CN104451882A - Garnet production technology - Google Patents
Garnet production technology Download PDFInfo
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- CN104451882A CN104451882A CN201410792092.1A CN201410792092A CN104451882A CN 104451882 A CN104451882 A CN 104451882A CN 201410792092 A CN201410792092 A CN 201410792092A CN 104451882 A CN104451882 A CN 104451882A
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- graphite
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the field of crystal growth and in particular relates to a garnet production technology. The garnet production technology comprises the steps of raw material preparing, press forming, charging, vacuumizing, system setting, melt heating, seed crystal dropping, seeding, diameter enlarging, stretching and furnace shut down. The garnet production technology has the beneficial effects that grown crystals are heated by adopting graphite resistance instead of expensive Pt-Ir alloys; crucible insulation materials are low in prices, so that the investment and the cost are reduced; molybdenum materials are adopted for insulation and are characterized in that the molybdenum materials can be reused for about one year in special growth atmospheres, so that the growth cycles of the crystals and the cost are reduced; in the implementation process, not only is the production capacity improved but also the production cost is reduced and no pollution, radiation or noise is achieved in the production process by adopting the new crystal growing technology provided by the invention; domestic gaps are filled in and valuable experience is provided for the development of the laser crystal growth industry by adopting the production technology.
Description
(1) technical field
The present invention relates to a kind of field of crystal growth, particularly the garnet production technique of one.
(2) background technology
Compared with conventional communication techniques, opticfiber communication has following features: (1) optical fiber volume is little, lightweight; (2) capacity is large, and speed is fast, and loss is low; (3) transmission reliability is high; (4) noise ratio, the error rate, information distortion degree are low etc.At present along with the fast development of near-infrared region optical fiber technology, optoisolator obtains more and more important application in information transmission.
Optoisolator can be used for eliminating the backlight produced in Optical Fiber Transmission.The existence of backlight can cause the self-coupling effect between system, makes excitaton source become unstable, produces reflect noise and autoexcitation, cause whole system normally to work.And optoisolator can eliminate above detrimentally affect.Such as, between semiconductor laser light source and optical transmission system, an optoisolator is installed, the detrimentally affect that reflected light produces the spectral output power stability of light source can be reduced to a great extent.In high speed directly modulation, direct-detection opticfiber communication system, reverse transfers light can produce additional noise, makes the performance degradation of system, and this also needs optoisolator to eliminate.
The center part of optoisolator is the magneto-optic Faraday rotor of 45 degree, mainly utilizes the Faraday effect of magneto-optical crystal.Faraday effect was found in 1845 by faraday.When line polarized light is propagated in media as well, if add a high-intensity magnetic field on the propagation direction being parallel to light, then optical vibration direction will deflect, the product that deflection angle Ψ passes through the length l of medium to magnetic induction density B and light is directly proportional, i.e. Ψ=VBl, scale-up factor V is called Verdet constant, relevant with medium character and frequency of light wave.Above-mentioned phenomenon is called Faraday effect or magnetic rotation effect.For the flashlight of forward entrance, by becoming line polarized light after the polarizer, Faraday rotation medium makes the polarization direction dextrorotation 45 degree of flashlight together with foreign field, and just makes less energy-consumption by becoming 45 degree of analyzers placed with the polarizer.For backlight, go out the line polarized light of analyzer through placing medium, polarization direction is dextrorotation 45 degree also, thus make the polarization direction of backlight orthogonal with polarizer direction, has blocked the transmission of backlight completely.
Garnet, as a kind of magneto-optical crystal of excellence, is main research object, and realizes commercialization.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides a kind of garnet production technique.
