CN105107431B - A kind of heater-type expands high pressure synthesis equipment - Google Patents
A kind of heater-type expands high pressure synthesis equipment Download PDFInfo
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- CN105107431B CN105107431B CN201510635170.1A CN201510635170A CN105107431B CN 105107431 B CN105107431 B CN 105107431B CN 201510635170 A CN201510635170 A CN 201510635170A CN 105107431 B CN105107431 B CN 105107431B
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Abstract
The invention discloses a kind of heater-type to expand high pressure synthesis equipment, including alloy cylinder body, the alloy cylinder body is divided into left and right cylinder body two parts, the heating coil being coaxial therewith is respectively provided with left and right two parts of alloy cylinder body, in the outer wall of heating coil, thermal insulating warm-keeping layer is set, high-pressure column is equipped with the two-part cental axial position in the left and right of alloy cylinder body, high-pressure column is separated out with heating coil by the B of alloy cylinder body, high pressure intercolumniation forms sample synthesis chamber, inventive samples blended space is larger, can reach 100mm3, outstanding advantages of cost is also far below diamond anvil cell high-tension apparatus, has design science, and the 5GPa of pressure limit 0, equipment investment cost is low, and safety is easy to operate, service life length, and temperature, pressure controllability is good；The experiment that can be prepared as material high pressure or production equipment, be widely used in national defence, new energy, new material, learn, the field such as planetary science, chemistry, Condensed Matter Physics, biomedicine.
Description
Technical field
The present invention relates to material high pressure synthesis equipment, especially a kind of heater-type expansion high pressure synthesis equipment.
Background technology
Static pressure technical equipment common at present mainly has the high-tension apparatuses such as cubic hinge press, top anvil high-pressure installation.Superelevation
Pressing forming apparatus cubic hinge press has many advantages, such as that as device structure is simple, synthetic operation is easy, and static pressure performance is good.But
With the development trend that press maximizes, complete machine is huger, and cost of investment is also with significantly improving, cubic hinge press in addition
The structures shape of pressure head cubic hinge press can not infinitely compress, i.e. hot compression stroke is smaller.
The content of the invention
The technical problems to be solved by the invention are：Kind of a heater-type expansion high pressure synthesis equipment is provided, in equal pressure strip
Under part, cost of investment significantly reduces, and designs different compression travels, is not limited by structure space, to overcome prior art
Deficiency.
What the present invention was realized in：A kind of heater-type expands high pressure synthesis equipment, including alloy cylinder body, the alloy cylinder body
It is divided into left and right cylinder body two parts, the heating coil being coaxial therewith is respectively provided with left and right two parts of alloy cylinder body, in heater wire
The outer wall of circle sets thermal insulating warm-keeping layer, and high-pressure column, high pressure are equipped with the two-part cental axial position in the left and right of alloy cylinder body
Post is separated out with heating coil by the B of alloy cylinder body, and high pressure intercolumniation forms sample synthesis chamber, and alloy cylinder body uses wolfram steel YG20
Or MGH4754 alloys are made, high-pressure column is made of fine copper, brass or manganin, and its general principle utilizes high-pressure column
Thermal coefficient of expansion is more than the thermal coefficient of expansion of alloy cylinder block material, under materials synthesis higher temperature, because of the expansion of high-pressure column
Make material be synthesized during and meanwhile there is higher pressure environment, specifically, heating coil be passed through the electric current of certain power from
And heat is produced, because thermal insulating warm-keeping layer can prevent heat to external diffusion, so that heat mainly inwardly transmits；Work as heat transfer
During to high-pressure column, because high-pressure column is the larger alloy material composition of linear expansion coefficient, so during isodose temperature change, it is stretched
Shrinkage is more than alloy cylinder body, therefore left and right two parts of high-pressure column will extrude to the sample synthesis chamber of centre, so that sample exists
During synthesis, there is certain hyperbaric environment；Part between alloy cylinder body, high-pressure column and heating coil is in production preparation process
In, there is autofrettage effeet；It is swollen due to high-pressure column under conditions of utilizing more than 1.1 times of temperature in use when equipment produces
Swelling pressure power makes the region A of inner wall layer（At the 1/3 of total wall thickness）It is plastically deformed, and B areas are still elastic deformation；Temperature drops
To normal temperature, after release reduces to normal pressure, there is residual stress without resilient, the B layers of elastic deformation in the A layers of plastic deformation
It can then restore to the original state, then B layers just generate the effect for compressing lock ring inward to A layers.
In a kind of foregoing heater-type expansion high pressure synthesis equipment, the outside of the alloy cylinder body is provided with for connecting a left side
The hinge of right cylinder body, one of hinge are fixed hinge, and another hinge is hinges, in order to keep internal high pressure,
Need preferable lock ring measure.Contining function is reached using hinge 7.
In a kind of foregoing heater-type expansion high pressure synthesis equipment, hard alloy is set on the relative termination of high-pressure column,
Hard alloy is made of tungsten carbide wc.
