CN107829133A - A kind of flame melt method numerical control crystal growing furnace - Google Patents

A kind of flame melt method numerical control crystal growing furnace Download PDF

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Publication number
CN107829133A
CN107829133A CN201711211207.3A CN201711211207A CN107829133A CN 107829133 A CN107829133 A CN 107829133A CN 201711211207 A CN201711211207 A CN 201711211207A CN 107829133 A CN107829133 A CN 107829133A
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CN
China
Prior art keywords
screen cloth
growing furnace
crystal growing
crystal
numerical control
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Pending
Application number
CN201711211207.3A
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Chinese (zh)
Inventor
毕孝国
周文平
唐坚
刘旭东
孙旭东
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Shenyang Institute of Engineering
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Shenyang Institute of Engineering
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Priority to CN201711211207.3A priority Critical patent/CN107829133A/en
Publication of CN107829133A publication Critical patent/CN107829133A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/04Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
    • C30B11/08Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt every component of the crystal composition being added during the crystallisation
    • C30B11/10Solid or liquid components, e.g. Verneuil method
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006Controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • C30B29/32Titanates; Germanates; Molybdates; Tungstates

Abstract

The invention belongs to field of new materials, is a kind of flame melt method numerical control crystal growing furnace, including:Crystal growth system, including crystal growing furnace, penetrate in crystal growing furnace, for the crystal growth pedestal bar of the carrier as crystal growth, the lifting speed controlling organization that quartz crystal grows pedestal bar and move up and down is transferred to by motor driven turn-screw;Material supply system, including taper raw material cabin, set screen cloth in the raw material cabin, and the charging aperture of the raw material cabin is provided with screen cloth vibrating mechanism;Fuel system, growth room is connected to by pipeline;Numerical control system, control signal is sent to lifting speed controlling organization, screen cloth vibration amplitude controlling organization, screen cloth vibration frequency control mechanism and gas handling system, and for setting control parameter.The present invention is particularly the high-temperature oxide monocrystal under melt state with decomposition tendency, such as strontium titanates, rutile monocrystal at a high temperature of can growing the complete high-quality of microstructure.

