CN100374626C - Method and device for growing sapphire crystal by laser - Google Patents
Method and device for growing sapphire crystal by laser Download PDFInfo
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- CN100374626C CN100374626C CNB2005100022798A CN200510002279A CN100374626C CN 100374626 C CN100374626 C CN 100374626C CN B2005100022798 A CNB2005100022798 A CN B2005100022798A CN 200510002279 A CN200510002279 A CN 200510002279A CN 100374626 C CN100374626 C CN 100374626C
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Abstract
The present invention belongs to the field of crystal growth. In the method, the lower end of Al2O3-doped ceramic rod is melted through laser irradiation, seed crystals are put on the lower end, and crystals rapidly grow from bottom to top. A device comprises a vacuum furnace, wherein the inner wall is surrounded by a side heat preservation screen (2), an upper heat preservation screen (7) and a lower heat preservation screen (8), and a crystallization rod (5) positioned on the central axis line of a furnace body and a lifting rod (1) are arranged in the vacuum furnace. The device is characterized in that the crystallization rod (5) whose top is connected with a seed crystal groove (4) penetrates through the lower heat preservation screen (8), the lifting rod (1) connected with a material clamp (10) penetrates through the upper heat preservation screen (7), a laser incidence window (3) is arranged on one side of the furnace body, an inspection window (9) which is not in the same horizontal line with the laser incidence window (3) is arranged on the other side of the furnace body, a vacuum system is additionally arranged outside the furnace body, two sets of servo motors and control systems are used as a lifting rotary system of the crystallization rod (5) and the lifting rod (1), and a thermoscope outside the inspection window (9) is used for temperature measurement and feedback. The present invention can rapidly produce sapphire crystals with the diameter of about 15mm.
Description
Technical field:
The invention belongs to the crystal preparation field.
Technical background:
Carry out the development of artificial sapphire crystal since mid-term in 20th century in the world, mainly adopt Czochralski grown sapphire crystal, and obtain initial success.But Czochralski grown sapphire has three shortcomings: 1. growth cycle is long, is generally several days to tens days, thereby yields poorly; 2. growth temperature surpasses 2000 ℃, need to use iridium crucible, thereby the cost height; 3. colored trace element spreads to the outside in the process of growth, and crystals is colourless, and it is blue having only an outside circle, can utilize volume seldom, so crystal pulling method does not really become the artificial sapphire effective ways of growth.
1995-1998, U.S. Penn State university has born the world's second largest artificial gem D.Swarovski﹠amp of company in the investigation of materials laboratory; Co. development project---adopt the laser heated pedestal method artificial sapphire of growing, and succeed.The advantage of this method is a fast growth, and color even does not need to use crucible.But shortcoming is that the size of growing crystal is smaller, and diameter is 2.5 millimeters to the maximum.The principle of laser heated pedestal method is the top that laser is focused on uniformly ceramic rod, make its fusing, form small melting zone, then seed end is goed deep into the melting zone, treat upwards to pull out again after its fusing, control ceramic rod and the speed that lifts seed crystal can grow crystal, and crystal is top-down growth.
Up to the present, still do not have a kind of comparatively easy method in the prior art, the sapphire crystal of the color even of growing large-size (more than the 15mm) has restricted artificial sapphire development to a certain extent fast.
Summary of the invention:
The objective of the invention is for the crystal growth cycle that overcomes crystal pulling method long, the little shortcoming of crystal growth size of the inhomogeneous and laser heated pedestal method of crystal color and a kind of novel method of proposing, and be the technical scheme of Method Of Accomplishment, designed the device of growing sapphire crystal by laser.
The method of growing sapphire crystal by laser is characterized in that in the technical scheme of the present invention, with high power laser irradiation doped with Al
2O
3The lower end of ceramic rod makes its fusion, places seed crystal at ceramic rod lower end relative position, forms sapphire crystal quick growth from the bottom to top.Because upwards lifting in the process of growth from the bottom to top with the inventive method of laser heated pedestal method, gravity role difference, the former gravity is to hinder crystalline size to become big, latter's gravity is to help the crystalline growth size to become big, therefore present method has overcome the little shortcoming of crystal growth size of laser heated pedestal method, adopt laser long simultaneously as the growth cycle that growth means itself have just overcome crystal pulling method, shortcomings such as crystal color is inhomogeneous successfully grow the sapphire crystal that diameter surpasses the color even of 15mm.
