CN104697331B - Semiconductor material Preparation equipment - Google Patents
Semiconductor material Preparation equipment Download PDFInfo
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- CN104697331B CN104697331B CN201310646928.2A CN201310646928A CN104697331B CN 104697331 B CN104697331 B CN 104697331B CN 201310646928 A CN201310646928 A CN 201310646928A CN 104697331 B CN104697331 B CN 104697331B
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 49
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- 238000004826 seaming Methods 0.000 claims abstract description 34
- 238000006073 displacement reaction Methods 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
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- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
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- 238000007789 sealing Methods 0.000 claims abstract description 4
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of semiconductor material Preparation equipments.It includes furnace body, induction coil, inductor, induction power supply, seaming chuck, push-down head, thermocouple, hydraulic system with sealing fire door；Seaming chuck, push-down head have velocity of displacement adjustable function；Inductor is graphite or stainless steel, has the function of hot pressing grinding tool and crucible；Induction coil is located at the intracavitary center of furnace body, and both ends are pierced by furnace body and are connected with the adjustable induction power supply of frequency；Thermocouple one end access furnace body is intracavitary and is inserted into the thermometer hole of inductor, and the other end accesses temperature control instrument；Furnace body is provided with inflating port, gas vent, vacuum system interface.The configuration of the present invention is simple; it is easy to operate; with multiple functions; it can be used for the quick solidification of the quick hot pressing of nanometer powder, the high melt of semiconductor material, alloy; the preparation of big crystal grain or single crystal samples; it can also be used in vacuum heat treatment, can be effectively reduced the preparation cost of semiconductor material, be especially suitable for the preparation of thermoelectric material.
Description
Technical field
The present invention relates to semiconductor material manufacturing technology, in particular to a kind of multi-functional semiconductor material Preparation equipment.
Background technique
The Seebeck effect of discovery in 1823 and the peltier effect of discovery in 1834 are thermoelectric energy converters and thermoelectricity
The application of refrigeration provides theoretical foundation.Thermoelectric material be it is a kind of can be by function semiconductor material that thermal energy and electric energy are mutually converted
Material, it is no moving parts, reliable flexible, environmentally protective, it is widely used in fields such as national defence, medical treatment, the people's livelihood.Based on heat to electricity conversion
Radiosotope thermoelectric generator (RTG) from the 1970s by the U.S. and Russia be used as spacecraft power supply, be so far still most
Reliable most long-lived deep space generation technology.Thermoelectric material can also by low-grade energy (solar energy, automotive residual heat, factory's waste heat,
Hot spring) etc. be directly translated into electric power, the companies such as BMW, Ford are developed out the environment-friendly vehicle using generating power by waste heat of tail gas of automobile
Type.The refrigeration modes that thermoelectricity also can be used as a kind of environmental protection convert electrical energy into the temperature difference, semiconductor water dispenser, semiconductor wine cabinet, vapour
Vehicle thermoelectricity seat is widely used.Thermoelectric material was greatly developed in recent years, for different warm areas Bi-Sb-Te,
The performance of the thermoelectric materials such as Mg-Si-Sn, PbTe, skutterudite, SiGe, AgPbTe-GeTe all makes a breakthrough.Thermoelectricity device
The transfer efficiency of part also rises to 12% or so, close to polysilicon solar cell and thin-film solar cells.
But current performance is higher, uses discharge plasma sintering mostly suitable for the block thermoelectric material preparation of power generation
The equipment such as furnace, vacuum sintering funace, monocrystal growing furnace, quick consolidation furnace, vacuum melting furnace.Discharge plasma agglomerating plant
It is expensive, and traditional vacuum hotpressing stove, monocrystal growing furnace, quick consolidation furnace, vacuum melting furnace only have simple function, answer
With being limited in scope.The complicated preparation process of existing high performance thermoelectric material and high request to equipment are research work and enterprise
Production increases extra cost, this is also that current international, domestic put into the research and development of pyroelectric technology and industry can not show a candle to photovoltaic skill
One of the reason of art.
Summary of the invention
The technical problem to be solved by the present invention is provide a kind of semiconductor material Preparation equipment, structure is simple, operation side
Just, there is quick hot pressing, high temperature sintering, the quickly multiple functions such as solidification, crystal growth, be able to solve existing thermoelectric material preparation
The disadvantages of functions of the equipments are single, expensive can not only effectively facilitate the large-scale production of thermoelectric material, can also use extensively
In the preparation of other semi-conductor thermoelectric materials, metal material.
