CN102517635A - Lithium potassium phosphorus oxide compound, lithium potassium phosphorus oxide crystal and preparation method of lithium potassium phosphorus oxygen compound and crystal - Google Patents

Lithium potassium phosphorus oxide compound, lithium potassium phosphorus oxide crystal and preparation method of lithium potassium phosphorus oxygen compound and crystal Download PDF

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CN102517635A
CN102517635A CN2012100087379A CN201210008737A CN102517635A CN 102517635 A CN102517635 A CN 102517635A CN 2012100087379 A CN2012100087379 A CN 2012100087379A CN 201210008737 A CN201210008737 A CN 201210008737A CN 102517635 A CN102517635 A CN 102517635A
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lithium potassium
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potassium phosphorus
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潘世烈
曹箭
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

The present invention relates to a kind of compound lithium potassium phosphorus oxygen and lithium potassium phosphorus oxygen crystal and preparation method thereof, the chemical formula of the compound is LiK3P2O7, molecular weight 298.18; The chemical formula of the crystal is LiK3P2O7, and molecular weight 298.18 does not have symmetrical centre, and crystal category rhombic system, space group C2221, cell parameter is
Figure DSA00000656677300013
Z=4,
Figure DSA00000656677300014
Figure DSA00000656677300015
Compound is synthesized using solid reaction process and high-temperature fusant method grows crystal, since compound L iK3P2O7 is congruent melting, it is suitble to use melt method for growing monocrystalline, and the melting point compound is low, viscosity is small, conducive to the ion transmission in melt, and does not need using fluxing agent, it is easy to operate, the advantages that speed of growth is fast, at low cost, is easy to get large scale, high quality crystal. The advantages that growth cycle of LiK3P2O7 crystal of the invention only needs several days, and resulting crystal has optical homogeneity good, and physicochemical properties are stablized, and hardness is moderate, easy to cut, polishing and preservation.

