CN105107431A - Heater-type expansive high pressure synthesis equipment - Google Patents

Heater-type expansive high pressure synthesis equipment Download PDF

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Publication number
CN105107431A
CN105107431A CN201510635170.1A CN201510635170A CN105107431A CN 105107431 A CN105107431 A CN 105107431A CN 201510635170 A CN201510635170 A CN 201510635170A CN 105107431 A CN105107431 A CN 105107431A
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heater
pressure
cylinder body
cylinder
alloy
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CN201510635170.1A
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CN105107431B (en
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张金柱
秦丙克
籍永华
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Guizhou University
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Guizhou University
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Abstract

The invention discloses heater-type expansive high pressure synthesis equipment, comprising an alloy cylinder, wherein the alloy cylinder consists of a left cylinder and a right cylinder; the left cylinder and the right cylinder are internally provided with heater coils, and the left cylinder and the right cylinder are coaxial with the respective heater coils; outer walls of the heater coils are provided with insulation layers; high-pressure columns are arranged at the center shaft positions of the left cylinder and the right cylinder of the alloy cylinder, the high-pressure columns are separated from the heater coils through a B area of the alloy cylinder, a sample synthesis room is formed between the high-pressure columns; the heater-type expansive high pressure synthesis equipment provided by the invention has a big sample synthesis space which can reach 100mm<3>, and the cost is far lower than the cost of diamond anvil cell high-voltage equipment; the heater-type expansive high pressure synthesis equipment has the outstanding advantages that the design is scientific, the pressure range is 0 to 5 GPa, the equipment investment cost is low, the safety and easy operation are realized, the service life is long, the controllability of temperature pressure is good, and the like; the heater-type expansive high pressure synthesis equipment can be used for the test or production equipment of high pressure preparation of materials, is widely used in the field such as national defenses, new energy resources, new materials, geonomy, planetary science, chemistry, condensed matter physics, biomedicine and the like.

