CN1308502C - Synthesis method for nonlinear optical crystal Nb2O5:KTP - Google Patents
Synthesis method for nonlinear optical crystal Nb2O5:KTP Download PDFInfo
- Publication number
- CN1308502C CN1308502C CNB2005100201641A CN200510020164A CN1308502C CN 1308502 C CN1308502 C CN 1308502C CN B2005100201641 A CNB2005100201641 A CN B2005100201641A CN 200510020164 A CN200510020164 A CN 200510020164A CN 1308502 C CN1308502 C CN 1308502C
- Authority
- CN
- China
- Prior art keywords
- ktp
- crystal
- synthetic method
- temperature
- linear optic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a method for synthesizing a nonlinear optical crystal material, namely a KTP crystal material (Nb: KTP) mixed with niobium. The method has the advantage that Nb: KTP single crystals with the niobium mix concentration of 0.1 to 15 wt% can be obtained; thus, Nb: KTP crystals with the advantages of perfect crystal mass are obtained, wherein niobium is uniformly distributed in the Nb: KTP crystals which can realize the blue shift of cutoff wavelength and can realize the noncritical phase match of the most frequently used wave bands of 1064 nm in a solid laser. The present invention enables the water solution of a KTP crystal raw material and a mixture containing a Nb2O5 reagent at high temperature under high pressure to reach definite degree of supersaturation so that KTP crystals mixed with niobium grow on Nb: KTP seed crystal plates. More specifically, the temperature of a growth zone in a reaction chamber accords with the temperature of a dissolution zone by a high-pressure autoclave and a resistance furnace matched with the high-pressure autoclave via reasonable temperature field design. When solution in a container generates convection because of the temperature difference between the upper part and the lower part, the saturated solution of the high-temperature zone is transmitted to the low-temperature zone; thus, an oversaturated state is formed to enable seed crystals to grow.
Description
(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 199928 (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, AppliedOptics., 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 and J.K.Liang, IEEE Journal ofQuantum Electronics, 2001,37 (3): 319 and Zhan De Ying, Shen Hongyuan, LiuWen, Zhang Ge ACTA PHOTONICA SINICA 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 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 the autoclave in " autoclave that has heat insulation blocking layer ".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
5Pulverous reagent or KNbO
3Pulverous reagent 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) 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 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, its structure mainly comprises: the vitellarium, dissolve area, steel cap, steel still.Present embodiment uses the gold lining pipe 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 inner chamber has 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, and baffle plate with holes is arranged at culture material top.Gold lining 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 of gold lining pipe bottom.
(2) prepare the mixing solutions of mineralizer and water again, the compactedness of pressing 70%-85% adds the mixing solutions of mineralizer 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 in echelon, cut KTP seed wafer and the two ends polishings (can reduce the defective of new growing crystal after the seed wafer polishing both surfaces) of 30 * 30 * 1.5mm by (011) direction, 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 the gold lining, good seal is put into autoclave more together, and slowly puts into resistance furnace.
(6) resistance furnace 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 (18)
1, the synthetic method of non-linear optic crystal Nb:KTP is characterized by this method and is to use and contains Nb
2O
5Reagent is by the synthetic ktp crystal of mixing niobium of hydrothermal synthesis method.
2, the synthetic method of non-linear optic crystal Nb:KTP according to claim 1 is characterized in that making the ktp crystal raw material and contains Nb
2O
5The aqueous solution of the mixture of reagent reaches degree of supersaturation, and the ktp crystal of niobium is mixed in growth on the KTP seed wafer.
3, the synthetic method of non-linear optic crystal Nb:KTP according to claim 1, it is characterized in that making the temperature of the vitellarium in the reaction chamber low, the temperature height of dissolve area, when the solution in the reaction chamber produces convection current owing to the temperature difference, the saturated solution of high-temperature zone is sent to cold zone, thereby the formation hypersaturated state makes seeded growth.
4, the synthetic method of non-linear optic crystal Nb:KTP according to claim 1 is characterized in that the device that uses autoclave and supporting with it temperature difference well formula resistance furnace to form.
5, according to the synthetic method of claim 3 or 4 described non-linear optic crystal Nb:KTP, it is characterized in that the dissolve area temperature is 450-520 ℃, the vitellarium temperature is 400-470 ℃, the temperature difference of dissolve area and vitellarium is 20-70 ℃.
6,, it is characterized in that operating pressure is 150-170Mpa according to the synthetic method of claim 3 or 4 described non-linear optic crystal Nb:KTP.
7, the synthetic method of non-linear optic crystal Nb:KTP according to claim 5 is characterized in that growing 30-90 days under the constant temperature.