Description

Compound lithium potassium phosphorus oxygen and lithium potassium phosphorus oxygen crystal and preparation method thereof
Technical field
The present invention relates to a kind of compound lithium potassium phosphorus oxygen and lithium potassium phosphorus oxygen crystal and preparation method thereof.
Background technology
Non-linear optical crystal material is one of important photoelectric information functional material; Be the particularly important substance basis of laser technology of photoelectron technology, be with a wide range of applications and huge using value in fields such as information, the energy, industrial manufacturing, medical science, military affairs.Because the phosphoric acid salt non-linear optic crystal is a current application laser frequency doubling crystal widely as important double-frequency material, in phosphate system, explores novel nonlinear optical crystal and realize that the high-level efficiency of optical maser wavelength is converted into the focus that laser field is paid close attention to always.At present main nonlinear optical material has: KDP (KH 2PO 4), KTP (KTiOPO 4) crystal, ADP (NH 4H 2PO 4) crystal.Though the crystal technique of these materials reaches its maturity, but still exist tangible weak point: as crystal be prone to deliquescence, growth cycle is long and cost an arm and a leg etc.Therefore, seek new non-linear optical crystal material and remain an extremely important and large order.Therefore; During novel nonlinear optical crystal, not only pay attention to crystalline optical property and mechanical property in development, and more and more pay attention to crystalline and prepare characteristic; Hope that new crystalline material prepares easily, can obtain the non-linear optic crystal of cheap large-size high-quality.
Summary of the invention
The objective of the invention is to, a kind of compound lithium potassium phosphorus oxygen is provided, the chemical formula of this compound is LiK 3P 2O 7, molecular weight 298.18 adopts the solid reaction process synthetic compound.
Another object of the present invention is to, a kind of lithium potassium phosphorus oxygen crystal is provided, this crystalline chemical formula is LiK 3P 2O 7, molecular weight 298.18 does not have symmetry centre, and crystal belongs to rhombic system, spacer C222 1, unit cell parameters does
Figure BSA00000656677600011
Figure BSA00000656677600012
Figure BSA00000656677600013
Z=4,
Figure BSA00000656677600014
Another object of the present invention is, a kind of compound lithium potassium phosphorus oxygen and lithium potassium phosphorus oxygen crystalline preparation method are provided, and this method adopts solid reaction process synthetic compound and high-temperature fusant method growing crystal, obtains transparent LiK 3P 2O 7Crystal.
A kind of compound lithium potassium phosphorus oxygen of the present invention, the chemical formula of this compound is LiK 3P 2O 7, molecular weight 298.18 adopts the solid reaction process synthetic compound.
A kind of lithium potassium phosphorus oxygen crystal, this crystalline chemical formula is LiK 3P 2O 7, molecular weight 298.18 does not have symmetry centre, and crystal belongs to rhombic system, spacer C222 1, unit cell parameters does
Figure BSA00000656677600021
Figure BSA00000656677600023
Figure BSA00000656677600024
Z=4,
Described compound lithium potassium phosphorus oxygen crystalline preparation method adopts solid reaction process synthetic compound and high-temperature fusant method growing crystal, and concrete operations follow these steps to carry out:
A, adopt solid reaction process, raw materials of compound is Li: K: P=1 in molar ratio: take by weighing at 3: 2 and to put into mortar, mix and careful the grinding, in the opening corundum crucible of the Ф 100mm * 100mm that packs into then; Put into retort furnace, slowly be warming up to 400 ℃, constant temperature 24 hours is cooled to room temperature; Fully grind, be warming up to 450 ℃ again, constant temperature 24 hours is cooled to room temperature; Fully grind, be warming up to 520 ℃ again, constant temperature 24 hours; Fully grind, obtain sintering lithium potassium phosphorus oxidation compound single-phase polycrystalline powder completely, again this polycrystal powder is carried out X-ray analysis;
B, with step a lithium potassium phosphorus oxygen LiK 3P 2O 7The powder heat temperature raising is to 680-850 ℃, and constant temperature 24 hours, fast cooling obtain lithium potassium phosphorus oxygen LiK to 633-810 ℃ 3P 2O 7Melt;
C, in bath surface or melt growing crystal: seed crystal is fixed on the seed rod, and seed crystal contacts with step b bath surface under the top, is cooled to 630-808 ℃;
D, with the rotating speed of 10-30rpm rotation seed crystal or crucible, with the speed of the 0.1mm/h pulling crystal that makes progress;
E, treat that required yardstick is arrived in single crystal growing after, strengthen pull rate, make crystal break away from melt liquid level, with the speed cooling of 10-50 ℃/h, slowly from burner hearth, take out then, can obtain lithium potassium phosphorus oxygen LiK 3P 2O 7Crystal.
Step a raw materials of compound contains the Li that is of lithium 2O, Li 2CO 3, LiNO 3Or LiOH, potassic is K 2CO 3, KNO 3Or KOH, phosphorated is H 3PO 4Or NH 4H 2PO 4
Below be severally typically can obtain LiK 3P 2O 7The reaction formula of compound:
(1)Li 2CO 3+3K 2CO 3+4NH 4H 2PO 4→2LiK 3P 2O 7+4CO 2↑+6H 2O↑+4NH 3↑
(2)LiNO 3+3KNO 3+2NH 4H 2PO 4→LiK 3P 2O 7+3NO 2↑+2NH 3↑+3H 2O↑+2O 2↑
(3)Li 2CO 3+3K 2CO 3+4H 3PO 4→2LiK 3P 2O 7+6H 2O↑+4CO 2↑
(4)LiOH+3KOH+2H 3PO 4→LiK 3P 2O 7+5H 2O↑
(5)Li 2O+3K 2CO 3+4H 3PO 4→2LiK 3P 2O 7+3CO 2↑+6H 2O↑
(6)LiNO 3+3KNO 3+2H 3PO 4→LiK 3P 2O 7+4NO 2↑+3H 2O↑+O 2↑
(7)2LiOH+3K 2CO 3+4H 3PO 4→2LiK 3P 2O 7+7H 2O↑+3CO 2↑
(8)Li 2CO 3+6KOH+4H 3PO 4→2LiK 3P 2O 7+9H 2O↑+CO 2↑
LiK among the preparation method of the present invention 3P 2O 7The growing apparatus of monocrystalline is:
1. single crystal pulling stove: the crystal lifting furnace or the vertical that generally use in the crystal growth industry can be made the resistance furnace that suitable thermograde makes crystal growth.
2. the monocrystalline bubble is given birth to stove: a suitable heating stove, this process furnace can be heated to 1000 ℃ at least, have accurate temperature controlling system, and temperature-controlled precision is ± 0.5 ℃, and the heating chamber of stove can be placed crucible.Seed rod is installed in stove top, the lower end of the seed rod LiK that can be installed 3P 2O 7Seed crystal, the upper end connects with a wheelwork mutually, and seed rod is done around axial rotatablely moving, this seed rod also can move up and down, so that can stretch into the appropriate location in the open pot, also is convenient to the crystal that is grown on the seed rod is lifted from liquid level.
