CN101323968A - Multicomponent compounds infrared crystal growth apparatus - Google Patents
Multicomponent compounds infrared crystal growth apparatus Download PDFInfo
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- CN101323968A CN101323968A CNA2008101385608A CN200810138560A CN101323968A CN 101323968 A CN101323968 A CN 101323968A CN A2008101385608 A CNA2008101385608 A CN A2008101385608A CN 200810138560 A CN200810138560 A CN 200810138560A CN 101323968 A CN101323968 A CN 101323968A
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Abstract
The invention provides a growth device of an infrared crystal of polynary compounds and comprises a stove, a hearth box inside the stove comprises three temperature regions of an upper high-temperature region, a middle gradient region and a lower low-temperature region from up to down, a heater with standalone temperature control is respectively arranged inside the upper high-temperature region and the lower low-temperature region, a thermocouple with temperature control is respectively positioned inside the upper high-temperature region and the lower low-temperature region, and the middle gradient region is a heat-insulating and fireproof layer with ventholes; a loading rod that is used for loading a crucible pot of crystal growth is arranged inside the hearth box, a lower end of the loading rod is connected with a rotary clamping head that is connected with an electric motor, and the electric motor is arranged on a spiral travel mechanism. The growth device can obtain temperature fields that are suitable for crystal growth according to the growth habits of different infrared crystals of polynary compounds, maintains the stability of a solid-liquid interface and realizes the crystal growth in the planar interface. By using the growth device and adopting the Bridgman method, the infrared crystal of polynary compounds with complete appearance and well crystal property can be prepared.
Description
Technical field
The present invention relates to a kind of growing apparatus of multicomponent compound infrared crystal, belong to mineral crystal growing technology field.
Background technology
The mid and far infrared coherent source has very important application at laser field, in military field, as: laser guidance, the infrared interference of laser orientation, laser communications, infrared remote sensing, thermal infrared imager, infrared distance measurement, laser aiming etc.; At civil area, as: all there is application quite widely aspects such as trace gas detection, biology, medicine in the environment.Present laser host material can produce tunable within the specific limits coherent source output, but because its tunable wavelength region is decided by the gain bandwidth of active ions in laser medium, so their tunable range and efficient are severely limited.Multicomponent compound infrared crystal is as AgGaS
2, AgGaSe
2, ZnGeP
2, CdGeAs
2, LiInS
2, LiInSe
2Deng having excellent non-linear optical property, can amplify (OPA) by optical parameter, optical parametric oscillation nonlinear frequency transformation technology such as (OPO) realizes tunable mid and far infrared laser output.The above-claimed cpd infrared crystal is the comparatively difficult crystal of growth of generally acknowledging, general available Bridgman method (Bridgman method) is carried out single crystal growing, the gradient zones of traditional Bridgman method temperature field is that the thermograde at solid-liquid interface place is less, and can't regulate according to different Growth Habit.These compound component are many, and the fusing point difference is big, and the saturated vapor pressure difference is big, and high temperature easily decomposes down; Especially in the crystallisation process, owing to form the segregation coefficient difference of each constituent element material of compound, the heat conductivility difference of solid and melt is big in addition, along with the variation of crystal growing process, the temperature field of crystallizing field is changed, cause solid-liquid interface to drift about, be difficult to keep required flat (or dimpling) interface growth of crystal growth, so common Bridgman method and existing growth apparatus are difficult to obtain the good compound semiconductor single crystal of integrity, the application of restriction infrared crystal.
Summary of the invention
The present invention is directed to the deficiency that existing multicomponent compound infrared crystal growing technology exists, a kind of multicomponent compounds infrared crystal growth apparatus that can prepare the multicomponent compound infrared crystal that outward appearance is complete, crystal property is good is provided.
Multicomponent compounds infrared crystal growth apparatus of the present invention adopts following technical solution:
This multicomponent compounds infrared crystal growth apparatus comprises body of heater, the intravital burner hearth of stove comprises high-temperature zone, top, middle part gradient zones and three kinds of warm areas of bottom cold zone from top to bottom, high-temperature zone, top and bottom cold zone are provided with the well heater of independent temperature control, high-temperature zone, top and bottom cold zone are all laid temperature-control heat couple, the middle part gradient zones is the insulating refractory layer of band ventilating pit, be provided with the support bar that supports crystal growing crucible in the burner hearth, the lower end of support bar is connected with the rotation dop, the rotation dop is connected with a motor, and motor is installed in the spiral travel mechanism.