The present invention is achieved through the following technical solutions:
A kind of garnet production technique, it is characterized in that: comprise the steps: prepared by (1) raw material: by the raw material such as raw material Y2O3, AL2O3, Nd2O3 or Ce2O3, Cr2O3, Er2O3, sintered by silicon molybdenum retort furnace, sintering temperature is 1400-1500 degree Celsius, and constant temperature 30 hours, remove moisture and other dirts;
(2) compression moulding: by the above-mentioned raw material prepared after automatic mixing machine batch mixing, be pressed into wafer type by press;
(3) shove charge: by burner hearth and graphite electrode plate wiped clean, by neat for parts assembling each in stove;
(4) vacuumize: before vacuum extraction, first check that whether vent valve is urgent, prevent from leaking gas in the process vacuumized; Start housing, open mechanical pump, vacuumize;
(5) system is set: crystal growth adopts and automatically controls weighing system, adopts JPG auto-control software, set the concentration of crystal type, size, external form and length setting and enter software.Product parameters counts computer controlled automatic processing parameter automatic growth;
(6) intensification melt: in the process of intensification melt, according to the situation that melting sources stays, promotes crucible position slowly, raw material is evenly melted;
(7) seed crystal under: first according to situation adjustment temperature in stove, and carry out constant temperature, decline seed crystal carries out preheating simultaneously, adjustment crystal rotation is 15r/min, when after temperature-adjusting constant temperature for some time, is turned down and melt contacts by seed crystal, examine and adjust furnace temperature, constant temperature 30-60min;
(8) seeding: open lift power supply, tune pulling rate is 1.0-2.0mm/h;
(9) shouldering: in the process of shouldering, is program controlly generally negative value, and the diameter along with shouldering becomes large, and program control value also strengthens, until start to turn shoulder.When shouldering is to Φ 20mm, pulling rate is lowered to 1mm/h with 0.1mm per hour;
(10) stretch: when growth length reaches 70mm.Pulling rate is down to 1.5mm/h by 1.5-2.5mm/h with reduction 0.1mm per hour, according to processing requirement, determines the length that will draw;
(11) blowing out: when terminating growth, manually mention crystal and make it depart from liquid level, then stop to draw and be slowly annealed to room temperature, annealing time is 20-40h.
Step 3 is specially: (1) should get out following article before shove charge: fix screen on urgent spanner, water level gauge, torch light, vernier callipers, pad, zirconia particles, the graphite connector cleaned up, crucible tray, table cooker, graphite pallet, graphite heater, graphite side screen, molybdenum side screen, molybdenum, graphite clamping, crucible, seed rod, centering rod, filter paper, molybdenum filament, seed crystal, dryout clean zirconium white side screen, clean gauze, alcohol, hairbrush; (2) checking burner hearth and graphite electrode plate whether wiped clean, if do not had, carrying out wiping with dipping in spirituous clean gauze; Check graphite electrode plate horizontality with water level gauge, Row sum-equal matrix of going forward side by side, graphite electrode plate horizontal plane and front-back are all up to the standard requirement; (3) aluminum oxide side screen is loaded onto, being tightened by graphite connector is fixed in underdrive, table cooker is installed on crucible tray, and one deck zirconia particles is spread uniformly on crucible tray, crucible tray entirety is forwarded on graphite connector, and carry out checking and adjustment level, crucible is placed on crucible tray, measuring and adjustation level; Dress graphite heater, uses graphite clamping itself and graphite electrode plate to be tightened, makes it contact well; Crucible is placed on crucible tray, surveys level peace crucible position and record; According to the height of graphite side screen, select the pad of three same thickness to be placed on graphite electrode plate, require that the difference of altitude on heating element and the upper edge of graphite side screen is 2-3mm, graphite side screen successively, molybdenum side is shielded, and requires that side is shielded and keeps concentric(al) circles with graphite heater, put screen and survey seeding crucible position and record.
Step 4 is specially: start housing, open mechanical pump, slowly pulled open by three-way valve, when vacuum tightness reaches-0.06MPa, open three-way valve completely, wait 5-10 minute and open vacuum measuring gauge, as 15Pa, close three-way valve, open recirculated water, open diffusion pump, open flapper valve; When vacuum tightness reaches 1-0.1Pa, record vacuum values, preheats.First open heating power supply, manually rise OP value, make current voltmeter have startup, then to arrange Prl be 3600uv/h, PL1 is 3mv, continue to vacuumize.
Step 6 is specially: when raw material collapse put down in crucible time, rise to optical flat crucible position, continue to observe material situation, and slowly promote crucible position according to material situation, when floating block in crucible is less than Φ 20mm, rises in seeding crucible, and be deflated to 20KPa; After rising to seeding crucible position, slowly adjust temperature variation, temperature adjustment has just been melted to floating block, constant temperature homogenizing.
Be filled with argon gas in described smelting furnace, smelting furnace adopts graphite resistance heating.
Described garnet crystal grows in molybdenum crucible.