8, the synthetic method of non-linear optic crystal Nb:KTP according to claim 1 is characterized in that with Nb
2O
5Or KNbO
3Or the two with the mixture of any proportional quantity proportioning as the raw material of mixing niobium.
9, the synthetic method of non-linear optic crystal Nb:KTP according to claim 8 is characterized in that wherein Nb
2O
5Be Nb
2O
5Pulverous reagent, or sinter blocky Nb into
2O
5Pottery, or granulous Nb
2O
5Crystal; KNbO
3Be KNbO
3Pulverous reagent, or sinter blocky KNbO into
3Pottery, or granulous KNbO
3Crystal.
10, the synthetic method of non-linear optic crystal Nb:KTP according to claim 9 is characterized in that wherein KNbO
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 KNbO 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.
11, the synthetic method of non-linear optic crystal Nb:KTP according to claim 4 is characterized in that described autoclave is the autoclave that has heat insulation blocking layer.
12, the synthetic method of non-linear optic crystal Nb:KTP according to claim 1 is characterized in that containing Nb
2O
5The preparation method of reagent is as follows:
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 to put into dissolve area after the ktp crystal raw material of 1.5-5mm mixes.
13, the synthetic method of non-linear optic crystal Nb:KTP according to claim 12 is characterized in that adding alkali-metal mineralizer and H by the compactedness of 60%-85% again
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
⑥K
2HPO
4(2.0-6.5mol/l)+KH
2PO
4(0.125-0.36mol/l)+H
2O。
14, the synthetic method of non-linear optic crystal Nb:KTP according to claim 13 is characterized in that the ratio of liquor capacity and all solids raw material weight, i.e. liquid-solid ratio L/S=1.0-5.0.
15, the synthetic method of non-linear optic crystal Nb:KTP according to claim 4 is characterized in that step is as follows:
(1) seed wafer that cuts is fixed on the trapezoidal seed crystal frame;
(2) 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;
(3) resistance furnace heats up, and adjusts temperature and pressure, constant temperature growth down;
(4) stay-warm case is opened in blowing out, and autoclave proposes burner hearth; Take out the seed crystal frame, take out crystal.
16, the synthetic method of non-linear optic crystal Nb:KTP according to claim 13 is characterized in that alkali-metal mineralizer and H
2The KNO that has also added 1-3wt% in the O mixing solutions
3Or H
2O
2
17, the synthetic method of non-linear optic crystal Nb:KTP according to claim 2, the cut direction that it is characterized in that seed wafer is (011) direction; Or (001) direction; Or (010) direction; Or (210) direction.
18, the synthetic method of non-linear optic crystal Nb:KTP according to claim 2 is characterized in that seed wafer passes through polishing both surfaces in advance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100201641A CN1308502C (en) | 2005-01-11 | 2005-01-11 | Synthesis method for nonlinear optical crystal Nb2O5:KTP |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100201641A CN1308502C (en) | 2005-01-11 | 2005-01-11 | Synthesis method for nonlinear optical crystal Nb2O5:KTP |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1673424A CN1673424A (en) | 2005-09-28 |
| CN1308502C true CN1308502C (en) | 2007-04-04 |
Family
ID=35046193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100201641A Active CN1308502C (en) | 2005-01-11 | 2005-01-11 | Synthesis method for nonlinear optical crystal Nb2O5:KTP |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1308502C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108448095A (en) * | 2018-03-23 | 2018-08-24 | 南开大学 | A kind of sodium ion battery electrode material KTiOPO4Synthesis and application |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0022193A1 (en) * | 1979-06-18 | 1981-01-14 | E.I. Du Pont De Nemours And Company | Improved process for growing crystal of KTiOPO4 and analogues thereof |
| CN85100836A (en) * | 1985-04-01 | 1986-08-06 | 国家建筑材料工业局人工晶体研究所 | The molten-salt growth method of KTP monocrystalline |
| US4654111A (en) * | 1985-12-02 | 1987-03-31 | At&T Laboratories | Hydrothermal growth of potassium titanyl phosphate |
