CN104697331A - Semiconductor material preparation equipment - Google Patents
Semiconductor material preparation equipment Download PDFInfo
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- CN104697331A CN104697331A CN201310646928.2A CN201310646928A CN104697331A CN 104697331 A CN104697331 A CN 104697331A CN 201310646928 A CN201310646928 A CN 201310646928A CN 104697331 A CN104697331 A CN 104697331A
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Abstract
The invention discloses semiconductor material preparation equipment. The semiconductor material preparation equipment comprises a furnace body having a sealing furnace door, an induction coil, an inductor, an induction light source, an upper pressure head, a lower pressure head, a thermocouple and a hydraulic system, wherein the upper pressure head and the lower pressure head have a displacement sped adjusting function; the inductor is graphite or stainless steel, and has functions of a thermal pressing grinding tool and a crucible; the induction coil is positioned in the center position in a cavity of the furnace body, and two ends thereof penetrate through the furnace body to be connected with the induction light source with adjustable frequency; one end of the thermocouple is connected into the cavity of the furnace body, and is inserted into a temperature measuring hole of the inductor, and the other end is connected into a temperature control meter; and the furnace body is provided with an air charging port, an air discharging port and a vacuum system interface. The semiconductor material preparation equipment is simple in structure and convenient for operation, has multiple functions, can be applied to quick thermal pressing of nanometer powder, high-temperature smelting of semiconductor materials, quick condensation of alloys, preparation of large crystal grain or single crystal samples and vacuum heat treatment, can effectively reduce the preparation cost of the semiconductor materials, and is particularly suitable for the preparation of thermoelectric materials.
Description
Technical field
The present invention relates to semi-conducting material manufacturing technology, particularly the multi-functional semi-conducting material Preparation equipment of one.
Background technology
The Seebeck effect found for 1823 and the peltier effect found for 1834 are that the application of thermoelectric energy converters and thermoelectric cooling provides theoretical foundation.Thermoelectric material is a kind of function semi-conducting material heat energy and electric energy can changed mutually, without moving-member, reliable flexible, environmental protection, is widely used in fields such as national defence, medical treatment, the people's livelihood.Radiosotope thermoelectric generator (RTG) based on thermoelectricity conversion is used as spacecraft power supply by the U.S. and Russia from 20 century 70s, is still reliable the most long-lived dark space generation technology so far.Thermoelectric material also can directly change into the electric power such as low-grade energy (solar energy, automotive residual heat, factory's used heat, hot spring), and the company such as BMW, Ford has developed the environmental protection vehicle utilizing generating power by waste heat of tail gas of automobile all.Converting electric energy is the temperature difference by the refrigeration modes that thermoelectricity also can be used as a kind of environmental protection, and semiconductor water dispenser, semiconductor wine cabinet, automobile thermoelectricity seat are used widely.Thermoelectric material was greatly developed in recent years, and the performance for the thermoelectric material such as Bi-Sb-Te, Mg-Si-Sn, PbTe, skutterudite, SiGe, AgPbTe-GeTe of different warm area all makes a breakthrough.The conversion efficiency of thermo-electric device also rises to about 12%, close to polysilicon solar cell and thin-film solar cells.
