CN103556214A - Method for growing rare earth lutetium phosphate laser host crystal - Google Patents
Method for growing rare earth lutetium phosphate laser host crystal Download PDFInfo
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- CN103556214A CN103556214A CN201310573930.1A CN201310573930A CN103556214A CN 103556214 A CN103556214 A CN 103556214A CN 201310573930 A CN201310573930 A CN 201310573930A CN 103556214 A CN103556214 A CN 103556214A
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Abstract
The invention belongs to the technical field of synthetic growth of functional materials and relates to a method for growing a rare earth lutetium phosphate laser host crystal. The method comprises the following steps: dissolving Pb(NO3)2 powder in distilled water to prepare a Pb(NO3)2 solution; heating and stirring the Pb(NO3)2 solution on a digital display heating magnetic stirrer until the solution is boiling; slowly dripping a phosphoric acid solution into the boiling Pb(NO3)2 solution, reacting to obtain a PbHPO4 precipitate, purifying the PbHPO4 precipitate, transferring the purified PbHPO4 precipitate into a vacuum drying oven, and drying to obtain white powder PbHPO4; weighing the PbHPO4 powder and Lu2O3 powder, uniformly mixing and putting into a platinum crucible, transferring into a chamber electric furnace, and setting a temperature control program for performing crystal growth. The growth process is simple, the growth period is short, a fewer reagents are used, the energy consumption is low, and the used device is simple, and easy and convenient to operate.
Description
Technical field:
The invention belongs to functional materials synthetically grown technical field, relate to a kind of Fast Growth technique of laser host crystal, particularly a kind of growth method of rare earth phosphoric acid lutetium laser host crystal.
Background technology:
In recent years, the solid statelaser development that the solid laser material of take is operation material rapidly, its energy is high, and output rating is large, and performance is relatively stable, sphere of life military affairs, medical science and people is widely used, laser crystals, as a kind of laser working medium of solid statelaser, has caused people's extensive concern, and rare earth phosphoric acid lutetium Crystallochemical Properties is stable, by most of pharmaceutical chemicalss, do not corroded, comprise nitric acid and hydrochloric acid; Its fusing point is higher than 2000 ℃, and Mohs' hardness is between 4 to 7.5; It has been proved the high-concentration dopant that can hold other lanthanide ions, and these performances of rare earth phosphoric acid lutetium crystal make it become a kind of good laser host crystal.
At present, less to the research of RE phosphate crystalloid growth both at home and abroad, growth method is mainly flux method, comprise fusing assistant sporadic nucleation method and fusing assistant top-seeded solution growth, but the device of these methods is too complicated, crystal growth cycle is longer, is unfavorable for the exploration of early stage to crystal growth condition and crystal property.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seeking design provides a kind of method of Fast Growth rare earth phosphoric acid lutetium laser host crystal, adopt chamber type electric resistance furnace to grow after phosphoric acid lutetium crystal with cooling rate faster, high temperature pours out crystal, device is simple, convenient operation, energy consumption is low.
To achieve these goals, the present invention includes raw material and synthesize and two steps of crystal growth, its concrete process of growth is:
(1) raw material is synthetic: the Pb(NO that is first 99.9% by purity
3)
2powder dissolution is prepared and is obtained the Pb(NO that mol ratio concentration is 0.3mol/L in distilled water
3)
2solution, then by Pb(NO
3)
2solution is placed into extremely boiling of heated and stirred on conventional digital display heating magnetic stirring apparatus; Then measure 45ml concentration and be 86% phosphoric acid solution and slowly splash into the Pb(NO of boiling
3)
2in solution, react, use magneton stirred solution between the reaction period always, stop heating and continue stirring after phosphoric acid solution drips off, after solution is cooled to room temperature, filtration obtains PbHPO
4precipitation, with distilled water repeatedly washing and filtering remove PbHPO
4residual ion in precipitation, the PbHPO after being purified
4precipitation, by the PbHPO after purifying
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 and mix after put into the platinum crucible with platinum lid, platinum crucible is moved in chamber type electric resistance furnace, by the temperature regulating device in chamber type electric resistance furnace, set temperature control program and carry out crystal growth, be first rapidly heated to 1360 ℃, 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; Be warming up to after 1360 ℃, be incubated 24 hours, make PbP in crucible
2o
7with LuPO
4the abundant mixed stability of melt forming also increases the stability of melt, then, with the cooling rate cooling of 3～6 ℃/h, crystal sporadic nucleation in melt is separated out; When temperature is down to 900 ℃, open the fire door of chamber type electric resistance furnace crystal is toppled over out together with fusing assistant, after the melt solidifying that pours out is cooling, grind, find out crystal, be the rare earth phosphoric acid lutetium laser host crystal that growth obtains.
The rare earth phosphoric acid lutetium laser host crystal that the present invention's growth obtains is uniaxial crystal, 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 in the present invention, and growth cycle is short, and medicine used is less, and energy consumption is low, and the device of use is simple, simple to operation, and growth cycle is short.
Accompanying drawing explanation:
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 present invention's rare earth phosphoric acid lutetium crystal of growing.
Fig. 3 is the structural representation of the present invention's rare earth phosphoric acid lutetium crystal of growing.
Embodiment:
Below by embodiment, be also described further by reference to the accompanying drawings.