| SU1583477A1 (en) * | 1988-06-23 | 1990-08-07 | Институт кристаллографии им.А.В.Шубникова | Method of hydrothermal growing of crystals |
| CN1014535B (en) * | 1988-12-30 | 1991-10-30 | 中国科学院物理研究所 | Utilize the method for improved mineralizer growth potassium titanium oxide phosphate monocrystalline |
| JP3289895B2 (en) * | 1990-01-05 | 2002-06-10 | イー・アイ・デユポン・ドウ・ヌムール・アンド・カンパニー | Hydrothermal method for growing optical quality single crystals |
-
2005
- 2005-01-11 CN CNB2005100201641A patent/CN1308502C/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0022193A1 (en) * | 1979-06-18 | 1981-01-14 | E.I. Du Pont De Nemours And Company | Improved process for growing crystal of KTiOPO4 and analogues thereof |
| CN85100836A (en) * | 1985-04-01 | 1986-08-06 | 国家建筑材料工业局人工晶体研究所 | The molten-salt growth method of KTP monocrystalline |
| US4654111A (en) * | 1985-12-02 | 1987-03-31 | At&T Laboratories | Hydrothermal growth of potassium titanyl phosphate |
| SU1583477A1 (en) * | 1988-06-23 | 1990-08-07 | Институт кристаллографии им.А.В.Шубникова | Method of hydrothermal growing of crystals |
| CN1014535B (en) * | 1988-12-30 | 1991-10-30 | 中国科学院物理研究所 | Utilize the method for improved mineralizer growth potassium titanium oxide phosphate monocrystalline |
| JP3289895B2 (en) * | 1990-01-05 | 2002-06-10 | イー・アイ・デユポン・ドウ・ヌムール・アンド・カンパニー | Hydrothermal method for growing optical quality single crystals |
Non-Patent Citations (5)
| Title |
|---|
| Growth and Properties of Nb-or Sn-Doped KTiOPO4 Crystals anovskii,V. K.,Voronkova,V. I.,Losevskaya,T. Yu.,Stefanovich,S. Yu.,Ivanov,S. A.,Simonov,V. I.,Sorokina,N. I,Crystallography Reports (Translation of Kristallografiya),Vol.47 No.1 2002 * |
| Growth and Properties of Nb-or Sn-Doped KTiOPO4 Crystals anovskii,V. K.,Voronkova,V. I.,Losevskaya,T. Yu.,Stefanovich,S. Yu.,Ivanov,S. A.,Simonov,V. I.,Sorokina,N. I,Crystallography Reports (Translation of Kristallografiya),Vol.47 No.1 2002;Hydrothermal growth of potassium titanyl phosphate (KTP)crystals in the medium range of temperature and pressure. Jia,Shouquan,Niu,Hongda,Tan,Jinge,Xu,Yanping,Tao,Ying,J. Cryst. Growth,Vol.99 No.1.4 1990;Studies on the phase-matching condition and the cut-offwavelength of Nb:KTiOPO4 crystal Liu,W.,Shen,H. Y.,Zhang,G. F.,Zhang,D. Y.,Zhang,G.,Lin,W. X.,Zeng,R. R.,Huang,C. H,Optics Communications,Vol.1 No.85 2000;掺铌KTP晶体的生长和性质研究 魏景谦 王继扬 刘耀岗 邵宗书 王长青 管庆才 蒋民华，人工晶体学报，第24卷第04期 1995 * |
| Hydrothermal growth of potassium titanyl phosphate (KTP)crystals in the medium range of temperature and pressure. Jia,Shouquan,Niu,Hongda,Tan,Jinge,Xu,Yanping,Tao,Ying,J. Cryst. Growth,Vol.99 No.1.4 1990 * |
| Studies on the phase-matching condition and the cut-offwavelength of Nb:KTiOPO4 crystal Liu,W.,Shen,H. Y.,Zhang,G. F.,Zhang,D. Y.,Zhang,G.,Lin,W. X.,Zeng,R. R.,Huang,C. H,Optics Communications,Vol.1 No.85 2000 * |
| 掺铌KTP晶体的生长和性质研究 魏景谦 王继扬 刘耀岗 邵宗书 王长青 管庆才 蒋民华，人工晶体学报，第24卷第04期 1995 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108448095A (en) * | 2018-03-23 | 2018-08-24 | 南开大学 | A kind of sodium ion battery electrode material KTiOPO4Synthesis and application |
| CN108448095B (en) * | 2018-03-23 | 2021-04-09 | 南开大学 | Sodium ion battery electrode material KTiOPO4Synthesis and application of |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1673424A (en) | 2005-09-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101435108B (en) | Large size nonlinear optical crystal lead bromoborate preparation method | |
| CN108070902B (en) | Compound sodium fluoborate and sodium fluoborate birefringece crystal and preparation method and purposes | |
| WO2007028326A1 (en) | LARGE-SIZE KBe2(BO3)F3 CRYSTAL, ITS PREPARATION METHOD AND FREQUENCY CONVERTER BY USING IT | |
| WO2010009597A1 (en) | Doped low temperature phase bab2o4 single crystal, the manufacturing method thereof and wave changing elements therefrom | |
| CN101435109B (en) | Growth method for fluxing medium of boron phosphate single crystal | |
| CN105668577A (en) | K3Ba3Li2Al4B6O20F compound, K3Ba3Li2Al4B6O20F nonlinear optical crystal, preparation method and application thereof | |