The device of growing sapphire crystal by laser comprises vacuum oven in the technical scheme of the present invention, inboard wall of furnace body is surrounded by side heat protection screen 2, last heat protection screen 7, following heat protection screen 8, structure in the stove comprises crystallizatio pole 5, the elevating lever 1 that is positioned on the body of heater axis, the crystallizatio pole 5 that it is characterized in that top connection seed slot 4 passes down heat protection screen 8, the elevating lever 1 that connects feed collet 10 passes heat protection screen 7, body of heater one side has laser entrance window 3, and opposite side has and the laser entrance window 3 infrared viewing window 9 on same sea line not; Attached vacuum system in addition outside the body of heater; 2 cover servomotor and Controlling System are respectively as the lifting rotational system of crystallizatio pole 5 and elevating lever 1; Be positioned at the infrared thermometer in infrared viewing window 9 outsides, be used for temperature survey and feedback are carried out in crystal growth.
The method of growing sapphire crystal by laser of the present invention and device thereof is characterized in that the technical process of growing crystal is as follows:
(1) puts into oriented seed in the seed slot;
(2) with doped with Al
2O
3Ceramic rod is fixed on the feed collet of stove internal upper part, is evacuated to 10
-3Pa charges into inert protective gas.
(3) doped with Al of rotating with high power laser illumination
2O
3Ceramic rod makes laser power density reach 650-850w/cm in 30-60s
2, make its end reach molten state.
(4) regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed slot touch the fused ceramic rod, and crystal growth begins.
(5) according to the Temperature Feedback of infrared thermometer, the lifting of servo electrical machinery system control ceramic rod and crystallizatio pole is carried out crystal growth automatically.
(6) treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to zero in 300-400s, crystal growth is finished on the crystallizatio pole.
Adopt the method for growing sapphire crystal by laser of the present invention and install obtained beneficial effect and be:
1. a kind of growing large-size sapphire crystalline novel method is provided, successfully grows the sapphire crystal that diameter surpasses the color even of 15mm.
2. device simplicity of design, practicality, low cost of manufacture.
3. process controllability is strong, and repeatability is high.
4. realize that the high-melting-point crystalline prepares fast, preparation sample purity height.
Description of drawings:
Fig. 1 is the internal structure synoptic diagram of the device-vacuum oven of growing sapphire crystal by laser of the present invention
Embodiment:
Device-the vacuum oven of growing sapphire crystal by laser of the present invention as shown in Figure 1, inboard wall of furnace body is by the side heat protection screen 2 of down heat protection screen 8 and driving fit, goes up heat protection screen 7 and constitute, the body of heater internal structure comprises crystallizatio pole 5, the elevating lever 1 that is positioned on the body of heater axis.The top has the crystallizatio pole 5 of seed slot 4 and the central position that water cooling plant 6 passes down heat protection screen 8 jointly, water cooling plant 6 and the accurate welding in body of heater bottom, between crystallizatio pole 5 and the water cooling plant 6 is to be slidingly matched, seed slot 4 is plugged in the top of crystallizatio pole 5, the elevating lever that has feed collet 10 1 that passes heat protection screen 7 reaches and its sleeve that becomes to be slidingly matched 11, sleeve 11 and the accurate welding of upper of furnace body, adopt between feed collet 10 and the elevating lever 1 and be threaded, body of heater one side has laser entrance window 3, opposite side has and the laser entrance window 3 infrared viewing window 9 on same sea line not, laser entrance window 3, infrared viewing window 9 adopts flange to be connected with body of heater.The material of seed slot 4 can be a molybdenum, materials processing such as tungsten and miramint and making, and last heat protection screen 7, side heat protection screen 2, heat protection screen 8 usefulness molybdenum sheets or tungsten sheet are made down, and crystallizatio pole 5 can be made by thermal conductivity good copper and alloy thereof.
Attached vacuum system in addition outside the body of heater, 2 cover servomotor and Controlling System, the lifting of crystallization control bar 5 and elevating lever 1 rotation respectively, laser is injected from laser entrance window 3, closely be positioned at the high precision infrared thermometer in the outside of infrared viewing window 9, be used for temperature survey and feedback are carried out in crystal growth.
Used laser apparatus is 2500 watts of CO
2Laser apparatus (German Rofin-Sinar company), infrared thermometer adopt U.S. EXERGEN standard type noncontact infrared thermometer Irt/c.100A.
Further specify the present invention below for example, carry out the sapphire crystal growth of different components with the method for above-mentioned growing sapphire crystal by laser and device thereof and technical process.
