CN205241849U - Induction heating rutile list crystal growth stove - Google Patents
Induction heating rutile list crystal growth stove Download PDFInfo
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- CN205241849U CN205241849U CN201520962478.2U CN201520962478U CN205241849U CN 205241849 U CN205241849 U CN 205241849U CN 201520962478 U CN201520962478 U CN 201520962478U CN 205241849 U CN205241849 U CN 205241849U
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- growth
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- crystal growth
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Abstract
The utility model relates to an induction heating rutile list crystal growth stove belongs to single crystal growth field. The problem of the distribution of temperature is hard to the accurate control, and following axial -temperature gradient is great at the crystal growth interface, easily has great stress in the crystal is solved, the growth stove includes: be divided into the cavity and the lower stove outer covering of cavity, a heating device, it is internal as the heating section to place the epicoele in including the conductive ceramic pipe, and the conductive ceramic pipe is the feed inlet and the feedstock channel of cavity down, and the quartz capsule is established to conductive ceramic outside of tubes cover, and the quartz capsule twines an electromagnetic induction coil outward, sets up in the internal growth room of cavity of resorption, and heating device below sets up the growth region into the growth room, the 2nd heating device, the two intraformational electromagnetic induction coil of heat preservation including the growth room of the below that sets up crystal growth district forms the soaking zone. The utility model discloses the change of possible temperature is more accurate, can adjust crystal growth's temperature gradient as required at any time.
Description
Technical field
The utility model relates to optical crystal growth furnace, particularly relates to a kind of eddy-current heating rutile monocrystalGrowth furnace, belongs to single crystal growth field.
Background technology
Rutile monocrystal receives much concern owing to having excellent physicochemical characteristics. Be mainly manifested in highRefractive index and birefringence, visible-infrared band permeability is good, is widely used in preparing optical communication systemIn the device such as optoisolator, light annular device, and the refractive power of electronic computer, polarizer, polarized light microscopyThe happy prism of Nico in mirror, polariscope, photometer, optically-active saccharimeter, interferes laser solution as instrument, chemistry pointAnalysing the colorimeter of use etc., is modern national defense, Aero-Space and the indispensable material of scientific research cause.
The method of growing rutile monocrystal has light float-zone method and flame melt method at present. The crystal of light float-zone method growthDislocation density is lower, but because the radial temperature profile of growth interface is that center is low, outside is high forever, growthInterface is in an unsure state, and is difficult to growing large-size crystal. Though tradition flame melt method can grow large scaleMonocrystal, but owing to using oxyhydrogen flame as origin of heat, the rutile single crystals physique of this method growth at presentMeasure still defectiveness, main cause is that the Temperature Distribution of oxyhydrogen flame is difficult to accurate control, and growth interface is subject to air-flowImpact, have a strong impact on crystal mass; The following axial-temperature gradient of crystal growth interface is larger, easy in crystalThere is larger stress; Crystal dislocation density is generally higher.
Utility model content
Technical problem to be solved in the utility model is to provide a kind of eddy-current heating rutile single crystals bulk-growthStove, by electromagnetic induction heating mode, can control temperature and Temperature Distribution in stove accurately, therebyIn body of heater, set up suitable thermograde to meet the requirement of growing optics-level rutile monocrystal.
The utility model is achieved in that a kind of eddy-current heating rutile monocrystal growth furnace, comprising:
Furnace shell; Furnace shell is upper cavity and the lower chamber separating by ceramic wafer, and the top of furnace shell is provided with chargingMouthful;
First heater, comprises that conductivity ceramics pipe is placed in upper cavity interior as bringing-up section, and conductivity ceramics pipe isThe feeding-passage of charging aperture and lower chamber, the outer sheathed quartz ampoule of conductivity ceramics pipe, quartz ampoule is wound around high-frequency electrical outwardMagnetic induction coil, fills heat preservation rock in upper cavity;
Growth room, is arranged in lower chamber, is total to central shaft communicates with conductivity ceramics pipe, in growth room, arrangesLiftable pedestal bar, first heater below is set to the vitellarium of growth room, the side of corresponding vitellariumFace is offered observation window;
Secondary heating mechanism, comprises the low frequency electricity in the heat-insulation layer of growth room of the below that crystal vitellarium is setMagnetic induction coil forms soaking zone.