But at present performance higher, the block thermoelectric material preparation that is applicable to generate electricity uses the equipment such as discharge plasma sintering furnace, vacuum sintering funace, monocrystal growing furnace, rapid solidification stove, vacuum melting furnace mostly.Discharge plasma agglomerating plant cost intensive, and traditional vacuum hotpressing stove, monocrystal growing furnace, rapid solidification stove, vacuum melting furnace only have simple function, are of limited application.The complicated preparation technology of existing high performance thermoelectric material and the high request to equipment, add extra cost for research work and enterprise produce, and this is also that the current world, the domestic research and development to pyroelectric technology and industry drop into one of reason that can not show a candle to photovoltaic technology.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of semi-conducting material Preparation equipment; structure is simple, easy to operate; there is the several functions such as quick hot pressing, high temperature sintering, rapid solidification, crystal growth; the shortcomings such as existing thermoelectric material Preparation equipment function singleness, cost intensive can be solved; effectively can not only promote that the scale of thermoelectric material is produced in batches, also can be widely used in the preparation of other semi-conductor thermoelectric material, metal material.。
For solving the problems of the technologies described above, semi-conducting material Preparation equipment provided by the invention, it comprises body of heater, induction coil, inductor, seaming chuck, push-down head, the thermocouple with sealing door;
Described seaming chuck, is positioned at the top of body of heater;
Described push-down head, is positioned at the bottom of body of heater;
Described induction coil is helical form, is positioned at the center of the cavity of body of heater, and two ends pass described body of heater, is connected with the heating head of induction power supply;
Seaming chuck, push-down head and induction coil are coaxial, and cross section is circular;
The cross-sectional area of induction coil is greater than the cross-sectional area of seaming chuck and push-down head;
Described inductor, for being placed between described induction coil, push-down head, seaming chuck;
Described thermocouple, one end is linked in the cavity of described body of heater;
Described body of heater, is provided with inflation inlet, gas vent, vacuum system interface;
Described inflation inlet, for inflation or liquid nitrogen in the cavity to described body of heater;
Described gas vent, for discharging the gas in the cavity of described body of heater;
Described vacuum system interface, for external pumped vacuum systems.
Preferably, described induction power supply, supply frequency is 1000-400000Hz;
Described inductor, material is graphite or stainless steel;
Described thermocouple, inserts the thermometer hole of described inductor in the cavity that one end is linked into described body of heater.
Preferably, semi-conducting material Preparation equipment, also comprises hydraulic system;
Described hydraulic system, for controlling displacement and the speed of seaming chuck and push-down head;
Described hydraulic system, comprises hydraulic pump, displacement transducer and pressure sensor;
Described hydraulic pump, for driving seaming chuck, push-down head;
Institute's displacement sensors, for detecting the displacement of seaming chuck, push-down head;
Described pressure sensor, for detecting the pressure of seaming chuck, push-down head.
Preferably, described body of heater, for bilayer or individual layer are around pipe water-cooled body of heater, body of heater and fire door is provided with cooling water connector.
Preferably, described seaming chuck, push-down head by flangeseal in body of heater top and bottom;
In described induction coil, the thermocouple cavity by flangeseal access body of heater.
Preferably, described fire door, is provided with visual window.
Preferably, described pumped vacuum systems, comprises high-vacuum pump, black vacuum pump, valve and vacuum meter.
Preferably, described high-vacuum pump is molecular pump, diffusion pump, ionic pump, cryogenic pump or lobe pump;
Described black vacuum pump is rotary vane mechanical pump, direct connection mechanical pump, water ring pump or without the dry pump of oil.
Semi-conducting material Preparation equipment of the present invention, structure is simple, easy to operate, there is several functions, nanocrystalline, polycrystalline, single-crystal semiconductor material can be prepared by methods such as vacuum/atmosphere Bidirectional hot press, vacuum/atmosphere Fast Sintering, rapid solidification, unidirectional sintering at a slow speed, also can be used for vacuum/atmosphere heat treatment, be particularly suitable for manufacturing semi-conductor thermoelectric material, effectively can reduce the preparation cost of semi-conductor thermoelectric material.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, below the accompanying drawing that will use required for the present invention is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the longitudinal sectional drawing of semi-conducting material Preparation equipment one embodiment of the present invention;
Fig. 2 is the top view of semi-conducting material Preparation equipment one embodiment of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, carry out clear, complete description to the technical scheme in the present invention, obviously, described embodiment is a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, other embodiments all that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belong to the scope of protection of the invention.