The invention has the beneficial effects as follows: the present invention adopts graphite resistance heat growth crystal to avoid using expensive iraurite, crucible heat insulation material price is low, same facility investment only has iridium crucible equipment about 20-25%, decrease investment, reduce cost, insulation adopts Mo, is characterized in reusing about 1 year cycle under special growth atmosphere, has saved the growth cycle of crystal and has reduced cost.In process of the invention process, adopt the production production capacity that crystal growth novel process of the present invention not only improves, and reduce production cost, accomplish pollution-free, radiationless, noiselessness in the process of producing.Production technique has filled up domestic blank, and the development for laser crystal growth industry provides valuable experience.
(4) embodiment
Embodiment 1:
Comprise the steps:
(1) raw material preparation: by the raw material such as raw material Y2O3, AL2O3, Nd2O3 or Ce2O3, Cr2O3, Er2O3, by silicon molybdenum retort furnace sintering, sintering temperature is 1400 degrees Celsius, and constant temperature 30 hours, remove moisture and other dirts;
(2) compression moulding: by the above-mentioned raw material prepared after automatic mixing machine batch mixing, be pressed into wafer type by press;
(3) shove charge: comprise the following steps: 1) following article should be got out before shove charge: fix screen on urgent spanner, water level gauge, torch light, vernier callipers, pad, zirconia particles, the graphite connector cleaned up, crucible tray, table cooker, graphite pallet, graphite heater, graphite side screen, molybdenum side screen, molybdenum, graphite clamping, crucible, seed rod, centering rod, filter paper, molybdenum filament, seed crystal, dryout clean zirconium white side screen, clean gauze, alcohol, hairbrush; 2) checking burner hearth and graphite electrode plate whether wiped clean, if do not had, carrying out wiping with dipping in spirituous clean gauze; Check graphite electrode plate horizontality with water level gauge, Row sum-equal matrix of going forward side by side, graphite electrode plate horizontal plane and front-back are all up to the standard requirement; 3) aluminum oxide side screen is loaded onto, being tightened by graphite connector is fixed in underdrive, table cooker is installed on crucible tray, and one deck zirconia particles is spread uniformly on crucible tray, crucible tray entirety is forwarded on graphite connector, and carry out checking and adjustment level, crucible is placed on crucible tray, measuring and adjustation level; Dress graphite heater, uses graphite clamping itself and graphite electrode plate to be tightened, makes it contact well; Crucible is placed on crucible tray, surveys level peace crucible position and record; According to the height of graphite side screen, select the pad of three same thickness to be placed on graphite electrode plate, require that the difference of altitude on heating element and the upper edge of graphite side screen is 2-3mm, graphite side screen successively, molybdenum side is shielded, and requires that side is shielded and keeps concentric(al) circles with graphite heater, put screen and survey seeding crucible position and record;
(4) vacuumize: before vacuum extraction, first check that whether vent valve is urgent, prevent from leaking gas in the process vacuumized; Start housing, open mechanical pump, vacuumize;
(5) system is set: crystal growth adopts and automatically controls weighing system, adopts JPG auto-control software, set the concentration of crystal type, size, external form and length setting and enter software.Product parameters counts computer controlled automatic processing parameter automatic growth;
(6) intensification melt: in the process of intensification melt, according to the situation that melting sources stays, promotes crucible position slowly, raw material is evenly melted;
(7) seed crystal under: first according to situation adjustment temperature in stove, and carry out constant temperature, decline seed crystal carries out preheating simultaneously, adjustment crystal rotation is 15r/min, when after temperature-adjusting constant temperature for some time, is turned down and melt contacts by seed crystal, examine and adjust furnace temperature, constant temperature 30-60min;
(8) seeding: open lift power supply, tune pulling rate is 1.0mm/h;
(9) shouldering: in the process of shouldering, is program controlly generally negative value, and the diameter along with shouldering becomes large, and program control value also strengthens, until start to turn shoulder.When shouldering is to Φ 20mm, pulling rate is lowered to 1mm/h with 0.1mm per hour;
(10) stretch: when growth length reaches 70mm.Pulling rate is down to 1.5mm/h by 1.5mm/h with reduction 0.1mm per hour, according to processing requirement, determines the length that will draw;
(11) blowing out: when terminating growth, manually mention crystal and make it depart from liquid level, then stop to draw and be slowly annealed to room temperature, annealing time is 20h.