Further, described growth room and conductivity ceramics pipe junction are arranged on pottery to the utility model growth furnaceOn plate, be wide-mouth structure, at wide-mouth structural region as crystal vitellarium.
Further, charging aperture is nozzle to the utility model growth furnace.
Further, the height of described bringing-up section is 120~160mm to the utility model growth furnace.
Further, the height of described soaking zone is 170~200mm to the utility model growth furnace.
Further, described high-frequency electromagnetic induction coil current adjustable extent is the utility model growth furnace50~130A, range of temperature is 900~2800 DEG C.
The utility model growth furnace further, described low frequency electromagnetic induction coil current range 10~50A, temperatureDegree is changed to 500~1500 DEG C.
Compared with prior art, beneficial effect is the utility model:
1. the utility model equipment is heated and is tied by the mode that adopts High-frequency and low-frequency electromagnetic induction to matchThe setting of structure, compared with traditional oxyhydrogen flame, the utility model can be by changing by the electric current of induction coilChange temperature and Temperature Distribution in stove, and can accomplish that the variation of temperature is more accurate, Ke YigenAccording to the thermograde that need to adjust at any time crystal growth.
2. by adopting the heating of the utility model growth furnace electromagnetic induction, can reduce to greatest extent golden redThe gas shock that stone growth interface is suffered, thus can make powder fusing more abundant, and crystallization is more complete, lacksSunken quantity significantly reduces.
3. adopt heat preservation rock to make the insulation material of body of heater, can alleviate body of heater quality.
4. the rutile monocrystal that prepared by the utility model meets optical grade requirement.
5. the flame fusion furnace of traditional growing rutile monocrystal is to adopt oxyhydrogen flame as origin of heat, combustion gas combustionBurn heat is passed to molten cap in the mode of conduction, crystalline size is larger, and the flow of required combustion gas just thereuponIncrease, this is that air-flow is just larger to the impact of molten cap, and the thing followed is that matter crystal internal defect increases, evenThere is the danger of overflow. The utility model method, in stove, temperature increases along with the increase of electric current, and with radiationForm transfer heat to molten cap, avoided the impact of air-flow, be therefore applicable to growing optics-level rutile listCrystal.
Brief description of the drawings
The growth furnace structural representation that Fig. 1 provides for the utility model embodiment;
The temperature temperature distribution state of the growth furnace that Fig. 2 provides for the utility model embodiment.
Detailed description of the invention
In order to make the purpose of this utility model, technical scheme and advantage clearer, below in conjunction with enforcementExample, is further elaborated to the utility model. Should be appreciated that specific embodiment described hereinOnly in order to explain the utility model, and be not used in restriction the utility model.