Description

A kind of flame melt method numerical control crystal growing furnace
Technical field
The invention belongs to field of new materials, is particularly a kind of flame melt method numerical control crystal growing furnace.
Background technology
Rutile monocrystal is preparing optoisolator, optical circulator, risen because having high birefringence and chemical stability There is irreplaceable advantage in the devices such as inclined device.As high temperature oxide single crystals such as rutile, melted using traditional flame The growth of method crystal growing furnace.
In traditional flame melt method crystal growing furnace, in crystal growth mechanism not using accurate turn-screw and numeral Control, fuel gas are not controlled without using accurate turn-screw sum using accurate gas mass flow gauge, raw material Word controls, and whole system does not have unified quality control system.Because growthing process parameter is without accurate digital control, growth For speed typically in more than 10mm/h, the speed of growth is fast, environment of crystal growth, especially temperature field, is unfavorable for complete optical grade Crystal, the speed of growth is very fast, growth interface, and entirely the Temperature Distribution in growth room, composition distribution cannot be guaranteed high-quality Crystal growth.Cause grown crystal in structural intergrity, for example dislocation density is high, stress is big, uneven etc., particularly The growth of rutile monocrystal, product qualified rate are very low.
For the method for crystal growth by crystal pulling stove being commonly used, because growth course is vacuum or the protection in high temperature Carried out down under atmosphere, there are strict requirements to the crucible material for containing melt.It is required that crucible material high temperature resistant, it is corrosion-resistant, Chemical erosion etc., typically valuable Iridium Crucible does not occur with melt so that the cost of whole growth furnace improves.To wanting The crystal of growth also has under strict requirements, such as high temperature, particularly solution, does not decompose.And as high temperature such as rutile Oxide single crystal at high temperature, is had very high decomposition pressure, is difficult to grow height using czochralski method particularly under melt state The rutile monocrystal of quality.
Rutile (TiO2) monocrystal birefringence is big, refractive index is big, for example optically isolated for spectroscope prism, polarizer Device, optical circulator, beam splitter etc..Above-mentioned device currently used for optical communication uses Yttrium Orthovanadate(YVO4)Crystal, high-end production Product must use rutile (TiO2) monocrystal.For another example, strontium titanates(STiO3)Monocrystal, it is very typical superconduction base Sheet material, but be difficult to grow using czochralski method.
Using traditional crystal growing furnace, because many growthing process parameters are not accurately controlled, the speed of growth is very fast, Temperature Distribution, composition distribution in growth interface, and whole growth room is it cannot be guaranteed that the crystal growth of high-quality.Cause to give birth to Long crystal is in structural intergrity, for example dislocation density is high, stress is big, uneven etc..
Establish the accurate temperature field for being adapted to crystalchecked growth and composition is distributed, removing influences crystalline substance in crystal growing process The factor of weight is extremely necessary to growing optics-level rutile monocrystal and other high-quality high-temp oxide crystals.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of flame melt method numerical control crystal growing furnace, can accurately controlled The parameters of crystal growth processed, Temperature Distribution, composition distribution and mechanics distribution in growth room are ensured, can be grown microcosmic Being particularly at a high temperature of the high-quality of structural integrity has the high-temperature oxide monocrystal for decomposing tendency, such as metatitanic acid under melt state The monocrystal such as strontium, rutile.
The present invention is achieved in that
A kind of flame melt method numerical control crystal growing furnace, it is characterised in that the growth furnace includes:
Crystal growth system, including crystal growing furnace, penetrate in crystal growing furnace, the crystal for the carrier as crystal growth Pedestal bar is grown, being transferred to quartz crystal by motor driven turn-screw grows the lifting speed control that moves up and down of pedestal bar Mechanism processed;
Material supply system, including taper raw material cabin, screen cloth, the charging aperture installation of the raw material cabin are set in the raw material cabin There is screen cloth vibrating mechanism;
Fuel system, growth room is connected to by pipeline;
Numerical control system, to lifting speed controlling organization, screen cloth vibration amplitude controlling organization, screen cloth vibration frequency control mechanism And gas handling system sends control signal, and for setting control parameter.
Further, the fuel system includes fuel gas source and fuel gas pipeline, float gas flow Meter, digital gas flowmeter, fuel gas controlling organization;Fuel gas source is connected to crystal growth by fuel gas pipeline Stove, set float gas flowmeter to be used for signal piping gas station on fuel gas pipeline, digital gas flowmeter is set For accurately controlling the flow of gas, fuel gas controlling organization is by sealing in the dehumidifying of fuel gas pipeline, drying, purify and set It is standby, the clean gas for meeting technological requirement is provided to digital gas flowmeter.
Further, Material supply system includes:
Screen cloth vibration amplitude controlling organization, regulation of the control screen cloth vibrating mechanism to the vibration amplitude of screen cloth;
Screen cloth vibration frequency control mechanism, regulation of the control screen cloth vibrating mechanism to the vibration frequency of screen cloth.
Further, the screen cloth vibration amplitude controlling organization includes the interior empty support column parallel with crystal growth pedestal bar I, is provided with connecting rod in the support column I, and the connecting rod passes through the lifting of a motor driven connecting rod, the connecting rod End connect a cross bar, the cross bar one end connection screen cloth vibrating mechanism.
Further, the screen cloth vibration frequency control mechanism exports transverse axis by a motor, at least a piece of on transverse axis Depression bar, transverse axis drive depression bar to rotate, the depression bar and the beam contact.
Further, the motor of the screen cloth vibration frequency control mechanism is fixed on the support column II parallel with support column I On.
Further, the crystal growing furnace and Material supply system are fixed on support column I periphery.
Further, the numerical control system passes through screen cloth vibration amplitude controlling organization and screen cloth vibration frequency control The amplitude and frequency of mechanism controls screen cloth reach the control of charging.