Embodiment 2:
Comprise the steps:
(1) raw material preparation: by the raw material such as raw material Y2O3, AL2O3, Nd2O3 or Ce2O3, Cr2O3, Er2O3, by silicon molybdenum retort furnace sintering, sintering temperature is 1500 degrees Celsius, and constant temperature 30 hours, remove moisture and other dirts;
(2) compression moulding: by the above-mentioned raw material prepared after automatic mixing machine batch mixing, be pressed into wafer type by press;
(3) shove charge: comprise the following steps: 1) following article should be got out before shove charge: fix screen on urgent spanner, water level gauge, torch light, vernier callipers, pad, zirconia particles, the graphite connector cleaned up, crucible tray, table cooker, graphite pallet, graphite heater, graphite side screen, molybdenum side screen, molybdenum, graphite clamping, crucible, seed rod, centering rod, filter paper, molybdenum filament, seed crystal, dryout clean zirconium white side screen, clean gauze, alcohol, hairbrush; 2) checking burner hearth and graphite electrode plate whether wiped clean, if do not had, carrying out wiping with dipping in spirituous clean gauze; Check graphite electrode plate horizontality with water level gauge, Row sum-equal matrix of going forward side by side, graphite electrode plate horizontal plane and front-back are all up to the standard requirement; 3) aluminum oxide side screen is loaded onto, being tightened by graphite connector is fixed in underdrive, table cooker is installed on crucible tray, and one deck zirconia particles is spread uniformly on crucible tray, crucible tray entirety is forwarded on graphite connector, and carry out checking and adjustment level, crucible is placed on crucible tray, measuring and adjustation level; Dress graphite heater, uses graphite clamping itself and graphite electrode plate to be tightened, makes it contact well; Crucible is placed on crucible tray, surveys level peace crucible position and record; According to the height of graphite side screen, select the pad of three same thickness to be placed on graphite electrode plate, require that the difference of altitude on heating element and the upper edge of graphite side screen is 2-3mm, graphite side screen successively, molybdenum side is shielded, and requires that side is shielded and keeps concentric(al) circles with graphite heater, put screen and survey seeding crucible position and record;
(4) vacuumize: before vacuum extraction, first check that whether vent valve is urgent, prevent from leaking gas in the process vacuumized; Start housing, open mechanical pump, vacuumize;
(5) system is set: crystal growth adopts and automatically controls weighing system, adopts JPG auto-control software, set the concentration of crystal type, size, external form and length setting and enter software.Product parameters counts computer controlled automatic processing parameter automatic growth;
(6) intensification melt: in the process of intensification melt, according to the situation that melting sources stays, promotes crucible position slowly, raw material is evenly melted;
(7) seed crystal under: first according to situation adjustment temperature in stove, and carry out constant temperature, decline seed crystal carries out preheating simultaneously, adjustment crystal rotation is 15r/min, when after temperature-adjusting constant temperature for some time, is turned down and melt contacts by seed crystal, examine and adjust furnace temperature, constant temperature 30-60min;
(8) seeding: open lift power supply, tune pulling rate is 2.0mm/h;
(9) shouldering: in the process of shouldering, is program controlly generally negative value, and the diameter along with shouldering becomes large, and program control value also strengthens, until start to turn shoulder.When shouldering is to Φ 20mm, pulling rate is lowered to 1mm/h with 0.1mm per hour;
(10) stretch: when growth length reaches 70mm.Pulling rate is down to 1.5mm/h by 2.5mm/h with reduction 0.1mm per hour, according to processing requirement, determines the length that will draw;
(11) blowing out: when terminating growth, manually mention crystal and make it depart from liquid level, then stop to draw and be slowly annealed to room temperature, annealing time is 40h.
