CN103556214B - A kind of growth method of rare earth lutetium phosphate laser host crystal - Google Patents
A kind of growth method of rare earth lutetium phosphate laser host crystal Download PDFInfo
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- CN103556214B CN103556214B CN201310573930.1A CN201310573930A CN103556214B CN 103556214 B CN103556214 B CN 103556214B CN 201310573930 A CN201310573930 A CN 201310573930A CN 103556214 B CN103556214 B CN 103556214B
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Abstract
The invention belongs to functional materials synthetically grown technical field, relate to a kind of growth method of rare earth lutetium phosphate laser host crystal, first by Pb(NO
3)
2powder dissolution is prepared and is obtained Pb(NO in distilled water
3)
2solution, then by Pb(NO
3)
2solution is placed into heated and stirred extremely boiling on digital display heating magnetic stirring apparatus; Then phosphoric acid solution is slowly added dropwise to the Pb(NO of boiling
3)
2carry out in solution being obtained by reacting PbHPO
4precipitation and to purification, by purify after PbHPO
4precipitation transfers to the PbHPO of drying in vacuum drying oven and obtaining white powder
4; Take PbHPO
4powder and Lu
2o
3powder is also put into platinum crucible after mixing and is moved into chamber type electric resistance furnace and set temperature control program and carry out crystal growth; Its process of growth is simple, and growth cycle is short, and medicine used is less, and energy consumption is low, and the device of use is simple, and simple to operation, growth cycle is short.
Description
Technical field:
The invention belongs to functional materials synthetically grown technical field, relate to a kind of quick growth technique of phosphate laser host crystal, particularly a kind of growth method of rare earth lutetium phosphate laser host crystal.
Background technology:
In recent years, the solid statelaser development taking solid laser material as operation material is rapid, its energy is high, and output rating is large, and performance is relatively stable, be widely used at the sphere of life of military, medical science and people, laser crystals, as a kind of laser working medium of solid statelaser, has caused the extensive concern of people, and rare earth lutetium Crystallochemical Properties is stablized, do not corroded by most of pharmaceutical chemicals, comprise nitric acid and hydrochloric acid; Its fusing point is higher than 2000 DEG C, and Mohs' hardness is between 4 to 7.5; It has been proved the high-concentration dopant that can hold other lanthanide ions, these performances of rare earth lutetium crystal, makes it become a kind of excellent phosphate laser host crystal.
At present, less to the research of RE phosphate crystalloid growth both at home and abroad, growth method is flux method mainly, comprise fusing assistant sporadic nucleation method and fusing assistant top-seeded solution growth, but the device of these methods is too complicated, crystal growth cycles is longer, is unfavorable for the exploration in earlier stage to crystal growth condition and crystal property.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art existence, seek to design a kind of method that quick growth rare earth lutetium phosphate laser host crystal is provided, adopt chamber type electric resistance furnace with after cooling rate grows lutetium crystal faster, high temperature pours out crystal, device is simple, convenient operation, energy consumption is low.
To achieve these goals, the present invention includes Material synthesis and crystal growth two steps, its concrete process of growth is:
(1) Material synthesis: be first the Pb(NO of 99.9% by purity
3)
2powder dissolution is prepared and is obtained the Pb(NO that mole specific concentration is 0.3mol/L in distilled water
3)
2solution, then by Pb(NO
3)
2solution is placed into heated and stirred extremely boiling on conventional digital display heating magnetic stirring apparatus; Then measure 45ml concentration be 86% phosphoric acid solution be slowly added dropwise to the Pb(NO of boiling
3)
2react in solution, use magneton stirred solution between the reaction period always, phosphoric acid solution drips off rear stopping and heating and continue to stir, and filters and obtain PbHPO after solution is cooled to room temperature
4precipitation, with distilled water repeatedly washing and filtering removal PbHPO
4ion residual in precipitation, obtains the PbHPO after purifying
4precipitation, by the PbHPO after purification
4precipitation is transferred in vacuum drying oven and is dried 24 hours, obtains the PbHPO of white powder
4;
(2) crystal growth: the proportioning of 12:1 takes PbHPO in mass ratio
4powder and Lu
2o
3powder the platinum crucible put into after mixing with platinum lid, platinum crucible is moved in chamber type electric resistance furnace, carry out crystal growth by the temperature regulating device setting temperature control program in chamber type electric resistance furnace, be first rapidly heated to 1360 DEG C, along with the rising of temperature, PbHPO
4be decomposed into PbP
2o
7, PbP
2o
7with Lu
2o
3reaction generates rare earth orthophosphoric acid salt LuPO
4, remaining PbP
2o
7as fusing assistant; After being warming up to 1360 DEG C, being incubated 24 hours, making PbP in crucible
2o
7with LuPO
4the abundant mixed stability of melt of composition also increases the stability of melt, then with the cooling of the cooling rate of 3 ~ 6 DEG C/h, make crystal in the melt sporadic nucleation separate out; When temperature is down to 900 DEG C, crystal topples over out together with fusing assistant by the fire door opening chamber type electric resistance furnace, grinds, find out crystal, be the rare earth lutetium phosphate laser host crystal growing and obtain after the melt solidifying cooling poured out.
It is uniaxial crystal that the present invention grows the rare earth lutetium phosphate laser host crystal obtained, and optical axis direction is along c-axis direction, and crystalline structure is tetragonal system body-centered cubic structure, and spacer is I4
1/ amd,
z=4.
Compared with prior art, its process of growth is simple, and growth cycle is short, and medicine used is less, and energy consumption is low in the present invention, and the device of use is simple, and simple to operation, growth cycle is short.
Accompanying drawing illustrates:
Fig. 1 is the crystal growing apparatus structural principle schematic diagram that the present invention uses, and comprises chamber type electric resistance furnace 1, resistance heating element 2, platinum crucible 3, crucible pad 4 and temperature regulating device 5.
Fig. 2 is the X-ray single crystal diffraction data of the rare earth lutetium crystal that the present invention grows.
Fig. 3 is the structural representation of the rare earth lutetium crystal that the present invention grows.
Embodiment:
Also be described further by reference to the accompanying drawings below by embodiment.
Embodiment:
The concrete steps that the present embodiment prepares rare earth lutetium crystal comprise Material synthesis and crystal growth two steps:
(1) Material synthesis: be the Pb(NO of 99.9% by 100g purity
3)
2powder dissolution in 1200ml distilled water, be then put into digital display heating magnetic stirring apparatus on stir be heated to seethe with excitement; Measure the phosphoric acid solution that 45ml concentration is 86% again, be slowly added dropwise in the solution of boiling and react, use magneton stirred solution between the reaction period always, phosphoric acid drips off rear stopping heating, continues stirring and is cooled to room temperature, then filters and obtains PbHPO
4precipitation, with ion residual in distilled water repeatedly washing and filtering removal precipitation, reaches the object of purification, after having purified, by PbHPO
4in precipitation transfer vacuum drying oven, dry 24 hours at 80 DEG C, obtain the PbHPO of white powder
4;
(2) crystal growth: the ratio being 12:1 according to mass ratio weighs PbHPO
4powder and concentration are the Lu of 99.99%
2o
3powder, puts into the platinum crucible 3 with platinum lid after mixing; Platinum crucible 3 is moved in chamber type electric resistance furnace 1, as shown in Figure 1, set temperature control program by the temperature regulating device 5 in chamber type electric resistance furnace 1 and carry out crystal growth, first in 5 hours, be warmed up to 1360 DEG C, along with the rising of temperature, PbHPO
4first be decomposed into PbP
2o
7, then PbP
2o
7with rare earth oxide Lu
2o
3reaction generates rare earth orthophosphoric acid salt LuPO
4, remaining PbP
2o
7then as fusing assistant, after being warmed up to 1360 DEG C, insulation for some time, the abundant mixed stability of the melt in crucible can being made and increase the stability of melt; Then 1200 DEG C are lowered the temperature with the cooling rate of 3 DEG C/h, be cooled to 900 DEG C with the cooling rate of 6 DEG C/h again, allow crystal in the melt sporadic nucleation separate out, finally when temperature is down to 900 DEG C, when melt will solidify, crystal topples over out together with fusing assistant by the fire door opening chamber type electric resistance furnace 1; To be poured go out melt solidifying cooling after, it is carefully ground, finds out crystal, be rare earth lutetium crystal.
The present embodiment carries out the data of X-ray single crystal diffraction gained as shown in Figure 2 to the crystal grown, and adopts the mapping of Diamond software to X-ray single crystal diffraction the data obtained, obtains crystalline structure schematic diagram, as shown in Figure 3; As can be seen from Figures 2 and 3, the present embodiment grows the crystal molecule formula obtained is LuPO
4, belong to tetragonal system, spacer is I4
1/ amd,
z=4, consistent with gross data, illustrate that the crystal grown is rare earth lutetium crystal, and crystal is comparatively pure, does not have stray crystal to occur.
The chamber type electric resistance furnace 1 that the present embodiment uses, resistance heating element 2, platinum crucible 3, crucible pad 4 and temperature regulating device 5 are commercially available prod conventional in prior art.
Claims (2)
1. a growth method for rare earth lutetium phosphate laser host crystal, it is characterized in that comprising Material synthesis and crystal growth two steps, its concrete process of growth is:
(1) Material synthesis: be first the Pb(NO of 99.9% by purity
3)
2powder dissolution is prepared and is obtained the Pb(NO that mole specific concentration is 0.3mol/L in distilled water
3)
2solution, then by Pb(NO
3)
2solution is placed into heated and stirred extremely boiling on conventional digital display heating magnetic stirring apparatus; Then measure 45ml concentration be 86% phosphoric acid solution be slowly added dropwise to the Pb(NO of boiling
3)
2react in solution, use magneton stirred solution between the reaction period always, phosphoric acid solution drips off rear stopping and heating and continue to stir, and filters and obtain PbHPO after solution is cooled to room temperature
4precipitation, with distilled water repeatedly washing and filtering removal PbHPO
4ion residual in precipitation, obtains the PbHPO after purifying
4precipitation, by the PbHPO after purification
4precipitation is transferred in vacuum drying oven and is dried 24 hours, obtains the PbHPO of white powder
4;
(2) crystal growth: the proportioning of 12:1 takes PbHPO in mass ratio
4powder and Lu
2o
3powder the platinum crucible put into after mixing with platinum lid, platinum crucible is moved in chamber type electric resistance furnace, carry out crystal growth by the temperature regulating device setting temperature control program in chamber type electric resistance furnace, be first rapidly heated to 1360 DEG C, along with the rising of temperature, PbHPO
4be decomposed into PbP
2o
7, PbP
2o
7with Lu
2o
3reaction generates rare earth orthophosphoric acid salt LuPO
4, remaining PbP
2o
7as fusing assistant; After being warming up to 1360 DEG C, being incubated 24 hours, making PbP in crucible
2o
7with LuPO
4the abundant mixed stability of melt of composition also increases the stability of melt, then with the cooling of the cooling rate of 3 ~ 6 DEG C/h, make crystal in the melt sporadic nucleation separate out; When temperature is down to 900 DEG C, crystal topples over out together with fusing assistant by the fire door opening chamber type electric resistance furnace, grinds, find out crystal, be the rare earth lutetium phosphate laser host crystal growing and obtain after the melt solidifying cooling poured out.
2. the growth method of rare earth lutetium phosphate laser host crystal according to claim 1, it is characterized in that growing the rare earth lutetium phosphate laser host crystal obtained is uniaxial crystal, optical axis direction is along c-axis direction, and crystalline structure is tetragonal system body-centered cubic structure, and spacer is I4
1/ amd,
z=4.
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| CN103556214B true CN103556214B (en) | 2015-11-04 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678125A (en) * | 2018-11-26 | 2019-04-26 | 合肥学院 | A kind of phosphate second-order non-linear optical materials preparation process |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568381A (en) * | 2014-10-15 | 2016-05-11 | 中国科学院新疆理化技术研究所 | Yttrium phosphate double-refraction crystal and growing method and application thereof |
| CN105603524A (en) * | 2014-11-19 | 2016-05-25 | 中国科学院新疆理化技术研究所 | Yttrium phosphate series laser crystal, preparation method and uses thereof |
| CN104577701B (en) * | 2015-01-29 | 2017-08-15 | 中国科学院福建物质结构研究所 | The 1.55 double-doped phosphate crystal lasers of micron waveband erbium ytterbium |
| CN109295497A (en) * | 2017-07-24 | 2019-02-01 | 中国科学院福建物质结构研究所 | A kind of phosphoric acid gadolinium crystal and its growing method and purposes |
| CN109097820A (en) * | 2018-09-06 | 2018-12-28 | 青岛大学 | A kind of preparation method and application for exempting to process sheet laser crystal |
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|---|---|---|---|---|
| CN1456714A (en) * | 2003-05-22 | 2003-11-19 | 北京大学 | Method for preparing phosphoric acid rare earth monocrystalline nano-thread |
| CN101435109A (en) * | 2007-11-14 | 2009-05-20 | 中国科学院理化技术研究所 | Fluxing agent growth method of boron phosphate single crystal |
| CN101768778A (en) * | 2010-02-05 | 2010-07-07 | 山东大学 | Self-activation crystal neodymium phosphate and preparation method thereof |
| CN102002752A (en) * | 2010-11-22 | 2011-04-06 | 福建福晶科技股份有限公司 | Process method for growing bismuth boronate crystals |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57140398A (en) * | 1981-02-19 | 1982-08-30 | Agency Of Ind Science & Technol | Manufacture of crystal of rare earth element phosphate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456714A (en) * | 2003-05-22 | 2003-11-19 | 北京大学 | Method for preparing phosphoric acid rare earth monocrystalline nano-thread |
| CN101435109A (en) * | 2007-11-14 | 2009-05-20 | 中国科学院理化技术研究所 | Fluxing agent growth method of boron phosphate single crystal |
| CN101768778A (en) * | 2010-02-05 | 2010-07-07 | 山东大学 | Self-activation crystal neodymium phosphate and preparation method thereof |
| CN102002752A (en) * | 2010-11-22 | 2011-04-06 | 福建福晶科技股份有限公司 | Process method for growing bismuth boronate crystals |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678125A (en) * | 2018-11-26 | 2019-04-26 | 合肥学院 | A kind of phosphate second-order non-linear optical materials preparation process |
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| CN103556214A (en) | 2014-02-05 |
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