Description

A kind of heater-type expansion high pressure synthesis equipment
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 contains the high-tension apparatus such as cubic hinge press, top anvil high-pressure installation.Super-pressure synthesis device cubic hinge press has plurality of advantages, and as device structure is simple, synthetic operation is easy, and static pressure performance is good.But along with the development trend that press maximizes, complete machine is huger, cost of investment is also along with significantly improving, and the structures shape cubic hinge press of the pressure head of cubic hinge press can not infinitely compress in addition, and instant heating compression travel is less.
Summary of the invention
Technical problem to be solved by this invention is: provide kind of a heater-type expansion high pressure synthesis equipment, under equal pressure condition, cost of investment significantly reduces, and designs different compression travel, not limited by structure space, to overcome the deficiencies in the prior art.
The present invention is achieved in that a kind of heater-type expansion high pressure synthesis equipment, comprise alloy cylinder body, this alloy cylinder body is divided into left and right cylinder body two parts, in left and right two parts of alloy cylinder body, all the heater coil coaxial with it is set, at the outer wall of heater coil, thermal insulating warm-keeping layer is set, the two-part cental axial position in the left and right of alloy cylinder body is equipped with high-pressure column, high-pressure column and heater coil are separated out by the B of alloy cylinder body, sample synthesis room is formed between high-pressure column, alloy cylinder body adopts wolfram steel YG20 or MGH4754 alloy to make, high-pressure column adopts fine copper, brass or manganin are made, its general principle is the thermal coefficient of expansion utilizing the thermal coefficient of expansion of high-pressure column to be greater than alloy cylinder block material, under materials synthesis higher temperature, make because of the expansion of high-pressure column material be synthesized in process and there is higher pressure environment simultaneously, concrete, heater coil passes into the electric current of certain power thus produces heat, because thermal insulating warm-keeping layer can stop heat to external diffusion, thus heat is mainly inwardly transmitted, when heat is delivered to high-pressure column, because high-pressure column is the alloy material composition that linear expansion coefficient is larger, so during isodose variations in temperature, its expansion and contraction is greater than alloy cylinder body, therefore left and right two parts of high-pressure column are by the sample synthesis room extruding to centre, thus make sample when synthesizing, there is certain hyperbaric environment, alloy cylinder body, part between high-pressure column and heater coil, in manufacture process, have autofrettage effeet, when device fabrication, adopt under exceeding the condition of serviceability temperature 1.1 times, the bulbs of pressure due to high-pressure column make the region A(of inner wall layer be less than 1/3 place of total wall thickness) there is plastic deformation, and B district is still elastic deformation, after temperature is down to normal temperature, after release reduces to normal pressure, there is residual stress and non-resilient in the A layer of plastic deformation, the B layer of elastic deformation then can restore to the original state, so B layer just creates the effect compressing lock ring inward to A layer.
In aforesaid a kind of heater-type expansion high pressure synthesis equipment, the outer setting of described alloy cylinder body has the hinge for connecting left and right cylinder body, one of them hinge to be fixed hinge, and another hinge is hinges, in order to keep inner high pressure, need good lock ring measure.Hinge 7 is adopted to reach contining function.
In aforesaid a kind of heater-type expansion high pressure synthesis equipment, the relative termination of high-pressure column arranges carbide alloy, carbide alloy adopts tungsten carbide wc to make.
Owing to have employed technique scheme, compared with prior art, the invention has the beneficial effects as follows:
(1) structural principle of the present invention is rationally reliable, and modern design may be used for the material of high-pressure synthesis large-size.
(2) pressure limit 0-5GPa of the present invention, the pressure that thermal expansion produces is highly stable.
(3) present device cost is low far below traditional high-tension apparatus.
(4) present device can sub computers software systems, and operability is good.
(5) present device running is without recirculated water, and heat loss is little, and energy consumption is very low.
(6) present device adopts heater-type, and by the heat trnasfer of heat coil, the temperature of high-pressure column raises and produces thermal expansion, and therefore produces high pressure.
(7) present device, key fitment is high-pressure column, hard alloy blocks and internal layer cylinder body, is non-moving parts, long service life.In addition can standardization, be easy to change.
Accompanying drawing explanation
Accompanying drawing 1 is structural representation of the present invention;
Accompanying drawing 2 is left and right of the present invention cylinder body open mode schematic diagrames;
Accompanying drawing 3 is A-A section left views of Fig. 1 of the present invention;
Accompanying drawing 4 is A-A section right views of Fig. 1 of the present invention
Accompanying drawing 5 is that alloy cylinder body is from contining function schematic diagram.
Detailed description of the invention
Embodiments of the invention: a kind of heater-type expansion high pressure synthesis equipment, comprise alloy cylinder body 2, it is characterized in that: this alloy cylinder body 2 is divided into left and right cylinder body two parts, in left and right two parts of alloy cylinder body 2, all the heater coil 3 coaxial with it is set, at the outer wall of heater coil 3, thermal insulating warm-keeping layer 4 is set, the two-part cental axial position in the left and right of alloy cylinder body 2 is equipped with high-pressure column 1, high-pressure column 1 and heater coil 3 are separated out by the B of alloy cylinder body 2, sample synthesis room 6 is formed between high-pressure column 1, alloy cylinder body 2 adopts wolfram steel YG20 or MGH4754 alloy to make, high-pressure column 1 adopts fine copper, brass or manganin are made, wherein the outer setting of alloy cylinder body 2 has the hinge 7 for connecting left and right cylinder body, one of them hinge 7 is fixed hinge, another hinge 7 is hinges, the relative termination of high-pressure column 1 arranges carbide alloy 5, carbide alloy 5 adopts tungsten carbide wc to make.
The general principle of the present embodiment is the thermal coefficient of expansion utilizing the thermal coefficient of expansion of high-pressure column 1 to be greater than alloy cylinder body 2 material, under materials synthesis higher temperature, because of the expansion of high-pressure column 1, material is synthesized in process and has higher pressure environment simultaneously.
The diameter of high-pressure column 1 is 10.6mm, and length is divided into 400mm, 600mm and 800mm tri-kinds of models according to the pressure difference of design; Left and right two edge lengths of high-pressure column are different, for accompanying drawing 1, left side high-pressure column is that full-length deducts 5mm, the diameter of carbide alloy 5 is 10.6mm, length is 20mm, alloy cylinder body 2 diameter is 230mm, and total length can be divided into 900mm, 1300mm and 1700mm according to the length of high-pressure column 1, and accompanying drawing 1 is specifically shown in other design of alloy cylinder body.
Particularly, heater coil 3 passes into the electric current of certain power thus produces heat, because thermal insulating warm-keeping layer 4 can stop heat to external diffusion, thus heat is mainly inwardly transmitted.When heat is delivered to high-pressure column 1, because high-pressure column 1 is the alloy material composition that linear expansion coefficient is larger, so during isodose variations in temperature, its expansion and contraction is greater than alloy cylinder body 2, therefore the sample synthesis room 6 to centre extrudes by left and right two parts of high-pressure column 1, thus make sample when synthesizing, there is certain hyperbaric environment.
Alloy cylinder body 2, part between high-pressure column 1 and heater coil 3, in manufacture process, have autofrettage effeet.When device fabrication, adopt under exceeding the condition of serviceability temperature 1.1 times, the bulbs of pressure due to high-pressure column 1 make the region A(of inner wall layer be less than 1/3 place of total wall thickness) there is plastic deformation, and B district is still for elastic deformation is as accompanying drawing 4).After temperature is down to normal temperature, after release reduces to normal pressure, there is residual stress and non-resilient in the A layer of plastic deformation.The B layer of elastic deformation then can restore to the original state.So B layer just creates the effect compressing lock ring inward to A layer.
In order to keep inner high pressure, need good lock ring measure.Adopt hinge 7 to reach contining function, meanwhile, in Fig. 2, lower hinge is fixed hinge, and upper hinge is for opening.
Concrete use procedure
When one, using, upper hinge is opened, then right half part cylinder body is rotated and fall fixed position, ceramic material is shaped to diameter 10mm, and height is the cylinder sample of 5mm.Sample puts into equipment sample synthesis room 6, then pull-up right half part cylinder body, when after upper hinge alignment, connects with locking hoop.Check lock ring situation, temperature-controlling system, after all are normal, by temperature control program setting sample synthesis temperature controlling curve, then run temperature control program, make equipment pass into the electric current of certain power.When high-pressure column reaches higher temperature, produce turgor pressure because of thermal expansion at device interior, sample also reaches synthesis temperature simultaneously.Be incubated after 120 minutes, powered-down, cool about 30 minutes sample temperatures and be reduced to close to room temperature, then open upper hinge, right half part cylinder body is rotated and falls fixed position, take out synthetic material sample.
When two, using, upper hinge is opened, then right half part cylinder body is rotated and fall fixed position, merit thermoelectric material is shaped to diameter 10mm, and height is the cylinder sample of 5mm.Sample puts into equipment sample synthesis room 6, then pull-up right half part cylinder body, when after upper hinge alignment, connects with locking hoop.Check lock ring situation, temperature-controlling system, after all are normal, by temperature control program setting sample synthesis temperature controlling curve, then run temperature control program, make equipment pass into the electric current of certain power.When high-pressure column reaches higher temperature, produce turgor pressure because of thermal expansion at device interior, sample also reaches synthesis temperature simultaneously.Be incubated after 60 minutes, powered-down, cool about 30 minutes sample temperatures and be reduced to close to room temperature, then open upper hinge, right half part cylinder body is rotated and falls fixed position, take out synthetic material sample.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to person skilled in the art can be understood content of the present invention and be implemented; can not as limiting the scope of the invention; all equivalent variations of doing according to Spirit Essence of the present invention or modification, all should be encompassed in protection scope of the present invention.