Compared with prior art, beneficial effect is the present invention:
The flame melt method numerical control crystal growing furnace of the present invention can be used for growing Special high-temperature oxide single crystal.Special high-temperature aoxidizes Thing monocrystal refers to that fusing point has the oxide single crystal of decomposition of components tendency more than 1600 DEG C, under high temperature fused state.By In realizing the precise figures control to parameter, temperature conditionss, composition condition and the mechanics bar required for crystal growth are improved The control accuracy of part, realizes accurate control of the speed of growth in 2-50mm/h sections, and the crystal perfection grown is good.High temperature Oxide single crystal, such as rutile monocrystal, strontium titanate monocrystal body, for preparing the optics such as the polarizer, superconductor substrate device Part etc., it is widely used in making the numerous areas such as optoisolator, optical circulator, superconductive device.
The present invention is by carrying out accurate mechanical structure to crystal growth mechanism, fuel organization of supply and raw material supply mechanism Design, increase corresponding control electricity, realize and gas flow, raw material supply amount and crystal growth speed are set in real time in control system Degree, realizes the digital control of crystal growth, storage technology data and can call at any time(It is shown on striking screen, computer screen On curtain, print).The present invention can establish suitable temperature field in body of heater, meet growing optics-level rutile monocrystal Requirement.According to retrieval result, there is presently no with function identical of the present invention disclosed in Special Equipment and device.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
A kind of flame melt method numerical control crystal growing furnace of the present invention, by crystal growth system, fuel system, raw material Supply system, the part of numerical control system four are formed, and see Fig. 1.
Referring to Fig. 1, crystal growth system of the present invention includes crystal growing chamber 5, crystal growth pedestal bar 4, transmission Leading screw 3 and lifting speed controlling organization 17.Crystal growth pedestal bar is penetrated in crystal growing furnace, for as crystal growth Carrier, lifting speed controlling organization drive turn-screw 3 to be transferred to quartz crystal growth pedestal bar 4 and do fortune up and down by motor 2 It is dynamic;
Turn-screw 3, which is arranged on, to be driven by controlled motor on a basic framework 1, forms the upper and lower of movement velocity controllable precise (Lifting)Motion, and crystal growth pedestal bar 4 is passed motion to, so as to accurately control the lifting speed of crystal.
Fuel system includes fuel gas source 7, fuel gas pipeline 6, float gas flowmeter 8, digital gas stream Gauge 9 and fuel gas controlling organization 19.Fuel gas source 7 includes fuel gas and combustion-supporting gas, and fuel gas can be Hydrogen, acetylene gas etc., combustion-supporting gas are oxygen.Fuel gas pipeline 6 is connected to crystal growing chamber, is stainless steel or polymer tube Line.Float gas flowmeter 8 is used for signal piping gas station, digital gas with the float gas flowmeter 8 of digital gas flowmeter 9 Flowmeter body 9 is used for the flow for accurately controlling gas.Fuel gas controlling organization 19 is by sealing in the dehumidifying of gas passage, doing Dry, cleaning equipment, the clean gas for meeting technological requirement is provided to digital gas flowmeter.
Material supply system includes raw material cabin 10, screen cloth 11, screen cloth vibrating mechanism 12, screen cloth vibration amplitude controlling organization 13rd, screen cloth vibration frequency control mechanism, screen cloth vibration frequency control motor 15, screen cloth vibration amplitude controlled motor 16 are formed.It is former Feed bin 10 is used to hold crystal raw material;Screen cloth 11 and screen cloth vibrating mechanism 12 are used to be fed;Screen cloth vibration amplitude controlling organization 13, Screen cloth vibration frequency control mechanism, screen cloth vibration frequency control motor 15, screen cloth vibration amplitude controlled motor 16 are used to accurately supply Material.
Screen cloth vibration amplitude controlling organization includes the interior empty support column I21 parallel with crystal growth pedestal bar, in support column Connecting rod is provided with I21, for connecting rod by the lifting of motor driven connecting rod, the end of connecting rod connects a cross bar 20, horizontal One end connection screen cloth vibrating mechanism of bar 20, screen cloth vibrating mechanism can be the hammer body of up-down vibration.
Screen cloth vibration frequency control mechanism exports transverse axis by screen cloth vibration frequency control motor 15, at least one on transverse axis Piece depression bar 14, transverse axis drive depression bar 14 to rotate, depression bar and beam contact, and the upper of cross bar is adjusted by the velocity of rotation for adjusting depression bar Bottom dynamic frequency is so as to controlling the vibration frequency of screen cloth vibrating mechanism.
The motor of screen cloth vibration frequency control mechanism is fixed on the support column II22 parallel with support column I.
Crystal growing furnace and Material supply system are fixed on support column I periphery.
Numerical control system passes through screen cloth vibration amplitude controlling organization and screen cloth vibration frequency control mechanism controls screen cloth Amplitude and frequency reach the control of charging.
Numerical control system of the present invention controls lifting speed controlling organization 2, digital gas flowmeter 9, screen cloth to shake Dynamic frequency controlling organization 14, screen cloth vibration frequency control motor 15, screen cloth vibration amplitude controlling organization 16, numerical control system tool There is computer 18 to be manipulated by touch-screen.Lifting speed controlling organization 2, digital gas flowmeter 9, screen cloth vibration frequency control mechanism 14 and screen cloth vibration amplitude controlling organization 16 by encoder and software, realize the both-way communication of data and computer 18.Pass through The growthing process parameters such as the lifting speed of touch-screen and computer input data instruction control crystal growth, feeding speed, temperature field, Control growth course;Pass through the real-time monitoring to growth course technological parameter in real time of touch-screen and computer;Technological parameter is carried out Storage, call, the exploitation for crystal growth new varieties, new technology.
The crystal grown using the numerical control crystal growing furnace of the present invention, speed of growth stability contorting are complete in 6mm/h, crystal Whole property is fine.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.

