CN2680686Y - Thermostable crystal annealing apparatus - Google Patents
Thermostable crystal annealing apparatus Download PDFInfo
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- CN2680686Y CN2680686Y CN 200420020209 CN200420020209U CN2680686Y CN 2680686 Y CN2680686 Y CN 2680686Y CN 200420020209 CN200420020209 CN 200420020209 CN 200420020209 U CN200420020209 U CN 200420020209U CN 2680686 Y CN2680686 Y CN 2680686Y
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- molybdenum
- crystal annealing
- elevated temperatures
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- crystal
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Abstract
The utility model relates to a thermostable crystal annealing apparatus, belonging to a crystal heat-treatment field, comprising a bell jar which is provided with a water inlet and a water outlet and is contacted with a chassis by a vacuum seal ring in manner of sea ling, and the bell jar is arranged on the chassis having vacuum vents. A thermal-insulation shielding system which comprises a side shielded barrel, an upper heat shield and a lower heat shield is arranged in a bell-jar body, and a charge valve and a gas outlet valve are arranged on the bell-jar body; a heater arranged on two sides of the side shielded barrel in the innermost layer is made of tungsten rods, and the heater is tightly fixed on a molybdenum electrode board by an electrode contact; the molybdenum electrode board is supported by an adamantine-spar insulating-ring bracing frame, and two ends are tightly fixed on a water cooled electrode pole; a crystal annealing chamber is arranged in the space enclosed by the heater above the molybdenum electrode board, and an insulating board is arranged on the inner side of the adamantine-spar insulating-ring bracing frame below the molybdenum electrode board. The utility model can substantially raise the quality-factor FOM values of the gem laser crystal mixed with titanium and can improve the optical quality of the thermostable oxide crystal.
Description
Technical field
The utility model belongs to crystalline thermal treatment field, relates to a kind of annealing device of high-temp oxide crystal, specifically, is a kind of resistant to elevated temperatures crystal annealing device.
Background technology
Along with science and technology development, manually breed the crystalline kind and constantly bring forth new ideas, the crystal of breeding by melt, because of the solid-liquid interface gradient temperature difference is bigger, the crystal of being bred, the one, thermal stresses is big, and crystal element making processes ftractures easily; The 2nd, some crystal structure integrity is relatively poor.The patent No. is: the utility model patent of ZL85100534.9 provides " a kind of resistant to elevated temperatures tgt crystal growth device ", it utilizes guiding temperature gradient method, and (be called for short: warm terraced method) growth mixes the titanium jewel, the crystal such as sapphire that thread light path is arranged, but must be through temperature recrystallization The high temperature anneal more than 1850 ℃, could improve the quality factor FOM value of mixing titanium jewel tunable laser crystal, and have the crystal of thread light path in the elimination sapphire crystal, make it become crystalline perfection, the gem-quality crystal that optical homogeneity is all excellent.
And the high temperature annealing method that in the past adopted is the High Temperature Furnaces Heating Apparatus that constitutes with molybdenum disilicide rod heating unit, and its limit Heating temperature is no more than 1750 ℃, and the hydrogen furnace Heating temperature also can only reach 1800 ℃.The graphite high-temperature annealing furnace that Suzhou Crystal Component Factory makes only is adapted to industrial jewel crystal thermal stresses anneal.The Frequency Induction Heating annealing furnace of Cai Yonging in the world, though induction heating temperature can reach more than 2000 ℃, its heating power is big, and the volume of crystal annealing chamber is little, and induction heating temperature is inhomogeneous, the crystal annealing poor effect.
The utility model content
For overcoming the deficiency of crystal high-temperature annealing furnace in the prior art, the utility model provides a kind of high temperature crystal that helps, the particularly annealing device of oxide crystal recrystallization, promptly a kind of resistant to elevated temperatures crystal annealing device.This annealing device adopts high vacuum degasification seal form, is provided with inflation inlet and air outlet, and the utmost point is suitable for crystal is carried out the high temperature annealing of circulated gases.Adopt the tungsten bar Heating element and the shielding heat-proof device of special methods processing and fabricating, treat that its temperature of annealed crystal watch-keeping cubicle can be up to more than 2000 ℃, and temperature is even, temperature is stable.