| CN102094245A (en) | Selenium-gallium-aluminum-barium compound, selenium-gallium-aluminum-barium nonlinear optical crystal and preparation methods and applications of compound and nonlinear optical crystal | |
| Route et al. | Growth of AgGaSe2 for infrared applications | |
| CN104609849B (en) | Terbium aluminium garnet Faraday magnetic rotation transparent ceramic of Si/Ti doping and preparation method thereof | |
| CN1308502C (en) | Synthesis method for nonlinear optical crystal Nb2O5:KTP | |
| CN1477239A (en) | Method for growing compound laser crystal | |
| CN103451730A (en) | Cd4RO(BO3)3 compound, Cd4RO(BO3)3 optical crystal, and preparation method and application thereof | |
| Liu et al. | Crystal growth, thermal and laser properties of Yb: CTGS single crystal | |
| Wang et al. | Applying the chemical bonding theory of single crystal growth to a Gd 3 Ga 5 O 12 Czochralski growth system: both thermodynamic and kinetic controls of the mesoscale process during single crystal growth | |
| CN115386954A (en) | Compound sodium lithium fluoroborate, lithium sodium fluoroborate birefringent crystal, preparation method and application | |
| CN115385351A (en) | Compound potassium lithium fluoborate, lithium potassium fluoborate birefringent crystal, preparation method and application | |
| CN104651933B (en) | Chlorine barium borate, chlorine barium borate nonlinear optical crystal, and preparation method and uses of chlorine barium borate nonlinear optical crystal | |
| CN1122732C (en) | Non-linear optical crystal of magnesium zinc bromophosphate and its preparing process and application | |
| CN100572615C (en) | A kind of alkali metal borate compounds and monocrystalline thereof and preparation method | |
| CN112505816B (en) | Compound potassium barium borate, potassium barium borate birefringent crystal, preparation method and application | |
| CN103305899A (en) | Method for growing large-size kalium titanyl arsenate single crystals through hydrothermal process | |
| CN107217300B (en) | Boronic acid compound sodium lithium and Boratex lithium optical crystal and preparation method and purposes | |
| US7744696B2 (en) | Method for preparing borate-based crystal and laser oscillation apparatus | |
| Zhou et al. | Bridgman growth and characterization of nonlinear optical single crystals Ca4GdO (BO3) 3 | |
| Cao et al. | Synthesis and characterization of a novel non-linear optical material La2SrB10O19 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: GUILIN RESEARCH INSTITUTE OF GEOLOGY FOR MINERAL R Free format text: FORMER NAME: GUILIN MINERALS + GEOLOGIC ACADEMY |
|
| CP03 | Change of name, title or address |
Address after: 541004 the Guangxi Zhuang Autonomous Region Guilin auxiliary Star Road, No. 9 Patentee after: China Nonferrous Metal Guilin Research Institute of Geology for Mineral Resources Co., Ltd. Address before: 541004 No. 2, Star Road, Guilin, the Guangxi Zhuang Autonomous Region Patentee before: Guilin Minerals & Geologic Academy |
|
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20050928 Assignee: GUILIN BAIRAY PHOTOELECTRIC TECHNOLOGY CO., LTD. Assignor: China Nonferrous Metal Guilin Research Institute of Geology for Mineral Resources Co., Ltd. Contract record no.: 2016450000005 Denomination of invention: Synthesis method for nonlinear optical crystal Nb2O5:KTP Granted publication date: 20070404 License type: Exclusive License Record date: 20160510 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| EC01 | Cancellation of recordation of patent licensing contract |
Assignee: GUILIN BAIRAY PHOTOELECTRIC TECHNOLOGY CO., LTD. Assignor: China Nonferrous Metal Guilin Research Institute of Geology for Mineral Resources Co., Ltd. Contract record no.: 2016450000005 Date of cancellation: 20160930 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20161020 Address after: 541004 the Guangxi Zhuang Autonomous Region Guilin auxiliary Star Road, No. 9 Patentee after: China Nonferrous Metal Guilin Research Institute of Geology for Mineral Resources Co., Ltd. Patentee after: GUILIN BAIRAY PHOTOELECTRIC TECHNOLOGY CO., LTD. Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin auxiliary Star Road, No. 9 Patentee before: China Nonferrous Metal Guilin Research Institute of Geology for Mineral Resources Co., Ltd. |