CN201224776Y - Multi-element compound infrared crystal growth apparatus - Google Patents

Multi-element compound infrared crystal growth apparatus Download PDF

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Publication number
CN201224776Y
CN201224776Y CNU2008200259957U CN200820025995U CN201224776Y CN 201224776 Y CN201224776 Y CN 201224776Y CN U2008200259957 U CNU2008200259957 U CN U2008200259957U CN 200820025995 U CN200820025995 U CN 200820025995U CN 201224776 Y CN201224776 Y CN 201224776Y
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China
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temperature
zone
crystal growth
growth apparatus
temperature zone
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Expired - Fee Related
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CNU2008200259957U
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Chinese (zh)
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王善朋
陶绪堂
蒋民华
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Shandong University
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Shandong University
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Abstract

The utility model provides a grower of multi-compound infrared crystal comprising a furnace body; the hearth inside the furnace body comprises an upper high-temperature zone, a middle temperature gradient zone and a lower low-temperature zone; a heater with independent temperature control is arranged at the upper high-temperature zone and the lower low-temperature zone respectively; a temperature control thermoelectric couple is arranged at the upper high-temperature zone and the lower low-temperature zone; the middle temperature gradient zone is a heat insulation and fire-resistant layer with ventholes; a supporting bar is positioned inside the hearth; the lower end of the supporting bar is connected with a rotating coupling; the rotating coupling is connected with an electric motor; the electric motor is arranged at a spiral travel mechanism. The utility model can easily adjust the temperature of temperature control of the high-temperature zone and low-temperature zone according to the growth habit of different compound infrared crystals, so a temperature field for meeting the growth of crystal can be obtained, and the stability of solid-liquid interface can be maintained, and the flat interface growth of crystal can be achieved. With the grower, a multi-compound infrared crystal with integrated appearance and good crystallization performance can be prepared by adopting the Bridgman method.

Description

Multicomponent compounds infrared crystal growth apparatus
Technical field
The utility model relates to a kind of growing apparatus of multicomponent compound infrared crystal, belongs 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 utility model provides 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 at the deficiency that existing multicomponent compound infrared crystal growing technology exists.
Multicomponent compounds infrared crystal growth apparatus of the present utility model 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 support bar 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 head box, is used for closed furnace.
The bottom of burner hearth is provided with heat insulation loop, to prevent that heat is to the atmosphere transmission.
Support bar inside is placed with temperature thermocouple, is used for measuring in real time the temperature of crucible tip.
Multicomponent compounds infrared crystal growth apparatus of the present utility model, 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 the outer crystal growth of different compound of red, 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
Accompanying drawing is the structural representation of multicomponent compounds infrared crystal growth apparatus of the present utility model.
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 utility model 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.
The utility model 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 the outer crystal growth of different compound of red, keep the stability of solid-liquid interface 17 in the plumbago crucible 3, realize the crystalline plane interface growth.

Claims (8)

1. multicomponent compounds infrared crystal growth apparatus, comprise body of heater, it is characterized in that: 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 support bar 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 head box.
6. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: the bottom of described burner hearth is provided with heat insulation loop.
7. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: described support bar inside is placed with temperature thermocouple.
8. multicomponent compounds infrared crystal growth apparatus according to claim 1 is characterized in that: described support bar is connected with motor by the rotation dop.
CNU2008200259957U 2008-07-24 2008-07-24 Multi-element compound infrared crystal growth apparatus Expired - Fee Related CN201224776Y (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102168305A (en) * 2011-04-02 2011-08-31 山东大学 Synthesis method of phosphorus-silicon-cadmium polycrystal material
CN104073872A (en) * 2014-06-26 2014-10-01 大庆佳昌晶能信息材料有限公司 Process for growing high-quality compound semiconductor single crystal by means of rotation-vertical gradient freeze (R-VGF) method
CN104651924A (en) * 2015-03-09 2015-05-27 中国工程物理研究院化工材料研究所 Tubular growth furnace
CN105220222A (en) * 2014-06-03 2016-01-06 长春理工大学 The crystal growing apparatus of multiple hot cell 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
CN109161972A (en) * 2018-11-14 2019-01-08 中国工程物理研究院激光聚变研究中心 Crystal growing ampoule apparatus for adjusting position and system
CN112827463A (en) * 2021-03-19 2021-05-25 深圳市一正科技有限公司 Continuous flow reaction system

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102168305A (en) * 2011-04-02 2011-08-31 山东大学 Synthesis method of phosphorus-silicon-cadmium polycrystal material
CN102168305B (en) * 2011-04-02 2012-06-27 山东大学 Synthesis method of phosphorus-silicon-cadmium polycrystal material
CN105220222A (en) * 2014-06-03 2016-01-06 长春理工大学 The crystal growing apparatus of multiple hot cell and method
CN104073872A (en) * 2014-06-26 2014-10-01 大庆佳昌晶能信息材料有限公司 Process for growing high-quality compound semiconductor single crystal by means of rotation-vertical gradient freeze (R-VGF) method
CN104651924A (en) * 2015-03-09 2015-05-27 中国工程物理研究院化工材料研究所 Tubular growth furnace
CN104651924B (en) * 2015-03-09 2017-06-06 中国工程物理研究院化工材料研究所 Tubular type growth furnace
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
CN109161972A (en) * 2018-11-14 2019-01-08 中国工程物理研究院激光聚变研究中心 Crystal growing ampoule apparatus for adjusting position and system
CN112827463A (en) * 2021-03-19 2021-05-25 深圳市一正科技有限公司 Continuous flow reaction system

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Granted publication date: 20090422

Termination date: 20100724