The technical scheme that its technical problem that solves the utility model adopts: a kind of resistant to elevated temperatures crystal annealing device, comprise and placing on the chassis that has vaccum exhaust outlet, and contact by the sealing of vaccum seal ring and chassis and to be respectively equipped with water-in and water outlet and barometric bell jar, be provided with the heat protection screen shielding apparatus that comprises the side shielding cylinder, goes up heat shield and following heat shield in the described bell body, its substantive distinguishing features is: also be provided with inflation valve and air outlet valve on the described bell body; The heating element that is arranged at innermost layer side shielding cylinder both sides adopts tungsten bar to be processed into, and described heating element is anchored on the molybdenum electrode plate by the molybdenum nut by the molybdenum electrode joint; Described molybdenum electrode plate is supported by corundum dead ring bracing frame, and its two ends are anchored on the water cooled electrode bar by high temperature steel gasket ring and high temperature steel nut; In the space that heating element surrounded, described molybdenum electrode plate top, be provided with a crystal annealing chamber; The below of described molybdenum electrode plate, the inboard of corundum dead ring bracing frame is provided with a thermal baffle.
Compared with prior art, the utlity model has following beneficial effect: after the resistant to elevated temperatures crystal annealing device anneal of the utility model, the quality factor FOM value of mixing titanium jewel tunable laser crystal improves greatly, the crystal optics quality also is greatly improved, and the titanium gem crystal blank of mixing that can not directly use originally that makes that warm terraced method grows out becomes high-quality and mixes titanium jewel tunable laser crystal.To the sapphire crystal blank decarbonization colour-removing of the terraced method growth of temperature, and the thread light path in the elimination crystal, effect is splendid.The transmitance of sapphire crystal, optical homogeneity and crystalline perfection all improve greatly, and make some original out of usely have thread light path crystal to become gem-quality crystal.This device can be used for the full annealed of various high temperature crystal, is specially adapted to various adulterated yttrium aluminum garnets, pure yttrium aluminum garnet, and sapphire is mixed the full annealed of high temperature oxide crystals such as titanium jewel.
Description of drawings
Fig. 1 is a sectional structure synoptic diagram of the present utility model.
Among the figure, 1. vaccum exhaust outlet; 2. chassis; 3. inflation valve; 4. baro-vacuum gauge; 5. bell jar; 6. water outlet; 7. corundum dead ring bracing frame; 8. two water cooled electrode bars; 9. thermal baffle; 10. high temperature steel gasket ring; 11. high temperature steel nut; 12. corundum insulation seat ring 13. corundum bench insulators; 14. tungsten comes thermopair; 15. molybdenum backing plate; 16. treat annealed crystal; 17. heat is thermostatic tube evenly; 18. heating element; 19. venting hole; 20. stainless steel stay-warm case; 21. last heat shield; 22. heat shield on the innermost layer; 23. stainless steel heat-preservation cylinder; 24. innermost layer side shielding cylinder; 25. zirconium white bracket; 26. side shielding cylinder base plate; 27. molybdenum electrode joint; 28. molybdenum electrode plate; 29. molybdenum nut; 30. following heat shield; 31. water-in; 32. air outlet valve; 33. crystal annealing chamber; 34. side shielding cylinder.
Embodiment
Below in conjunction with drawings and Examples the utility model is described in further detail.
A kind of resistant to elevated temperatures crystal annealing device as shown in Figure 1, comprise and placing on the chassis 2 that has vaccum exhaust outlet 1, and contact the bell jar 5 that is respectively equipped with water-in 31 and water outlet 6 and baro-vacuum gauge 4 by 2 sealings of vaccum seal ring and chassis, be provided with the heat protection screen shielding apparatus that comprises side shielding cylinder 34, goes up heat shield 21 and following heat shield 30 in described bell jar 5 bodies, its principal character is: also be provided with inflation valve 3 and air outlet valve 32 on the described bell body 5; The heating element 18 that is arranged at innermost layer side shielding cylinder 24 both sides adopts tungsten bar to be processed into, and described heating element 18 is anchored on two blocks of molybdenum electrode plates 28 by molybdenum nut 29 by molybdenum electrode joint 27; Described two blocks of molybdenum electrode plates 28 are supported by corundum dead ring bracing frame 7, and its two ends are anchored on the water cooled electrode bar 8 by high temperature steel gasket ring 10 and high temperature steel nut 11; In the space that described molybdenum electrode plate 28 top heating elements 18 are surrounded, be provided with a crystal annealing chamber 33; The below of described molybdenum electrode plate 28, the inboard of corundum dead ring bracing frame 7 is provided with a thermal baffle 9.