Embodiment one
Semi-conducting material Preparation equipment, as shown in Figure 1 and Figure 2, comprises body of heater 1, induction coil 11, inductor 12, seaming chuck 8, push-down head 4, the thermocouple 6 with sealing door 18;
Described seaming chuck 8, is positioned at the top of body of heater 1;
Described push-down head 4, is positioned at the bottom of body of heater 1;
Described induction coil 11 is helical form, is positioned at the center of the cavity of body of heater 1, and two ends pass described body of heater 1, are connected with the heating head of induction power supply 16;
Described induction power supply 16, has frequency-adjustable function, frequency range 1000-400000Hz;
Seaming chuck 8, push-down head 4 and induction coil 11 are coaxial, and cross section is circular;
The cross-sectional area of induction coil 11 is greater than the cross-sectional area of seaming chuck 8 and push-down head 4;
Described inductor 12, for being placed between described induction coil 11, push-down head 4, seaming chuck 8;
Described thermocouple 6, one end is linked into the cavity of described body of heater 1, for detecting heating-up temperature;
Described body of heater 1, is provided with inflation inlet 2, gas vent 7, vacuum system interface 5;
Described inflation inlet 2, for external inertia gas cylinder or liquid nitrogen, inflates or is filled with liquid nitrogen in the cavity of described body of heater 1;
Described gas vent 7, for discharging the gas in the cavity of described body of heater 1;
Described vacuum system interface 5, for external pumped vacuum systems.
Preferably, semi-conducting material Preparation equipment also comprises hydraulic system, described hydraulic system, for controlling displacement and the speed of seaming chuck and push-down head; Described hydraulic system comprises hydraulic pump, displacement transducer and pressure sensor; Described hydraulic pump is for driving seaming chuck 8, push-down head 4, and institute's displacement sensors is for detecting the displacement of seaming chuck 8, push-down head 4, and described pressure sensor is for detecting the pressure of seaming chuck 8, push-down head 4.
Preferably, described body of heater 1 be Double water-cooled or individual layer around pipe furnace body, body of heater and fire door are provided with cooling water connector 3.
Preferably, described seaming chuck 8, push-down head 4 are sealed in body of heater 1 top and bottom by ring flange 9; In described induction coil 11, thermocouple 6 cavity by flangeseal access body of heater 1.
Described inductor, material is graphite or stainless steel;
Described thermocouple, described thermocouple, one end to be linked in the cavity of described body of heater by insulating flange and to insert the thermometer hole of inductor, and the part cover that thermocouple is positioned at cavity has insulating ceramics pipe;
According to the difference of power used (1-30kW) and induction coil size, induction power supply adopts the radio frequency induction power supply of 1000-400000Hz, graphite susceptor surface and internal temperature can be made within a few second, a few minutes to rise to 1000-2000 degree Celsius, realize the Fast Heating to sample.
Preferably, described fire door 18 is provided with visual window 17.
Preferably, described pumped vacuum systems, comprises high-vacuum pump (one namely in molecular pump, diffusion pump, ionic pump, cryogenic pump, lobe pump), black vacuum pump (rotary vane mechanical pump, direct connection mechanical pump, water ring pump, without the one in oily dry pump), valve and vacuum meter.
The semi-conducting material Preparation equipment of embodiment one, induction power supply, hydraulic system, thermocouple, temperature control instrument, vacuum instrumentation dispatch control system are integrated in electrical control cubicles 15 by human-computer dialogue function software, to the endoceliac heat temperature raising of stove, pressure shows and Real-Time Monitoring and control are carried out in the control of vacuum valve, and induction power supply utilizes thermocouple 6 and temperature control instrument to control the output of power supply thus the sample temperature in accurate control sensor 12.Equipment is furnished with pumped vacuum systems and multiple gas interface, and the parts such as induction coil 11, seaming chuck 8, push-down head 4, thermocouple 6 and containment portion connecting portion adopt " O " type flat seal and axial flange dish to seal, and in body of heater cavity, vacuum can be low to moderate 10
-5pa, also can be filled with several atmospheric inert gas, can realize the hot pressing under the different conditions such as high vacuum, high pressure inert atmosphere, mobility atmosphere or sintering.The semi-conducting material Preparation equipment of embodiment one, utilizes the inductor such as graphite or stainless steel, coordinates pumped vacuum systems and inert gas interface can realize the melting sintering of semi-conducting material; The semi-conducting material Preparation equipment of embodiment one, primer fluid pressing system, takes Bidirectional-pressure pattern and high pressure resistant conductor inductor (such as graphite, stainless steel, the highest can withstand voltage 100MPa), can prepare the bulk nanometer semi-conducting material that density is greater than 95%; Also can stop heating when melt is in high temperature, inductor is down to stove inner bottom part, then simultaneously spray inert gas from gas interface 2 to inductor (having the function of grinding tool/crucible concurrently) or liquid nitrogen realizes rapid solidification; In addition, the semi-conducting material Preparation equipment of embodiment one can also realize monocrystalline/large grain size growth, between inductor and coil, add heat-insulation layer, by induction power supply fused raw material, controlled the velocity of displacement (adjustable within the scope of 0.01-150mm/s) of push-down head by displacement transducer.
