CN1445388A - Preparation method of neodymium-doped yttrium aluminate and yttrium aluminate composite laser crystal - Google Patents
Preparation method of neodymium-doped yttrium aluminate and yttrium aluminate composite laser crystal Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000012047 saturated solution Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 230000012010 growth Effects 0.000 claims description 33
- 230000006798 recombination Effects 0.000 claims description 26
- 238000005215 recombination Methods 0.000 claims description 26
- 238000000137 annealing Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 239000002178 crystalline material Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000012856 packing Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 230000007423 decrease Effects 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 230000007306 turnover Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract 1
- 230000004907 flux Effects 0.000 abstract 1
- 238000004943 liquid phase epitaxy Methods 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 description 11
- 230000000694 effects Effects 0.000 description 6
- 239000004568 cement Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000011555 saturated liquid Substances 0.000 description 2
- 230000001225 therapeutic effect Effects 0.000 description 2
- 241000931526 Acer campestre Species 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 230000000025 haemostatic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 244000144985 peep Species 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
一种掺钕铝酸钇和铝酸钇复合激光晶体的制备方法，其特征在于它是将晶面方向为(010)或(100)或(001)的Nd：YAP单晶衬底作大面积籽晶，在YAP单晶的结晶温度下，在电阻加热液相外延炉中与含有YAP多晶料的助熔剂饱和溶液接触的两个界面上生长等厚的YAP单晶，形成YAP/Nd：YAP/YAP复合激光晶体，该晶体的两种晶体间无明显分界、晶体完整性好、重复性好。本发明适宜批量生产，能够满足激光器件制造上的市场需求，具有良好的经济效益。
A preparation method of neodymium-doped yttrium aluminate and yttrium aluminate composite laser crystal is characterized in that it uses a Nd:YAP single crystal substrate with a crystal plane direction of (010) or (100) or (001) as a large area Seed crystal, at the crystallization temperature of YAP single crystal, grow YAP single crystal of equal thickness on the two interfaces in contact with the flux saturated solution containing YAP polycrystalline material in the resistance heating liquid phase epitaxy furnace to form YAP/Nd: YAP/YAP composite laser crystal, there is no obvious boundary between the two crystals of this crystal, the crystal integrity is good, and the repeatability is good. The invention is suitable for batch production, can meet the market demand in the manufacture of laser devices, and has good economic benefits.
Description
Technical field:
The invention relates to neodymium-doped yttrium aluminate (Nd:YAP) and yttrium aluminate (YAP) recombination laser crystalline preparation method.Relate to the pure yttrium aluminate of both ends of the surface growth particularly, be combined into the recombination laser crystalline material of neodymium-doped yttrium aluminate and yttrium aluminate: YAP/Nd:YAP/YAP at neodymium-doped yttrium aluminate monocrystalline.
Background technology:
Neodymium-doped yttrium aluminate (Nd:YAP) laser crystals is the novel laser crystal that comes out at the initial stage seventies.Except to the Nd:YAG laser crystals has similar thermomechanical property, Nd:YAP also have the wide energy storage of photoluminescence line big, can output polarization laser and optical maser wavelength with crystallographic axis to different and equal characteristics.Especially, Nd:YAP can export the laser of 1.34um, this wavelength laser has the advantage that the 1.06um haemostatic effect is good and the 10.6um laser cutting is fast concurrently. interior peep in the operation safe and reliable, can be widely used in the laser medicine therapeutic equipment (referring to people's such as Shen Hong unit of Fujian Inst. of Matter Structure, Chinese Academy of Sciences patent, " a kind of laser cure apparatus ", notification number are 1335117).Utilize the polarized light 1.079um of the Nd:YAP crystal output of b axle can make the ophthalmology laser therapeutic equipment of certain characteristic simultaneously.