Claims (8)

1. a kind of flame melt method numerical control crystal growing furnace, it is characterised in that the growth furnace includes:
Crystal growth system, including crystal growing furnace, penetrate in crystal growing furnace, the crystal for the carrier as crystal growth Pedestal bar is grown, being transferred to quartz crystal by motor driven turn-screw grows the lifting speed control that moves up and down of pedestal bar Mechanism processed;
Material supply system, including taper raw material cabin, screen cloth, the charging aperture installation of the raw material cabin are set in the raw material cabin There is screen cloth vibrating mechanism;
Fuel system, growth room is connected to by pipeline;
Numerical control system, to lifting speed controlling organization, screen cloth vibration amplitude controlling organization, screen cloth vibration frequency control mechanism And gas handling system sends control signal, and for setting control parameter.
2. according to the flame melt method numerical control crystal growing furnace described in claim 1, it is characterised in that the fuel system includes Fuel gas source and fuel gas pipeline, float gas flowmeter, digital gas flowmeter, fuel gas controlling organization;Fuel Gas source is connected to crystal growing furnace by fuel gas pipeline, sets float gas flowmeter to be used on fuel gas pipeline Signal piping gas station, sets digital gas flowmeter to be used for the flow for accurately controlling gas, and fuel gas controlling organization leads to Cross and seal in the dehumidifying, dry of fuel gas pipeline, cleaning equipment, the cleaning for meeting technological requirement is provided to digital gas flowmeter Gas.
3. according to the flame melt method numerical control crystal growing furnace described in claim 1, it is characterised in that Material supply system includes:
Screen cloth vibration amplitude controlling organization, regulation of the control screen cloth vibrating mechanism to the vibration amplitude of screen cloth;
Screen cloth vibration frequency control mechanism, regulation of the control screen cloth vibrating mechanism to the vibration frequency of screen cloth.
4. according to the flame melt method numerical control crystal growing furnace described in claim 3, it is characterised in that the screen cloth vibration amplitude control Mechanism includes the interior empty support column I parallel with crystal growth pedestal bar, and connecting rod, the company are provided with the support column I For extension bar by the lifting of motor driven connecting rod, the end of the connecting rod connects a cross bar, one end connection sieve of the cross bar Net vibrating mechanism.
5. according to the flame melt method numerical control crystal growing furnace described in claim 4, it is characterised in that the screen cloth vibration frequency control Mechanism exports transverse axis, at least a piece of depression bar on transverse axis by motor, and transverse axis drives depression bar to rotate, the depression bar and the cross bar Contact.
6. according to the flame melt method numerical control crystal growing furnace described in claim 5, it is characterised in that the screen cloth vibration frequency The motor of controlling organization is fixed on the support column II parallel with support column I.
7. according to the flame melt method numerical control crystal growing furnace described in claim 4, it is characterised in that the crystal growing furnace and original Material supply system is fixed on support column I periphery.
8. according to the flame melt method numerical control crystal growing furnace described in claim 4, it is characterised in that the numerical control system passes through The amplitude and frequency of screen cloth vibration amplitude controlling organization and screen cloth vibration frequency control mechanism controls screen cloth reach the control of charging System.
CN201711211207.3A 2017-11-28 2017-11-28 A kind of flame melt method numerical control crystal growing furnace Pending CN107829133A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109161960A (en) * 2018-11-07 2019-01-08 沈阳工程学院 A kind of plasma method numerical control crystal growing furnace
CN111005063A (en) * 2019-12-27 2020-04-14 沈阳工程学院 High-precision crystal growth powder setting control device

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109161960A (en) * 2018-11-07 2019-01-08 沈阳工程学院 A kind of plasma method numerical control crystal growing furnace
CN111005063A (en) * 2019-12-27 2020-04-14 沈阳工程学院 High-precision crystal growth powder setting control device

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Application publication date: 20180323