CN2400459Y - High temp. oxide crystal growth furnace - Google Patents
High temp. oxide crystal growth furnace Download PDFInfo
- Publication number
- CN2400459Y CN2400459Y CN 99252128 CN99252128U CN2400459Y CN 2400459 Y CN2400459 Y CN 2400459Y CN 99252128 CN99252128 CN 99252128 CN 99252128 U CN99252128 U CN 99252128U CN 2400459 Y CN2400459 Y CN 2400459Y
- Authority
- CN
- China
- Prior art keywords
- crucible
- melt
- bonnet
- growth furnace
- melt crucible
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model relates to a growth furnace for high temperature oxide crystals. The utility model is mainly suitable for high temperature oxide crystals, such as YVO4 and Nd: YNV4, which grow in a crystal pulling method. The utility model comprises a fusant crucible which is arranged in the central position of a furnace mantle and is used for being filled with fusant, wherein, a gap layer, a crucible-shaped or cylindrical heat carrier, an insulating layer and an induction heating coil are orderly arranged between the fusant crucible and the furnace mantle. The induction heating coil inducts the heat carrier through the insulating layer, and the heat carrier irradiates heat quantity to the fusant crucible in order to cause fusant temperature inside the fusant crucible to slowly and uniformly rise. The temperature gradient formed in a thermal field is small, and thereby, the crystals with large size and good quality can be cultivated.
Description
The utility model relates to employing Czochralski grown large size high-quality high-temp oxide crystal, as vanadic acid yttrium (YVO
4) and Nd-doped yttrium vanadate (Nd:YVO
4) a kind of growth furnace of high-temp oxide crystal of crystal etc.
Prior art:
Chinese Academy of Sciences's Fujian structure of matter in 1994 Li Gansheng (Gansheng Li), Guo Xibin (Xibin Guo), execute natural pearls (Zhenzhu Shi) and woods refined (Bin Lin) (The InternationalChina Fiber-com ' 94 in Shanghai China in the international optical-fibre communications academic conference of Chinese Shanghai, May 15-18th, 1994), with the grow high-quality YVO of successful Φ 25 * 50mm of the used growth furnace of crystal pulling method
4Crystal impels this crystal to reach practicability and industrialization.At present, YVO
4And Nd:YVO
4Crystalline industrialization growing technology is the growth furnace of crystal pulling method and (consults the artificial lens journal, the 28th volume, the 1st phase (1999) 27), still, along with the fast development that laser technology is used and optical fiber technology is used, more and more higher to this crystalline quality and dimensional requirement.Above-mentioned mention is generally adopted radio frequency (intermediate frequency or high frequency) induction heating iridium crucible with the growth furnace of crystal pulling method, and iridium crucible is a container of putting material, is again heating element, has bigger temperature ladder, and this will cause 2 kinds of consequences: on the one hand, because YVO
4Melt viscosity is very little, makes convection current disorder in the melt, and crystal diameter is difficult to control, and easily forms defective such as filamentous growth striped in crystal; On the other hand, big warm ladder can cause V
2O
5Volatilization and resolve into the at a low price oxide compound of vanadium under superheat state makes the crystal blackening of growth useless.
The purpose of this utility model: use Czochralski grown YVO in the above-mentioned prior art in order to overcome
4And Nd:YVO
4The defective of this type high temp oxide crystal growth furnace, provide a kind of can growing large-size, the growth furnace of the high-temp oxide crystal of high quality crystal that subsurface defect is few.
Growth furnace of the present utility model comprises as depicted in figs. 1 and 2: bonnet 1, in bonnet 1 and on the central position of bonnet 1 concentricity axis, be equipped with the melt crucible 7 that holds melt 6, and the crystal 3 of band seed rod 2 just in this slowly growth above melt 6, becomes big.There is stay-warm case 4 on the top of melt crucible 7 between the crystal 3 of band seed rod 2 and the bonnet 1, and stay-warm case 4 has the view port 5 that communicates with bonnet 1.Be equipped with load coil 12 near bonnet 1 between melt crucible 7 and the bonnet 1.There is thermofin 10 on one side near load coil 12 between load coil 12 and the melt crucible 7.Being close to thermofin 10 between thermofin 10 and the melt crucible 7 has thermophore 9, gapped layer 8 between thermophore 9 and melt crucible 7.Temperature thermocouple 13 is arranged at the bottom that puts in melt crucible 7 in the bonnet 1, and temperature and control growing temperature are used for measuring.