Resistant to elevated temperatures crystal annealing device described in the utility model is commonly referred to bell-jar resistance high-temperature annealing furnace.
For the vacuum-sealing that reaches a high temperature down, the double-layer stainless steel structure of logical recirculated water is adopted on bell jar 5 and chassis 2.Battery lead rod 8 water flowings cooling guarantees that battery lead rod 8 contacts with chassis 2 insulated enclosures with sealing-ring by resistant to elevated temperatures fluorinated ethylene propylene.
For fear of annealing device parts high temperature oxidation, treat that annealed crystal 16 puts into crystal annealing chamber 33, stove sealing back is vented to high vacuum (usually above 5 * 10 by the vacuum unit earlier
-3Pa), the different needs according to treating annealed crystal 16 can adopt to vacuumize annealing, gas-flow closure annealing, and annealing way such as the through-flow body annealing of taking offence, the inflation heating step is decided according to different demands.
Carry out circulated gases annealing in order to treat annealed crystal 16, carry out special oxide crystal annealing operation (as: the flowing hydrogen annealing of titanium jewel), bell jar 5 is provided with inflation valve 3 and air outlet valve 32.
In order to reach special heat (greater than 2000 ℃), not only non-volatile but also not loss of Heating element, and not with the high-temperature hydrogen reaction, adopt the tungsten bar heating element 18 of special processing and fabricating, be fixed on the molybdenum electrode plate 28 by molybdenum nut 29 by molybdenum electrode joint 27.
For fear for the treatment of that annealed crystal 16 conducts because of local heating and the thermal radiation influence is ftractureed, treat annealed crystal 16 and the hot evenly thermostatic tubes 17 of heating element 18 middle placements.Treat that annealed crystal 16 does not contact with the even thermostatic tube 17 of heat, make and treat to obtain even thermal conduction and thermal radiation heating around the annealed crystal, reach stable elevation temperature annealing process.
Zirconium white is from conduction when temperature is higher than 1800 ℃, placement corundum bench insulator 13 between zirconium white bracket 25 and battery lead plate 28.
For the temperature of energy micrometric measurement and control crystal annealing chamber 33,33 belows, crystal annealing chamber are provided with W-Re (WRe3-WRe25) thermopair 14 outside the chassis 2 that extends to bell jar 5.The whole process of whole cycle of annealing is finished by precision meter is program control.
Temperature is even all around in order to make crystal annealing chamber 33, thermal field is stable, around heating element 18 and crystal annealing chamber 33, be provided with tight heat protection screen shielding apparatus, shielding unit comprises the corundum thermal baffle 9 of battery lead plate 28 belows, following heat shield 30, last heat shield 21 and side shielding cylinder 34, last heat shield 21 and side shielding cylinder 34 guarantee at high temperature not melt, indeformable.
The resistant to elevated temperatures crystal annealing device of the utility model shown in Figure 1, its bell jar 5 adopts the double-layer stainless steel structure, and during for fear of high temperature annealing, furnace wall sealing place and burner hearth burn out, and are provided with water-in 31, water outlet 6 logical recirculated water coolings.Consider that some crystal must carry out the high temperature full annealed in flowing gas, therefore, burner hearth also has inflation valve 3, air outlet valve 32, baro-vacuum gauge 4.
Heating element 18 adopts that tungsten bar is special to be processed into, and is anchored on the molybdenum electrode plate 28 by molybdenum nut 29 by molybdenum electrode joint 27.The space size of crystal annealing chamber 33 according to the bell jar stove and treat anneal crystal 16 volume and decide.Two blocks of molybdenum electrode plates 28 are supported by corundum dead ring bracing frame 7, its two ends are anchored on the battery lead rod 8 by high temperature steel gasket ring 10 and high temperature steel nut 11, battery lead rod 8 is made of the red copper bar or the stainless steel of logical recirculated water cooling, battery lead rod 8 is no more than 100 ℃ Celsius with the temperature that contacts on chassis 2, guarantees that battery lead rod 8 contacts with the absolute seal on chassis 2.The below of battery lead plate 28, a corundum thermal baffle 9 is placed in the inboard of corundum dead ring bracing frame 7, to reduce the thermal radiation and the thermal conduction of 33 belows, crystal annealing chamber.
