CN1673424A - Synthesis method for nonlinear optical crystal Nb2O5:KTP - Google Patents

Synthesis method for nonlinear optical crystal Nb2O5:KTP Download PDF

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CN1673424A
CN1673424A CN 200510020164 CN200510020164A CN1673424A CN 1673424 A CN1673424 A CN 1673424A CN 200510020164 CN200510020164 CN 200510020164 CN 200510020164 A CN200510020164 A CN 200510020164A CN 1673424 A CN1673424 A CN 1673424A
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ktp
crystal
knbo
autoclave
temperature
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CN1308502C (en
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张昌龙
黄凌雄
周卫宁
张戈
霍汉德
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Guilin Bairay Photoelectric Technology Co Ltd
China Nonferrous Metal Guilin Geology and Mining Co Ltd
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Guilin Minerals & Geologic Academy
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Abstract

The present invention relates to non-linear optical crystal material, and is especially Nb doped KTP crystal synthesizing process. The process can obtain Nb:KTP monocrystal with Nb doped concentration of 0.1-15 wt%, and the monocrystal has high quality and homogeneously distributed Nb and can realize the blue shift of cut-off wavelength and non-critical phase matching in 1064 waveband for normal solid laser. Under high temperature and high pressure, KTP crystal material and Nb2O5 reagent containing mixture aqua are made to reach certain over saturation, so that Nb doped KTP crystal is grown on Nb:KTP seed crystal. The present invention has high pressure reactor and resistive furnace adopted and reasonable temperature field designed for seed crystal to grow.

Description

Non-linear optic crystal Nb 2O 5: the synthetic method of KTP
(1) technical field:
The present invention relates to a kind of non-linear optical crystal material, promptly mix the synthetic method of the ktp crystal material (Nb:KTP) of niobium, this non-linear optic crystal is a critical material of realizing frequency inverted, modulation, deflection and the Q-switch of laser.
(2) background technology:
Potassium titanium oxide phosphate (KTP) crystal is the very good non-linear optic crystal of a kind of performance, it has big nonlinear optics and electro-optic coefficient, high laser damage threshold, can in wide temperature range, realize phase matched, stable chemistry and thermal property and wide transmission region etc., be the 1064nm place particularly at Nd ion laser radiation wavelength, the frequency-doubled effect of ktp crystal is that other nonlinear optical materials are incomparable, therefore over nearly 20 years, ktp crystal is considered to the frequency-doubling crystal of middle low power laser apparatus the best always.But ktp crystal still exists some shortcomings in actual applications.For example: 1. the degree of birefringence of ktp crystal is less, and when making double-frequency material, the cutoff wavelength of phase matched only is 994nm.Therefore can't directly make the ktp crystal frequency multiplication produce blue light, thereby limit the application of ktp crystal in important blue-light device.2. ktp crystal promptly can't be realized 90 ° of noncritical phase matchings, thereby limit the raising of green glow efficiency of conversion for the frequency multiplication optimum phase matching angle θ of 1064nm Nd:YAG laser commonly used=90 °, φ=23.1 °.
In order further to improve the performance of ktp crystal, remedy its deficiency on using, many scientific workers have done a large amount of unremitting efforts.C.T.Chen in 1994, L.K.Cheng, (Appl.Phys.Lett.1994 64:155-157) has reported and mixes niobium (Nb) can increase its degree of birefringence in ktp crystal, thereby expanded its phase matched cutoff wavelength for R.L.Harlow and J.D.Bierlein.Subsequently, Wei Jingqian, Wang Jiyang, Liu Yaogang (artificial lens journal, 1995,24 (4): 291), Liu Yaogang, Wang Jiyang, Wei Jingqian (artificial lens journal, 1997,26 (1): 1), Wang Wanyan, Zhang Kecong, Zhang Hong, Wang Ximin (artificial lens journal, 1997,26 (3-4): 384), Zhang Kecong, Wang Wanyan, Wang Ximin, good and expensive, (Beijing University of Technology's journal 1998,24 (1): 1) such as Chang Xinan, Chang Xinan, Zhang Kecong, good and your etc. 124) etc. (artificial lens journal 2000,29 (5): all carried out molten-salt growth and mixed niobium ktp crystal and growthhabit thereof, the research of aspect such as defective and crystal property.