Claims (3)

1. a heater-type expansion high pressure synthesis equipment, comprise alloy cylinder body (2), it is characterized in that: this alloy cylinder body (2) is divided into left and right cylinder body two parts, in left and right two parts of alloy cylinder body (2), all the heater coil (3) coaxial with it is set, at the outer wall of heater coil (3), thermal insulating warm-keeping layer (4) is set, the two-part cental axial position in left and right of alloy cylinder body (2) is equipped with high-pressure column (1), high-pressure column (1) and heater coil (3) are separated out by the B of alloy cylinder body (2), form sample synthesis room (6) between high-pressure column (1).
2. a kind of heater-type expansion high pressure synthesis equipment according to claim 1, it is characterized in that: the outer setting of described alloy cylinder body (2) has the hinge (7) for connecting left and right cylinder body, one of them hinge (7) is fixed hinge, and another hinge (7) is hinges.
3. a kind of heater-type expansion high pressure synthesis equipment according to claim 1, is characterized in that: on the relative termination of high-pressure column (1), arrange carbide alloy (5).
CN201510635170.1A 2015-09-30 2015-09-30 A kind of heater-type expands high pressure synthesis equipment Active CN105107431B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020240213A1 (en) 2019-05-30 2020-12-03 Gull Corporation Ltd Apparatus and methods for the manufacture of synthetic diamonds
US11623194B2 (en) 2019-05-30 2023-04-11 Gull Corporation Ltd Apparatus for the manufacture of synthetic diamonds using differential expansion

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CN203710985U (en) * 2013-12-24 2014-07-16 中国科学院上海硅酸盐研究所 High-pressure mold
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101819104A (en) * 2010-04-16 2010-09-01 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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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020240213A1 (en) 2019-05-30 2020-12-03 Gull Corporation Ltd Apparatus and methods for the manufacture of synthetic diamonds
GB2587058A (en) * 2019-05-30 2021-03-17 Gull Corp Ltd Apparatus and Methods for the Manufacture of Synthetic Diamonds
US11623194B2 (en) 2019-05-30 2023-04-11 Gull Corporation Ltd Apparatus for the manufacture of synthetic diamonds using differential expansion
GB2587058B (en) * 2019-05-30 2023-08-09 Gull Corp Ltd Apparatus and Methods for the Manufacture of Synthetic Diamonds
JP7431455B2 (en) 2019-05-30 2024-02-15 ガル コーポレーション リミテッド Synthetic diamond manufacturing equipment and manufacturing method

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