CN2745959Y - Crystal growing device by biheating temperature gradient method - Google Patents
Crystal growing device by biheating temperature gradient method Download PDFInfo
- Publication number
- CN2745959Y CN2745959Y CN 200420082546 CN200420082546U CN2745959Y CN 2745959 Y CN2745959 Y CN 2745959Y CN 200420082546 CN200420082546 CN 200420082546 CN 200420082546 U CN200420082546 U CN 200420082546U CN 2745959 Y CN2745959 Y CN 2745959Y
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- crucible
- heating
- heater
- molybdenum
- heating element
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Abstract
The design of the utility model relates to a crystal growing device by biheating temperature gradient method, belonging to the field of the crystallization technology, comprising a bell-jar fine vacuum single crystal furnace. Four electrodes, two pairs of electrode plates and a bi-heater are arranged in the bell-jar fine vacuum single crystal furnace; in addition, a double power supply and a double temperature-controlling heating system are arranged in the bell-jar fine vacuum single crystal furnace. The heater is composed of a main heater of the rectangular wave-shaped batten-type graphite barrel and a minor heater of the back taper type heteromorphic batten; an upper heat screen which has good effect in thermal insulation, a lower heat screen and a side shielded device are provided above the main heater and the minor heater, below the main heater and the minor heater and around the main heater and the minor heater; a crystal growing chamber is formed by an obconic copple with seed crystal grooves in the space enclosed by the main heater and the minor heater. The crystal growing device designed by the utility model has good sealed performance and stable thermal field, and the crystal growing device by biheating temperature gradient method is suitable for middle-temperature crystals and high-temperature crystals with large diameters, such as sapphire crystals, yttrium aluminium garnet crystals, yttrium aluminate crystals and calcium-fluoride crystals, etc.
Description
Technical field
The utility model belongs to crystallization processes and learns the field, two heating tgt crystal growth devices specifically, are the single warm area tgt crystal growth devices of two heating, the major diameter refractory oxide crystal that is specially adapted to grow also is applicable to the crystal of other type of growth certainly.
Background technology
Though two heating, two warm areas are added hot many warm areas method growth III-V family's semiconductor crystal and calcium fluoride crystal and are extensively adopted for a long time in the world, as Beijing non-ferrous metal institute, adopt many warm areas method growth GaAs crystal.But two heating in the past, adding heat all is to create two warm areas, many warm areas method is engaged in the thermograde falling crucible method or crucible moves method growing crystal (being the Tammann-Bridgman method), the mobile system of aforesaid method easily causes a temperature unstable, the major diameter high temperature crystal of many components proportioning of especially growing is as the yttrium aluminum garnet (Nd of growth major diameter neodymium-doped
3+: YAG) crystal, except that traditional crystal pulling method, still do not have other crystallization method so far and can succeed.
" a kind of resistant to elevated temperatures tgt crystal growth device " (patent No. 85100534.9) of Zhou Yongzong invention in 1985, successfully to grow diameter be 120 millimeters to the pure static temperature gradient method (being the Tammann method) of the single warm area of the single heating of initiative in the world, the yag crystal (Nd of the 3300 gram high-quality neodymium-dopeds that weigh
3+: YAG), doped titanium titanium gem crystal (Ti
3+: Al
2O
3), sapphire crystal (Al
2O
3).And single heating, single warm area growth fusing point is higher than 1950 ℃ major diameter crystal, and as when crystal diameter during greater than 6 inches, the interior central temperature head that reaches up and down of back taper crucible reaches more than 200～300 ℃.About 2100 ℃ of the softening point temperature of molybdenum product material under carbon containing (C) atmosphere, the excessive crystal growing chamber temperature difference will cause crucible and insulation shielding to damage, can't growing crystal.
The utility model design content
The purpose of this utility model is the shortcoming that overcomes the warm terraced method growing crystal of above-mentioned single heating, and the tgt crystal growth devices of the single warm area of two heating are provided, for the growth melt temperature provides good warm field condition near 2100 ℃ major diameter high temperature crystal.