Said to place the thermophore 9 between melt crucible 7 and the thermofin 10 be to constitute with melt crucible 7 same materials, is the crucible shape, as shown in Figure 1.Or drum, as shown in Figure 2.
Said thermofin 10 is to constitute by filling zirconia powder in the silica tube, or zirconium white piece formation, or by magnesium oxide, or aluminum oxide, or the powder of other high-temperature oxides or piece formation.
The said crucible holder 11 that places bottom, melt crucible 7 lower ends, when thermophore 9 was drum, crucible holder 11 was monoblocks, as shown in Figure 2.When thermophore 9 was the crucible shape, crucible holder 11 was divided into two by thermophore 9, and one is between melt crucible 7 bottoms and thermophore 9 bottoms, is supporting melt crucible 7, with existing of the clearance layer 8 between maintenance melt crucible 7 and the thermophore 9.Another piece is so as to supporting thermophore 9 in thermophore 9 bottoms.
Above-mentioned growth furnace of the present utility model claims lifting furnace, or claims vacuum oven.The key of the utility model growth furnace is that load coil 12 is by thermofin 10, induction heating thermophore 9, thermophore 9 is given melt crucible 7 with heat radiation again, the heat that is to say melt crucible 7 is to obtain by the thermophore 9 that places its outside, be not the melt crucible 7 that direct heating is placed melt 6, therefore reduced the temperature ladder in the melt crucible 7.
Specifically, radio-frequency induction heating thermophore 9, by the thermal radiation melt heating crucible 7 of thermophore 9, and then melt heating 6.Temperature distribution in the melt 6 is: edge and bottom temp height, centre and head temperature are low, form a rational temperature gradient.As Fig. 3 curve 1 is radial temperature profile curve reasonably, compares with the melt temperature distribution curve 2 of the growth furnace of prior art crystal pulling method, and obviously the thermograde of curve 1 is little.
The utility model has the advantages that growth furnace of the present utility model compared with the prior art, the utility model is a radio-frequency induction heating thermophore 9, thermal radiation by thermophore 9 comes melt heating crucible 7, reduced the thermograde of the melt 6 in the melt crucible 7 with this, also just weakened the turbulent convection of melt 6, just can grow high-quality high-temp oxide crystal greater than Φ 30 * 60mm size, therefore crystal so that the crystal mass that grows among the embodiment is grown apparently higher than prior art can satisfy the market requirement that optical-fibre communications and Laser Devices are made.
Description of drawings:
Fig. 1 is the growth furnace of high-temp oxide crystal of the present utility model, the internal structure cross-sectional schematic when thermophore 9 is the crucible shape.
Fig. 2 is the growth furnace of high-temp oxide crystal of the present utility model, the internal structure cross-sectional schematic when thermophore 9 is drum.
Fig. 3 is warm curve of field distribution figure, wherein curve 2 is warm field distribution in the melt that growth furnace obtained 6 of prior art, curve 1 is warm field distribution in the melt 6 that growth furnace of the present utility model obtained, X-coordinate is the radial distances of melt crucible 7 center O to the edge, is equivalent to the radius R of melt crucible 7.
Embodiment 1:
As above-mentioned structure shown in Figure 1, wherein thermophore 9 is crucible shapes.Melt crucible 7 and thermophore 9 crucibles all use the iridium material to constitute.Melt 6 is vanadic acid yttrium (YVO
4).Attached vacuum system in addition outside the above-mentioned bonnet 1,50kw radio-frequency induction heating power supply is added on the load coil 12, uses 818P
4Ou Lu precise temperature control system monitoring and thermometric use the Ir-Rh thermopair as temperature thermocouple 13.