In recent years, one of applicant is mixed in niobium ktp crystal and the correlated performance research in molten-salt growth and has been obtained certain progress, has grown and has mixed 3mol%, 5mol%, 7.5mol%, Nb:KTP monocrystalline (the Zhang Deying of 13mol%, Shen Hongyuan, Liu Wen, Zhang Guofang, Chen wenzhi, artificial lens journals such as Zhang Ge 1,999 28 (3): 298), and 7.5mol% and 13mol%Nb:KTP crystalline cutoff wavelength (W.Liu, H.Y.Shen, G.F.Zhang have been measured, D.Y.Zhang, G.Zhang, W.X.Lin, R.R.Zeng and C.H.Huang, Optics communications2000,185:191), detailed measurements 7.5mol%Nb:KTP crystalline specific refractory power and temperature factor (H.Y.Shen, D.Y.Zheng, W.Liu, G.F.Zhang, W.Z.Chen, G.Zhang, Applied Optics., 1999 (38): 987 and Zhang Deying, Shen Hongyuan, Liu Wen, Zhang Guofang, Chen wenzhi, Xiamen University's journals (natural science edition) such as Zhang Ge 2000,39 (6): 764 and Zhang Deying, Shen Hongyuan, Liu Wen, Zhang Guofang, Chen wenzhi, functional materialss such as Zhang Ge 2000,31 (5): 539), carried out research (D.Y.Zhang, the H.Y.Shen of frequency doubling property, W.Liu, G.Zhang, G.F.Zhang, W.Z.Chen, R.R.Zeng, C.H.Huang, W.X.Lin andJ.K.Liang, IEEE Journal of Quantum Electronics, 2001,37 (3): 319 and Zhan De Ying, Shen Hongyuan, Liu Wen, Zhang Ge ACTA PHOTONICASINICA 2001,30 (8): 966).By mixing niobium, the cutoff wavelength success blue shift of ktp crystal is to 937nm.In addition, after mixing Nb, ktp crystal is expected to realize the noncritical phase matching of 1064nm wave band the most frequently used in the solid statelaser, and the deviation angle of noncritical phase matching is little, parameters such as tolerance angle, tolerance wavelength are bigger, help carrying out the frequency multiplication research of more high efficiency 1064nm wave band.
But, all be to adopt molten-salt growth method in Nb:KTP crystalline growth aspect synthetic both at home and abroad at present, so everybody has also just run into a common difficult problem, that is exactly: molten-salt growth Nb:KTP crystal is relatively more difficult, and crystal mass is relatively poor.Owing to after adding niobium in the system, cause crystal speed of growth difference of each crystal face in the heavy-gravity melt further to increase, grow up to laminar easily.The heavy-gravity melt also is unfavorable for the diffusion of solute in the process of growth in addition, causes the difference of crystal each several part composition easily, need grow under comparatively high temps, and this makes the niobium ktp crystal of mixing of molten-salt growth be difficult to enter the practical stage.
(3) summary of the invention
The present invention will disclose the synthetic method of a kind of non-linear optic crystal Nb:KTP.
Nb:KTP crystalline synthetic method among the present invention is to make the ktp crystal raw material under the High Temperature High Pressure and contain Nb 2O 5(as Nb 2O 5, KNbO 3Deng) aqueous solution of the mixture of reagent reaches certain degree of supersaturation, the ktp crystal of niobium is mixed in growth on the Nb:KTP seed wafer.Specifically be exactly to adopt autoclave and supporting with it resistance furnace, by the design of rational temperature, make the temperature of interior vitellarium of reaction chamber and dissolve area suitable, when the solution in the container produces convection current owing to the temperature difference between the top and the bottom, the saturated solution of high-temperature zone is sent to cold zone, thereby the formation hypersaturated state makes seeded growth.