This solves the technical scheme that its technical problem is taked, design two heating tgt crystal growth devices, comprise bell-jar high vacuum single crystal growing furnace, in establish 4 water-cooled electroplaxs, 2 water-cooled main electrodes, 2 water-cooled auxiliary electrodes, main heating element is slit into the cylinder of the wavy lath power circuit of rectangle for groove about the quilt, and whole cylinder is installed on the battery lead plate that links to each other with the water-cooled main electrode.Because the conduction of heat of the battery lead plate that links to each other with the water-cooled main electrode, in the space, it is poor to produce strong thermograde about crystal growing chamber.Molten the collapsing in order to prevent thermograde difference that major diameter molybdenum crucible upper limb and seed crystal position are excessive, the auxiliary heating element of inverted cone-shaped abnormity is set around below molybdenum crucible, groove is slit into the auxilliary heating element of inverted cone-shaped abnormity lath about the quilt, be installed on the auxiliary electrode plate that links to each other with the water-cooled auxiliary electrode, crucible bottom is heated, reduce the indoor top of crystal growth, middle part, the bottom temperature difference.By two temperature controls raw material is heated, treat that the raw material of growing crystal all melts, behind the temperature balance and stability, by auxilliary heating element temperature controlling system, reduce heating power gradually, until zero heating power, make the interior melt formation temperature gradient difference of crucible of crystal growing chamber, and the beginning solidification and crystallization.After this main heating element temperature controlling system begins cooling, makes the whole solidification and crystallizations of melt in the crucible.
In addition, the auxilliary heating element of this design can also significantly reduce the thermal shocking of thermal convection to the crucible bottom xln, and the major diameter crystal that assurance grows is not easy to crack.
In order to guarantee crystal growing chamber, airtight performance is good, and thermal field is stable, and on major-minor heating element, the below reaches
Be provided with tight heat protection screen shielding apparatus all around.Shielding unit comprises heat shield, last heat shield and side shielding cylinder down.
Compared with prior art, the present invention has following characteristics, two single warm areas of thermal control that add, crystal growing chamber is not disturbed by thermal convection and any transmission system, thermal field stability is good, two heating temperature controlling systems can be created the thermograde that makes progress of enough big intimate linearity, and the major diameter refractory oxide crystal that is particularly suitable for growing is as gem crystal series (Al
2O
3Ti
3+: Al
2O
3CR
3+: Al
2O
3); (YAG is Y to yag crystal series
3Al
5O
12Nd
3+: YAG; Yb
3+: YAG; Ce
3+: YAG) and various adulterated yttrium aluminate (YAlO
3) crystal and CaF
2Crystal.
Description of drawings
Fig. 1 is a sectional structure synoptic diagram of the present utility model.
Among the figure, 1. crucible pole; 2. auxiliary electrode bar; 3. main electrode bar; 4. auxiliary electrode plate; 5. main electrode plate; 6. auxilliary heating element; 7. main heating element; 8. auxilliary temperature-control heat couple; 9. the warm galvanic couple of master control; 10. crucible; 11. seed crystal; 12. crucible locating bar; 13. molybdenum seat; 14. main heating element pressure ring; 15. auxilliary heating element pressure ring; 16. zirconium white insulation seat ring; 17. corundum dead ring; 18. corundum dead ring; 19. corundum dead ring; 20. main electrode nut; 21. auxiliary electrode nut; 22. side shielding cylinder seat board; 23. inner shield tube; 24. side shielding cylinder; 25. heat shield on the internal layer; 26. last heat shield; 27. center production well; 28. following heat shield; 29. stainless steel protection tube; 30. stainless steel stay-warm case; 31. crystal growing chamber; 32. bell-jar high vacuum single crystal growing furnace chassis.
Embodiment
Below in conjunction with drawings and Examples the utility model is described in further detail.