The temperature-control heat couple of high-temperature zone, top is placed in 1/2～2/3 position of high-temperature zone, top height, and the temperature-control heat couple of bottom cold zone is placed in 1/3～1/2 position of bottom cold zone height.
The upper and lower end of insulating refractory layer is provided with baffle plate, and the position of regulating upper and lower baffle plate can change the thickness of heat insulation fireproof plate.
Add one deck Zirconium oxide fibre blanket above the insulating refractory layer, be delivered to cold zone further to stop the high-temperature zone heat.
The top of burner hearth is provided with the head box that is used for closed furnace.
The bottom of burner hearth is provided with the heat insulation loop that prevents that heat from transmitting to atmosphere.
Support bar inside is placed with the temperature thermocouple that is used for measuring in real time crucible tip temperature.
This chamber design can realize the adjusting of warm curvature of field line in the burner hearth easily by control temperature and middle gradient zones lagging material of adjustment and the distance that changes high-temperature zone, cold zone, satisfies the requirement of the outer crystal growth of different compound of red to the temperature field.Roof of the furnace head box closed furnace, can effectively prevent " chimneyeffect ", guarantee to keep in the bigger scope in high-temperature zone constant temperature, the fusing and the homogeneity that help the multi-element compounds crystal raw material, the heat that prevents that the bottom is provided with can be guaranteed to keep constant temperature in cold zone in a big way to the heat insulation loop of atmosphere transmission.The heat insulation fireproof plate of middle gradient zones band ventilating pit can stop effectively that the high-temperature zone heat is to radiation, convection current and the conduction of cold zone to gradient zones, to reduce the temperature difference of high-temperature zone, keep the stable of temperature field, can produce bigger thermograde effectively in gradient zones, the spacing that can regulate high-temperature zone and cold zone easily by the thickness of regulating the insulating refractory layer, thus the size of thermograde changed.Adopt the thermofin of different effect of heat insulation in addition, the size that perhaps changes the middle ventilating pit of thermofin can change the size of thermograde equally, satisfies the needs of the outer crystal growth of Different Red.The support bar of support crucible can be realized the rotation of crucible in the crystal growing process, the inner temperature thermocouple of placing of support bar can be measured the temperature of crucible tip in real time, can real-time monitor crucible residing position in the temperature field, also help to realize the successful welding of seed crystal for seeded growth technology.
Multicomponent compounds infrared crystal growth apparatus of the present invention, crystal is grown in the different temperature fields of high-temperature zone, cold zone and three kinds of warm areas of gradient zones, can obtain to regulate in gradient zones than big thermograde and thermograde, thereby can be according to the habit of different multicomponent compound infrared crystals, regulate the control temperature of high-temperature zone, cold zone easily, obtain to be fit to the temperature field of crystal growth, keep the stability of solid-liquid interface, realize the crystalline plane interface growth.Use this growing apparatus, adopt Bridgman method (Bridgman method) can prepare the multicomponent compound infrared crystal that outward appearance is complete, crystal property is good.
Description of drawings
Fig. 1 is the structural representation of multicomponent compounds infrared crystal growth apparatus of the present invention.
Fig. 2 is the warm curvature of field line of multicomponent compounds infrared crystal growth apparatus of the present invention.
Among the figure: 1, body of heater, 2, silica tube, 3, plumbago crucible, 4, upper heater, 5, high-temperature zone temperature-control heat couple, 6, the zirconium white heat-insulation blanket, 7, overhead gage, 8, the insulating refractory layer, 9, lower baffle plate, 10, the cold zone temperature-control heat couple, 11, well heater down, 12, support bar, 13, heat insulation loop, 14, temperature thermocouple, 15, dop, 16, head box, 17, solid-liquid interface, 18, the high-temperature zone, 19, gradient zones, 20, cold zone, 21, ventilating pit.