The present invention adopts hydrothermal method to synthesize the Nb:KTP crystal, the device that uses autoclave and supporting with it temperature difference well formula resistance furnace to form, wherein employed autoclave is preferably the autoclave that has heat insulation blocking layer, as application number is 200420033375.X, and name is called " autoclave that has heat insulation blocking layer " autoclave.Said apparatus mainly comprises the vitellarium, dissolve area, steel cap, devices such as steel still.In order to prolong the life-span of autoclave, prevent basic solution corrosion to autoclave under High Temperature High Pressure, generally need to use gold, platinum or other uncorruptible metals or the nonmetal lining pipe of making as protecting lining and basic solution and autoclave inwall being separated.The lining pipe inner chamber has mineralizer and H 2The mixing solutions of O is by the ktp crystal raw material with contain Nb 2O 5The culture material that reagent is formed is positioned at the bottom (dissolve area just) of lining pipe inner chamber, and baffle plate with holes is arranged at culture material top, and baffle plate is divided into two parts of dissolve area and vitellarium with lining pipe.Also be provided with trapezoidal seed crystal frame in the lining pipe, the seed crystal chord position is (just in the vitellarium) above lining pipe top, baffle plate.The seed wafer that cuts is fixed on the seed crystal frame.Seed wafer need be by the cutting of certain direction because (001) and (010) crystal plane direction speed of growth is the fastest, but after the crystal growth soon these exponential crystal faces will disappear; And the crystal face of (011), (210) direction can appear always, the speed of growth slower slightly but the crystal mass that grows out is better, and other directions or crystalline growth velocity are very slow, the crystal mass that grows out is very poor, so the cut direction of seed wafer is preferably directions such as (011), (210), (001), (010).
The synthetic Nb:KTP crystalline step of the present invention is as follows:
(1) contains Nb 2O 5The preparation of reagent
Use Nb 2O 5Or KNbO 3Or the two with arbitrary proportion blended mixture as the raw material of mixing niobium, with Nb 2O 5/ or KNbO 3Press: Nb 2O 5(or KNbO 3, or the mixture of the two)/ratio and the particle diameter of KTP=0.1-30wt% is the dissolve area of putting into the lining pipe bottom after the ktp crystal raw material of 1.5-5mm mixes.
Nb wherein 2O 5Or KNbO 3Can directly use Nb 2O 5The reagent of powdered or KNbO 3The reagent of powdered sinters blocky Nb into but use 2O 5Pottery, KNbO 3Pottery or granulous Nb 2O 5Or KNbO 3Crystal is better effects if then.As with K 2CO 3And Nb 2O 5In 1～1.2: 1 ratio (mol ratio) was mixed and grinding evenly was fired into KNbO in the back in 700-1050 ℃ of following 12-36 hour 3Powder will bake KNbO again 3Powder grinds behind thin and the briquetting and to sinter blocky KNbO in 700-1050 ℃ of following 12-36 hour into 3Ceramic block.
(2) compactedness (compactedness is meant the percentage ratio of the shared lining pipe free volume of solution in the autoclave lining pipe of packing under the room temperature) by 60%-85% adds alkali-metal mineralizer and H 2The O mixing solutions, this mixing solutions proportioning is
①KF(1.5-6.5mol/l)+H 2O；
Or 2.
KF(1.5-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O；
Or 3.
KF(1.5-6.5mol/l)+K 2HPO 4(2.0-6.5mol/l)+H 2O；
Or 4.
KF(1.5-6.5mol/l)+K 2HPO 4(2.0-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O；
Or 5.
K 2HPO 4(2.0-6.5mol/l)+H 2O；
Or 6.
K 2HPO 4(2.0-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O。
In order to improve crystal quality, eliminate the oxygen room in the crystal, also need add the KNO of 1-3wt% in the solution 3Or H 2O 2(KNO 3Or H 2O 2/ alkali-metal mineralizer and H 2The O mixing solutions=1-3wt%).
