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CN1292106C - Growth method of yttrium aluminate crystal - Google Patents

Growth method of yttrium aluminate crystal Download PDF

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CN1292106C
CN1292106C CN 200510027322 CN200510027322A CN1292106C CN 1292106 C CN1292106 C CN 1292106C CN 200510027322 CN200510027322 CN 200510027322 CN 200510027322 A CN200510027322 A CN 200510027322A CN 1292106 C CN1292106 C CN 1292106C
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crystal
diameter
cooling
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growth
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CN1724724A (en
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王俊
陆燕玲
孙宝德
杨扬
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Shanghai Jiao Tong University
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Abstract

一种属于光电子材料技术领域的铝酸钇晶体的生长方法，本发明在YAP晶体生长后期，即晶体等径部分达到预定尺寸后，为避免晶体开裂，减慢提拉速度，缓慢升温使晶体直径逐渐变细，待晶体直径达到6-8mm时，然后恒温生长晶体一段时间，最后分六阶段缓慢降至室温，在降温过程中，若晶体已被拉出保温罩，则将提拉速度设置为零，若没有被拉出保温罩，则继续上引，为防止晶体被扭断，埚内余料凝固前需关掉晶转，开炉后取出坩埚，此时晶体与坩埚内余料粘在一起，将晶体与熔体在细径处分离，即可得到完整的YAP晶体。本发明简单易行，可操作性强，不但减少了晶体开裂的几率，而且提高了铝酸钇晶体的成品率和光学均匀性，节约了电能，降低了生产成本。A method for growing yttrium aluminate crystals belonging to the technical field of optoelectronic materials. In the later stage of YAP crystal growth, that is, after the equal-diameter part of the crystal reaches a predetermined size, in order to avoid crystal cracking, the pulling speed is slowed down, and the temperature is slowly raised to make the crystal diameter Gradually become thinner, when the diameter of the crystal reaches 6-8mm, then grow the crystal at a constant temperature for a period of time, and finally slowly drop to room temperature in six stages. During the cooling process, if the crystal has been pulled out of the heat preservation cover, set the pulling speed to Zero, if it is not pulled out of the insulation cover, continue to lead upwards. In order to prevent the crystal from being twisted, the crystal rotor should be turned off before the remaining material in the crucible solidifies, and the crucible should be taken out after the furnace is turned on. Together, the crystal and the melt are separated at a small diameter, and the complete YAP crystal can be obtained. The invention is simple and easy to operate, and has strong operability, not only reduces the probability of crystal cracking, but also improves the yield and optical uniformity of the yttrium aluminate crystal, saves electric energy and reduces production costs.

Description

The growth method of yttrium aluminate crystal
Technical field
What the present invention relates to is a kind of method of photoelectron material technical field, specifically, and a kind of growth method of yttrium aluminate crystal.
Background technology
YAP (yttrium aluminate) is a kind of laser crystals substrate material of excellent property, and molecular formula is YAlO 3, the Y-O bond distance in the YAP crystalline structure in the oxygen dodecahedron (2.65 ) is greater than the Y-O bond distance (2.45 ) in YAG (yttrium aluminum garnet) crystal, and this matrix structure helps mixing of active ions.And Y 3+Ionic radius and rare earth ion radius are comparatively approaching, therefore mix the Nd of certain number 3+, Ho 3+, Tm 3+, Er 3+Y in the ionic replacement YAP lattice 3+Case, can not cause that big distortion takes place lattice; YAP matrix also can be mixed transition group ion (Fe simultaneously 3+, Co 3+, Ni 3+) make laser crystals as activator, Al in these transition group ionic replacement YAP lattice 3+Case.Because the anisotropy of YAP crystallophy character, its thermal expansivity is quite big along different crystallographic axis differences, is respectively 4.2 * 10 along a, b, c axle thermal expansivity -6/ ℃, 11.7 * 10 -6/ ℃, 5.1 * 10 -6/ ℃, so the YAP serial crystal very easily ftractures under bigger thermograde.When adopting Czochralski grown crystal, after crystalline size reaches predetermined length, usually adopt quick crystal pulling method or manual crystal pulling method to make crystal break away from melt.But crystal will be subjected to very big thermal shocking in the moment that breaks away from melt, easily make crystal cracking occur.