Embodiment
Multicomponent compounds infrared crystal growth apparatus of the present invention comprises body of heater 1 as shown in Figure 1, fills up lagging material between the shell of body of heater 1 and the burner hearth.The intravital burner hearth of stove comprises high-temperature zone, top 18, middle part gradient zones 19 and bottom cold zone 20 3 parts from top to bottom.The top of burner hearth is provided with the head box of being made by alumina firebrick that is used for closed furnace 16, can effectively prevent " chimneyeffect ", guarantees to keep constant temperature in the bigger scope in high-temperature zone, helps the fusing and the homogeneity of polycrystal raw material.Burner hearth bottom adds a heat insulation loop 13, prevents that heat from causing calorific loss to the atmosphere transmission, keeps the warm field stability of cold zone, guarantees to keep constant temperature in cold zone in a big way.Be provided with the upper heater 4 by independent F P23 precise temperature control instrument control temperature control in the high-temperature zone, top 18, high-temperature zone temperature-control heat couple 5 is placed in 1/2～2/3 position of high-temperature zone, top height.Be provided with the well heater 11 by independent F P23 precise temperature control instrument control temperature control in the bottom cold zone 20, cold zone temperature-control heat couple 10 is placed in 1/3～1/2 position of bottom cold zone height.The centrally aligned burner hearth central axis of following well heater 11 is positioned over burner hearth, guarantee in the flat-temperature zone temperature radially evenly.Middle part gradient zones 19 is the insulating refractory layer of being made by the light-weight mullite lagging material 8 of one deck band ventilating pit 21, the upper and lower ends of insulating refractory layer 8 is provided with the overhead gage 7 and the lower baffle plate 9 of stainless material, and the thickness of insulating refractory layer 8 is adjusted by the distance of regulating between overhead gage 7 and the lower baffle plate 9.Put one deck zirconium white heat-insulation blanket 6 on insulating refractory layer 8, to increase effect of heat insulation, the internal diameter of insulating refractory layer 8 and zirconium white heat-insulation blanket 6 will be complementary with the outside dimension of crucible, guarantees can pass through when crucible moves down.Insulating refractory layer 8 and Zirconium oxide fibre blanket 6 are to be used to stop radiation, convection current and the conduction of the heat of high-temperature zone to gradient zones, to reduce the temperature difference of high-temperature zone, keep the stable of temperature field; Because the thermal conductivity of air is less, the middle ventilating pit of insulating refractory layer 8 can effectively stop the heat of high-temperature zone to the gradient zones transmission, increases the thermograde of gradient zones.By regulating the distance between overhead gage 7 and the lower baffle plate 9, the size that changes insulating refractory layer 8 middle ventilating pit can realize bigger thermograde in narrower gradient zones, satisfy the growth demand of different multicomponent compound infrared crystals.Also be provided with the support bar 12 of support crucible 3 in the burner hearth, support bar 12 is connected with motor by rotation dop 15.In order to keep the radial temperature profile in the crucible even, by rotation dop 15 support bar 12 is connected with motor in the crystal growing process, realizes the rotation of crucible, motor is installed in the spiral travel mechanism (not drawing among the figure), can realize the decline of crucible.The silica tube 2 that plumbago crucible 3 is housed is placed in the hydraucone of support bar 12 upper ends, be placed with temperature thermocouple 14 in tip, be used for monitoring in real time the temperature of crucible tip, understand crystal growing process near crucible 3, in seeded growth technology, also help to realize the successful welding of seed crystal.
This chamber design can be by control temperature and middle gradient zones lagging material of adjustment and the distance that changes high-temperature zone, cold zone, realize the adjusting of warm curvature of field line in the burner hearth easily, satisfy the requirement of the outer crystal growth of different compound of red to the temperature field, keep the stability of solid-liquid interface 17 in the plumbago crucible 3, realize the crystalline plane interface growth.The warm curvature of field line of multicomponent compounds infrared crystal growth apparatus of the present invention as shown in Figure 2.
Utilize above-mentioned multicomponent compounds infrared crystal growth apparatus growth infrared crystal, comprise following technological process:
(1) cleans silica tube
(2) feed and vacuumize, the sealed knot silica tube
The multi-element compounds crystal powder is packed in the crucible 3, in the silica tube 2 after the cleaning of again crucible of charging being packed into, be heated to then under 200 ℃～300 ℃ and vacuumize, the vacuum tightness in crucible reaches 10
-3～10
-4During Pa, with oxyhydrogen flame sealed knot silica tube.