Embodiment 3:
Comprise the steps:
(1) raw material preparation: by the raw material such as raw material Y2O3, AL2O3, Nd2O3 or Ce2O3, Cr2O3, Er2O3, by silicon molybdenum retort furnace sintering, sintering temperature is 1450 degrees Celsius, and constant temperature 30 hours, remove moisture and other dirts;
(2) compression moulding: by the above-mentioned raw material prepared after automatic mixing machine batch mixing, be pressed into wafer type by press;
(3) shove charge: comprise the following steps: 1) following article should be got out before shove charge: fix screen on urgent spanner, water level gauge, torch light, vernier callipers, pad, zirconia particles, the graphite connector cleaned up, crucible tray, table cooker, graphite pallet, graphite heater, graphite side screen, molybdenum side screen, molybdenum, graphite clamping, crucible, seed rod, centering rod, filter paper, molybdenum filament, seed crystal, dryout clean zirconium white side screen, clean gauze, alcohol, hairbrush; 2) checking burner hearth and graphite electrode plate whether wiped clean, if do not had, carrying out wiping with dipping in spirituous clean gauze; Check graphite electrode plate horizontality with water level gauge, Row sum-equal matrix of going forward side by side, graphite electrode plate horizontal plane and front-back are all up to the standard requirement; 3) aluminum oxide side screen is loaded onto, being tightened by graphite connector is fixed in underdrive, table cooker is installed on crucible tray, and one deck zirconia particles is spread uniformly on crucible tray, crucible tray entirety is forwarded on graphite connector, and carry out checking and adjustment level, crucible is placed on crucible tray, measuring and adjustation level; Dress graphite heater, uses graphite clamping itself and graphite electrode plate to be tightened, makes it contact well; Crucible is placed on crucible tray, surveys level peace crucible position and record; According to the height of graphite side screen, select the pad of three same thickness to be placed on graphite electrode plate, require that the difference of altitude on heating element and the upper edge of graphite side screen is 2-3mm, graphite side screen successively, molybdenum side is shielded, and requires that side is shielded and keeps concentric(al) circles with graphite heater, put screen and survey seeding crucible position and record;
(4) vacuumize: before vacuum extraction, first check that whether vent valve is urgent, prevent from leaking gas in the process vacuumized; Start housing, open mechanical pump, vacuumize;
(5) system is set: crystal growth adopts and automatically controls weighing system, adopts JPG auto-control software, set the concentration of crystal type, size, external form and length setting and enter software.Product parameters counts computer controlled automatic processing parameter automatic growth;
(6) intensification melt: in the process of intensification melt, according to the situation that melting sources stays, promotes crucible position slowly, raw material is evenly melted;
(7) seed crystal under: first according to situation adjustment temperature in stove, and carry out constant temperature, decline seed crystal carries out preheating simultaneously, adjustment crystal rotation is 15r/min, when after temperature-adjusting constant temperature for some time, is turned down and melt contacts by seed crystal, examine and adjust furnace temperature, constant temperature 30-60min;
(8) seeding: open lift power supply, tune pulling rate is 1.5mm/h;
(9) shouldering: in the process of shouldering, is program controlly generally negative value, and the diameter along with shouldering becomes large, and program control value also strengthens, until start to turn shoulder.When shouldering is to Φ 20mm, pulling rate is lowered to 1mm/h with 0.1mm per hour;
(10) stretch: when growth length reaches 70mm.Pulling rate is down to 1.5mm/h by 2.2mm/h with reduction 0.1mm per hour, according to processing requirement, determines the length that will draw;
(11) blowing out: when terminating growth, manually mention crystal and make it depart from liquid level, then stop to draw and be slowly annealed to room temperature, annealing time is 30h.
Claims (6)
1. a garnet production technique, it is characterized in that: comprise the steps: prepared by (1) raw material: by the raw material such as raw material Y2O3, AL2O3, Nd2O3 or Ce2O3, Cr2O3, Er2O3, sintered by silicon molybdenum retort furnace, sintering temperature is 1400-1500 degree Celsius, and constant temperature 30 hours, remove moisture and other dirts;
(2) compression moulding: by the above-mentioned raw material prepared after automatic mixing machine batch mixing, be pressed into wafer type by press;
(3) shove charge: by burner hearth and graphite electrode plate wiped clean, by neat for parts assembling each in stove;
(4) vacuumize: before vacuum extraction, first check that whether vent valve is urgent, prevent from leaking gas in the process vacuumized; Start housing, open mechanical pump, vacuumize;
(5) arrange system: crystal growth adopts and automatically controls weighing system, adopt JPG auto-control software, set the concentration of crystal type, size, external form and length setting and enter software, product parameters counts computer controlled automatic processing parameter automatic growth;
(6) intensification melt: in the process of intensification melt, according to the situation that melting sources stays, promotes crucible position slowly, raw material is evenly melted;
(7) seed crystal under: first according to situation adjustment temperature in stove, and carry out constant temperature, decline seed crystal carries out preheating simultaneously, adjustment crystal rotation is 15r/min, when after temperature-adjusting constant temperature for some time, is turned down and melt contacts by seed crystal, examine and adjust furnace temperature, constant temperature 30-60min;
(8) seeding: open lift power supply, tune pulling rate is 1.0-2.0mm/h;
(9) shouldering: in the process of shouldering, is program controlly generally negative value, and the diameter along with shouldering becomes large, and program control value also strengthens, until start to turn shoulder, when shouldering is to Φ 20mm, pulling rate is lowered to 1mm/h with 0.1mm per hour;
(10) stretch: when growth length reaches 70mm, pulling rate is down to 1.5mm/h by 1.5-2.5mm/h with reduction 0.1mm per hour, according to processing requirement, determines the length that will draw;
(11) blowing out: when terminating growth, manually mention crystal and make it depart from liquid level, then stop to draw and be slowly annealed to room temperature, annealing time is 20-40h.