Because the Nd ion has more excited state, quantum yield is little, therefore the radiationless transition probability is big, and electronics transits to upper laser level from highly excited level will produce a large amount of heats, tends to thermal lensing effect occur and the efficient and the beam quality that influence laser at Nd activated gain media.Equally, in the Nd:YAP crystal, also there is such problem.People adopt usually optical cement bonding or adopt improved crystal pulling method etc. at the two ends of gain medium the bonding or pure laser host material of growing to improve laser characteristics, for example, propose at the pure YAG crystalline of Nd:YAG laser bar two ends optical cement composite structure people such as R..Weber in 1998, on the one hand, pure YAG crystal is absorptive pumping light or oscillation light not, gain media be can effectively cool off, heat effect and thermal lensing effect reduced; On the other hand, at pure YAG rod two ends plated film, the laser damage threshold that improves rete there is positive effect, thereby improved the laser activity of Nd:YAG greatly, reduced laser threshold (referring to IEEE Journal of Quantum Electronics, the 6th phase, the 34th the volume, 1998 the 1046th page).People such as D.Ehrentraut in 2002 have reported with improved crystal pulling method in pure YAG pipe growth inside Yb doped YAG (Journal of Crystal the 242nd phase of Growth, 2002 years the 375th page) etc.Adopt can the grow composite laser material of YAG/Nd:YAG/YAG of these methods.
Yet, adopt the composite laser material of above-mentioned prior art for preparing, significant disadvantages is arranged: the composite laser material that (1) forms by optical coupled agent or direct superimposed optical cement, because the mismatch of optical coupled agent and single crystal, and have significantly boundary between pure crystal and doped crystal, optical loss is big; (2) with the composite single crystal of growths such as the crystal pulling method that has improved, the complicated control difficulty of equipment, crystal mass is poor, have defectives such as a large amount of bubbles and wrap, and repeatability is low, does not obtain practical application so far in device.
Summary of the invention:
Shortcomings such as the optical loss that the problem to be solved in the present invention is to overcome prior art for preparing recombination laser crystalline material is big, of poor quality, repeatability is low, a kind of preparation method of YAP/Nd:YAP/YAP recombination laser crystalline material is proposed, to enhance productivity, satisfy the needs of growing Laser Devices manufacturing technology.
Technical solution of the present invention is as follows:
A kind of neodymium-doped yttrium aluminate and yttrium aluminate recombination laser crystalline preparation method, its fundamental point is that crystal plane direction is made the big area seed crystal for the Nd:YAP single crystalline substrate of (010) or (100) or (001), under the Tc of YAP monocrystalline, in resistive heating rheotaxy stove with two interfaces that the fusing assistant saturated solution that contains the YAP polycrystal contacts on the YAP monocrystalline of growth uniform thickness.
This is that the preparation of YAP/Nd:YAP/YAP recombination laser crystalline adopts resistive heating rheotaxy stove to carry out, its structure mainly comprises: body of heater, the body of heater bottom is a main furnace body, upper of furnace body is the annealing body of heater, central authorities are equipped with crucible in body of heater, crucible is coaxial with body of heater, be provided with the side heating element around the crucible relatively in the main furnace body, the periphery of side heating element is a thermal insulation layer, thermal insulation layer is arranged under the crucible and can regulate crucible collet just, have in the annealing furnace upside heating element (, main furnace body also is provided with middle temperature thermocouple, and annealing furnace is provided with temperature thermocouple, is extended with a rotary pulling bar under the upper top cover mediad of body of heater, the lower end of this rotary pulling bar is a substrate clamp, and the rotary pulling bar is coaxial with body of heater.