(3) crystal growth
A. the silica tube behind the sealed knot 2 is put into the burner hearth of growing apparatus shown in Figure 1, make the crucible 3 of charging all be positioned at high-temperature zone, top 18, make high-temperature zone, top 18 be warming up to more than the multi-element compounds crystalline melting point 50 ℃～100 ℃, make the multi-element compounds crystal powder fully melt and overheated with the speed of 1 ℃ of/minute kind～3 ℃/minute kind; Bottom cold zone 20 is warming up to below the multi-element compounds crystalline melting point with same speed, after the temperature of high-temperature zone, top 18 and bottom cold zone 20 rises to target temperature, promptly obtains the needed temperature of crystal growth field, is incubated 24 hours～48 hours.
B. after holding stage finishes, crucible is descended with the speed of 10mm/ hour～20mm/ hour, the solid-liquid interface place of gradient zones in the middle part of the crucible tip is reduced to, promptly the position of multi-element compounds crystalline melting point correspondence stops to descend, after being incubated 4 hours～6 hours, crucible descends with the speed of 0.2mm/ hour～1mm/ hour, and the beginning crystal growth is through 2 week～3 time-of-weeks, allow the whole solid-liquid interface by the middle part gradient zones of melt in the crucible, the crystal growth end.
(4) crystal aftertreatment
After crystal growth finishes, crucible is dropped to the bottom cold zone annealed 2 days～4 days, take out crystal after reducing to room temperature with 10 ℃/hour～50 ℃/hour speed then.
Claims (7)
1. multicomponent compounds infrared crystal growth apparatus, comprise body of heater, it is characterized in that: the intravital burner hearth of stove comprises the high-temperature zone, top from top to bottom, middle part gradient zones and three kinds of warm areas of bottom cold zone, high-temperature zone, top and bottom cold zone are provided with the well heater of independent temperature control, high-temperature zone, top and bottom cold zone are all laid temperature-control heat couple, the middle part gradient zones is the insulating refractory layer of band ventilating pit, be provided with the support bar that supports crystal growing crucible in the burner hearth, the lower end of support bar is connected with the rotation dop, the rotation dop is connected with a motor, and motor is installed in the spiral travel mechanism.
2. multicomponent compounds infrared crystal growth apparatus according to claim 1, it is characterized in that: the temperature-control heat couple of high-temperature zone, described top is placed in 1/2～2/3 position of high-temperature zone, top height, and the temperature-control heat couple of bottom cold zone is placed in 1/3～1/2 position of bottom cold zone height.
3. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: the upper and lower end of described insulating refractory layer is provided with baffle plate.
4. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: add one deck Zirconium oxide fibre blanket above the described insulating refractory layer.
5. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: the top of described burner hearth is provided with the head box that is used for closed furnace.
6. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: the bottom of described burner hearth is provided with the heat insulation loop that prevents that heat from transmitting to atmosphere.
7. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: described support bar inside is placed with the temperature thermocouple that is used for measuring in real time crucible tip temperature.
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| CN2008101385608A CN101323968B (en) | 2008-07-24 | 2008-07-24 | Multicomponent compounds infrared crystal growth apparatus |
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Cited By (12)
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|---|---|---|---|---|
| CN102304753A (en) * | 2011-08-31 | 2012-01-04 | 中山大学 | Crystal growth preparation system |
| CN102787350A (en) * | 2012-09-03 | 2012-11-21 | 上海硅酸盐研究所中试基地 | Device and method of growing 500-1000mm long bismuth germanate crystals by descent method |
| CN102925957A (en) * | 2011-08-12 | 2013-02-13 | 昆山中辰矽晶有限公司 | Crystal growth device |