In the crystal annealing chamber 33, the central authorities on two electrode plate 28 are provided with corundum bench insulator 13, place zirconium white bracket 25 on the corundum bench insulator 13, avoid zirconium white bracket 25 high-temperature electric conductions, heat conduction.Zirconium white bracket 25 tops are provided with molybdenum backing plate 15 (or tungsten backing plate) and thermal balance thermostatic tube 17 (molybdenum or tungsten).Treat that annealed crystal 16 places on the molybdenum backing plate 15 and is positioned at the middle position of thermal balance thermostatic tube 17 for one or many.In order to prevent to treat that annealed crystal 16 local heatings are inhomogeneous and ftracture, treat that annealed crystal 16 must not contact with thermal balance thermostatic tube 17, its distance is advisable greater than 3 millimeters.For the ease of accurate precise temperature measurement, temperature control and accurate program control operation are carried out automatic crystal annealing heating and cooling program, are equipped with the Wolfram rhenium heat electric couple 14 that extends to outside the bell jar stove below treating annealed crystal 16.
For the thermal field that keeps crystal annealing chamber 33 is stablized, temperature is even, is provided with tight heat protection screen shielding apparatus around crystal annealing chamber 33, and this heat protection screen shielding apparatus comprises thermal baffle 9, following heat shield 30, side shielding cylinder 34 and last heat shield 21 and corundum insulation seat ring 12.
Following heat shield 30 is made up of several layers of (for example 10-22 layer) molybdenum sheet, is placed on the below of corundum thermal baffle 9, and the inboard of corundum dead ring bracing frame 7 further stops to come thermal conduction and thermodiffusion to 33 belows, crystal annealing chamber.
Be provided with side shielding cylinder 34 around heating element 18, it is by inner shield tube 24, and side shielding cylinder 34 and stainless steel protection tube 23 are formed.Innermost layer side shielding cylinder 24 both can be individual layer molybdenum tube also internal layer molybdenum tube of being lined with the tungsten sheet form, need and durable life requirements determines according to the art breading for the treatment of annealed crystal 16.Side shielding cylinder 34 is made of the co-axial molybdenum tube of multilayer, both can put the wave parting bead of molybdenum matter between molybdenum tube and the molybdenum tube into, also can adopt molybdenum filament serial connection fixedly to make and equally spacedly between each molybdenum tube guarantee the temperature field symmetrically.The skin of side shielding cylinder 34 is stainless steel protection tubes 23, by screw the stainless steel heat-preservation cylinder is fixed on the base plate 26, is beneficial to the installation of shielding unit, is supported on the corundum insulation seat ring 12, and this base plate 26 is processed into by individual layer or double-deck molybdenum plate.Innermost layer side shielding cylinder 24 is located by interior positioned centrally screw, and side shielding cylinder 34 is located by outer dog screw.
Last heat shield 21 places the top of crystal annealing chamber 33 and heating element 18, mainly be made of the molybdenum sheet that has central row pore 19, heat shield 22 is 1.5-3 millimeter molybdenum plate (or tungsten plate) on its innermost layer, can guarantee that long-time high temperature annealing does not melt, indeformable, durable in use.A stainless steel stay-warm case 20 is being arranged with the gaseous exchange inside and outside the minimizing shielding unit above stainless steel protection tube 23 and the last heat shield 21.
Claims (15)
1, a kind of resistant to elevated temperatures crystal annealing device, comprise and placing on the chassis that has vaccum exhaust outlet, and contact by the sealing of vaccum seal ring and chassis and to be respectively equipped with water-in and water outlet and barometric bell jar, be provided with the heat protection screen shielding apparatus that comprises the side shielding cylinder, goes up heat shield and following heat shield in the described bell body, it is characterized in that: also be provided with inflation valve and air outlet valve on the described bell body; The heating element that is arranged at innermost layer side shielding cylinder both sides adopts tungsten bar to be processed into, and described heating element is anchored on the molybdenum electrode plate by the molybdenum nut by the molybdenum electrode joint; Described molybdenum electrode plate is supported by corundum dead ring bracing frame, and its two ends are anchored on the water cooled electrode bar by high temperature steel gasket ring and high temperature steel nut; In the space that heating element surrounded, described molybdenum electrode plate top, be provided with a crystal annealing chamber; The below of described molybdenum electrode plate, the inboard of corundum dead ring bracing frame is provided with a thermal baffle.
2, according to the described resistant to elevated temperatures crystal annealing device of claim 1, it is characterized in that: described heating element adopts molybdenum bar to be processed into.