Referring to Fig. 1, a kind of eddy-current heating rutile monocrystal growth furnace, comprising: stainless steel furnace shell, furnace shell 1The upper cavity 11 and the lower chamber 12 that separate by ceramic wafer, the top of furnace shell 1 is provided with charging aperture 7, housingOn be provided with ceramic cap 2; First heater, comprises that conductivity ceramics pipe 8 is placed in the interior conduct of upper cavity 11 and addsHot arc, conductivity ceramics pipe 8 is the feeding-passage of charging aperture 7 and lower chamber 12, conductivity ceramics pipe 8 is outer sheathedQuartz ampoule 3, outer winding the first electromagnetic induction coil 5 of quartz ampoule 3, the interior filling heat preservation rock 4 of upper cavity 11,The internal diameter of conductivity ceramics pipe 8 is 20mm, and the height of the bringing-up section that the first electromagnetic induction coil 5 forms is120~160mm;
Growth room is arranged in lower chamber, is total to central shaft communicates with conductivity ceramics pipe 8, in growth room, arrangesLiftable pedestal bar 13, first heater below is set to the vitellarium of growth room, corresponding vitellariumObservation window 9 is offered in side; Growth room and conductivity ceramics pipe junction are arranged on ceramic wafer 6, are wide-mouth knotStructure, at wide-mouth structural region as crystal vitellarium. Include secondary heating mechanism, in crystal vitellariumThe heat-insulation layer of growth room of below in the second electromagnetic induction coil 10 form soaking zone. The second electromagnetic inductionThe height that coil 10 forms soaking zone is 170~200mm. Bringing-up section matches with soaking zone, jointly formsThe rutile needed thermograde of growing. The charging aperture of growth furnace is selected nozzle.
In the present embodiment, the first electromagnetic induction coil electric current adjustable extent is 50~130A, range of temperatureIt is 900~2800 DEG C. Second low frequency electromagnetic induction coil current range 10~50A, variations in temperature is500~1500℃。
This growth furnace makes full use of radiation, conduction, convection heat transfer' heat-transfer by convection principle, and in stove, temperature is the highest can be heated to2800 DEG C, can meet the requirement of most of high-temp oxide crystals. For growing rutile monocrystal, twoTitanium oxide powder is carried from nozzle and is entered in body of heater by oxygen, then by heating element heater electromagnetic induction coil andHigh temperature resistant conductivity ceramics heats by radiation mode, makes it to heat up, and melts in growth room, formsMolten cap, heating-up temperature is regulated by the electric current by induction coil. The effect of quartz ampoule is protection electromagnetic inductionCoil, in order to avoid melted by heat.
The fusing point of rutile is 1850 DEG C, can know according to Fig. 2, and the utility model growth furnace of employing,When the flow of adjusting oxygen is 0.1m/s, bringing-up section temperature is heated to 2400 DEG C, and bringing-up section is adjusted into 150mm,Soaking zone is adjusted into 180mm, can guarantee that growth interface center temperature is a little more than 1850 DEG C, and warm aroundDegree, a little less than 1850 DEG C, meets growing rutile monocrystal and expands shoulder requirement.
The utility model is prepared rutile according to above-mentioned growth furnace for eddy-current heating:
1) first adjust induced-current to the about 0.5h of body of heater preheating, bringing-up section electric current is started by 50A, withThe speed of 1.5A/min increases bringing-up section electric current, until temperature reaches 1500 DEG C of left and right in bringing-up section;
2) move being equipped with on the pedestal bar of seed crystal, make seed crystal top planes be positioned at 1/3 place of observation window height,Then progressively increase induced-current, increase bringing-up section electric current according to the speed of 1.5A/min, make seed crystal top fromFour jiaos start to melt and form molten drop, observe obvious liquid-solid interface;
3) start powder supplying mechanism, and pass into oxygen initial flow 0.1m/s, oxygen is carrying powder and is falling molten dropUpper, and all melt, more progressively increase bringing-up section electric current, increase electric current extremely according to the speed of 0.5A/min130A, and increase for powder amount according to molten cap state, ensure oxygen flow 0.5m/s, control seed rod and move down speedDegree 5~8mm/h, makes liquid-solid line of demarcation keep stable, and crystal starts to expand shoulder growth;
4) regulate soaking zone, low frequency electromagnetic induction coil current range 10~50A, temperature is 500~1500 DEG C;
5) in the time that crystal expansion is takeed on to required size, keep for powder speed and bringing-up section electric current, crystal starts isometricalGrowth. When crystal grows to after Len req, in reducing for powder amount, subtract with the speed of 1.5A/minFew bringing-up section electric current, the indoor temperature that makes to grow is reduced to below 1850 DEG C gradually, molten cap attenuation now, straightFootpath diminishes and fades away, and receives shoulder and finishes;
6) then stop air feed, feed and induced-current, body of heater is incubated to processing, treat that crystal is cooled toAfter room temperature, send into and in annealing furnace, carry out annealing in process.