Find through literature search prior art, Chinese patent publication number: 1544711, denomination of invention is: the growth method of gadolinium silicate single crystal, this method is grown the later stage at gadolinium orthosilicate, take certain tailing-in technique to make crystalline afterbody and shoulder shape symmetry, can reduce the probability of crystal cleavage.But it is comparatively complicated that this method actually operating is got up, and choosing of laser bar be that whether beautiful tail shape is in the crystalline equal-diameter part, its actual having little significance.In addition, though this patent has also been mentioned slow cooling, do not provide concrete working method.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of yttrium aluminate laser crystalline growth method is provided, make it solve the easy rimose problem of crystal, improve the crystal yield rate.
The present invention is achieved by the following technical solutions, the present invention is in Czochralski grown, take following ending cooling process: in the YAP crystal growth later stage, after promptly the crystal equal-diameter part reaches predetermined size, for avoiding crystal cleavage, pull rate slows down, reduce to 1.0mm/h by 1.5mm/h, slowly heating up is tapered crystal diameter, when treating that crystal diameter reaches 6-8mm, constant temperature is grown for some time then, length is 8-10mm, divides for six stages slowly reduced to room temperature at last, in temperature-fall period, if crystal has been drawn out stay-warm case, then pull rate is set to zero, if be not drawn out stay-warm case, draws on then continuing, for preventing that crystal from being twisted off, need turn off brilliant the commentaries on classics before clout solidifies in the crucible, take out crucible after the blow-on, the interior clout of this moment crystal and crucible sticks together, crystal is separated at place, thin footpath with melt, can obtain complete YAP crystal.
Concrete steps of the present invention are as follows:
(1) adopt Frequency Induction Heating Czochralski grown yttrium aluminate crystal, heating element is an iridium crucible, and raw material is Al 2O 3(99.995%), Y 2O 3(99.999%), is doped to high-purity rare earth oxide Tm 2O 3(99.999%) or Nd 2O 3(99.999%).Raw material through claim to join, grind be mixed even after, be compacted into piece on the hydropress and sintering generation solid state reaction under 1300 ℃ of high temperature, the raw material that sinters places iridium crucible, and with following direction: the YAP seed crystal of [100], [010] or [001] is packed in the seed chuck, in the monocrystalline burner hearth of packing in the lump;
(2) single crystal growing furnace pumping high vacuum is made stay-warm case and lagging material with zirconium white, adopts protection of inert gas; 1900 ℃ of growth temperatures, pull rate 1.5mm/h, crystal rotating speed 25rpm; and adopt sapphire sheet and corundum sheet to build better heat-insulation system, the thermal field that is fit to crystal growth is provided.
(3) strict carry out roasting brilliant, sow, necking down, slowly shouldering, receive shoulder, balanced isometrical stage of control, the especially isometrical stage, even diameter changes, also to be controlled to gradual change, avoid forming cracking because of the crystal diameter sudden change causes internal stress to concentrate.
(4) after the crystal equal-diameter part reaches predetermined size, slowly finish up.For avoiding crystal cracking to occur, the pull rate that slows down is reduced to 1.0mm/h by 1.5mm/h, and slowly heating up is tapered crystal diameter, when treating that crystal diameter reaches 6-8mm, and constant temperature growing crystal length 8-10mm.
(5) divided for six stages slowly reduced to room temperature.In temperature-fall period, if crystal has been drawn out stay-warm case, then pull rate is set to zero; If be not drawn out stay-warm case, draw on then continuing.For preventing that crystal from being twisted off, need turn off brilliant the commentaries on classics before clout solidifies in the crucible.Take out crucible after the blow-on, the interior clout of this moment crystal and crucible sticks together, and crystal is separated at place, thin footpath with melt.Concrete cool-down method is as follows:
1. 15 ℃/h, cooling continues 6h, 1900 ℃-1810 ℃;
2. 20 ℃/h, cooling continues 9h, 1810 ℃-1630 ℃;
3. 25 ℃/h, cooling continues 10h, 1630 ℃-1380 ℃;
4. 30 ℃/h, cooling continues 12h, 1380 ℃-1020 ℃;
5. 38 ℃/h, cooling continues 15h, 1020 ℃-450 ℃;
6. 55 ℃/h, cooling continues 8h, 450 ℃-room temperature.