3, according to claim 1 or 2 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: described heating element adopts tungsten thorium rod to be processed into.
4, resistant to elevated temperatures crystal annealing device according to claim 1 is characterized in that: described battery lead rod is made by the red copper bar or the stainless steel that can lead to recirculated cooling water.
5, according to the described resistant to elevated temperatures crystal annealing device of claim 1, it is characterized in that: described crystal annealing chamber comprises and is positioned at two battery lead rod central authorities tops and places corundum bench insulator on the molybdenum electrode plate, be arranged at zirconium white bracket on the corundum bench insulator, be arranged at evenly thermostatic tube of backing plate on the zirconium white bracket and heat.
6, according to claim 1 or 5 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: described crystal annealing chamber also comprises to be arranged at treats that the annealed crystal below extends to the outer Wolfram rhenium heat electric couple of bell jar stove.
7, according to the described resistant to elevated temperatures crystal annealing device of claim 5, it is characterized in that: backing plate that described crystal annealing is indoor and heat evenly thermostatic tube can be made by molybdenum or tungsten material.
8, according to the described resistant to elevated temperatures crystal annealing device of claim 1, it is characterized in that: the innermost layer shielding cylinder of described side shielding cylinder adopts individual layer molybdenum sheet structure; The outermost layer of described side shielding cylinder is the stainless steel protection tube; Described going up in the heat shield with the immediate the first layer baffle plate of heating element is molybdenum plate or tungsten plate.
9, according to claim 1 or 8 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: the innermost layer shielding cylinder of described side shielding cylinder adopts internal layer to be lined with the molybdenum barrel structure of tungsten sheet.
10, described according to Claim 8 resistant to elevated temperatures crystal annealing device is characterized in that: the top of described stainless steel protection tube and last heat shield is provided with a stainless steel stay-warm case.
11, according to the described resistant to elevated temperatures crystal annealing device of claim 1, it is characterized in that: described thermal baffle is the corundum plate.
12, according to claim 1 or 11 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: described thermal baffle is a hollow ball corundum plate.
13, according to claim 1 or 11 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: described thermal baffle is the zirconium white plate of grain pattern.
14, according to claim 1 or 11 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: described thermal baffle is the heatproof ceramic plate.
15, according to claim 1 or 11 described resistant to elevated temperatures crystal annealing devices, it is characterized in that: described thermal baffle is molybdenum plate or tungsten plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200420020209 CN2680686Y (en) | 2004-02-17 | 2004-02-17 | Thermostable crystal annealing apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200420020209 CN2680686Y (en) | 2004-02-17 | 2004-02-17 | Thermostable crystal annealing apparatus |
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| Publication Number | Publication Date |
|---|---|
| CN2680686Y true CN2680686Y (en) | 2005-02-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200420020209 Expired - Fee Related CN2680686Y (en) | 2004-02-17 | 2004-02-17 | Thermostable crystal annealing apparatus |
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| CN (1) | CN2680686Y (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321922A (en) * | 2011-10-09 | 2012-01-18 | 广州市晶蓝灯饰有限公司 | Protective screen for water cooled electrode of resistance high-temperature vacuum furnace |
| CN102404884A (en) * | 2011-10-09 | 2012-04-04 | 广州市晶蓝灯饰有限公司 | Transitional connection method for heating rod and water cooling electrode of crystal growing furnace |
| CN103409794A (en) * | 2013-08-16 | 2013-11-27 | 哈尔滨工业大学 | Sapphire single-crystal resistor growth furnace |
| CN105603534A (en) * | 2016-02-26 | 2016-05-25 | 吕远芳 | Germanium crystal stress elimination method |
-
2004
- 2004-02-17 CN CN 200420020209 patent/CN2680686Y/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321922A (en) * | 2011-10-09 | 2012-01-18 | 广州市晶蓝灯饰有限公司 | Protective screen for water cooled electrode of resistance high-temperature vacuum furnace |
| CN102404884A (en) * | 2011-10-09 | 2012-04-04 | 广州市晶蓝灯饰有限公司 | Transitional connection method for heating rod and water cooling electrode of crystal growing furnace |
| CN103409794A (en) * | 2013-08-16 | 2013-11-27 | 哈尔滨工业大学 | Sapphire single-crystal resistor growth furnace |
| CN105603534A (en) * | 2016-02-26 | 2016-05-25 | 吕远芳 | Germanium crystal stress elimination method |
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| 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 |