The described proportioning raw materials that contains YAP polycrystal fusing assistant saturated solution is as follows:
1. the set of dispense of fusing assistant solution is than being the PbO of 10-13mol and lmol B
2O
3, or 8-12molBi
2O
3B with 1-3mol
2O
3
2. the weight percent of YAP polycrystalline and fusing assistant is: YAP/ fusing assistant solution=10wt%-50wt%
Neodymium-doped yttrium aluminate and yttrium aluminate recombination laser crystalline preparation method comprise following concrete steps:
＜1〉according to the selected YAP polycrystalline and the proportioning raw materials weighing of fusing assistant, in the crucible of packing into after thorough mixing is even and in the body of heater of packing into;
＜2〉crystal plane direction is inserted in the substrate clamp for the substrate wafer of the Nd:YAP of (100) or (010) or (001), adjusted the rotary pulling bar, make it to be on the coaxial position of crucible;
＜3〉heat-up rate with 100 ℃/Hr is warming up to 1000～1150 ℃, fused raw material YAP and fusing assistant PbO-B
2O
3Or Bi
2O
3-B
2O
3, make it become saturated solution, treat all dissolvings after, 1050～1150 ℃ of constant temperature 5 hours;
＜4〉the rotary pulling bar that descends gradually drops to from saturated fusing assistant liquid level 3～5mm place substrate wafer, again constant temperature 2～4 hours under 900～1050 ℃ of conditions of YAP crystallization range;
＜5〉decline rotary pulling bar immerses in the homothermic saturated solution substrate wafer fully, the rotary pulling bar rotates with 100～250r/min speed, regulate corresponding growth time according to required growth YAP crystal face thickness, after growth time finishes, mention the rotary pulling bar immediately, make substrate make it break away from liquid level;
＜6〉annealing, the rotary pulling bar will be continued to mention, make substrate wafer and precipitating thereof uniform thickness YAP monocrystalline thereon enter the interior upside heating element interval of annealing furnace, the power of heating element makes its temperature at 900 ℃ of constant temperature after 5 hours in the adjustment, be cooled to room temperature with 50 ℃/Hr speed then, finish the preparation of YAP/Nd:YAP/YAP composite laser material.
Technique effect of the present invention is as follows:
The present invention compared with prior art on the one hand, compares with existing optical coupled agent directly superimposed (optical cement), and there are not lattice mismatch in Nd:YAP and YAP direct growth, do not have tangible interface, optical loss is very little together; On the other hand, compare with the existing composite single crystal that improves growth such as crystal pulling method, do not have obviously between two kinds of crystal of YAP/Nd:YAP/YAP of liquid phase epitaxial method growth demarcate, good, the good reproducibility of perfection of crystal.Suitable batch of the present invention is produced, and can satisfy the market requirement that Laser Devices are made, and has good economic benefit.
Description of drawings:
Fig. 1 is that the present invention prepares the used growing apparatus sectional view of YAP/Nd:YAP/YAP recombination laser crystalline material.
Embodiment:
A kind of neodymium-doped yttrium aluminate and yttrium aluminate recombination laser crystalline preparation method, be characterized in crystal plane direction is made the big area seed crystal for the Nd:YAP single crystalline substrate of (010) or (100) or (001), under the Tc of YAP monocrystalline, with the YAP monocrystalline of growth uniform thickness on two interfaces that the fusing assistant saturated solution that contains the YAP polycrystal contacts.
Preparation YAP/Nd:YAP/YAP recombination laser crystal carries out in resistive heating rheotaxy stove, and the structure of this stove mainly comprises: body of heater 1, and body of heater 1 bottom is a main furnace body 101, body of heater 1 top is annealing body of heater 102.In body of heater 101, central authorities are equipped with crucible 9, crucible 9 is coaxial with body of heater 1, be provided with side heating element 2 around the crucible 9 relatively in the main furnace body 101, the periphery of side heating element 2 is a thermal insulation layer 11, thermal insulation layer 13 is arranged under the crucible 9 and can regulate crucible 9 collet 12 just, upside heating element 5 is arranged in the annealing furnace 102, main furnace body 101 also is provided with middle temperature thermocouple 3, annealing furnace 102 is provided with temperature thermocouple, be extended with a rotary pulling bar 6 under the upper top cover mediad of body of heater 1, the lower end of this rotary pulling bar 6 is a substrate clamp 7, and rotary pulling bar 6 is coaxial with body of heater 1.