Temperature-fall period amounts to 60h, cooling rate 15-55 ℃/h.If cooling rate is too fast,, also be prone to cracking even original crystal is fine.If adopt constant cooling at a slow speed always, then waste electric energy, increase production cost.
The crystal growth later stage is adopted above-mentioned ending and cooling process, has significantly reduced the probability of crystal cleavage.Think: epilogue lifts the thermal shocking that crystal is caused when having avoided crystal growth to finish fast, has reduced intracrystalline thermograde, has effectively improved its thermal field, makes crystal avoid growing under the rimose thermal field condition helping; On the other hand, multistage cooling process has reduced to occur in the convection current of cold and hot atmosphere in the growth chamber, and remaining crystal has suitable thermograde, has overcome the serious rimose phenomenon of crystal.Slowly cooling also is a kind of method for annealing simultaneously, not only can reduce the probability of crystal cleavage, also can improve the crystalline optical homogeneity.So after adopting aforesaid method, significantly reduced the crystal cleavage phenomenon.Under these conditions we can successfully grow do not ftracture, YAP crystal that integrity is good.
The present invention has overcome the problem that original YAP crystal easily causes cracking defect, and is simple, workable, not only reduced the probability of crystal cleavage, and improved the yield rate and the optical homogeneity of yttrium aluminate crystal, saved electric energy, reduced production cost.
Embodiment
Embodiment 1: induction heating Czochralski grown b axle Tm:YAP crystal.
Utilize Frequency Induction Heating, in the Iridium Crucible of Φ 66 * 45mm, put into the Tm:YAP raw material 590g of tablet forming, charge into 99.999% high pure nitrogen behind the body of heater pumping high vacuum, adopt crystal pulling method, growth b axialite body as shielding gas.Growth velocity 1.5mm/h, rotating speed 25rpm controls protruding interface growth.When the crystal equal-diameter part reached 70mm, directly manually quick pulling crystal broke away from itself and melt, obtains a transparent b axle Tm:YAP crystal, and weight is 200g.Crystal is pale brown look, local cracking phenomena occurs.
Embodiment 2: the multistage induction heating Czochralski grown b axle Tm:YAP crystal of slowly lowering the temperature.
Utilize Frequency Induction Heating, in the Iridium Crucible of Φ 66 * 45mm, put into the Tm:YAP raw material 590g of tablet forming; charge into 99.999% high pure nitrogen behind the body of heater pumping high vacuum as shielding gas; adopt crystal pulling method, select for use b axle YAP crystal to make seed crystal, growth Tm:YAP crystal.Growth velocity 1.5mm/h, rotating speed 25rpm controls protruding interface growth.When the crystal equal-diameter part reached 70mm, pull rate slowed to 1.0mm/h, and slowly heating up is tapered crystal diameter, and when treating that crystal diameter reaches 6-8mm, constant temperature is grown for some time then, length 8-10mm.Divided for six stages slowly reduced to room temperature at last.This moment, crystal was not pulled out stay-warm case, drew in the continuation, when clout is near curdled appearance by the time, stopped brilliant the commentaries on classics.Take out crucible after the blow-on, crystal is separated at place, thin footpath with melt, obtaining one ruler very little is the b axle Tm:YAP crystal of Φ 21 * 100mm, and weight is 250g.Crystal is pale brown look, does not see cracking phenomena, and integrity is good, and scattering particles are few, and optical property is preferably arranged.
Embodiment 3: the multistage induction heating Czochralski grown c axle Tm:YAP crystal of slowly lowering the temperature.