Melt crucible 7 is of a size of Φ 80 * 60mm, and thermophore 9 is of a size of Φ 100 * 100mm.[100] oriented seed all is evacuated to 10 in clearance layer 8 and the bonnet 1
-2Behind the Pa, charge into high pure nitrogen to 1 normal atmosphere, melt 6 is warming up to 1810 ℃ of fusing points in the melt crucible 7, after being superheated to 1850 ℃, constant temperature 30 minutes, seed crystal rotating speed 25rpm is with 2mm/hr growth velocity pulling crystal, with the shouldering of 0.2 ℃/hr rate of temperature fall, after isometrical, ending, crystallization is finished, be cooled to room temperature with the rate of temperature fall about 200 ℃/hr, the growth whole process finishes.Take out the YVO of Φ 30 * 60mm size
4Crystal, this crystal on crystalline perfection and transparency and the size all apparently higher than prior art.
Embodiment 2:
With above-mentioned same growth furnace structure and condition, just melt 6 is Nd-doped yttrium vanadate (Nd:YVO
4), grow high-quality Nd:YVO greater than Φ 30 * 60mm size
4Crystal.Warm field distribution in the melt that records 6 is shown in curve among Fig. 31, and by finding out among Fig. 3, the warm field distribution of the curve 1 obviously thermograde than the curve 2 of prior art is little.
Above-mentioned two embodiment have proved that fully the growth furnace of high-temp oxide crystal of the present utility model can grow the crystal of large-size high-quality.
Claims (5)
1. the growth furnace of a high-temp oxide crystal, comprise and placing on the interior central position of bonnet (1), hold the melt crucible (7) that confession has the melt (6) of seed rod (2) crystal (3) growth with the inside of the concentricity axis of bonnet (1), above the melt crucible (7), the stay-warm case (4) that the view port (5) that communicates with bonnet (1) is arranged between crystal (3) and the bonnet (1) of band seed rod (2), be equipped with load coil (12) near bonnet (1) between melt crucible (7) and the bonnet (1), there is thermofin (10) on one side near load coil (12) between load coil (12) and the melt crucible (7), temperature thermocouple (13) is arranged at the bottom that puts in the interior melt crucible of bonnet (1) (7), it is characterized in that being close to thermofin (10) between melt crucible (7) and the thermofin (10) is equipped with thermophore (9), gapped layer (8) between thermophore (9) and melt crucible (7), bottom, melt crucible (7) lower end is equipped with crucible holder (11).
2. the growth furnace of high-temp oxide crystal according to claim 1, it is characterized in that said to place the thermophore (9) between melt crucible (7) and the thermofin (10) be to constitute with melt crucible (7) same material, be the crucible shape, or drum.
3. the growth furnace of high-temp oxide crystal according to claim 1 is characterized in that the clearance layer (8) between said thermophore (9) and the melt crucible (7) is a layer of inert, or vacuum layer.
4. the growth furnace of high-temp oxide crystal according to claim 1, it is characterized in that said thermofin (10) is constituted by filling zirconia powder in the silica tube, or constitute by the zirconium white piece, or by magnesium oxide, or aluminum oxide, or the powder of other high-temperature oxides or piece formation.
