer 1, be respectively equipped with conductive electrode 3, between described conductive electrode 3 and corresponding described top hammer 1, insulate; Make the described conductive cap 61 on the synthetic alms bowl 5 of described pyrophillite corresponding with described conductive electrode 3;
(4) start cubic apparatus, top hammer 1 is pushed the synthetic alms bowl 5 of pyrophillite, and the pressure in the synthetic alms bowl 5 of pyrophillite raises, and treats that pressure is increased to 2.1~5.8Gpa, simultaneously by conductive electrode 3 and power connection, the synthetic piece 4 energising heating of raw material, temperature is increased to 1100~1500 ℃, is incubated after 2~5 minutes, slowly cool to below 80 ℃, then slowly removal pressure, to normal pressure, is removed the synthetic alms bowl 5 of pyrophillite, finally takes out and contains adamantine sintered body.
Because equal die mould diamond synthesizer can guarantee that raw material synthesizes all even being heated evenly of piece 4 pressurizeds, i.e. pressure conduction equilibrium, current trend equilibrium; Pyrophillite synthesizes the inside cavity temperature equalization that alms bowl 5 surrounds, and not only can improve the efficiency of diamond synthesis, and the grade of diamond synthesis is higher, form is more complete.
As mentioned above, describe particularly embodiments of the invention in the above, but the invention is not restricted to this.It should be appreciated by those skilled in the art, can carry out various modifications, combination, sub-portfolio or replacement according to designing requirement or other factors, and they are in the scope of claims and equivalent thereof.

Claims (1)

1. equal die mould diamond synthesizer, it is characterized in that: comprise cubic apparatus, the top hammer of described cubic apparatus has indent arched top pressure surface, described indent arched top pressure surface forms pressure chamber, spherical top, wherein in a pair of relative described top hammer, be respectively equipped with conductive electrode, between described conductive electrode and corresponding described top hammer, insulate;
Also comprise the synthetic piece of the spherical raw material of being made by graphite and catalyst, the synthetic alms bowl of the spherical pyrophillite mating with pressure chamber, described spherical top is installed on the synthetic piece of described raw material, the conductive communication device corresponding with described conductive electrode and the synthetic piece of described raw material is installed on the synthetic alms bowl of described pyrophillite;
Described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate.
2. equal die mould diamond synthesizer as claimed in claim 1, is characterized in that: six described indent arched top pressure surface shapes are identical.
3. equal die mould diamond synthesizer as claimed in claim 1 or 2, is characterized in that: the synthetic alms bowl of described spherical pyrophillite comprises two synthetic alms bowls of hemispherical pyrophillite of coupling mutually.
4. the diamond synthetic method based on equal die mould diamond synthesizer claimed in claim 1, is characterized in that, comprises the steps:
(1) graphite powder and catalyst are mixed, be made into the synthetic piece of spherical raw material;
(2) make the synthetic alms bowl of spherical pyrophillite, the synthetic alms bowl of described spherical pyrophillite has the cavity that holds the synthetic piece of described spherical raw material, and synthetic described raw material piece is installed in the synthetic alms bowl of described spherical pyrophillite; The conductive communication device corresponding with described conductive electrode and the synthetic piece of described raw material is installed on the synthetic alms bowl of described pyrophillite; Described conductive communication device comprises the conductive cap corresponding with described conductive electrode and the synthetic piece of described raw material, between described conductive cap and all described top hammers, insulate;
(3) then the assembly of synthetic pyrophillite alms bowl and the synthetic piece of raw material is placed on the workbench of cubic apparatus, the top hammer of described cubic apparatus has indent arched top pressure surface, described indent arched top pressure surface forms pressure chamber, spherical top, the assembly of the synthetic alms bowl of described pyrophillite and the synthetic piece of raw material is positioned at pressure chamber, described spherical top, wherein in a pair of relative described top hammer, be respectively equipped with conductive electrode, between described conductive electrode and corresponding described top hammer, insulate; Make the described conductive communication device on the synthetic alms bowl of described pyrophillite corresponding with described conductive electrode;
(4) start cubic apparatus, the synthetic alms bowl of top hammer extruding pyrophillite, the pressure in the synthetic alms bowl of pyrophillite raises, and treats that pressure is increased to 2.1~5.8GPa, simultaneously by conductive electrode and power connection, the synthetic piece energising of raw material heating, temperature is increased to 1100~1500 ℃, is incubated after 2~5 minutes, slowly cool to below 80 ℃, then slowly removal pressure, to normal pressure, is removed the synthetic alms bowl of pyrophillite, finally takes out and contains adamantine sintered body.
5. diamond synthetic method as claimed in claim 4, is characterized in that: the synthetic alms bowl of described spherical pyrophillite comprises two synthetic alms bowls of hemispherical pyrophillite of coupling mutually.
6. the diamond synthetic method as described in claim 4 or 5, is characterized in that: six described indent arched top pressure surface shapes are identical.
CN201210115199.3A 2012-04-19 2012-04-19 Pressure-equalizing type diamond synthesis device and diamond synthesis method based on device Expired - Fee Related CN102658061B (en)

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CN103521134B (en) * 2013-10-29 2015-06-17 河南晶锐超硬材料有限公司 Assembly for super-hard material synthesis
CN106422983A (en) * 2016-11-10 2017-02-22 郑州磨料磨具磨削研究所有限公司 Ultrahigh-pressure pressurizing and heating device
CN111167377B (en) * 2020-01-14 2021-09-14 燕山大学 Arc top hammer type four-side top ultrahigh-pressure device
CN113290926B (en) * 2021-04-26 2021-11-05 杭州超然金刚石有限公司 Preparation device and preparation process of diamond semiconductor

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IE74960B1 (en) * 1995-01-05 1997-08-13 Sii Megadiamond Inc Synthetic gasket materials for use in high-pressure presses
CN2235855Y (en) * 1995-10-14 1996-09-25 徐宏舫 Conducting stop of artificial diamond pyrophyllite block
JP2006231277A (en) * 2005-02-28 2006-09-07 Okayama Univ Single crystal synthesizing method and device
CN100441282C (en) * 2006-12-25 2008-12-10 张甜 Super high pressure mould of six top surfaced diamond synthesis pressure equipment
CN201020356Y (en) * 2007-03-06 2008-02-13 四川大学原子与分子物理研究所 Temperature measuring and controlling device in hexahedral top pressure airtight synthetic cavity
CN101329376A (en) * 2008-07-29 2008-12-24 中国科学院物理研究所 Device and method for measuring dielectric constant and dielectric loss of sample under low high temperature and high voltage
CN202516531U (en) * 2012-04-19 2012-11-07 山东日能超硬材料有限公司 Pressure-equalizing diamond synthesizing device

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