In order to solve the above technical problems, semiconductor material Preparation equipment provided by the invention comprising have sealing fire door
Furnace body, induction coil, inductor, seaming chuck, push-down head, thermocouple；
The seaming chuck, positioned at the top of furnace body；
The push-down head, positioned at the bottom of furnace body；
The induction coil is helical form, and positioned at the center of the cavity of furnace body, both ends are pierced by the furnace body, with sense
The heating head of power supply is answered to be connected；
Seaming chuck, push-down head and induction coil are coaxial, and cross section is circle；
The cross-sectional area of induction coil is greater than the cross-sectional area of seaming chuck and push-down head；
The inductor, for being placed on the induction coil, push-down head, between seaming chuck；
The thermocouple, one end are linked into the cavity of the furnace body；
The furnace body is provided with inflating port, gas vent, vacuum system interface；
The inflating port, for inflation or liquid nitrogen into the cavity of the furnace body；
The gas vent, for the intracorporal gas of the chamber of the furnace body to be discharged；
The vacuum system interface is used for external pumped vacuum systems.
Preferably, the induction power supply, supply frequency 1000-400000Hz；
The inductor, material are graphite or stainless steel；
The thermocouple, one end are linked into the cavity of the furnace body and are inserted into the thermometer hole of the inductor.
Preferably, semiconductor material Preparation equipment, further includes hydraulic system；
The hydraulic system, for controlling the displacement and speed of seaming chuck and push-down head；
The hydraulic system, including hydraulic pump, displacement sensor and pressure sensor；
The hydraulic pump, for driving seaming chuck, push-down head；
Institute's displacement sensors, for detecting the displacement of seaming chuck, push-down head；
The pressure sensor, for detecting the pressure of seaming chuck, push-down head.
Preferably, the furnace body, is provided with cooling water on pipe water cooling furnace body, furnace body and fire door and connects for double-deck or single layer
Mouthful.
Preferably, the seaming chuck, push-down head are by flangeseal at the top and bottom of furnace body；
The induction coil, thermocouple are accessed by flangeseal in the cavity of furnace body.
Preferably, the fire door, is provided with visual window.
Preferably, the pumped vacuum systems, including high-vacuum pump, rough vacuum pump, valve and vacuum meter.
Preferably, the high-vacuum pump, is molecular pump, diffusion pump, ionic pump, cryogenic pump or lobe pump；
The rough vacuum pump is rotary vane mechanical pump, direct connection mechanical pump, water ring pump or oil-free dry pump.
Semiconductor material Preparation equipment of the invention, structure are simple and convenient to operate, and have multiple functions, can be by true
Sky/atmosphere Bidirectional hot press, vacuum/atmosphere Fast Sintering, quickly solidification, unidirectional the methods of sintering at a slow speed prepare nanocrystalline, polycrystalline,
Single-crystal semiconductor material, it may also be used for vacuum/atmosphere heat treatment is particularly suitable for manufacture semi-conductor thermoelectric material, can effectively drop
The preparation cost of low semi-conductor thermoelectric material.
Detailed description of the invention
In order to illustrate more clearly of technical solution of the present invention, the required attached drawing of the present invention is made below simple
It introduces, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ordinary skill people
For member, without creative efforts, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is the longitudinal sectional drawing of one embodiment of semiconductor material Preparation equipment of the invention；
Fig. 2 is the top view of one embodiment of semiconductor material Preparation equipment of the invention.