Two heating tgt crystal growth devices as shown in Figure 1 on bell-jar high vacuum single crystal growing furnace chassis 33, are provided with 4 battery lead rods, 2 auxiliary electrode bars, 2 main electrode bars 3.Battery lead rod 2,3 water flowings cooling guarantees that battery lead rod 2,3 contacts with single crystal growing furnace chassis 32 insulated enclosures with airtight circle by resistant to elevated temperatures fluorinated ethylene propylene.
In order to reduce the temperature difference at molybdenum crucible 10 upper ends to seed crystal 11 places, below crucible 10, be provided with the auxilliary heating element 6 of inverted cone shape abnormity lath, auxilliary heating element 6 is pressed on the auxiliary electrode plate 4 of ring-type dovetail groove by auxilliary heating element pressure ring 15, and auxiliary electrode plate 4 is anchored on the water cooled electrode bar 2 by heat-resistance stainless steel nut 21.Auxilliary heating element 6 is by the auxilliary temperature controller control heating and cooling heating schedule that is connected with auxilliary temperature-control heat couple 8.
The main heating element 7 of the wavy strip type graphite tube of rectangle, press on the main electrode plate 5 of ring-type dovetail groove by main heating element pressure ring 14, main electrode plate 5 is anchored on the water cooled electrode bar 3 by heat-resistance stainless steel nut 20, and main heating element 7 has the temperature controller control heating power that is connected with the warm galvanic couple 9 of master control.Corundum dead ring 17 is put in ring groove interior the support-side shielding cylinder and the last heat shield of battery lead plate 5 and the temperature stable effect that keeps is arranged.The ring groove below of battery lead plate 5 is provided with corundum dead ring 19 and plays load-bearing and reduce the gaseous exchange effect.
Graphite tube main heating element 7 has separated n by inscribed angle etc. and has gone up groove and n groove down, and to constitute the wavy lath power circuit of rectangle, the thermograde difference of crystal growing chamber is by the thermal conduction creation of graphite tube main heating element and battery lead plate.Near the temperature seed crystal main leaning on the thermal conduction of crucible pole and the temperature-fall period of auxilliary heating element produces jointly.
Crystal growing chamber is made of the turbination molybdenum matter crucible 10 of band seed slot.Crucible 10 places in the circular groove of crucible locating bar 12 of molybdenum matter, pass zirconium white insulating ring 16 centre holes, place in the groove of molybdenum seat 13, molybdenum seat 13 bottoms have the crucible pole bracket just in time to be enclosed within the top of cold-crucible bar 1, and the crucible locating bar constitutes the passage with certain thermal conduction capability by molybdenum seat and cold-crucible bar.The crucible pole liftable is with the position of suitable adjusting crucible.
In order to keep the stable thermal field of crystal growing chamber, on crucible and heating element, around reaching, the below is provided with the heat protection screen shielding apparatus, and this device comprises heat shield 28, corundum dead ring 18, side shielding cylinder and last heat shield down.
Following heat shield divides 2 groups to constitute by the multilayer molybdenum sheet, is placed on auxiliary electrode plate below, and corundum dead ring 18 is except that playing insulation effect, and main is to reduce the influence of thermal convection to crystal growing chamber.
The side shielding cylinder is set around the heating element, and it is by inner shield tube 23, and side shielding cylinder 24 and stainless steel protection tube 29 constitute.Stainless steel protection tube bottom outward flange is anchored on side shielding cylinder seat board 22 by screw.Fixation side shielding cylinder device is so that lifting is moved.
Last heat shield places crystal growing chamber and main heating element top, mainly is made of center production well 27, it is characterized in that with the immediate internal layer of heating element on heat shield 25 for having certain thickness molybdenum plate or tungsten plate, to prevent softening transform.Last heat shield 26 divides 5～7 groups to constitute by the multilayer molybdenum sheet, above stainless steel protection tube 29 and last heat shield 26 a stainless steel stay-warm case 30 is arranged, with the gaseous exchange inside and outside the minimizing shielding unit.Production well 27 is used to drain the indoor volatile foreign-matter contamination of crystal growth.