| CN103603033A (en) * | 2013-12-02 | 2014-02-26 | 中国工程物理研究院化工材料研究所 | Vertical Bridgman multi-component compound crystal growth system and application method thereof |
| CN103993355A (en) * | 2014-05-09 | 2014-08-20 | 上海大学 | Preparation method of CuInS2 monocrystals and preparation device of CuInS2 monocrystals |
| CN104165898A (en) * | 2014-08-21 | 2014-11-26 | 共慧冶金设备科技(苏州)有限公司 | Large-temperature-gradient Bridgman furnace |
| CN104593860A (en) * | 2015-02-03 | 2015-05-06 | 中国电子科技集团公司第四十六研究所 | Support structure for VB/VGF single crystal growth and processing method of support structure |
| CN105369361A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and apparatus for preparing sapphire single crystals by moving thermal field |
| CN105401213A (en) * | 2015-12-03 | 2016-03-16 | 河南西格马晶体科技有限公司 | Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method |
| CN105714375A (en) * | 2016-04-20 | 2016-06-29 | 黑龙江工程学院 | Synthesis method of Li-containing I-III-VI2 type mid and far infrared polycrystalline |
| CN106149051A (en) * | 2015-04-03 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | The thermal control Bridgman method single-crystal growing apparatus of fluoride single crystal body and method |
| CN115029770A (en) * | 2021-03-04 | 2022-09-09 | 北京一轻研究院有限公司 | Crucible atmospheric descending furnace device and method |
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2008
- 2008-07-24 CN CN2008101385608A patent/CN101323968B/en not_active Expired - Fee Related
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| CN102925957A (en) * | 2011-08-12 | 2013-02-13 | 昆山中辰矽晶有限公司 | Crystal growth device |
| CN102925957B (en) * | 2011-08-12 | 2015-06-17 | 昆山中辰矽晶有限公司 | Crystal growth device |
| CN102304753A (en) * | 2011-08-31 | 2012-01-04 | 中山大学 | Crystal growth preparation system |
| CN102787350B (en) * | 2012-09-03 | 2016-04-06 | 上海硅酸盐研究所中试基地 | The apparatus and method of the long bismuth-germanium-oxide crystal of descent method for growing 500-1000mm |
| CN102787350A (en) * | 2012-09-03 | 2012-11-21 | 上海硅酸盐研究所中试基地 | Device and method of growing 500-1000mm long bismuth germanate crystals by descent method |
| CN103603033A (en) * | 2013-12-02 | 2014-02-26 | 中国工程物理研究院化工材料研究所 | Vertical Bridgman multi-component compound crystal growth system and application method thereof |
| CN103603033B (en) * | 2013-12-02 | 2016-02-03 | 中国工程物理研究院化工材料研究所 | Vertical Bridgman multi-component compound crystal growth system and using method thereof |
| CN103993355A (en) * | 2014-05-09 | 2014-08-20 | 上海大学 | Preparation method of CuInS2 monocrystals and preparation device of CuInS2 monocrystals |
| CN103993355B (en) * | 2014-05-09 | 2016-11-02 | 上海大学 | CuInS2the preparation method of monocrystal and CuInS2monocrystal preparation facilities |
| CN104165898A (en) * | 2014-08-21 | 2014-11-26 | 共慧冶金设备科技(苏州)有限公司 | Large-temperature-gradient Bridgman furnace |
| CN104593860B (en) * | 2015-02-03 | 2017-02-22 | 中国电子科技集团公司第四十六研究所 | Support structure for VB/VGF single crystal growth and processing method of support structure |
| CN104593860A (en) * | 2015-02-03 | 2015-05-06 | 中国电子科技集团公司第四十六研究所 | Support structure for VB/VGF single crystal growth and processing method of support structure |
| CN106149051A (en) * | 2015-04-03 | 2016-11-23 | 中国科学院上海硅酸盐研究所 | The thermal control Bridgman method single-crystal growing apparatus of fluoride single crystal body and method |
| CN105401213A (en) * | 2015-12-03 | 2016-03-16 | 河南西格马晶体科技有限公司 | Method for preparing large flake-like sapphire single crystals by utilizing crucible rising pulling method |
| CN105369361A (en) * | 2015-12-03 | 2016-03-02 | 洛阳西格马炉业股份有限公司 | Method and apparatus for preparing sapphire single crystals by moving thermal field |
| CN105369361B (en) * | 2015-12-03 | 2018-04-10 | 河南西格马晶体科技有限公司 | A kind of thermal field movement prepares the method and device of sapphire monocrystal |
| CN105714375A (en) * | 2016-04-20 | 2016-06-29 | 黑龙江工程学院 | Synthesis method of Li-containing I-III-VI2 type mid and far infrared polycrystalline |
| CN105714375B (en) * | 2016-04-20 | 2017-12-15 | 黑龙江工程学院 | A kind of Li III VI2 types mid and far infrared polycrystalline synthetic method |
| CN115029770A (en) * | 2021-03-04 | 2022-09-09 | 北京一轻研究院有限公司 | Crucible atmospheric descending furnace device and method |
| CN115029770B (en) * | 2021-03-04 | 2024-05-03 | 北京一轻研究院有限公司 | Crucible atmospheric lowering furnace device and method |
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