(3) put into the ratio of liquor capacity and all solids raw material weight in the lining pipe, i.e. liquid-solid ratio (L/S (milliliter/gram))=1.0-5.0.
(4) use gold, platinum or other uncorruptible metals or the nonmetal trapezoidal seed crystal frame of making, the seed wafer that cuts is fixing on the top of the shelf.
(5) the seed crystal frame is slowly put into lining pipe and good seal and put into autoclave more together, correspondingly pressing 60%-85% compactedness filling distilled water between autoclave reaction chamber and the lining pipe with the pressure inside and outside the balance bush pipe simultaneously.Again resistance furnace is also slowly put in the autoclave sealing.
(6) resistance furnace heats up, and adjusts temperature and pressure, controls the required temperature and the temperature difference, reaches the autoclave reaction chamber internal and external equilibrium temperature of design, and is in constant temperature under and grew 30-90 days; The dissolve area temperature is 450-520 ℃, and the vitellarium temperature is 400-470 ℃, and the temperature difference of dissolve area and vitellarium is 20-70 ℃; Operating pressure 150-170MPa (the interior operating pressure of the operating pressure in the autoclave and lining pipe is the same).When autoclave heated up, The faster the better for heat-up rate, can avoid the seed wafer excessive dissolution like this, but attainable generally speaking heat-up rate is 50-100 ℃/h.
(7) stay-warm case is opened in blowing out, and autoclave proposes burner hearth.Take out the seed crystal frame, take out crystal.
The present invention compares with technology formerly, this method can access mixes the Nb:KTP monocrystalline that niobium concentration is 0.1-15wt%, and the crystal mass that obtains with this method is intact, niobium is evenly distributed in crystal, can realize the cutoff wavelength blue shift and can realize the noncritical phase matching of 1064nm wave band the most frequently used in the solid statelaser.And present method good reproducibility, cost is low, is applicable to batch process.
(4) description of drawings:
Fig. 1 is that the present invention adopts hydrothermal method to synthesize the used growing apparatus diagrammatic cross-section of Nb:KTP crystal.
(5) embodiment:
In the present embodiment, request for utilization of the present invention number is 200420033375.X, name is called the described device of utility model of " autoclave that has heat insulation blocking layer ", this device as shown in Figure 1, it is by the high temperature and high pressure kettle of a tyre stay-warm case and the growing apparatus that supporting with it temperature difference well formula resistance furnace is formed, and its structure mainly comprises: vitellarium 1, dissolve area 2, steel cap 3, steel still 4.Present embodiment uses gold lining pipe 5 as protecting lining pipe and solution and autoclave inwall being separated, use the gold silk to make seed crystal frame in echelon simultaneously, and make a call to an aperture on the seed wafer that will cut by (011) direction, with the gold silk it is linked to each other with the seed crystal frame then and be fixed on the seed crystal frame.Gold lining pipe 5 inner chambers have mineralizer and H 2The mixing solutions of O, ktp crystal raw material and contain Nb 2O 5The culture material that reagent is formed is positioned at dissolve area 2, and baffle plate with holes is arranged at culture material top.Gold lining 5 inner cavity size Φ 38mm * 750mm, thickness of pipe 0.8mm.
(1) with K 2CO 3And Nb 2O 5Mix and grind evenly the back by 1: 1 (mol ratio) and sintered KNbO in following 24 hours in 1050 ℃ 3Powder will bake KNbO again 3Powder grinds behind thin and the briquetting in 1000 ℃ and sintered blocky KNbO in following 24 hours into 3Ceramic block;
With 280 gram particles directly is ktp crystal raw material, the 10 gram KNbO of 1.5-5mm 3Ceramic block is put into the dissolve area 2 of gold lining pipe 5 bottoms.