Specific embodiment
Below in conjunction with attached drawing, clear, complete description is carried out to the technical solution in the present invention, it is clear that described
Embodiment is a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
Embodiment one
Semiconductor material Preparation equipment, as shown in Figure 1 and Figure 2, including having furnace body 1, the induction coil of sealing fire door 18
11, inductor 12, seaming chuck 8, push-down head 4, thermocouple 6；
The seaming chuck 8, positioned at the top of furnace body 1；
The push-down head 4, positioned at the bottom of furnace body 1；
The induction coil 11 is helical form, and positioned at the center of the cavity of furnace body 1, both ends are pierced by the furnace body 1,
It is connected with the heating head of induction power supply 16；
The 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 circle；
The cross-sectional area of induction coil 11 is greater than the cross-sectional area of seaming chuck 8 and push-down head 4；
The inductor 12, for being placed on the induction coil 11, push-down head 4, between seaming chuck 8；
The thermocouple 6, one end is linked into the cavity of the furnace body 1, for detecting heating temperature；
The furnace body 1 is provided with inflating port 2, gas vent 7, vacuum system interface 5；
The inflating port 2 is used for external inertia gas cylinder or liquid nitrogen, inflates or be filled with liquid nitrogen in the cavity of Xiang Suoshu furnace body 1；
The gas vent 7, for the intracorporal gas of the chamber of the furnace body 1 to be discharged；
The vacuum system interface 5 is used for external pumped vacuum systems.
Preferably, semiconductor material Preparation equipment further includes hydraulic system, the hydraulic system, for control seaming chuck and
The displacement and speed of push-down head；The hydraulic system includes hydraulic pump, displacement sensor and pressure sensor；The hydraulic pump
For driving seaming chuck 8, push-down head 4, institute's displacement sensors are used to detect the displacement of seaming chuck 8, push-down head 4, the pressure
Sensor is used to detect the pressure of seaming chuck 8, push-down head 4.
Preferably, the furnace body 1 is that Double water-cooled or single layer are provided with cooling water connector on pipe furnace body, furnace body and fire door
3。
Preferably, the seaming chuck 8, push-down head 4 are sealed in 1 top and bottom of furnace body by ring flange 9；The line of induction
Circle 11, thermocouple 6 are accessed by flangeseal in the cavity of furnace body 1.
The inductor, material are graphite or stainless steel；
The thermocouple, the thermocouple, one end are linked into the cavity of the furnace body by insulating flange and are inserted into sense
The thermometer hole of device is answered, thermocouple part within the cavity is cased with ceramics pipe outer；
According to the difference of power used (1-30kW) and induction coil size, induction power supply uses 1000-
The radio frequency induction power supply of 400000Hz can be such that graphite susceptor surface and internal temperature rises within several seconds, a few minutes
1000-2000 degrees Celsius, realize the quick heating to sample.
Preferably, the fire door 18 is provided with visual window 17.
Preferably, the pumped vacuum systems, including high-vacuum pump (i.e. molecular pump, diffusion pump, ionic pump, cryogenic pump, Roots
Pump one of), rough vacuum pump (one of rotary vane mechanical pump, direct connection mechanical pump, water ring pump, oil-free dry pump), valve and
Vacuum meter.
The semiconductor material Preparation equipment of embodiment one, induction power supply, hydraulic system, thermocouple, temperature control instrument, vacuscope
Table dispatch control system is integrated in power control cabinet 15 by human-computer dialogue operating software, shows to the endoceliac heat temperature raising of furnace, pressure
And the control of vacuum valve carries out real-time monitoring and control, induction power supply control power supply using thermocouple 6 and temperature control instrument
Output to the sample temperature in accurate control sensor 12.Equipment is furnished with pumped vacuum systems and multiple gas interfaces, induction
The components such as coil 11, seaming chuck 8, push-down head 4, thermocouple 6 and containment portion connecting portion use " O " type flat seal and axial direction
Flangeseal, vacuum degree can be down to 10 in furnace body cavity-5Pa can also be filled with the inert gas of several atmospheric pressure, can be realized
Hot pressing or sintering under the different conditions such as high vacuum, high pressure inert atmosphere, mobility atmosphere.The semiconductor material system of embodiment one
Standby equipment cooperates pumped vacuum systems and inert gas interface that semiconductor material may be implemented using inductors such as graphite or stainless steels
The melting of material is sintered；The semiconductor material Preparation equipment of embodiment one starts hydraulic system, takes Bidirectional-pressure mode and Nai Gao
Press conductor inductor (such as graphite, stainless steel, highest can pressure resistance 100MPa), can prepare consistency be greater than 95% it is nanocrystalline
Bulk semiconductor material；Can also stop when melt is in high temperature heating, inductor is down to bottom in furnace, then simultaneously from
Gas interface 2 sprays inert gas to inductor (having both grinding tool/crucible function) or liquid nitrogen realizes quickly solidification；In addition, real
The semiconductor material Preparation equipment for applying example one can also realize monocrystalline/big crystal grain growth, be added and protect between inductor and coil
Warm layer controls velocity of displacement (the 0.01-150mm/s range of push-down head by displacement sensor by induction power supply fused raw material
It is interior adjustable).