Embodiment 1:
(composition is (Al with sapphire polycrystalline ceramics rod
2O
3)
0.988(Fe
2O
3)
0.006(FeTiO
3)
0.006) be fixed on the feed collet 10, put into [0001] oriented seed in the seed slot 4, charge into high-purity argon gas to 1 normal atmosphere after vacuumizing, regulate laser power density in the 30s to 750w/cm
2, make its end reach molten state, regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed crystal frame touch the fused ceramic rod, and crystal growth begins.According to the Temperature Feedback of infrared thermometer, servo electrical machinery system is pressed the lifting of blas control ceramic rod and crystallizatio pole, and crystal growth is carried out automatically.Treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to 0 in the time at 400s, crystal growth is finished on the crystallizatio pole.After treating that crystal is cooled to room temperature, take out sapphire crystal, crystal diameter reaches 14.9mm, and perfect crystalline does not ftracture, and is evenly blue, can be used for decorating using jewel.
Embodiment 2:
(composition is (Al with sapphire polycrystalline ceramics rod
2O
3)
0.99(Fe
2O
3)
0.004(FeTiO
3)
0.006) be fixed on the feed collet 10, put into [0001] oriented seed in the seed slot 4, charge into high-purity argon gas to 1 normal atmosphere after vacuumizing, regulate laser power density in the 30s to 800w/cm
2, make its end reach molten state, regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed crystal frame touch the fused ceramic rod, and crystal growth begins.According to the Temperature Feedback of infrared thermometer, servo electrical machinery system is pressed the lifting of blas control ceramic rod and crystallizatio pole, and crystal growth is carried out automatically.Treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to 0 in the time at 300s, crystal growth is finished on the crystallizatio pole.After treating that crystal is cooled to room temperature, take out sapphire crystal, crystal diameter reaches 15.2mm, and perfect crystalline does not ftracture, and it is light blue and more even that crystal is, and can be used for decorating using jewel.
Embodiment 3:
(composition is (Al with sapphire polycrystalline ceramics rod
2O
3)
0.986(Fe
2O
3)
0.008(FeTiO
3)
0.006) be fixed on the feed collet 10, put into [0001] oriented seed in the seed slot 4, charge into high-purity argon gas to 1 normal atmosphere after vacuumizing, regulate laser power density in the 30s to 650w/cm
2, make its end reach molten state, regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed crystal frame touch the fused ceramic rod, and crystal growth begins.According to the Temperature Feedback of infrared thermometer, servo electrical machinery system is pressed the lifting of blas control ceramic rod and crystallizatio pole, and crystal growth is carried out automatically.Treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to 0 in the time at 400s, crystal growth is finished on the crystallizatio pole.After treating that crystal is cooled to room temperature, take out sapphire crystal, crystal diameter reaches 15.1mm, and perfect crystalline does not ftracture, and it is more even that crystal is blueness, can be used as to decorate to use jewel.
Embodiment 4:
(composition is (Al with sapphire polycrystalline ceramics rod
2O
3)
0.984(Fe
2O
3)
0.008(FeTiO
3)
0.008) be fixed on the feed collet 10, put into [0001] oriented seed in the seed slot 4, charge into high-purity argon gas to 1 normal atmosphere after vacuumizing, regulate laser power density in the 30s to 820w/cm
2, make its end reach molten state, regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed crystal frame touch the fused ceramic rod, and crystal growth begins.According to the Temperature Feedback of infrared thermometer, servo electrical machinery system is pressed the lifting of blas control ceramic rod and crystallizatio pole, and crystal growth is carried out automatically.Treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to 0 in the time at 400s, crystal growth is finished on the crystallizatio pole.After treating that crystal is cooled to room temperature, take out sapphire crystal, crystal diameter reaches 15mm, and perfect crystalline does not ftracture, and crystal color is dark blue more even, can be used as to decorate to use jewel.
Embodiment 5:
(composition is (Al with sapphire polycrystalline ceramics rod
2O
3)
0.984(Fe
2O
3)
0.01(FeTiO
3)
0.006) be fixed on the feed collet 10, put into [0001] oriented seed in the seed slot 4, charge into high-purity argon gas to 1 normal atmosphere after vacuumizing, regulate laser power density in the 30s to 850w/cm
2, make its end reach molten state, regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed crystal frame touch the fused ceramic rod, and crystal growth begins.According to the Temperature Feedback of infrared thermometer, servo electrical machinery system is pressed the lifting of blas control ceramic rod and crystallizatio pole, and crystal growth is carried out automatically.Treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to 0 in the time at 400s, crystal growth is finished on the crystallizatio pole.After treating that crystal is cooled to room temperature, take out sapphire crystal, crystal diameter reaches 15.2mm, and perfect crystalline does not ftracture, and crystal is light blue and slightly pink colour is not too even, uses jewel but can be used as after the cutting process to decorate.
Claims (3)
1. the method for a growing sapphire crystal by laser is characterized in that, makes its fusion with the lower end of laser irradiation doped with Al 2O3 ceramic rod, places seed crystal at this ceramic rod lower end relative position, forms sapphire crystal quick growth from the bottom to top.