2. according to garnet production technique according to claim 1, it is characterized in that: step 3 is specially: (1) should get out following article before shove charge: fix screen on urgent spanner, water level gauge, torch light, vernier callipers, pad, zirconia particles, the graphite connector cleaned up, crucible tray, table cooker, graphite pallet, graphite heater, graphite side screen, molybdenum side screen, molybdenum, graphite clamping, crucible, seed rod, centering rod, filter paper, molybdenum filament, seed crystal, dryout clean zirconium white side screen, clean gauze, alcohol, hairbrush; (2) checking burner hearth and graphite electrode plate whether wiped clean, if do not had, carrying out wiping with dipping in spirituous clean gauze; Check graphite electrode plate horizontality with water level gauge, Row sum-equal matrix of going forward side by side, graphite electrode plate horizontal plane and front-back are all up to the standard requirement; (3) aluminum oxide side screen is loaded onto, being tightened by graphite connector is fixed in underdrive, table cooker is installed on crucible tray, and one deck zirconia particles is spread uniformly on crucible tray, crucible tray entirety is forwarded on graphite connector, and carry out checking and adjustment level, crucible is placed on crucible tray, measuring and adjustation level; Dress graphite heater, uses graphite clamping itself and graphite electrode plate to be tightened, makes it contact well; Crucible is placed on crucible tray, surveys level peace crucible position and record; According to the height of graphite side screen, select the pad of three same thickness to be placed on graphite electrode plate, require that the difference of altitude on heating element and the upper edge of graphite side screen is 2-3mm, graphite side screen successively, molybdenum side is shielded, and requires that side is shielded and keeps concentric(al) circles with graphite heater, put screen and survey seeding crucible position and record.
3. according to garnet production technique according to claim 1, it is characterized in that: step 4 is specially: start housing, open mechanical pump, three-way valve is slowly pulled open, when vacuum tightness reaches-0.06MPa, open three-way valve completely, wait 5-10 minute and open vacuum measuring gauge, as 15Pa, close three-way valve, open recirculated water, open diffusion pump, open flapper valve; When vacuum tightness reaches 1-0.1Pa, record vacuum values, preheats, first opens heating power supply, manually rise OP value, make current voltmeter have startup, then to arrange Prl be 3600uv/h, PL1 is 3mv, continues to vacuumize.
4. according to garnet production technique according to claim 1, it is characterized in that: step 6 is specially: when raw material collapse put down in crucible time, rise to optical flat crucible position, continue to observe material situation, and slowly promote crucible position according to material situation, when floating block in crucible is less than Φ 20mm, rises in seeding crucible, and be deflated to 20KPa; After rising to seeding crucible position, slowly adjust temperature variation, temperature adjustment has just been melted to floating block, constant temperature homogenizing.
5. according to garnet production technique according to claim 1, it is characterized in that: be filled with argon gas in described smelting furnace, smelting furnace adopts graphite resistance heating.
6. according to garnet production technique according to claim 1, it is characterized in that: described garnet crystal grows in molybdenum crucible.
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| US4957712A (en) * | 1989-05-30 | 1990-09-18 | Nkk Corporation | Apparatus for manufacturing single silicon crystal |
| CN101671844A (en) * | 2009-09-30 | 2010-03-17 | 中国科学院安徽光学精密机械研究所 | Ca, Mg, Zr, Gd and Ga garnet doped with Sm and melt method crystal growth method thereof |
| CN103409805A (en) * | 2013-08-13 | 2013-11-27 | 安徽环巢光电科技有限公司 | Yttrium aluminum garnet crystal doped with neodymium, cerium and chromium, and preparation method thereof |
| CN103710755A (en) * | 2013-12-27 | 2014-04-09 | 中国科学院合肥物质科学研究院 | Rare earth co-doping activated yttrium-aluminum-scandium garnet luminescent material and melt crystal growth method thereof |
| 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 |
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