The described proportioning raw materials that contains YAP polycrystal fusing assistant saturated solution is as follows:
1. the set of dispense of fusing assistant solution is than being the PbO of 10-13mol and lmol B
2O
3, or 8-12molBi
2O
3B with 1-3mol
2O
3
2. the weight percent of YAP polycrystalline and fusing assistant is: YAP/ fusing assistant solution=10wt%-50wt%
The preparation method of YAP/Nd:YAP/YAP recombination laser crystalline material of the present invention mainly contains following two kinds: a kind of method can be described as " two-sided pickling process ", just in grow the simultaneously method of pure YAP monocrystalline of Nd:YAP crystalline both ends of the surface; Another kind method can be called " single-side impregnated method ", the first pure YAP monocrystalline of growth on end face of Nd:YAP crystalline just, and then on its another corresponding end face the method for the YAP monocrystalline of growth equal thickness.
The inventive method comprises following concrete steps:
＜1〉according to the selected YAP polycrystalline and the proportioning raw materials weighing of fusing assistant, in the crucible 9 of packing into after thorough mixing is even and in the body of heater 1 of packing into;
＜2〉crystal plane direction is inserted in the substrate clamp 7 for the substrate wafer 8 of the Nd:YAP of (100) or (010) or (001), adjusted rotary pulling bar 6, make it to be on the coaxial position of crucible 9;
＜3〉heat-up rate with 100 ℃/Hr is warming up to 1000～1150 ℃, fused raw material YAP and fusing assistant PbO-B
2O
3Or Bi
2O
3-B
2O
3Make it become saturated solution 10, treat all dissolvings after, 1050～1150 ℃ of constant temperature 5 hours;
＜4〉the rotary pulling bar 6 that descends gradually drops to from saturated fusing assistant liquid level 3～5mm place substrate wafer 8, again constant temperature 2～4 hours under 900～1050 ℃ of conditions of YAP crystallization range;
＜5〉decline rotary pulling bar 6 immerses in the homothermic saturated solution 10 substrate wafer 8 fully, rotary pulling bar 6 rotates with 100～250r/min speed, regulate corresponding growth time according to required growth YAP crystal face thickness, after growth time finishes, mention rotary pulling bar 6 immediately, make substrate 8 make it break away from liquid level;
＜6〉annealing, rotary pulling bar 6 will be continued to mention, make substrate wafer 8 and precipitating thereof uniform thickness YAP monocrystalline thereon enter upside heating element 5 intervals in the annealing furnace 102, the power of heating element 5 makes its temperature at 900 ℃ of constant temperature after 5 hours in the adjustment, be cooled to room temperature with 50 ℃/Hr speed then, finish the preparation of YAP/Nd:YAP/YAP composite laser material.
Preparation YAP/Nd:YAP/YAP recombination laser crystal, also can adopt single-side impregnated method, promptly earlier as stated above＜1,＜2 〉,＜3 〉,＜4〉step carries out, and step＜5 be the heating power of adjusting the side heating element 2 of main furnace body 101, temperature thermocouple 3 is designated as 900～1050 ℃ in making, constant temperature 1～2h again, rotary pulling bar 6 then descends, the lower surface of substrate wafer 8 is contacted with homothermic saturated solution 10, this rotary pulling bar 6 is with the rotation of the speed of 100～250r/min, regulates corresponding growth time according to the thickness of the YAP crystal face of required growth, and growth time finishes, mention rotary pulling bar 6 immediately, make substrate wafer 8 break away from liquid level;
＜6〉the annealing back obtains single-ended YAP/Nd:YAP crystalline material with YAP crystal layer;
＜7〉will insert once more in the substrate clamp 7 behind prepared substrate wafer 8 turn-overs, adjust rotary pulling bar 6 and make it to be on the coaxial position of crucible 9;
＜8〉through step＜3〉＜4＜5＜6 after finish the preparation of YAP/Nd:YAP/YAP recombination laser crystalline material.