(2) prepare the mixing solutions of mineralizer and water again, the compactedness of pressing 70%-85% adds the mixing solutions of mineralizer 7 and water.Any in the optional following proposal of the compound method of the mixing solutions of mineralizer and water:
The scheme numbering Mineralizer concentration
1 KF (1.5-6.5mol/l)+H 2O (aqueous solution of KF, its concentration are 1.5-6.5mol/l)
2 KF (1.5-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O (KF and KH 2PO 4Mixed aqueous solution, wherein the concentration of KF is 1.5-6.5mol/l; K 2HPO 4Concentration be 0.125-0.36mol/l)
3 KF (1.5-6.5mol/l)+K 2HPO 4(2.0-6.5mol/l)+H 2O (KF and K 2HPO 4Mixed aqueous solution, wherein the concentration of KF is 1.5-6.5mol/l; K 2HPO 4Concentration be 2.0-6.5mol/l)
4 KF (1.5-6.5mol/l)+K 2HPO 4(2.0-6.5mol/l)+KH 2PO 4(0.125-0.36mol/ l)+H 2O (KF and K 2HPO 4And KH 2PO 4Mixed aqueous solution, wherein the concentration of KF is 1.5-6.5mol/l; K 2HPO 4Concentration be 2.0-6.5mol/l; KH 2PO 4Concentration be 0.125-0.36mol/l)
5 K 2HPO 4(2.0-6.5mol/l)+H 2O (K 2HPO 4The aqueous solution, its concentration is 2.0-6.5mol/l)
6 K 2HPO 4(2.0-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O.(K 2HPO 4And KH 2PO 4Mixed aqueous solution, K wherein 2HPO 4Concentration be 2.0-6.5mol/l; KH 2PO 4Concentration be 0.125-0.36mol/l)
(3) for guaranteeing the synthetic crystal quality, in the present embodiment, also added the KNO of 1-3wt% in the solution 3Or H 2O 2, to guarantee the oxygen room not occur in the crystal.
(4) use the gold silk to make seed crystal frame 6 in echelon, the Nb:KTP seed wafer of 30 * 30 * 1.5mm that cuts by (011) direction and two ends polishings (can reduce the defective of new growing crystal after the seed wafer polishing both surfaces), spile at the edge, connect aperture with the gold silk, and fix on the top of the shelf, whenever next ladder frame can be hung ten (deciding on the seed crystal size).
(5) the seed crystal frame is slowly put into gold lining 5, and good seal puts into autoclave more together, and slowly put into resistance furnace 10.
(6) resistance furnace 10 heats up, and adjusts temperature and pressure.The dissolve area temperature is 450-520 ℃, and the vitellarium temperature is 400-470 ℃, 50 ℃ of the temperature difference; Operating pressure 150-170MPa; Heat-up rate is 80 ℃/h, and the autoclave internal and external temperature reaches balance, and the constant temperature growth is 45 days under this temperature.
(7) stay-warm case is opened in cooling, blowing out, and autoclave proposes burner hearth, takes out 10 in crystal, uses warm water cleaning, and crystal is sparkling and crystal-clear transparent, and the nothing cotton does not have to be split, and integrity is good.
After the polishing of gained crystal-cut, can be used as the blue laser double-frequency material or the 1064nm wave band is realized noncritical phase matching, thereby but make the Nb:KTP crystal enter the practicability stage.

Claims (7)

1, the device that the hydrothermal method synthetic method of non-linear optic crystal Nb:KTP, this method use autoclave and supporting with it temperature difference well formula resistance furnace to form, concrete steps are as follows:
(1) contains Nb 2O 5The preparation of reagent
Use Nb 2O 5Or KNbO 3Or the two with the mixture of any proportional quantity proportioning as the raw material of mixing niobium, with Nb 2O 5And/or KNbO 3Press: (Nb 2O 5And/or KNbO 3The ratio of)/KTP=0.1-30wt% and particle diameter are the dissolve area of putting into the lining pipe bottom after the ktp crystal raw material of 1.5-5mm mixes;
Nb wherein 2O 5And KNbO 3Reagent for powdered; Perhaps for sintering blocky Nb into 2O 5Or KNbO 3Pottery; Perhaps be granulous Nb 2O 5Or KNbO 3Crystal;
(2) compactedness by 60%-85% adds alkali-metal mineralizer and H 2The O mixing solutions, this mixing solutions proportioning is 1. KF (1.5-6.5mol/l)+H 2O or 2. KF (1.5-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O or 3. KF (1.5-6.5mol/l)+K 2HPO 4(2.0-6.5mol/l)+H 2O or 4. KF (1.5-6.5mol/l)+K 2HPO 4(2.0-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O or 5. K 2HPO 4(2.0-6.5mol/l)+H 2O or 6. K 2HPO 4(2.0-6.5mol/l)+KH 2PO 4(0.125-0.36mol/l)+H 2O.