Said apparatus is in the bell-jar high vacuum single crystal growing furnace of general growing crystal, regulate by two heating temperature controls, can create the thermograde that makes progress that enough is close to linearity that surpasses more than 300 ℃, the thermal field good stability, the dystectic gem-quality crystal of major diameter is suitable for growing.The crucible that the raw material that will be used to grow (crystal block material or powder compact material) is put into the growth room installs stove; the heating edge exhaust of pumping high vacuum back meets the requirements of vacuum tightness; charge into inert protective gas; be warming up to the fixed temperature material by two heating temperature controllers again; after treating that thermal field is fully stable; lower the temperature by set cooling process by auxilliary temperature controller earlier, create enough being close to the linear thermograde that makes progress, and make the seed crystal position begin solidification and crystallization.After this finish whole single crystal growing by main temperature controller voluntarily by set cooling process.
Claims (7)
1. two heating tgt crystal growth devices, be included on the bell-jar high vacuum single crystal growing furnace chassis (33), 4 battery lead rods are set, 2 auxiliary electrode bars (2), 2 main electrode bars (3), it is characterized in that described two heating is to be made of the main generating body (7) of the wavy strip type graphite tube of rectangle and the auxilliary heating element (6) of inverted cone-shaped abnormity lath power circuit, in the space that major-minor heating element surrounds, constitute crystal growing chamber by the turbination crucible (10) that has seed slot, on the major-minor heating element, around the below reaches the heat protection screen shielding apparatus is set.
2. according to claims 1 described two heating tgt crystal growth devices, it is characterized in that: described two heating tgt crystal growth devices have 4 battery lead rods, and battery lead rod is made of the red copper bar or the stainless steel that can lead to water coolant.
3. according to the described two heating tgt crystal growth devices of claims 1, it is characterized in that: described graphite tube main heating element by inscribed angle etc. separated n go up groove and n down groove to constitute wavy lath power circuit.
4. according to claims 1 described two heating tgt crystal growth devices, it is characterized in that: the crucible below of described crystal growing chamber, the auxilliary heating element of inverted cone-shaped abnormity graphite product is set, auxilliary heating element by inscribed angle etc. separated n go up groove and n down groove to constitute inverted cone-shaped abnormity lath power circuit.
5. according to claims 1 described two heating tgt crystal growth devices, it is characterized in that: the bottom of the tapered bottom of described molybdenum crucible has seed slot, and the tapered bottom of crucible is less than 120 °, and the best is 95 °-110 °, the gradient of sidewall of crucible is greater than 1: 100, and the best is 1: 30-1: 40.Crucible can adopt pure molybdenum or miramint material.
6. according to claims 1 described two heating tgt crystal growth devices, it is characterized in that: described heat protection screen shielding apparatus, contain side shielding cylinder (23) (24); Last heat shield (25) (26) and following heat shield (28).The internal layer of the inner shield tube (23) of described side shielding cylinder is lined with the molybdenum tube of tungsten sheet; described side shielding cylinder outermost layer is stainless steel protection tube (29); described going up in the heat shield; with heat shield (25) on the immediate internal layer of main heating element for having certain thickness molybdenum plate or tungsten plate, there is a stainless steel stay-warm case top of last heat shield (26).