By adopting the above-described technical solution, compared with prior art, the beneficial effects of the invention are as follows：
（1）Structural principle of the present invention is rationally reliable, and modern design can be used for the material of high-pressure synthesis large-size.
（2）Pressure limit 0-5GPa of the present invention, pressure caused by thermal expansion are highly stable.
（3）Present device cost is low to be far below traditional high-tension apparatus.
（4）Present device can sub computers software systems, operability is good.
（5）Present device running is without recirculated water, and heat loss is seldom, and energy consumption is very low.
（6）Present device uses heater-type, and by the heat transfer of heat coil, the temperature rise generation heat of high-pressure column is swollen
It is swollen, and therefore produce high pressure.
（7）Present device, key fitment are high-pressure column, hard alloy blocks and internal layer cylinder body, are non-moving parts, make
Use long lifespan.It can standardize, be easily changed in addition.
Brief description of the drawings
Accompanying drawing 1 is schematic structural view of the invention；
Accompanying drawing 2 is cylinder body open mode schematic diagram in left and right of the present invention；
Accompanying drawing 3 is Fig. 1 of the present invention A-A section left views；
Accompanying drawing 4 is Fig. 1 of the present invention A-A section right views
Accompanying drawing 5 is alloy cylinder body from contining function schematic diagram.
Embodiment
Embodiments of the invention：A kind of heater-type expands high pressure synthesis equipment, including alloy cylinder body 2, it is characterised in that：Should
Alloy cylinder body 2 divides for left and right cylinder body two parts, and the heating coil being coaxial therewith is respectively provided with left and right two parts of alloy cylinder body 2
3, thermal insulating warm-keeping layer 4 is set in the outer wall of heating coil 3, is all provided with the two-part cental axial position in the left and right of alloy cylinder body 2
There is high-pressure column 1, high-pressure column 1 is separated out with heating coil 3 by the B of alloy cylinder body 2, and sample synthesis chamber 6 is formed between high-pressure column 1,
Alloy cylinder body 2 is made of wolfram steel YG20 or MGH4754 alloy, and high-pressure column 1 is made of fine copper, brass or manganin, its
The outside of middle alloy cylinder body 2 is provided with the hinge 7 for connecting left and right cylinder body, and one of hinge 7 is fixed hinge, another
Hinge 7 is hinges, and hard alloy 5 is set on the relative termination of high-pressure column 1, and hard alloy 5 is made of tungsten carbide wc.
The general principle of the present embodiment is to be more than the thermal expansion of the material of alloy cylinder body 2 using the thermal coefficient of expansion of high-pressure column 1
Coefficient, under materials synthesis higher temperature, during being synthesized material because of the expansion of high-pressure column 1 while there is higher pressure
Force environment.
A diameter of 10.6mm of high-pressure column 1, length are divided into 400mm, 600mm and 800mm tri- according to the pressure difference of design
Kind model；Left and right two edge lengths of high-pressure column are different, and by taking accompanying drawing 1 as an example, left side high-pressure column is that full-length subtracts 5mm, and hard closes
The a diameter of 10.6mm, length 20mm, 2 a diameter of 230mm of alloy cylinder body of gold 5, total length can divide according to the length of high-pressure column 1
For 900mm, 1300mm and 1700mm, the other designs of alloy cylinder body are specifically shown in accompanying drawing 1.
Specifically, heating coil 3 is passed through the electric current of certain power so as to produce heat, because thermal insulating warm-keeping layer 4 can prevent
Heat is to external diffusion, so that heat mainly inwardly transmits.When heat transfer is to high-pressure column 1, because high-pressure column 1 is line expansion
The larger alloy material composition of coefficient, so during isodose temperature change, its expansion and contraction is more than alloy cylinder body 2, therefore high-pressure column 1
Left and right two parts will to centre sample synthesis chamber 6 extrude so that sample synthesis when, there is certain hyperbaric environment.
Part between alloy cylinder body 2, high-pressure column 1 and heating coil 3 has self-reinforcing effect in preparation process is produced
Should.When equipment produces, under conditions of utilizing more than 1.1 times of temperature in use, because the bulbs of pressure of high-pressure column 1 make inner wall layer
Region A（At the 1/3 of total wall thickness）It is plastically deformed, and B areas are still elastic deformation such as accompanying drawing 4).Temperature is down to normal temperature
Afterwards, after release reduces to normal pressure, there is residual stress without resilient in the A layers of plastic deformation.The B layers of elastic deformation then can be extensive
Restore shape.Then B layers just generate the effect for compressing lock ring inward to A layers.
In order to keep the high pressure of inside, it is necessary to preferably lock ring measure.Contining function is reached using hinge 7, meanwhile, Fig. 2
In, lower hinge is fixed hinge, and upper hinge is to open.