The semi-conducting material Preparation equipment of embodiment one, structure is simple, easy to operate, there is several functions, nanocrystalline, polycrystalline, single-crystal semiconductor material can be prepared by methods such as vacuum/atmosphere Bidirectional hot press, vacuum/atmosphere Fast Sintering, rapid solidification, unidirectional sintering at a slow speed, also can be used for vacuum/atmosphere heat treatment, be particularly suitable for manufacturing semi-conductor thermoelectric material, effectively can reduce the preparation cost of semi-conductor thermoelectric material.
Embodiment two
Based on the semi-conducting material Preparation equipment of embodiment one, prepare process that is nanocrystalline, crystallite bulk semiconductor material as follows:
Open fire door 18, by the center of nanometer being housed, the graphite susceptor 12 of micron powder sample 14 is put into push-down head 4, primer fluid pressing system, push-down head 4 is raised to suitable position, seaming chuck 8 is down to suitable position simultaneously, thermocouple 6 is inserted in the thermometer hole of graphite susceptor 12, closes fire door 18, start vacuum system by induction power supply heat temperature raising.Until after vacuum meets the requirements, characteristic per sample, can select keep vacuum or be filled with inert gas in body of heater cavity.Carry out heat temperature raising by induction power supply to sample, after reaching required temperature, primer fluid pressing system, carries out two-way or uniaxial hot pressing to sample 14.Nanocrystalline, crystallite bulk semiconductor material that density reaches 99% can be obtained.
Embodiment three
Based on the semi-conducting material Preparation equipment of embodiment one, the sintering fusion process of semi-conducting material is as follows:
Open fire door 18, the graphite susceptor 12 that raw material sample 14 is housed is put into the center of push-down head 4, primer fluid pressing system, push-down head 4 is raised to the centre position in coil 11, thermocouple 6 is inserted in the thermometer hole of graphite susceptor 12, close fire door 18.Until after vacuum meets the requirements, can select keep vacuum or be filled with inert gas in body of heater cavity.After reaching required atmosphere, by induction power supply, heat-agglomerating is implemented to sample.The sintering melting of semi-conducting material within the scope of room temperature-2000 DEG C can be realized.
Embodiment four
Based on the semi-conducting material Preparation equipment of embodiment one, prepare the large grain size even process of single-crystal semiconductor material as follows:
Open fire door 18, the graphite susceptor 12 that sample 14 is housed is put into the center of push-down head 4, aluminium oxide insulation quilt is added between inductor 12 and coil, primer fluid pressing system, push-down head 4 is raised to the centre position in coil 11, thermocouple 6 is inserted in the thermometer hole of graphite susceptor 12, closes fire door 18.Until after vacuum meets the requirements, can select keep vacuum or be filled with inert gas in body of heater cavity.After reaching required atmosphere, by induction power supply, heat temperature raising is implemented to sample.Rise to temperature required and be incubated, ((adjustable within the scope of 0.01-150mm/s) can obtain large grain size even monocrystal material to control the decrease speed of push-down head 4 by displacement transducer.