The rutile of above-mentioned preparation is optical grade, the monocrystal that defect is few.
The foregoing is only preferred embodiment of the present utility model, not in order to limit the utility model,All any amendments of doing within spirit of the present utility model and principle, be equal to and replace and improvement etc., all shouldWithin being included in protection domain of the present utility model.
Claims (7)
1. an eddy-current heating rutile monocrystal growth furnace, is characterized in that, comprising:
Furnace shell; Furnace shell is upper cavity and the lower chamber separating by ceramic wafer, and the top of furnace shell is provided with chargingMouthful;
First heater, comprises that conductivity ceramics pipe is placed in upper cavity interior as bringing-up section, and conductivity ceramics pipe isThe feeding-passage of charging aperture and lower chamber, the outer sheathed quartz ampoule of conductivity ceramics pipe, quartz ampoule is wound around the first electricity outwardMagnetic induction coil, fills heat preservation rock in upper cavity;
Growth room, is arranged in lower chamber, is total to central shaft communicates with conductivity ceramics pipe, in growth room, arrangesLiftable pedestal bar, first heater below is set to the vitellarium of growth room, the side of corresponding vitellariumFace is offered observation window;
Secondary heating mechanism, comprises the second electricity in the heat-insulation layer of growth room of the below that crystal vitellarium is setMagnetic induction coil forms soaking zone.
2. according to growth furnace claimed in claim 1, it is characterized in that described growth room and conductivity ceramics pipeJunction is arranged on ceramic wafer, is wide-mouth structure, at wide-mouth structural region as crystal vitellarium.
3. according to growth furnace claimed in claim 1, it is characterized in that, charging aperture is nozzle.
4. according to growth furnace claimed in claim 1, it is characterized in that, the height of described bringing-up section is120~160mm。
5. according to growth furnace claimed in claim 1, it is characterized in that, the height of described soaking zone is170~200mm。
6. according to growth furnace claimed in claim 1, it is characterized in that described the first electromagnetic induction coil electricityStream adjustable extent is 50~130A, and range of temperature is 900~2800 DEG C.
7. according to growth furnace claimed in claim 1, it is characterized in that described the second electromagnetic induction coil electricityStream scope 10~50A, variations in temperature is 500~1500 DEG C.
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CN201520962478.2U CN205241849U (en) | 2015-11-25 | 2015-11-25 | Induction heating rutile list crystal growth stove |
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CN201520962478.2U CN205241849U (en) | 2015-11-25 | 2015-11-25 | Induction heating rutile list crystal growth stove |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105369342A (en) * | 2015-11-25 | 2016-03-02 | 东北大学 | Inductively heated rutile single crystal growth furnace and method for preparing rutile by using same |
CN114318510A (en) * | 2021-12-30 | 2022-04-12 | 无锡晶名光电科技有限公司 | Indium antimonide crystal growth method and crystal growth furnace |
-
2015
- 2015-11-25 CN CN201520962478.2U patent/CN205241849U/en not_active Withdrawn - After Issue
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105369342A (en) * | 2015-11-25 | 2016-03-02 | 东北大学 | Inductively heated rutile single crystal growth furnace and method for preparing rutile by using same |
CN114318510A (en) * | 2021-12-30 | 2022-04-12 | 无锡晶名光电科技有限公司 | Indium antimonide crystal growth method and crystal growth furnace |
CN114318510B (en) * | 2021-12-30 | 2023-09-19 | 无锡晶名光电科技有限公司 | Indium antimonide crystal growth method and crystal growth furnace |
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Granted publication date: 20160518 Effective date of abandoning: 20171031 |