Utilize Frequency Induction Heating, in the Iridium Crucible of Φ 66 * 45mm, put into the Tm:YAP raw material 590g of tablet forming; charge into 99.999% high pure nitrogen behind the body of heater pumping high vacuum as shielding gas; adopt crystal pulling method, select for use c axle YAP crystal to make seed crystal, growth Tm:YAP crystal.Growth velocity 1.5mm/h, rotating speed 25rpm controls protruding interface growth.When the crystal equal-diameter part reaches 75mm, the pull rate that slows down, slowly heating up is tapered crystal diameter, and when treating that crystal diameter reaches 6-8mm, constant temperature is grown for some time then, length 8-10mm.Divided for six stages slowly reduced to room temperature at last.This moment, crystal was not pulled out stay-warm case, drew in the continuation, when waiting clout near curdled appearance, stopped brilliant the commentaries on classics.Take out crucible after the blow-on, crystal is separated at place, thin footpath with melt, obtaining one ruler very little is the c axle Tm:YAP crystal of Φ 21 * 110mm, and weight is 270g.Crystal is pale brown look, does not see cracking phenomena, and integrity is good, and scattering particles are few, and optical property is preferably arranged.
Embodiment 4: the multistage induction heating Czochralski grown b axle Nd:YAP crystal of slowly lowering the temperature.
Utilize Frequency Induction Heating, in the Iridium Crucible of Φ 66 * 45mm, put into the Nd:YAP raw material 590g of tablet forming; charge into 99.999% high pure nitrogen behind the body of heater pumping high vacuum as shielding gas; adopt crystal pulling method, select for use b axle YAP crystal to make seed crystal, growth of Nd: the YAP crystal.Growth velocity 1.5mm/h, rotating speed 25rpm controls protruding interface growth.When the crystal equal-diameter part reaches 70mm, the pull rate that slows down, slowly heating up is tapered crystal diameter, and when treating that crystal diameter reaches 6-8mm, constant temperature is grown for some time then, length 8-10mm.Divided for six stages slowly reduced to room temperature at last.This moment, crystal was not pulled out stay-warm case, drew in the continuation, when waiting clout near curdled appearance, stopped brilliant the commentaries on classics.Take out crucible after the blow-on, crystal is separated at place, thin footpath with melt, obtaining one ruler very little is the b axle Nd:YAP crystal of Φ 21 * 100mm, and weight is 250g.Crystal is a lavender, does not see cracking phenomena, and integrity is good, and scattering particles are few.
Embodiment 5: the pure YAP crystal of induction heating Czochralski grown.
Utilize Frequency Induction Heating, in the Iridium Crucible of Φ 66 * 45mm, put into the YAP raw material 590g of tablet forming, charge into 99.999% high pure nitrogen behind the body of heater pumping high vacuum, adopt crystal pulling method, growth b axialite body as shielding gas.Growth velocity 1.5mm/h, rotating speed 25rpm controls protruding interface growth.When the crystal equal-diameter part reaches 80mm, the pull rate that slows down, slowly heating up is tapered crystal diameter, and when treating that crystal diameter reaches 6-8mm, constant temperature is grown for some time then, length 8-10mm.Divided for six stages slowly reduced to room temperature at last.Crystal will be drawn out stay-warm case this moment, draw on stopping.During near curdled appearance, stop brilliant the commentaries on classics Deng clout.Take out crucible after the blow-on, crystal is separated at place, thin footpath with melt, obtain to be of a size of the pure YAP crystal of b axle of Φ 21 * 120mm, weight is 280g.Crystal is not seen cracking phenomena, and integrity is good, and scattering particles are few.