The semiconductor material Preparation equipment of embodiment one, structure are simple and convenient to operate, and are had multiple functions, can be passed through
Vacuum/atmosphere Bidirectional hot press, vacuum/atmosphere Fast Sintering, quickly solidification, unidirectional the methods of sintering at a slow speed prepare nanocrystalline, more
Brilliant, single-crystal semiconductor material, it may also be used for vacuum/atmosphere heat treatment is particularly suitable for manufacture semi-conductor thermoelectric material, can be effective
Reduce the preparation cost of semi-conductor thermoelectric material.
Embodiment two
Semiconductor material Preparation equipment based on embodiment one prepares the process of nanocrystalline crystallite bulk semiconductor material
It is as follows:
Fire door 18 is opened, the centre bit of push-down head 4 will be put into equipped with nanometer, the graphite susceptor 12 of micron powder sample 14
It sets, starts hydraulic system, push-down head 4 is raised to suitable position, while seaming chuck 8 is down to suitable position, by thermocouple 6
It is inserted into the thermometer hole of graphite susceptor 12, closes fire door 18, vacuum system is started by induction power supply heat temperature raising.Until true
After reciprocal of duty cycle meets the requirements, according to the characteristic of sample, it can choose and keep vacuum or be filled with inert gas into furnace body cavity.It is logical
It crosses induction power supply and heat temperature raising is carried out to sample, after reaching required temperature, start hydraulic system, sample 14 is carried out two-way
Or uniaxial hot pressing.Consistency be can get up to 99% nanocrystalline, crystallite bulk semiconductor material.
Embodiment three
The sintering fusion process of semiconductor material Preparation equipment based on embodiment one, semiconductor material is as follows:
Fire door 18 is opened, the graphite susceptor 12 equipped with raw material sample 14 is put into the center of push-down head 4, starting
Push-down head 4 is raised to the middle position in coil 11, thermocouple 6 is inserted into the thermometer hole of graphite susceptor 12 by hydraulic system,
Close fire door 18.After vacuum degree meets the requirements, it can choose and keep vacuum or be filled with inert gas into furnace body cavity.
After reaching required atmosphere, heat-agglomerating is implemented to sample by induction power supply.Semiconductor within the scope of -2000 DEG C of room temperature can be achieved
The sintering melting of material.
Example IV
Semiconductor material Preparation equipment based on embodiment one, preparation the big crystal grain even process of single-crystal semiconductor material are such as
Under:
Fire door 18 is opened, the graphite susceptor 12 equipped with sample 14 is put into the center of push-down head 4, in inductor 12
Aluminium oxide insulation quilt is added between coil, starts hydraulic system, push-down head 4 is raised to the middle position in coil 11, it will be hot
Galvanic couple 6 is inserted into the thermometer hole of graphite susceptor 12, closes fire door 18.After vacuum degree meets the requirements, holding can choose
Vacuum is filled with inert gas into furnace body cavity.After reaching required atmosphere, sample is implemented to heat by induction power supply
Heating.It rises to required temperature and keeps the temperature, decrease speed ((the 0.01-150mm/s range of push-down head 4 is controlled by displacement sensor
It is interior adjustable), big crystal grain even monocrystal material can be obtained.
Embodiment five
The quick solidification preparation process of semiconductor material Preparation equipment based on embodiment one, semiconductor material is as follows:
Fire door 18 is opened, the graphite susceptor 12 equipped with sample 14 is put into the center of push-down head 4, starts hydraulic pressure system
System, is raised to the middle position in coil 11 for push-down head 4, thermocouple 6 is inserted into the thermometer hole of graphite susceptor 12, closes furnace
Door 18.After vacuum degree meets the requirements, it can choose and keep vacuum or be filled with inert gas into furnace body cavity.When reaching
After required atmosphere, heat-agglomerating is implemented to sample by induction power supply.After rising to required temperature, power supply is closed, while passing through position
Displacement sensor, which controls push-down head 4 and quickly declines inductor 12, causes bottom in furnace, then by the interfaces 2,5 of two sides to inductor
Liquid nitrogen or inert gas are sprayed into, then starts vacuum system and extracts gas, realizes quickly solidification.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent substitution, improvement and etc. done be should be included within the scope of the present invention.