Embodiment:
The concrete steps that the present embodiment is prepared rare earth phosphoric acid lutetium crystal comprise that raw material synthesizes and two steps of crystal growth:
(1) raw material is synthetic: the Pb(NO that is 99.9% by 100g purity
3)
2powder dissolution, in 1200ml distilled water, stirs and is heated to boiling while be then put on digital display heating magnetic stirring apparatus; Measure again 45ml concentration and be 86% phosphoric acid solution, slowly splash in the solution of boiling and react, between the reaction period, use magneton stirred solution always, after phosphoric acid drips off, stop heating, continue to stir and be cooled to room temperature, then filter and obtain PbHPO
4precipitation, with distilled water repeatedly washing and filtering remove residual ion in precipitation, reach the object of purification, after having purified, by PbHPO
4precipitation shifts in vacuum drying oven, dries 24 hours at 80 ℃, obtains the PbHPO of white powder
4;
(2) crystal growth: the ratio that is 12:1 according to mass ratio weighs PbHPO
4powder and concentration are 99.99% Lu
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, by the temperature regulating device 5 in chamber type electric resistance furnace 1, set temperature control program and carry out crystal growth, first in 5 hours, be warmed up to 1360 ℃, along with the rising of temperature, PbHPO
4first be decomposed into PbP
2o
7, PbP then
2o
7with rare earth oxide Lu
2o
3reaction generates rare earth orthophosphoric acid salt LuPO
4, remaining PbP
2o
7, as fusing assistant, be warmed up to after 1360 ℃, insulation for some time, can make the abundant mixed stability of melt in crucible and increase the stability of melt; Then with the cooling rate of 3 ℃/h, lower the temperature 1200 ℃, cooling rate with 6 ℃/h is cooled to 900 ℃ again, allows crystal sporadic nucleation in melt separate out, finally when temperature is down to 900 ℃, when melt will solidify, open the fire door of chamber type electric resistance furnace 1 crystal is toppled over out together with fusing assistant; After the melt solidifying pouring out is cooling, it is carefully ground, find out crystal, be rare earth phosphoric acid lutetium crystal.
The data that the present embodiment carries out X ray single crystal diffraction gained to the crystal growing as shown in Figure 2, and adopt the mapping of Diamond software to X ray single crystal diffraction the data obtained, obtain crystalline structure schematic diagram, as shown in Figure 3; As can be seen from Figures 2 and 3, the crystal molecule formula that the present embodiment growth obtains is LuPO
4, belonging to tetragonal system, spacer is I4
1/ amd,
z=4, consistent with gross data, illustrate that the crystal growing is rare earth phosphoric acid lutetium crystal, and crystal is comparatively pure, do not have stray crystal to occur.
Chamber type electric resistance furnace 1, resistance heating element 2, platinum crucible 3, crucible pad 4 and temperature regulating device 5 that the present embodiment is used are commercially available prod conventional in prior art.
Claims (2)
1. a growth method for rare earth phosphoric acid lutetium laser host crystal, is characterized in that comprising that raw material synthesizes and two steps of crystal growth, and its concrete process of growth is:
(1) raw material is synthetic: the Pb(NO that is first 99.9% by purity
3)
2powder dissolution is prepared and is obtained the Pb(NO that mol ratio concentration is 0.3mol/L in distilled water
3)
2solution, then by Pb(NO
3)
2solution is placed into extremely boiling of heated and stirred on conventional digital display heating magnetic stirring apparatus; Then measure 45ml concentration and be 86% phosphoric acid solution and slowly splash into the Pb(NO of boiling
3)
2in solution, react, use magneton stirred solution between the reaction period always, stop heating and continue stirring after phosphoric acid solution drips off, after solution is cooled to room temperature, filtration obtains PbHPO
4precipitation, with distilled water repeatedly washing and filtering remove PbHPO
4residual ion in precipitation, the PbHPO after being purified
4precipitation, by the PbHPO after purifying
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 and mix after put into the platinum crucible with platinum lid, platinum crucible is moved in chamber type electric resistance furnace, by the temperature regulating device in chamber type electric resistance furnace, set temperature control program and carry out crystal growth, be first rapidly heated to 1360 ℃, 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; Be warming up to after 1360 ℃, be incubated 24 hours, make PbP in crucible
2o
7with LuPO
4the abundant mixed stability of melt forming also increases the stability of melt, then, with the cooling rate cooling of 3～6 ℃/h, crystal sporadic nucleation in melt is separated out; When temperature is down to 900 ℃, open the fire door of chamber type electric resistance furnace crystal is toppled over out together with fusing assistant, after the melt solidifying that pours out is cooling, grind, find out crystal, be the rare earth phosphoric acid lutetium laser host crystal that growth obtains.
2. the growth method of rare earth phosphoric acid lutetium laser host crystal according to claim 1, it is characterized in that the rare earth phosphoric acid lutetium laser host crystal that growth obtains 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104577701A (en) * | 2015-01-29 | 2015-04-29 | 中国科学院福建物质结构研究所 | Erbium and ytterbium co-doped phosphate crystal laser device with wave bands of 1.55 micrometers |
| 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 |
| 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 |
| 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 |
Families Citing this family (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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| JPS57140398A (en) * | 1981-02-19 | 1982-08-30 | Agency Of Ind Science & Technol | Manufacture of crystal of rare earth element phosphate |
| 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 | Growth method for fluxing medium 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 |
-
2013
- 2013-11-15 CN CN201310573930.1A patent/CN103556214B/en not_active Expired - Fee Related
Patent Citations (5)
| 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 |
| 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 | Growth method for fluxing medium 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 (6)
| 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 |
| CN104577701A (en) * | 2015-01-29 | 2015-04-29 | 中国科学院福建物质结构研究所 | Erbium and ytterbium co-doped phosphate crystal laser device with wave bands of 1.55 micrometers |
| 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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| CN103556214B (en) | 2015-11-04 |
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