Claims (7)

1.一种铝酸钇晶体的生长方法，其特征在于，在YAP晶体生长后期，即晶体等径部分达到预定尺寸后，减慢提拉速度，缓慢升温使晶体直径逐渐变细，待晶体直径达到6-8mm时，然后恒温生长，最后分六阶段缓慢降至室温，在降温过程中，若晶体已被拉出保温罩，则将提拉速度设置为零，若没有被拉出保温罩，则继续上引，埚内余料凝固前需关掉晶转，开炉后取出坩埚，此时晶体与坩埚内余料粘在一起，将晶体与熔体在细径处分离，即可得到完整的YAP晶体，所述的降温，是指：降温过程共计60小时，降温速度15-55℃/小时，具体方法如下：①15℃/h，降温持续6h，1900℃-1810℃；②20℃/h，降温持续9h，1810℃-1630℃；③25℃/h，降温持续10h，1630℃-1380℃；④30℃/h，降温持续12h，1380℃-1020℃；⑤38℃/h，降温持续15h，1020℃-450℃；⑥55℃/h，降温持续8h，450℃-室温。1. a growth method of yttrium aluminate crystal, it is characterized in that, in the later stage of YAP crystal growth, after the equal-diameter portion of the crystal reaches a predetermined size, the pulling speed is slowed down, and the crystal diameter is gradually thinned by slowly heating up, until the crystal diameter When it reaches 6-8mm, then grow at a constant temperature, and finally slowly drop to room temperature in six stages. During the cooling process, if the crystal has been pulled out of the heat preservation cover, set the pulling speed to zero. If the crystal has not been pulled out of the heat preservation cover, Then continue to lead upwards. Before the remaining material in the crucible solidifies, the crystal rotor needs to be turned off, and the crucible is taken out after the furnace is turned on. At this time, the crystal and the remaining material in the crucible stick together, and the crystal and the melt are separated at a small diameter to obtain a complete For YAP crystals, the mentioned cooling refers to: the cooling process is 60 hours in total, and the cooling rate is 15-55°C/hour. The specific method is as follows: ①15°C/h, cooling for 6h, 1900°C-1810°C; ②20°C/h , cooling for 9 hours, 1810°C-1630°C; ③25°C/h, cooling for 10h, 1630°C-1380°C; ④30°C/h, cooling for 12h, 1380°C-1020°C; ⑤38°C/h, cooling for 15h, 1020°C-450°C; ⑥55°C/h, cooling for 8 hours, 450°C-room temperature. 2.根据权利要求1所述的铝酸钇晶体的生长方法，其特征是，包括如下步骤：2. the growth method of yttrium aluminate crystal according to claim 1, is characterized in that, comprises the steps: (1)采用中频感应加热提拉法生长铝酸钇晶体，发热体为铱坩埚，原料为Al2O3和Y2O3，掺杂为Tm2O3或Nd2O3，原料经称配、研混均匀后，在液压机上压紧成块并在1300℃高温下烧结发生固相反应，烧结好的原料置于铱坩埚中，并将以下方向：[100]、[010]或[001]的YAP籽晶装入籽晶夹头中，一并装入单晶炉膛内；(1) The yttrium aluminate crystal is grown by medium-frequency induction heating and pulling method. The heating element is an iridium crucible, and the raw materials are Al 2 O 3 and Y 2 O 3 , doped with Tm 2 O 3 or Nd 2 O 3 . After blending and mixing evenly, press it into a block on a hydraulic press and sinter at a high temperature of 1300 ° C to undergo a solid phase reaction. The sintered raw materials are placed in an iridium crucible, and the following directions: [100], [010] or [ The YAP seed crystal of 001] is packed in the seed crystal chuck, and is packed in the single crystal hearth together; (2)单晶炉抽高真空，用氧化锆作保温罩及保温材料，采用惰性气体保护，生长温度1900℃，提拉速度1.5mm/h，晶体转速25rpm，并采用蓝宝石片及刚玉片以营造更好的保温系统，提供适合晶体生长的热场；(2) The single crystal furnace is evacuated to a high vacuum, using zirconia as the insulation cover and insulation material, using inert gas protection, the growth temperature is 1900°C, the pulling speed is 1.5mm/h, the crystal rotation speed is 25rpm, and the sapphire sheet and corundum sheet are used. Create a better thermal insulation system and provide a thermal field suitable for crystal growth; (3)严格执行烤晶、下种、缩颈、缓慢放肩、收肩、均衡控制等径阶段；(3) Strictly implement the equal-diameter stages of crystal roasting, seeding, necking, slow shouldering, shouldering, and balanced control; (4)晶体等径部分达到预定尺寸后，缓慢收尾，为避免晶体出现开裂，减慢提拉速度，缓慢升温使晶体直径逐渐变细，待晶体直径达到6-8mm时，恒温生长晶体一段时间；(4) After the equal-diameter part of the crystal reaches the predetermined size, it is slowly closed. In order to avoid cracking of the crystal, the pulling speed is slowed down, and the temperature is raised slowly to make the diameter of the crystal gradually thinner. When the diameter of the crystal reaches 6-8mm, the crystal is grown at a constant temperature for a period of time ; (5)分六阶段缓慢降至室温：在降温过程中，若晶体已被拉出保温罩，则将提拉速度设置为零，若没有被拉出保温罩，则继续上引，埚内余料凝固前需关掉晶转，开炉后取出坩埚，此时晶体与坩埚内余料粘在一起，将晶体与熔体在细径处分离。