5. the growth furnace of high-temp oxide crystal according to claim 1 is characterized in that said to place the crucible holder (11) of bottom, melt crucible (7) lower end be a monoblock, or constitutes by two.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99252128 CN2400459Y (en) | 1999-12-16 | 1999-12-16 | High temp. oxide crystal growth furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99252128 CN2400459Y (en) | 1999-12-16 | 1999-12-16 | High temp. oxide crystal growth furnace |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2400459Y true CN2400459Y (en) | 2000-10-11 |
Family
ID=34036431
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99252128 Expired - Fee Related CN2400459Y (en) | 1999-12-16 | 1999-12-16 | High temp. oxide crystal growth furnace |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2400459Y (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460571C (en) * | 2006-12-16 | 2009-02-11 | 杭州慧翔电液技术开发有限公司 | Linear guide rail type crucible lifting device |
| CN100460572C (en) * | 2006-12-16 | 2009-02-11 | 杭州慧翔电液技术开发有限公司 | Sensor built-out type crystal lifting device |
| CN103806102A (en) * | 2014-02-14 | 2014-05-21 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN104534879A (en) * | 2015-01-14 | 2015-04-22 | 中国科学院合肥物质科学研究院 | Method and minicrystal growing furnace for in-situ measurement of fusion method crystal growth microstructures through synchrotron radiation mu-XRD technology |
-
1999
- 1999-12-16 CN CN 99252128 patent/CN2400459Y/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460571C (en) * | 2006-12-16 | 2009-02-11 | 杭州慧翔电液技术开发有限公司 | Linear guide rail type crucible lifting device |
| CN100460572C (en) * | 2006-12-16 | 2009-02-11 | 杭州慧翔电液技术开发有限公司 | Sensor built-out type crystal lifting device |
| CN103806102A (en) * | 2014-02-14 | 2014-05-21 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN103806102B (en) * | 2014-02-14 | 2017-01-11 | 闽能光电集团有限公司 | Thermal field structure for growth of sapphire crystal |
| CN104534879A (en) * | 2015-01-14 | 2015-04-22 | 中国科学院合肥物质科学研究院 | Method and minicrystal growing furnace for in-situ measurement of fusion method crystal growth microstructures through synchrotron radiation mu-XRD technology |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1084398C (en) | Equipment for growing high-temp oxide crystal | |
| CN102758249B (en) | A kind of preparation method of colourless boule monocrystal | |
| CZ303673B6 (en) | Preparation of doped garnet structure single crystals with diameters of up to 500 mm | |
| WO2016078321A1 (en) | Method for preparing large size yb-yag laser crystal through kyropoulos method | |
| CN104109904A (en) | Seeding method of sapphire crystal growth kyropoulos method | |
| CN101649486A (en) | Device and method for growing terbium gallium garnet (TGG) crystal by pulling method | |
| CN104109906A (en) | Apparatus For Manufacturing Single Crystal, Method For Manufacturing Single Crystal, And Single Crystal | |
| CN102703970A (en) | Kyropous method growth of titanium doped sapphire crystals | |
| CN109868503A (en) | A kind of crucible assembly and long crystal furnace | |
| CN2400459Y (en) | High temp. oxide crystal growth furnace | |
| CN104120488A (en) | Dynamic-temperature-field preparation method for large-size C-axis sapphire crystal | |
| CN204138819U (en) | Kyropoulos sapphire single crystal growth furnace insulation side screen | |
| CN206033931U (en) | Crystal growing device | |
| CN103469304B (en) | Branched shaping sapphire crystallization device and long crystal method thereof | |
| CN100552096C (en) | A kind of improved BaY that is applicable to 2F 8The temperature gradient method of single crystal growth and device thereof | |
| CN215517747U (en) | Preparation device of germanium window material for large-size infrared optics | |
| CN104894637B (en) | The grower and growing method of a kind of crystal | |
| CN114737253A (en) | Single crystal furnace thermal field structure and method for growing large-size sapphire single crystal plate | |
| CN208038588U (en) | Incude kyropoulos crystal growing apparatus | |
| CN114875480A (en) | Single crystal furnace, heating and heat-preserving system thereof and method for growing gallium oxide crystals | |
| JP2828118B2 (en) | Single crystal manufacturing method and single crystal pulling apparatus | |
| CN103266346B (en) | The growth apparatus of a kind of crystal Pulling YVO4 crystal and growing method based on this growth apparatus | |
| Machida et al. | Growth of TiO2 single crystals using the edge-defined, film-fed growth technique | |
| CN214736215U (en) | Lithium niobate crystal growth outer heat preservation cover | |
| CN1062319C (en) | Growth method for high-temp. phase barium metaborate (alpha-BaB*O*) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C53 | Correction of patent for invention or patent application | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: PATENTEE; FROM: SHANGHAI OPTICS AND PRECISION MECHANICS INSTITUTE, CHINESE ACADEMY OF SCIENCES TO: SHANGHAI ZHONGKE JIAPU PHOTOELECTRON MATERIAL CO., LTD. |
|
| CP03 | Change of name, title or address |
Address after: 201000 No. 1411, Yecheng Road, Shanghai, Jiading District Patentee after: Shanghai Zhongke Jiapu Optoelectronic Materials Co., Ltd. Address before: Shanghai 800-211 post office box Patentee before: Shanghai Optical Precision Machinery Inst., Chinese Academy of Sciences |
|
| 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 |