(3) put into the ratio of liquor capacity and all solids raw material weight in the lining pipe, i.e. liquid-solid ratio L/S=1.0-5.0;
(4) seed wafer that cuts is fixed on the trapezoidal seed crystal frame;
(5) the seed crystal frame is slowly put into lining pipe and good seal and put into autoclave more together, correspondingly pressing 60%-85% compactedness filling distilled water between autoclave reaction chamber and the lining pipe with the pressure inside and outside the balance bush pipe simultaneously; Again resistance furnace is also slowly put in the autoclave sealing;
(6) resistance furnace heats up, and adjusts temperature and pressure, and the dissolve area temperature is 450-520 ℃, and the vitellarium temperature is 400-470 ℃, and the temperature difference of dissolve area and vitellarium is 20-70 ℃; Operating pressure 150-170Mpa; Constant temperature was grown 30-90 days down;
(7) stay-warm case is opened in blowing out, and autoclave proposes burner hearth; Take out the seed crystal frame, take out crystal.
2, the hydrothermal method synthetic method of non-linear optic crystal Nb:KTP according to claim 1 is characterized in that: Nb wherein 2O 5And KNbO 3Be Nb 2O 5The reagent of powdered or KNbO 3The reagent of powdered, or sinter blocky Nb into 2O 5Pottery, or granulous Nb 2O 5Or KNbO 3Crystal.
3, the hydrothermal method synthetic method of non-linear optic crystal Nb:KTP according to claim 2 is characterized in that: KNbO wherein 3Pottery is made by following method, with K 2CO 3And Nb 2O 5By 1～1.2: 1 mixed in molar ratio and grinding evenly back were fired into the KNbO3 powder in 700-1050 ℃ of following 12-36 hour, will bake KNbO again 3Powder grinds behind thin and the briquetting and to sinter blocky KNbO in 700-1050 ℃ of following 12-36 hour into 3Ceramic block.
4, according to the hydrothermal method synthetic method of any one described non-linear optic crystal Nb:KTP of claim 1-3 kind, it is characterized in that: described autoclave is the autoclave that has heat insulation blocking layer.
5, according to the hydrothermal method synthetic method of any one described non-linear optic crystal Nb:KTP of claim 1-3 kind, it is characterized in that: in the step (2), alkali-metal mineralizer and H 2The KNO that has also added 1-3wt% in the O mixing solutions 3Or H 2O 2
6, according to the hydrothermal method synthetic method of any one described non-linear optic crystal Nb:KTP of claim 1-3 kind, it is characterized in that: the cut direction of seed wafer is (011) direction; Or (001) direction; Or (010) direction; Or (210) direction.
7, according to the hydrothermal method synthetic method of any one described non-linear optic crystal Nb:KTP of claim 1-3 kind, it is characterized in that: seed wafer is passed through polishing both surfaces in advance.
CNB2005100201641A 2005-01-11 2005-01-11 Synthesis method for nonlinear optical crystal Nb2O5:KTP Active CN1308502C (en)

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US4654111A (en) * 1985-12-02 1987-03-31 At&T Laboratories Hydrothermal growth of potassium titanyl phosphate
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Address after: 541004 the Guangxi Zhuang Autonomous Region Guilin auxiliary Star Road, No. 9

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