Embodiment 1: the concrete steps of " two-sided pickling process " preparation YAP/Nd:YAP/YAP recombination laser crystalline material are as follows:
Selected resistive heating rheotaxy stove device as shown in Figure 1, the crucible 9 in the main body stove 101 is a platinum crucible.According to above-mentioned step of preparation process＜1〉with polycrystal raw material YAG and solubility promoter (PbO: B
2O
3=10mol: 1mol) be YAP/ (PbO+B by weight percentage
2O
3The proportioning of)=0.20 is carried out weighing 1000g altogether, in the platinum crucible 9 of the φ 80 * 80mm that packs into after mixing; By processing step＜2〉will be of a size of φ 30 * 0.5mm, crystal plane direction places in the anchor clamps 7 for the Nd:YAP substrate 8 of (010), and with anchor clamps 7 rotary pulling bar 6 bottoms of packing into, the position of adjusting crucible 9 and substrate wafer 8 makes it coaxial, and all is in the central authorities of main furnace body 101; By above-mentioned steps＜.3〉body of heater 101 is warming up to 1150 ℃, make raw material and fusing assistant be melt into saturated solution 10, and at 1150 ℃ of constant temperature after 5 hours, the rotary pulling bar 6 that descends gradually set by step＜4 〉, make substrate wafer 8 apart from saturated liquid level 4mm, again constant temperature 3 hours under 950 ℃ of temperature of YAP crystallization range; By above-mentioned processing step＜5〉decline rotary pulling bar 6 immerses in the saturated solution 10 substrate wafer 8 fully, and rotary pulling bar 6 is rotated with 200r/min speed, after constant temperature under 950 ℃ of temperature was grown 5 hours, lift from rapidly rotary pulling bar 6 make substrate wafer and on monocrystalline break away from liquid level, crystallization is so far finished; By above-mentioned processing step＜6〉anneal, the YAP monocrystalline of growth is lifted to heating element 5 intervals of body of heater 1 top annealing furnace 102 together with substrate wafer 8, constant temperature is after 5 hours under 900 ℃ of temperature, be cooled to room temperature with 50 ℃/Hr speed, annealing finishes, and the preparation of YAP/Nd:YAP/YAP recombination laser crystalline material finishes.
Embodiment 2: the step of " single-side impregnated method " growth YAP/Nd:YAP/YAP recombination laser crystalline material is as follows:
According to step＜1 in the foregoing description 1〉with YAP polycrystal and solubility promoter (Bi
2O
3: B
2O
3=8mol: 2mol) be YAG/ (Bi by weight percentage
2O
3+ B
2O
3The proportioning of)=0.40 is carried out weighing 1000g altogether, repeat step＜2 in the foregoing description 1 〉, by in the foregoing description 1＜.3 body of heater 101 is warming up to 1100 ℃, make raw material and fusing assistant be melt into saturated solution 10, and at 1100 ℃ of constant temperature after 5 hours, by in the foregoing description 1＜4 rotary pulling bar 6 gradually descends, make substrate wafer 8 apart from saturated liquid level 4mm, constant temperature 3 hours under 1000 ℃ of temperature of YAP crystallization range again, by in the foregoing description 1＜5〉decline rotary pulling bars 6 make an end face of substrate wafer 8 contact with saturated solution 10 liquid levels, and rotary pulling bar 6 is rotated with 200r/min speed, after constant temperature under 1000 ℃ of temperature was grown 5 hours, lift from rapidly rotary pulling bar 6 make substrate wafer and on monocrystalline break away from liquid level, crystallization is so far finished; Step＜6 by the foregoing description 1〉to anneal, the YAP monocrystalline that is about to growth lifts to the hot zone of body of heater 1 top annealing furnace 102 together with substrate wafer 8, and constant temperature was cooled to room temperature with 50 ℃/Hr speed after 5 hours under 900 ℃ of temperature, and annealing finishes; Obtain single-ended YAP/Nd:YAP with YAG crystal layer, prepared substrate material is inserted in the substrate clamp 7 after together with the monocrystalline turn-over once more, adjust rotary pulling bar 6, make it to be in the coaxial position of crucible 9, repeat above＜3 〉～＜6〉step (wherein growth times and above-mentioned＜5〉growth time identical), obtain uniform thickness YAP monocrystalline, finish the preparation of YAP/Nd:YAP/YAP composite laser material.