7. according to claims 1 described two heating tgt crystal growth devices, it is characterized in that: described crystal growing chamber is made of the turbination molybdenum matter crucible (10) of band seed slot, crucible (10) places in the circular groove of crucible locating bar (12) of molybdenum matter, pass zirconium white insulating ring (16) centre hole, place in the groove of molybdenum seat (13), molybdenum seat (13) bottom has the crucible pole bracket just in time to be enclosed within the top of cold-crucible bar (1), and the crucible locating bar constitutes the passage with certain thermal conduction capability by molybdenum seat and cold-crucible bar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200420082546 CN2745959Y (en) | 2004-09-06 | 2004-09-06 | Crystal growing device by biheating temperature gradient method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200420082546 CN2745959Y (en) | 2004-09-06 | 2004-09-06 | Crystal growing device by biheating temperature gradient method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2745959Y true CN2745959Y (en) | 2005-12-14 |
Family
ID=35582542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200420082546 Expired - Fee Related CN2745959Y (en) | 2004-09-06 | 2004-09-06 | Crystal growing device by biheating temperature gradient method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2745959Y (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100400720C (en) * | 2006-04-21 | 2008-07-09 | 罗建国 | Precise vertical temperature-difference gradient condensation single crystal growth device and method thereof |
| WO2008080304A1 (en) * | 2006-12-29 | 2008-07-10 | Jiaxing University | Crystal producing system containing multiple crucibles used in temperature gradient method |
| CN100547124C (en) * | 2007-10-31 | 2009-10-07 | 中国科学院上海光学精密机械研究所 | The growth method of carbon-doped sapphire crystal |
| CN102212871A (en) * | 2011-05-23 | 2011-10-12 | 无锡斯达新能源科技有限公司 | Growth method for sapphire crystals and crystal growth furnace structure for growing sapphire crystals |
| CN103243378A (en) * | 2012-02-09 | 2013-08-14 | 洛阳金诺机械工程有限公司 | Multilayer-sleeve-formed temperature gradient control structure for crystal growth and method thereof |
| CN103757708A (en) * | 2014-01-17 | 2014-04-30 | 中国科学院福建物质结构研究所 | High temperature inorganic scintillation crystal growth crucible |
| CN103757702A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院福建物质结构研究所 | Method for preparing high-temperature inorganic scintillation crystal |
| CN109338461A (en) * | 2018-12-18 | 2019-02-15 | 北方民族大学 | The auxiliary heating means and device and single crystal growing furnace of induction heating monocrystalline growth with czochralski |
| CN110484968A (en) * | 2019-09-30 | 2019-11-22 | 山西中科晶电信息材料有限公司 | A kind of crystal growing furnace being provided with furnace body elevating mechanism |
-
2004
- 2004-09-06 CN CN 200420082546 patent/CN2745959Y/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100400720C (en) * | 2006-04-21 | 2008-07-09 | 罗建国 | Precise vertical temperature-difference gradient condensation single crystal growth device and method thereof |
| WO2008080304A1 (en) * | 2006-12-29 | 2008-07-10 | Jiaxing University | Crystal producing system containing multiple crucibles used in temperature gradient method |
| CN100422393C (en) * | 2006-12-29 | 2008-10-01 | 嘉兴学院 | Temperature gradient method rotary multiple crucible crystal growth system |
| CN100547124C (en) * | 2007-10-31 | 2009-10-07 | 中国科学院上海光学精密机械研究所 | The growth method of carbon-doped sapphire crystal |
| CN102212871A (en) * | 2011-05-23 | 2011-10-12 | 无锡斯达新能源科技有限公司 | Growth method for sapphire crystals and crystal growth furnace structure for growing sapphire crystals |
| CN103243378A (en) * | 2012-02-09 | 2013-08-14 | 洛阳金诺机械工程有限公司 | Multilayer-sleeve-formed temperature gradient control structure for crystal growth and method thereof |
| CN103243378B (en) * | 2012-02-09 | 2016-12-14 | 洛阳金诺机械工程有限公司 | Thermograde control structure and method that multilamellar sleeve formed is utilized during crystal growth |
| CN103757708A (en) * | 2014-01-17 | 2014-04-30 | 中国科学院福建物质结构研究所 | High temperature inorganic scintillation crystal growth crucible |
| CN103757702A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院福建物质结构研究所 | Method for preparing high-temperature inorganic scintillation crystal |
| CN109338461A (en) * | 2018-12-18 | 2019-02-15 | 北方民族大学 | The auxiliary heating means and device and single crystal growing furnace of induction heating monocrystalline growth with czochralski |
| CN110484968A (en) * | 2019-09-30 | 2019-11-22 | 山西中科晶电信息材料有限公司 | A kind of crystal growing furnace being provided with furnace body elevating mechanism |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |