CN103088401B - A kind of employing fusing assistant molten-salt growth KTiOAsO 4the method of crystal - Google Patents

A kind of employing fusing assistant molten-salt growth KTiOAsO 4the method of crystal Download PDF

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CN103088401B
CN103088401B CN201310032669.4A CN201310032669A CN103088401B CN 103088401 B CN103088401 B CN 103088401B CN 201310032669 A CN201310032669 A CN 201310032669A CN 103088401 B CN103088401 B CN 103088401B
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crystal
ktioaso
growth
temperature
fluorochemical
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CN103088401A (en
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王世武
贾延伟
王鸿雁
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QINGDAO HAITAI PHOTOELECTRIC TECHNOLOGY Co Ltd
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QINGDAO HAITAI PHOTOELECTRIC TECHNOLOGY Co Ltd
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Abstract

The present invention proposes a kind of employing new flux molten-salt growth KTiOAsO 4the method of crystal, solves the KTiOAsO of existing molten-salt growth 4there is growth line and multidomain defect in crystal, the problem that wrap is many, crystal homogeneity is poor, is characterized in comprising the following steps: KH 2asO 4decaptitate after recrystallization and truncate; By the KH after recrystallization 2asO 4with K 2cO 3, TiO 2, fluorochemical adds platinum crucible, synthesis KTiOAsO 4, K 4as 2o 7, fluorochemical uniformly mixing raw material; Top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal crystal orientation is Z-direction <001>, seed rod rotating speed 20 ~ 60rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 850 ~ 950 DEG C, thermograde 0.2 ~ 2 DEG C/cm, rate of temperature fall 0.5 ~ 2 DEG C/day, lower the temperature 40 ~ 60 DEG C.Present invention achieves high quality KTiOAsO 4the repeatability growth of crystal, improves KTiOAsO 4the homogeneity of crystal.

Description

A kind of employing fusing assistant molten-salt growth KTiOAsO 4the method of crystal
Technical field
The present invention relates to field of crystal growth, refer to a kind of employing new flux molten-salt growth KTiOAsO especially 4the method of crystal.
Background technology
KTiOAsO 4crystal is a kind of excellent middle infrared nonlinear material, is KTiOPO 4a member in crystal family, transparency range is 0.35 ~ 5.3 μm, in the absorption loss of 3 ~ 5 mu m wavebands far below KTiOPO 4crystal, few to the absorption of idle light, can be applicable to mid and far infrared optical parametric oscillation (being called for short OPO) field.
Domestic and international KTiOAsO at present 4crystal technique is all immature, KTiOAsO 4the defects such as crystal exists growth line, multidomain, inner homogeneous is poor, OPO efficiency of conversion is low, limit KTiOAsO 4the application of crystal in device.Current KTiOAsO 4crystal mainly adopts molten-salt growth, and the fusing assistant that growth uses is generally K 6p 4o 13system, this fusing assistant viscosity is large, and mass transfer is poor, causes the KTiOAsO obtained 4crystal homogeneity is poor, wrap is many.Recent years, people were devoted to change fusing assistant, attempt arsenate fusing assistant (J.Crystal Growth, 1994, Vo1.137(107-115)), tungstate fusing assistant (J.Crystal Growth, 1991, Vo1.33(197-203)) and molybdate fusing assistant (J.Crystal Growth, 1991, Vo1.33(197-203)) etc. to obtaining the less KTiOAsO of defect 4crystal, but all do not obtain remarkable achievement.People's report (Appl.Phys., 1993, Lett.62 (4), 346-348) such as U.S. CR & D Scientific Engineering laboratory L.K.Cheng in 1992 are by doped F e 2o 3, Sc 2o 3, In 2o 3be conducive to obtaining single domain KTiOAsO 4crystal, but crystals lack of homogeneity, wrap are many.Up to now, have no and realize single domain KTiOAsO 4the report of crystal repeatability growth, high-quality single domain crystal is difficult to obtain, and is still puzzlement KTiOAsO 4the subject matter of crystal application.
Summary of the invention
The present invention proposes a kind of employing new flux molten-salt growth KTiOAsO 4the method of crystal, solves the KTiOAsO of existing molten-salt growth 4there is growth line and multidomain defect, wrap is many, crystal homogeneity is poor problem in crystal.
Technical scheme of the present invention is achieved in that
A kind of employing new flux molten-salt growth KTiOAsO 4the method of crystal, is characterized in that, comprises the following steps:
(1) with pure water by KH 2asO 4heating for dissolving, filtration, cooling, precipitation, decaptitate after recrystallization and truncate;
(2) in ultra-clean room, by the KH after recrystallization 2asO 4with K 2cO 3, TiO 2, fluorochemical adds in platinum crucible;
(3) be positioned over by platinum crucible in conjunction material stove, high temperature 1000 ~ 1200 DEG C stirs synthesis KTiOAsO 4, K 4as 2o 7, fluorochemical homogeneous mixture of material, be cooled to room temperature afterwards;
(4) platinum crucible is put into rapidly dry molten salt furnace;
(5) top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal crystal orientation is Z-direction <001>, seed rod rotating speed 20 ~ 60rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 850 ~ 950 DEG C, thermograde 0.2 ~ 2 DEG C/cm, rate of temperature fall 0.5 ~ 2 DEG C/day, lower the temperature 40 ~ 60 DEG C;
(6) after crystal growth terminates, molten salt furnace is down to room temperature, takes out obtained KTiOAsO 4crystal.
Preferred fluorochemical is: BaF 2in NaF or KF any one or multiple.
Preferred KTiOAsO 4, K 4as 2o 7, fluorochemical mixed system in, KTiOAsO 4with K 4as 2o 7mol ratio be 0.4 ~ 0.8.
Preferred KTiOAsO 4, K 4as 2o 7, fluorochemical mixed system in, F element and KTiOAsO 4mol ratio be 0.02 ~ 0.06.
Common molten-salt growth method generally adopts K 6p 4o 13system is fusing assistant, and compared with prior art, present method adopts K 4as 2o 7for fusing assistant, this fusing assistant viscosity is little, and mass transfer is good, grows the KTiOAsO obtained 4crystal is without growing line, without wrap, having good uniformity.The invention solves the KTiOAsO of common molten-salt growth 4crystal exist growth line, multidomain defect, wrap is many, crystal homogeneity is poor, can not repeatability growth problem.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the single domain KTiOAsO obtained 4pictorial diagram;
Fig. 2 is KTiOAsO 4microscope photograph after the chemical corrosion of <001> crystal face;
Fig. 3 is KTiOAsO 4<001> crystal face synchrotron radiation X-ray shape appearance figure.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
A kind of employing new flux molten-salt growth KTiOAsO 4the method of crystal, is characterized in that, comprises the following steps:
(1) with pure water by KH 2asO 4heating for dissolving, filtration, cooling, precipitation, decaptitate after recrystallization and truncate;
(2) in ultra-clean room, by the KH after recrystallization 2asO 4with K 2cO 3, TiO 2, fluorochemical adds in platinum crucible;
(3) be positioned over by platinum crucible in conjunction material stove, high temperature 1000 ~ 1200 DEG C stirs synthesis KTiOAsO 4, K 4as 2o 7, fluorochemical homogeneous mixture of material, be cooled to room temperature afterwards;
Concrete chemical reaction is: 2KH 2asO 4+ K 2cO 3=K 4as 2o 7+ CO 2↑+2H 2o, KH 2asO 4+ TiO 2=KTiOAsO 4+ H 2o;
(4) platinum crucible is put into rapidly dry molten salt furnace;
(5) top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal crystal orientation is Z-direction <001>, seed rod rotating speed 20 ~ 60rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 850 ~ 950 DEG C, thermograde 0.2 ~ 2 DEG C/cm, rate of temperature fall 0.5 ~ 2 DEG C/day, lower the temperature 40 ~ 60 DEG C;
(6) after crystal growth terminates, molten salt furnace is down to room temperature, takes out obtained KTiOAsO 4crystal.
Preferred fluorochemical is: BaF 2in NaF or KF any one or multiple.
Preferred KTiOAsO 4, K 4as 2o 7, fluorochemical mixed system in, KTiOAsO 4with K 4as 2o 7mol ratio be 0.4 ~ 0.8.
Preferred KTiOAsO 4, K 4as 2o 7, fluorochemical mixed system in, F element and KTiOAsO 4mol ratio be 0.02 ~ 0.06.
Embodiment 1:
First, with pure water by KTiOAsO 4heating for dissolving, filtration, cooling, precipitation, decaptitate after recrystallization and truncate;
Second step, in ultra-clean room, by the KTiOAsO after recrystallization 4with K 2cO 3, TiO 2, BaF 2add in platinum crucible;
3rd step, is placed in platinum crucible and closes material stove, rise to 1100 DEG C and constant temperature 48h with the temperature rise rate of 50 DEG C/h, stirs synthesis mol ratio KTiOAsO 4/ K 4as 2o 7=0.4, F/KTiOAsO 4the homogeneous mixture of material of=0.02, is down to room temperature with the rate of temperature fall of 40 DEG C/h afterwards;
4th step, puts into rapidly dry molten salt furnace by platinum crucible;
5th step, with the temperature rise rate of 50 DEG C/h, molten salt furnace is warming up to 1100 DEG C, first 865 DEG C are down to the rate of temperature fall of 30 DEG C/h after constant temperature 48h, 850 DEG C are cooled to again with the rate of temperature fall of 5 DEG C/h, then melt is entered by under the seed crystal after preheating, after treating seed portion melt back, top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal direction is Z-direction <001>, seed rod rotating speed 20rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 850 DEG C, thermograde 0.2 DEG C/cm, rate of temperature fall 0.5 DEG C/day, lowers the temperature 40 DEG C;
6th step, after crystal growth terminates, is down to room temperature with the rate of temperature fall of 40 DEG C/h by molten salt furnace, takes out obtained KTiOAsO 4crystal.
With reference to Fig. 2, KTiOAsO prepared by aforesaid method 4crystal pro cessing becomes 8 × 8 × 1mm 3kTiOAsO 4sample, puts into the corrosive fluid (mol ratio: KOH/KNO of 220 DEG C 3=2) take out after corrosion 7-10s in, with water cleaning after naturally cooling, observe under 500 power microscopes, test display: image uniform, without the region that light and shade is different.Show: the KTiOAsO of this technology growth 4crystal is single domain crystal.
With reference to Fig. 3, KTiOAsO prepared by aforesaid method 4crystal pro cessing becomes 3 × 3 × 10mm 3kTiOAsO 4sample, with the shape appearance figure of synchrotron radiation X-ray topography test <001> crystal face, test display: the feature image of <001> crystal face is even, does not observe multidomain region.Show: the KTiOAsO of this technology growth 4crystal is single domain crystal.
Embodiment 2:
First, with pure water by KTiOAsO 4heating for dissolving, filtration, cooling, precipitation, decaptitate after recrystallization and truncate;
Second step, in ultra-clean room, by the KTiOAsO after recrystallization 4with K 2cO 3, TiO 2, NaF adds in platinum crucible;
3rd step, is placed in platinum crucible and closes material stove, rise to 1100 DEG C and constant temperature 48h with the temperature rise rate of 50 DEG C/h, stirs synthesis mol ratio KTiOAsO 4/ K 4as 2o 7=0.6, F/KTiOAsO 4the homogeneous mixture of material of=0.04, is down to room temperature with the rate of temperature fall of 40 DEG C/h afterwards;
4th step, puts into rapidly dry molten salt furnace by platinum crucible;
5th step, with the temperature rise rate of 50 DEG C/h, molten salt furnace is warming up to 1100 DEG C, first 925 DEG C are down to the rate of temperature fall of 30 DEG C/h after constant temperature 48h, 910 DEG C are cooled to again with the rate of temperature fall of 5 DEG C/h, then melt is entered by under the seed crystal after preheating, after treating seed portion melt back, top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal direction is Z-direction <001>, seed rod rotating speed 40rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 910 DEG C, thermograde 1 DEG C/cm, rate of temperature fall 1.2 DEG C/day, lowers the temperature 50 DEG C;
6th step, after crystal growth terminates, is down to room temperature with the rate of temperature fall of 40 DEG C/h by molten salt furnace, takes out obtained KTiOAsO 4crystal.
KTiOAsO prepared by aforesaid method 4crystal pro cessing becomes 8 × 8 × 1mm 3kTiOAsO 4sample, puts into the corrosive fluid (mol ratio: KOH/KNO of 220 DEG C 3=2) take out after corrosion 7-10s in, with water cleaning after naturally cooling, observe under 500 power microscopes and find: image uniform, without the region that light and shade is different.Show: the KTiOAsO of this technology growth 4crystal is single domain crystal.
KTiOAsO prepared by aforesaid method 4crystal pro cessing becomes 3 × 3 × 1mm 3kTiOAsO 4sample, with the shape appearance figure of synchrotron radiation X-ray topography test <001> crystal face, test finds: <001> crystal face pattern is even, does not observe multidomain region.Show: the KTiOAsO of this technology growth 4crystal is single domain crystal.
Embodiment 3:
First, with pure water by KTiOAsO 4heating for dissolving, filtration, cooling, precipitation, decaptitate after recrystallization and truncate;
Second step, in ultra-clean room, by the KTiOAsO after recrystallization 4with K 2cO 3, TiO 2, KF adds in platinum crucible;
3rd step, is placed in platinum crucible and closes material stove, rise to 1100 DEG C and constant temperature 48h with the temperature rise rate of 50 DEG C/h, stirs synthesis mol ratio KTiOAsO 4/ K 4as 2o 7=0.8, F/KTiOAsO 4the homogeneous mixture of material of=0.06, is down to room temperature with the rate of temperature fall of 40 DEG C/h afterwards;
4th step, puts into rapidly dry molten salt furnace by platinum crucible;
5th step, with the temperature rise rate of 50 DEG C/h, molten salt furnace is warming up to 1100 DEG C, first 965 DEG C are down to the rate of temperature fall of 30 DEG C/h after constant temperature 48h, 950 DEG C are cooled to again with the rate of temperature fall of 5 DEG C/h, then melt is entered by under the seed crystal after preheating, after treating seed portion melt back, top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal direction is Z-direction <001>, seed rod rotating speed 60rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 950 DEG C, thermograde 2 DEG C/cm, rate of temperature fall 2 DEG C/day, lowers the temperature 60 DEG C;
6th step, after crystal growth terminates, is down to room temperature with the rate of temperature fall of 40 DEG C/h by molten salt furnace, takes out obtained KTiOAsO 4crystal.
KTiOAsO prepared by aforesaid method 4crystal pro cessing becomes 8 × 8 × 1mm 3kTiOAsO 4sample, puts into the corrosive fluid (mol ratio: KOH/KNO of 220 DEG C 3=2) take out after corrosion 7-10s in, with water cleaning after naturally cooling, observe under 500 power microscopes and find: image uniform, without the region that light and shade is different.Show: the KTiOAsO of this technology growth 4crystal is single domain crystal.
KTiOAsO prepared by aforesaid method 4crystal pro cessing becomes 3 × 3 × 1mm 3kTiOAsO 4sample, with the shape appearance figure of synchrotron radiation X-ray topography test <001> crystal face, test finds: <001> crystal face pattern is even, does not observe multidomain region.Show: the KTiOAsO of this technology growth 4crystal is single domain crystal.
In addition to the implementation, also respectively above-mentioned parameter is reconfigured and carried out verification experimental verification, all achieve good effect.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (2)

1. one kind adopts fusing assistant molten-salt growth KTiOAsO 4the method of crystal, is characterized in that, comprises the following steps:
(1) with pure water by KH 2asO 4heating for dissolving, filtration, cooling, precipitation, decaptitate after recrystallization and truncate;
(2) in ultra-clean room, by the KH after recrystallization 2asO 4with K 2cO 3, TiO 2, fluorochemical adds in platinum crucible; Described fluorochemical is BaF 2in NaF or KF any one or multiple;
(3) be positioned over by platinum crucible in conjunction material stove, high temperature 1000 ~ 1200 DEG C stirs synthesis KTiOAsO 4, K 4as 2o 7, fluorochemical homogeneous mixture of material, be cooled to room temperature afterwards; KTiOAsO 4, K 4as 2o 7, fluorochemical mixed system in, F element and KTiOAsO 4mol ratio be 0.02 ~ 0.06;
(4) platinum crucible is put into rapidly dry molten salt furnace;
(5) top-seeded solution growth growth KTiOAsO 4crystal, wherein: seed crystal crystal orientation is Z-direction <001>, seed rod rotating speed 20 ~ 60rpm, seed rod rotation mode is for rotating forward-stopping-reversion, crystal growth starting temperature 850 ~ 950 DEG C, thermograde 0.2 ~ 2 DEG C/cm, rate of temperature fall 0.5 ~ 2 DEG C/day, lower the temperature 40 ~ 60 DEG C;
(6) after crystal growth terminates, molten salt furnace is down to room temperature, takes out obtained KTiOAsO 4crystal.
2. method according to claim 1, is characterized in that, KTiOAsO 4, K 4as 2o 7, fluorochemical mixed system in, KTiOAsO 4with K 4as 2o 7mol ratio be 0.4 ~ 0.8.
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CN110055586B (en) * 2019-05-23 2021-08-06 山东华特知新材料有限公司 Preparation method of large-size KTA crystal
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5334365A (en) * 1992-05-26 1994-08-02 E. I. Du Pont De Nemours And Company Single cesium titanyl arsenate-type crystals, and their preparation
CN101319386A (en) * 2008-04-30 2008-12-10 烁光特晶科技有限公司 Preparation method of KTP crystal with anti-soil performance

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5334365A (en) * 1992-05-26 1994-08-02 E. I. Du Pont De Nemours And Company Single cesium titanyl arsenate-type crystals, and their preparation
CN101319386A (en) * 2008-04-30 2008-12-10 烁光特晶科技有限公司 Preparation method of KTP crystal with anti-soil performance

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