Specifically used process
First, in use, upper hinge is opened, the rotation of right half part cylinder body is then fallen on fixed position, function ceramics
Material is shaped to diameter 10mm, a height of 5mm cylinder sample.Sample is put into equipment sample synthesis chamber 6, then pull-up right half part
Cylinder body, after upper hinge is alignd, connected with hoop is locked.Lock ring situation, temperature-controlling system are checked, after all going well, passes through temperature control journey
Sequence sets sample synthesis temperature controlling curve, then runs temperature control program, equipment is passed through the electric current of certain power.Work as high-pressure column
When reaching higher temperature, turgor pressure is produced in device interior because of thermal expansion, while sample also reaches synthesis temperature.Insulation 120
After minute, power supply is closed, 30 minutes or so sample temperatures of cooling are reduced to close to room temperature, upper hinge are then opened, right side
Divide cylinder body rotation to fall on fixed position, take out synthetic material sample.
2nd, in use, upper hinge is opened, the rotation of right half part cylinder body is then fallen on fixed position, work(thermoelectricity material
Material is shaped to diameter 10mm, a height of 5mm cylinder sample.Sample is put into equipment sample synthesis chamber 6, then pull-up right half part cylinder
Body, after upper hinge is alignd, connected with hoop is locked.Lock ring situation, temperature-controlling system are checked, after all going well, passes through temperature control program
Sample synthesis temperature controlling curve is set, temperature control program is then run, equipment is passed through the electric current of certain power.When high-pressure column reaches
During to higher temperature, turgor pressure is produced in device interior because of thermal expansion, while sample also reaches synthesis temperature.Insulation 60 minutes
Afterwards, power supply is closed, 30 minutes or so sample temperatures of cooling are reduced to close to room temperature, upper hinge are then opened, right half part cylinder
Body rotation falls on fixed position, takes out synthetic material sample.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and be carried out, can not be all according to this hair as limiting the scope of the invention
The equivalent variations or modification that bright Spirit Essence is made, it should all cover within the scope of the present invention.
Claims (3)
1. a kind of heater-type expands high pressure synthesis equipment, including alloy cylinder body (2), it is characterised in that：The alloy cylinder body (2) is divided into
Left and right cylinder body two parts, the heating coil (3) being coaxial therewith is respectively provided with left and right two parts of alloy cylinder body (2), is being heated
The outer wall of coil (3) sets thermal insulating warm-keeping layer (4), is equipped with the two-part cental axial position in left and right of alloy cylinder body (2)
High-pressure column (1), high-pressure column (1) and heating coil (3) by be located in alloy cylinder body (2) high-pressure column (1) and heating coil (3) it
Between A areas, B separate out, between high-pressure column (1) formed sample synthesis chamber (6).
A kind of 2. heater-type expansion high pressure synthesis equipment according to claim 1, it is characterised in that：The alloy cylinder body
(2) outside is provided with the hinge (7) for connecting left and right cylinder body, and one of hinge (7) is fixed hinge, another hinge
(7) it is hinges.
A kind of 3. heater-type expansion high pressure synthesis equipment according to claim 1, it is characterised in that：In high-pressure column (1)
With respect to setting hard alloy (5) on termination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510635170.1A CN105107431B (en) | 2015-09-30 | 2015-09-30 | A kind of heater-type expands high pressure synthesis equipment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510635170.1A CN105107431B (en) | 2015-09-30 | 2015-09-30 | A kind of heater-type expands high pressure synthesis equipment |
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| Publication Number | Publication Date |
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| CN105107431A CN105107431A (en) | 2015-12-02 |
| CN105107431B true CN105107431B (en) | 2018-02-09 |
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| CN201510635170.1A Active CN105107431B (en) | 2015-09-30 | 2015-09-30 | A kind of heater-type expands high pressure synthesis equipment |
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| GB201907655D0 (en) | 2019-05-30 | 2019-07-17 | Gull Corp Ltd | Apparatus and methods for the manufacture of synthetic diamonds |
| KR20220015409A (en) | 2019-05-30 | 2022-02-08 | 걸 코포레이션 리미티드 | Apparatus and method for producing synthetic diamonds |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0523573A (en) * | 1991-07-24 | 1993-02-02 | Sumitomo Electric Ind Ltd | Pressure control in superhigh device |
| US5512235A (en) * | 1994-05-06 | 1996-04-30 | General Electric Company | Supported polycrystalline compacts having improved physical properties and method for making same |
| CN200991645Y (en) * | 2006-12-16 | 2007-12-19 | 山东理工大学 | Device for producing pressure by expand with heat and contract with cold |
| CN101819104B (en) * | 2010-04-16 | 2011-07-20 | 北京工业大学 | Small-sized heated supercharging device |
| CN203710985U (en) * | 2013-12-24 | 2014-07-16 | 中国科学院上海硅酸盐研究所 | High-pressure mold |
| CN204973811U (en) * | 2015-09-30 | 2016-01-20 | 贵州大学 | Heater -type inflation high pressure synthesis equipment |
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