Behind the YAP/Nd:YAP/YAP recombination laser crystalline material cutting of aforesaid method growth, round as a ball, processing, plated film, make all-solid state continuous laser, laser apparatus has good laser activity, low laser threshold.This recombination laser crystal has wide application background in fields such as high power laser systems.
Claims (5)
1. a neodymium-doped yttrium aluminate (hereinafter to be referred as Nd:YAP) and yttrium aluminate (hereinafter to be referred as YAP) recombination laser crystalline preparation method, it is characterized in that it is that crystal plane direction is made the big area seed crystal for the Nd:YAP single crystalline substrate of (010) or (100) or (001), under the Tc of YAP monocrystalline, in resistive heating rheotaxy stove with two interfaces that the fusing assistant saturated solution that contains the YAP polycrystal contacts on the YAP monocrystalline of growth uniform thickness.
2. Nd:YAP according to claim 1 and YAP recombination laser crystalline preparation method, the structure that it is characterized in that preparing the resistive heating rheotaxy stove that YAP/Nd:YAP/YAP recombination laser crystal adopted mainly comprises: body of heater (1), body of heater (1) bottom is main furnace body (101), body of heater (1) top is annealing body of heater (102), central authorities are equipped with crucible (9) in body of heater (101), crucible (9) is coaxial with body of heater (1), relative crucible (9) is provided with side heating element (2) on every side in the main furnace body (101), the periphery of side heating element (2) is thermal insulation layer (11), thermal insulation layer (13) is arranged under the crucible (9) and can regulate crucible (9) collet (12) just, upside heating element (5) is arranged in the annealing furnace (102), main furnace body (101) also is provided with middle temperature thermocouple (3), annealing furnace (102) is provided with temperature thermocouple, under the upper top cover mediad of body of heater (1), be extended with a rotary pulling bar (6), the lower end of this rotary pulling bar (6) is substrate clamp (7), and rotary pulling bar (6) is coaxial with body of heater (1).
3. Nd:YAP according to claim 1 and YAP recombination laser crystalline preparation method is characterized in that the proportioning raw materials of the described YAP of containing polycrystal fusing assistant saturated solution is as follows:
1. the set of dispense of fusing assistant solution is than being the PbO of 10-13mol and lmol B
2O
3, or 8-12molBi
2O
3B with 1-3mol
2O
3
2. the weight percent of YAP polycrystalline and fusing assistant is: YAP/ fusing assistant solution=10wt%-50wt%
4. Nd:YAP according to claim 1 and YAP recombination laser crystalline preparation method is characterized in that this method comprises the following steps:
＜1〉according to the selected YAP polycrystalline and the proportioning raw materials weighing of fusing assistant, in the crucible (9) of packing into after thorough mixing is even and in the body of heater of packing into (1);
＜2〉crystal plane direction is inserted in the substrate clamp (7) for the substrate wafer (8) of the Nd:YAP of (100) or (010) or (001), adjusted rotary pulling bar (6), make it to be on the coaxial position of crucible (9);
＜3〉heat-up rate with 100 ℃/Hr is warming up to 1000～1150 ℃, fused raw material YAP and fusing assistant PbO-B
2O
3Or Bi
2O
3-B
2O
3, make it become saturated solution (10), treat all dissolvings after, 1050～1150 ℃ of constant temperature 5 hours;
＜4〉the rotary pulling bar (6) that descends gradually drops to from saturated fusing assistant liquid level 3～5mm place substrate wafer (8), again constant temperature 2～4 hours under 900～1050 ℃ of conditions of YAP crystallization range;
＜5〉decline rotary pulling bar (6) immerses in the homothermic saturated solution (10) substrate wafer (8) fully, rotary pulling bar (6) rotates with 100～250r/min speed, regulate corresponding growth time according to required growth YAP crystal face thickness, after growth time finishes, mention rotary pulling bar (6) immediately, make substrate (8) make it break away from liquid level;
＜6〉annealing, rotary pulling bar (6) will be continued to mention, make substrate wafer (8) and precipitating thereof uniform thickness YAP monocrystalline thereon enter interior upside heating element (5) interval of annealing furnace (102), the power of heating element in the adjustment (5) makes its temperature at 900 ℃ of constant temperature after 5 hours, be cooled to room temperature with 50 ℃/Hr speed then, finish the preparation of YAP/Nd:YAP/YAP composite laser material.