Embodiment five
Based on the semi-conducting material Preparation equipment of embodiment one, the rapid solidification preparation process of semi-conducting material is as follows:
Open fire door 18, the graphite susceptor 12 that sample 14 is housed is put into the center of push-down head 4, primer fluid pressing system, push-down head 4 is raised to the centre position in coil 11, thermocouple 6 is inserted in the thermometer hole of graphite susceptor 12, close fire door 18.Until after vacuum meets the requirements, can select keep vacuum or be filled with inert gas in body of heater cavity.After reaching required atmosphere, by induction power supply, heat-agglomerating is implemented to sample.Rise to temperature required after, powered-down, controls push-down head 4 by displacement transducer simultaneously and fast inductor 12 decline is caused stove inner bottom part, then spray into liquid nitrogen or inert gas by the interface 2,5 of both sides to inductor, then start vacuum system and extract gas, realize rapid solidification.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within the scope of protection of the invention.
Claims (8)
1. a semi-conducting material Preparation equipment, is characterized in that, comprises body of heater, induction coil, inductor, seaming chuck, push-down head, the thermocouple with sealing door;
Described seaming chuck, is positioned at the top of body of heater;
Described push-down head, is positioned at the bottom of body of heater;
Described induction coil is helical form, is positioned at the center of the cavity of body of heater, and two ends pass described body of heater, is connected with the heating head of the induction power supply of frequency-adjustable;
Seaming chuck, push-down head and induction coil are coaxial, and cross section is circular;
The cross-sectional area of induction coil is greater than the cross-sectional area of seaming chuck and push-down head;
Described inductor, for being placed between described induction coil, push-down head, seaming chuck;
Described thermocouple, one end is linked in the cavity of described body of heater;
Described body of heater, is provided with inflation inlet, gas vent, vacuum system interface;
Described inflation inlet, for inflation or liquid nitrogen in the cavity to described body of heater;
Described gas vent, for discharging the gas in the cavity of described body of heater;
Described vacuum system interface, for external pumped vacuum systems.
2. semi-conducting material Preparation equipment according to claim 1, is characterized in that,
Described induction power supply, supply frequency is 1000-400000Hz;
Described inductor, material is graphite or stainless steel;
Described thermocouple, inserts the thermometer hole of described inductor in the cavity that one end is linked into described body of heater.
3. semi-conducting material Preparation equipment according to claim 1, is characterized in that,
Semi-conducting material Preparation equipment, also comprises hydraulic system;
Described hydraulic system, for controlling displacement and the speed of seaming chuck and push-down head;
Described hydraulic system, comprises hydraulic pump, displacement transducer and pressure sensor;
Described hydraulic pump, for driving seaming chuck, push-down head;
Institute's displacement sensors, for detecting the displacement of seaming chuck, push-down head;
Described pressure sensor, for detecting the pressure of seaming chuck, push-down head.
4. semi-conducting material Preparation equipment according to claim 2, is characterized in that,
Described body of heater, for bilayer or individual layer are around pipe water-cooled body of heater, body of heater and fire door is provided with cooling water connector.
5. semi-conducting material Preparation equipment according to claim 2, is characterized in that,
Described seaming chuck, push-down head by flangeseal in body of heater top and bottom;
In described induction coil, the thermocouple cavity by flangeseal access body of heater.
6. semi-conducting material Preparation equipment according to claim 2, is characterized in that,
Described fire door, is provided with visual window.
7. semi-conducting material Preparation equipment according to claim 2, is characterized in that,
Described pumped vacuum systems, comprises high-vacuum pump, black vacuum pump, valve and vacuum meter.
8. semi-conducting material Preparation equipment according to claim 6, is characterized in that,
Described high-vacuum pump is molecular pump, diffusion pump, ionic pump, cryogenic pump or lobe pump;
Described black vacuum pump is rotary vane mechanical pump, direct connection mechanical pump, water ring pump or without the dry pump of oil.