2. the method for growing sapphire crystal by laser according to claim 1 is characterized in that, may further comprise the steps:
(1) puts into oriented seed in the seed slot;
(2) with doped with Al
2O
3Ceramic rod is fixed on the feed collet of stove internal upper part, is evacuated to 10
-3Pa charges into inert protective gas;
(3) doped with Al of rotating with high power laser illumination
2O
3Ceramic rod makes laser power density reach 650-850w/cm in 30-60s
2, make its end reach molten state;
(4) regulation and control 2 cover servo electrical machinery systems make doped with Al
2O
3Ceramic rod is slowly downward, and crystallizatio pole upwards makes the seed crystal in the seed slot touch the fused ceramic rod, and crystal growth begins;
(5) according to the Temperature Feedback of infrared thermometer, the lifting of servo electrical machinery system control ceramic rod and crystallizatio pole is carried out crystal growth automatically;
(6) treat doped with Al
2O
3After ceramic rod has melted, regulate laser power, make it to reduce to zero in 300-400s, crystal growth is finished on the crystallizatio pole.
3. implement the method equipment therefor of claim 1 or 2 described growing sapphire crystal by laser, comprise vacuum oven, inboard wall of furnace body is by side heat protection screen (2), last heat protection screen (7), following heat protection screen (8) surrounds, comprise the crystallizatio pole (5) that is positioned on the body of heater axis in the vacuum oven, elevating lever (1), it is characterized in that, the crystallizatio pole (5) that the top connects seed slot (4) passes down heat protection screen (8), the elevating lever (1) that connects feed collet (10) passes heat protection screen (7), body of heater one side has laser entrance window (3), and opposite side has and laser entrance window (3) the infrared viewing window (9) on same sea line not; Attached vacuum system in addition outside the body of heater, 2 cover servomotor and Controlling System are respectively as the lifting rotational system of crystallizatio pole (5) and elevating lever (1); Be positioned at the infrared thermometer in infrared viewing window (9) outside, be used for temperature survey and feedback are carried out in crystal growth.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100022798A CN100374626C (en) | 2005-01-20 | 2005-01-20 | Method and device for growing sapphire crystal by laser |
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|---|---|---|---|
| CNB2005100022798A CN100374626C (en) | 2005-01-20 | 2005-01-20 | Method and device for growing sapphire crystal by laser |
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| CN100374626C true CN100374626C (en) | 2008-03-12 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101984150A (en) * | 2010-10-29 | 2011-03-09 | 北京工业大学 | Method of growing sapphire crystal by floating zone method |
| CN102020458B (en) * | 2010-11-04 | 2013-05-08 | 西北工业大学 | Method for getting structure appearance of aluminum oxide-based ternary melt growth ceramic |
| CN102050617B (en) * | 2010-11-04 | 2013-04-17 | 西北工业大学 | Method for obtaining microstructure of alumina-based binary eutectic melt-grown ceramic |
| CN102864496A (en) * | 2012-09-20 | 2013-01-09 | 上海大学 | Device for growing tellurium-zinc-cadmium crystals by traveling heater method |
| CN104180927B (en) * | 2014-08-28 | 2017-04-12 | 洛阳西格马炉业股份有限公司 | Measurement platform and measurement method for standard temperature of super-high-temperature hearth |
| CN112410887A (en) * | 2020-11-17 | 2021-02-26 | 通辽精工蓝宝石有限公司 | Welding method of sapphire rods |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63242989A (en) * | 1987-03-31 | 1988-10-07 | Fujikura Ltd | Production of single crystal fiber |
| US5427051A (en) * | 1993-05-21 | 1995-06-27 | General Electric Company | Solid state formation of sapphire using a localized energy source |
| US5607506A (en) * | 1994-10-21 | 1997-03-04 | University Of South Florida | Growing crystalline sapphire fibers by laser heated pedestal techiques |
-
2005
- 2005-01-20 CN CNB2005100022798A patent/CN100374626C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63242989A (en) * | 1987-03-31 | 1988-10-07 | Fujikura Ltd | Production of single crystal fiber |
| US5427051A (en) * | 1993-05-21 | 1995-06-27 | General Electric Company | Solid state formation of sapphire using a localized energy source |
| US5607506A (en) * | 1994-10-21 | 1997-03-04 | University Of South Florida | Growing crystalline sapphire fibers by laser heated pedestal techiques |
Non-Patent Citations (1)
| Title |
|---|
| 提拉法生长蓝宝石晶体的工艺特征及晶体质量检测. 秦友兰等.重庆大学学报，第17卷第6期. 1994 * |
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| CN1670268A (en) | 2005-09-21 |
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