5. Nd:YAP according to claim 4 and YAP recombination laser crystalline preparation method, it is characterized in that described step＜5〉be the heating power of adjusting the side heating element (2) of main furnace body (101), make middle temperature thermocouple (3) be designated as 900～1050 ℃, constant temperature 1～2h again, rotary pulling bar (6) then descends, the lower surface of substrate wafer (8) is contacted with homothermic saturated solution (10), this rotary pulling bar (6) is with the speed rotation of 100～250r/min, thickness according to the YAP crystal face of required growth is regulated corresponding growth time, growth time finishes, mention rotary pulling bar (6) immediately, make substrate wafer (8) break away from liquid level;
＜6〉the annealing back obtains single-ended YAP/Nd:YAP crystalline material with YAP crystal layer;
＜7〉will insert once more in the substrate clamp (7) behind prepared substrate wafer (8) turn-over, adjust rotary pulling bar (6) and make it to be on the coaxial position of crucible (9);
＜8〉through step＜3〉＜4＜5＜6 after finish the preparation of YAP/Nd:YAP/YAP recombination laser crystalline material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116631 CN1236112C (en) | 2003-04-25 | 2003-04-25 | Preparation method of neodymium-doped yttrium aluminate and yttrium aluminate composite laser crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116631 CN1236112C (en) | 2003-04-25 | 2003-04-25 | Preparation method of neodymium-doped yttrium aluminate and yttrium aluminate composite laser crystal |
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| Publication Number | Publication Date |
|---|---|
| CN1445388A true CN1445388A (en) | 2003-10-01 |
| CN1236112C CN1236112C (en) | 2006-01-11 |
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| CN 03116631 Expired - Fee Related CN1236112C (en) | 2003-04-25 | 2003-04-25 | Preparation method of neodymium-doped yttrium aluminate and yttrium aluminate composite laser crystal |
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| Country | Link |
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| CN (1) | CN1236112C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021661A (en) * | 2010-12-30 | 2011-04-20 | 北京华进创威电子有限公司 | Seed crystal bonding device |
| 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 |
| CN109280963A (en) * | 2018-08-24 | 2019-01-29 | 中国科学院合肥物质科学研究院 | A kind of composite plate-shaped laser crystal and method for producing the same |
-
2003
- 2003-04-25 CN CN 03116631 patent/CN1236112C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021661A (en) * | 2010-12-30 | 2011-04-20 | 北京华进创威电子有限公司 | Seed crystal bonding device |
| CN102021661B (en) * | 2010-12-30 | 2012-09-19 | 北京华进创威电子有限公司 | Seed crystal bonding device |
| 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 |
| CN109280963A (en) * | 2018-08-24 | 2019-01-29 | 中国科学院合肥物质科学研究院 | A kind of composite plate-shaped laser crystal and method for producing the same |
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| Publication number | Publication date |
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| CN1236112C (en) | 2006-01-11 |
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