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| CN201310646928.2A CN104697331B (en) | 2013-12-04 | 2013-12-04 | Semiconductor material Preparation equipment |
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| CN201310646928.2A CN104697331B (en) | 2013-12-04 | 2013-12-04 | Semiconductor material Preparation equipment |
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| CN105682270A (en) * | 2016-01-27 | 2016-06-15 | 福州大学 | High-frequency electromagnetic induction hot-pressing sintering and brazing device |
| CN105783501A (en) * | 2016-03-16 | 2016-07-20 | 中国科学院宁波材料技术与工程研究所 | Vacuum hot-pressing sintering furnace |
| CN108645212A (en) * | 2018-07-17 | 2018-10-12 | 浙江晨华科技有限公司 | Small size vacuum smelting furnace |
| CN109346596A (en) * | 2018-09-11 | 2019-02-15 | 中国科学院上海硅酸盐研究所 | A kind of preparation facilities of annular thermo-electric device and its method for preparing annular thermo-electric device |
| CN109373761A (en) * | 2018-11-27 | 2019-02-22 | 成都易飞得材料科技有限公司 | A kind of multi- scenarios method material handling system |
| CN109623106A (en) * | 2018-12-26 | 2019-04-16 | 常州市乐萌压力容器有限公司 | The welding procedure of semiconductor monocrystal furnace cavity |
| CN109765088A (en) * | 2019-01-23 | 2019-05-17 | 李明霞 | A kind of semiconductor material Preparation equipment |
| CN110094974A (en) * | 2018-01-31 | 2019-08-06 | 中国科学院金属研究所 | A kind of modular combination material high throughput hot pressing sintering equipment and its application method |
| CN110116206A (en) * | 2019-04-22 | 2019-08-13 | 武汉科技大学 | A kind of dedicated AC power frequency discharge sintering equipment of thermoelectric material and sintering method |
| CN111036915A (en) * | 2019-12-26 | 2020-04-21 | 河海大学常州校区 | Pressure nano-particle sintering device |
| WO2021208363A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Device for preparing large-size single crystal |
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| CN105682270B (en) * | 2016-01-27 | 2019-07-09 | 福州大学 | A kind of high-frequency electromagnetic induction hot pressed sintering and brazing device |
| CN105682270A (en) * | 2016-01-27 | 2016-06-15 | 福州大学 | High-frequency electromagnetic induction hot-pressing sintering and brazing device |
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| CN108645212A (en) * | 2018-07-17 | 2018-10-12 | 浙江晨华科技有限公司 | Small size vacuum smelting furnace |
| CN109346596A (en) * | 2018-09-11 | 2019-02-15 | 中国科学院上海硅酸盐研究所 | A kind of preparation facilities of annular thermo-electric device and its method for preparing annular thermo-electric device |
| CN109346596B (en) * | 2018-09-11 | 2020-06-12 | 中国科学院上海硅酸盐研究所 | Preparation device and method for annular thermoelectric device |
| CN109373761A (en) * | 2018-11-27 | 2019-02-22 | 成都易飞得材料科技有限公司 | A kind of multi- scenarios method material handling system |
| CN109373761B (en) * | 2018-11-27 | 2023-12-15 | 成都易飞得材料科技有限公司 | Multi-field coupling material processing system |
| CN109623106A (en) * | 2018-12-26 | 2019-04-16 | 常州市乐萌压力容器有限公司 | The welding procedure of semiconductor monocrystal furnace cavity |
| CN109623106B (en) * | 2018-12-26 | 2020-10-20 | 常州市乐萌压力容器有限公司 | Welding process of semiconductor single crystal furnace cavity |
| CN109765088A (en) * | 2019-01-23 | 2019-05-17 | 李明霞 | A kind of semiconductor material Preparation equipment |
| CN109765088B (en) * | 2019-01-23 | 2021-05-25 | 托特半导体(山东)有限公司 | Semiconductor material preparation equipment |
| CN110116206A (en) * | 2019-04-22 | 2019-08-13 | 武汉科技大学 | A kind of dedicated AC power frequency discharge sintering equipment of thermoelectric material and sintering method |
| CN111036915A (en) * | 2019-12-26 | 2020-04-21 | 河海大学常州校区 | Pressure nano-particle sintering device |
| WO2021208363A1 (en) * | 2020-04-17 | 2021-10-21 | 中国电子科技南湖研究院 | Device for preparing large-size single crystal |
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