(5) Slowly drop to room temperature in six stages: during the cooling process, if the crystal has been pulled out of the heat preservation cover, set the pulling speed to zero; Before the solidification of the material, the crystal converter needs to be turned off, and the crucible is taken out after the furnace is turned on. At this time, the crystal and the remaining material in the crucible stick together, and the crystal and the melt are separated at a small diameter. 3.根据权利要求2所述的铝酸钇晶体的生长方法，其特征是，所述的Al2O3纯度为99.995％，Y2O3纯度为99.999％。3. The method for growing yttrium aluminate crystals according to claim 2, characterized in that the purity of Al 2 O 3 is 99.995%, and the purity of Y 2 O 3 is 99.999%. 4.根据权利要求2所述的铝酸钇晶体的生长方法，其特征是，所述的稀土氧化物是指：纯度为99.999％ Tm2O3或纯度为99.999％ Nd2O3。4 . The method for growing yttrium aluminate crystal according to claim 2 , wherein the rare earth oxide refers to a purity of 99.999% Tm 2 O 3 or a purity of 99.999% Nd 2 O 3 . 5.根据权利要求1或2所述的铝酸钇晶体的生长方法，其特征是，所述的提拉速度，由1.5mm/h降为1.0mm/h。5. The growth method of yttrium aluminate crystal according to claim 1 or 2, characterized in that, the pulling speed is reduced from 1.5mm/h to 1.0mm/h. 6.根据权利要求1或2所述的铝酸钇晶体的生长方法，其特征是，所述的恒温生长是指晶体长度达到8-10mm。6. The method for growing yttrium aluminate crystal according to claim 1 or 2, characterized in that, the constant temperature growth means that the crystal length reaches 8-10 mm. 7.根据权利要求2所述的铝酸钇晶体的生长方法，其特征是，所述的均衡控制等径阶段是指：即使直径有变化，也要控制成渐变的，避免因晶体直径突变造成内部应力集中而形成开裂。7. The growth method of yttrium aluminate crystal according to claim 2, characterized in that, the equal-diameter stage of balanced control refers to: even if the diameter changes, it should be controlled to gradually change, so as to avoid the sudden change of crystal diameter. Cracks are formed due to internal stress concentration.
CN 200510027322 2005-06-30 2005-06-30 Growth method of yttrium aluminate crystal Expired - Fee Related CN1292106C (en)

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US8438893B2 (en) 2006-10-26 2013-05-14 Industrial Origami, Inc. Method of forming two-dimensional sheet material into three-dimensional structure
US8505258B2 (en) 2000-08-17 2013-08-13 Industrial Origami, Inc. Load-bearing three-dimensional structure

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CN106319635A (en) * 2016-09-30 2017-01-11 中国电子科技集团公司第二十六研究所 Method for enhancing light output of cerium-doped lutetium yttrium aluminate (LuYAP) scintillation crystals
CN107841789A (en) * 2017-09-19 2018-03-27 同济大学 Yttrium aluminate visible waveband laser crystal that a kind of dysprosium terbium is co-doped with and preparation method thereof
CN108018601A (en) * 2017-12-19 2018-05-11 清远先导材料有限公司 Crystal growing apparatus, growing method and its application
CN108330541A (en) * 2018-01-19 2018-07-27 暨南大学 A kind of GYAP laser crystals and preparation method thereof
CN108893778A (en) * 2018-07-16 2018-11-27 苏州四海常晶光电材料有限公司 A kind of ABO3Mixed crystal and growing method

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US8114524B2 (en) 2002-09-26 2012-02-14 Industrial Origami, Inc. Precision-folded, high strength, fatigue-resistant structures and sheet therefor
US8377566B2 (en) 2002-09-26 2013-02-19 Industrial Origami, Inc. Precision-folded, high strength, fatigue-resistant structures and sheet therefor
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