Claims (6)
1. a kind of semiconductor material Preparation equipment, which is characterized in that including having furnace body, the induction coil, induction of sealing fire door
Device, seaming chuck, push-down head, thermocouple；
The seaming chuck, positioned at the top of furnace body；
The push-down head, positioned at the bottom of furnace body；
The induction coil is helical form, and positioned at the center of the cavity of furnace body, both ends are pierced by the furnace body, can with frequency
The heating head of the induction power supply of tune is connected；
Seaming chuck, push-down head and induction coil are coaxial, and cross section is circle；
The cross-sectional area of induction coil is greater than the cross-sectional area of seaming chuck and push-down head；
The inductor, for being placed on the induction coil, push-down head, between seaming chuck；
The thermocouple, one end are linked into the cavity of the furnace body；
The furnace body is provided with inflating port, gas vent, vacuum system interface；
The inflating port, for inflation or liquid nitrogen into the cavity of the furnace body；
The gas vent, for the intracorporal gas of the chamber of the furnace body to be discharged；
The vacuum system interface is used for external pumped vacuum systems；
The induction power supply, supply frequency 1000-400000Hz；
The inductor, material are graphite or stainless steel；
The thermocouple, one end are linked into the cavity of the furnace body and are inserted into the thermometer hole of the inductor；
The seaming chuck, push-down head are by flangeseal at the top and bottom of furnace body；
The induction coil, thermocouple are accessed by flangeseal in the cavity of furnace body.
2. semiconductor material Preparation equipment according to claim 1, which is characterized in that
Semiconductor material Preparation equipment further includes hydraulic system；
The hydraulic system, for controlling the displacement and speed of seaming chuck and push-down head；
The hydraulic system, including hydraulic pump, displacement sensor and pressure sensor；
The hydraulic pump, for driving seaming chuck, push-down head；
Institute's displacement sensors, for detecting the displacement of seaming chuck, push-down head；
The pressure sensor, for detecting the pressure of seaming chuck, push-down head.
3. semiconductor material Preparation equipment according to claim 1, which is characterized in that
The furnace body is provided with cooling water connector on pipe water cooling furnace body, furnace body and fire door for double-deck or single layer.
4. semiconductor material Preparation equipment according to claim 1, which is characterized in that
The fire door, is provided with visual window.
5. semiconductor material Preparation equipment according to claim 1, which is characterized in that
The pumped vacuum systems, including high-vacuum pump, rough vacuum pump, valve and vacuum meter.
6. semiconductor material Preparation equipment according to claim 5, which is characterized in that
The high-vacuum pump is molecular pump, diffusion pump, ionic pump, cryogenic pump or lobe pump；
The rough vacuum pump is rotary vane mechanical pump, direct connection mechanical pump, water ring pump or oil-free dry pump.
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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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| CN104697331A CN104697331A (en) | 2015-06-10 |
| CN104697331B true CN104697331B (en) | 2019-04-23 |
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| CN201311179Y (en) * | 2008-09-28 | 2009-09-16 | 锦州航星真空设备有限公司 | Multifunction vacuum high temperature hot pressing furnace |
-
2013
- 2013-12-04 CN CN201310646928.2A patent/CN104697331B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH1038466A (en) * | 1996-07-24 | 1998-02-13 | Fuji Electric Co Ltd | Vacuum float dissolving apparatus and dissolving and casting method |
| CN201122048Y (en) * | 2007-09-07 | 2008-09-24 | 上海中加电炉有限公司 | Large vacuum hotpressing stove |
| CN101183093A (en) * | 2007-11-08 | 2008-05-21 | 武汉科技大学 | Measuring equipment of non-metallic material high-temperature expansive power and method of use thereof |
| CN101187611A (en) * | 2007-11-08 | 2008-05-28 | 武汉科技大学 | Heating device for determining non-metal material high temperature compressive strength |
| CN201311179Y (en) * | 2008-09-28 | 2009-09-16 | 锦州航星真空设备有限公司 | Multifunction vacuum high temperature hot pressing furnace |
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| CN104697331A (en) | 2015-06-10 |
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