3. the monocrystal growing furnace that uses of falling crucible method: give birth on the basis of stove at the monocrystalline bubble; Let the platform of putting crucible in the furnace chamber be connected with a mechanism; Platform speed is on request moved up and down; Or well heater can be moved up and down, type of heating can be the wire spiral heating, also can be the heating of globars or Si-Mo rod.
Description of drawings
Fig. 1 is LiK of the present invention 3P 2O 7Crystalline x-ray powder diffraction pattern.
Fig. 2 is LiK of the present invention 3P 2O 7The fundamental diagram of the device for non-linear optical that crystal is made, wherein 1 is laser apparatus, and 2 for sending light beam, and 3 is LiK 3P 2O 7Crystal, 4 is outgoing beam, 5 is filter plate.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated:
Embodiment 1:
Prepare Powdered LiK 3P 2O 7Compound
In molar ratio for Li: K: P=1: take by weighing at 3: 2 and to put into mortar, mix and careful the grinding, in the opening corundum crucible of the Ф 100mm * 100mm that packs into then, put into retort furnace; Slowly be warming up to 400 ℃, constant temperature 24 hours is cooled to room temperature, takes out after fully grinding for the second time and puts into retort furnace; Be warming up to 450 ℃ again, constant temperature 24 hours is cooled to room temperature; Take out after fully grinding for the third time and put into retort furnace, be warming up to 520 ℃ again, constant temperature 24 hours; Take out through grinding and make lithium potassium phosphorus oxidation compound single-phase polycrystalline powder, this product is carried out X-ray analysis, gained X-ray spectrogram and lithium potassium phosphorus oxygen LiK 3P 2O 7The X-ray spectrogram that single crystal structure obtains is consistent;
Adopt crystal pulling method to prepare LiK 3P 2O 7Crystal
Press reaction formula: Li 2CO 3+ 3K 2CO 3+ 4NH 4H 2PO 4→ 2LiK 3P 2O 7+ 4CO 2↑+6H 2O ↑+4NH 3↑ synthetic compound LiK 3P 2O 7
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, and crucible is put into the crystal lifting furnace, is warming up to 800 ℃, and constant temperature is after 24 hours, and fast cooling to 760 ℃ obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
At the bath surface growing crystal: the seed crystal of [010] direction is fixed on the seed rod with platinum filament, and seed crystal under the top makes seed crystal contact with melt liquid level; Be cooled to 755 ℃;
With the rotating speed rotary seed crystal rod of 20rpm, with the speed of the 0.1mm/h pulling crystal that makes progress, the vitellarium thermograde is 20-30 ℃/cm;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, slowly from burner hearth, take out then, can obtain the lithium potassium phosphorus oxygen LiK of 30mm * 22mm * 15mm with the speed annealing of 10 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 2:
Press reaction formula: LiNO 3+ 3KNO 3+ 2NH 4H 2PO 4→ LiK 3P 2O 7+ 3NO 2↑+2NH 3↑+3H 2O ↑+2O 2↑ preparation compound L iK 3P 2O 7Crystal:
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, puts into crystal growing furnace to crucible, is warming up to 700 ℃, and constant temperature was cooled to 660 ℃ after 24 hours, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
At the bath surface growing crystal: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, and seed crystal is contacted with melt liquid level, is cooled to 659 ℃;
With the rotating speed of 10rpm rotation seed crystal, with the speed of the 0.1mm/h pulling crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 28mm * 19mm * 11mm with the speed of 15 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 3:
Press reaction formula: Li 2CO 3+ 3K 2CO 3+ 4H 3PO 4→ 2LiK 3P 2O 7+ 6H 2O ↑+4CO 2↑ preparation compound L iK 3P 2O 7Crystal:
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of the Ф 80mm * 80mm that packs into, slowly is heated to 790 ℃, and constant temperature 24 hours is cooled to 735 ℃, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
Growing crystal in melt: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, makes seed crystal directly put into melt, is cooled to 732 ℃;
With the rotating speed of 30rpm rotation crucible, with the speed of the 0.1mm/h pulling crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 23mm * 15mm * 10mm with the speed of 20 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 4:
Press reaction formula: LiOH+3KOH+2H 3PO 4→ LiK 3P 2O 7+ 5H 2O ↑ preparation compound L iK 3P 2O 7Crystal::
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, slowly is heated to 720 ℃, and constant temperature 24 hours is cooled to 680 ℃, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
At the bath surface growing crystal: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, and seed crystal is contacted with melt liquid level, is cooled to 679 ℃;
With the rotating speed of 15rpm rotation crucible, with the speed of the 0.1mm/h pulling crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 18mm * 12mm * 10mm with the speed of 25 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 5:
Press reaction formula: Li 2O+3K 2CO 3+ 4H 3PO 4→ 2LiK 3P 2O 7+ 3CO 2↑+6H 2O ↑ preparation compound L iK 3P 2O 7Crystal:
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, slowly is heated to 850 ℃, and constant temperature 24 hours is cooled to 810 ℃, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
Growing crystal in melt: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, makes seed crystal place melt, is cooled to 808 ℃;
With the rotating speed of 25rpm rotation seed crystal, with the speed of the 0.1mm/h pulling crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 25mm * 20mm * 12mm with the speed of 40 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 6:
Press reaction formula: LiNO 3+ 3KNO 3+ 2H 3PO 4→ LiK 3P 2O 7+ 4NO 2↑+3H 2O ↑+O 2↑ preparation compound L iK 3P 2O 7Crystal:
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, slowly is heated to 680 ℃, and constant temperature 24 hours is cooled to 633 ℃, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
At the bath surface growing crystal: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, and seed crystal is contacted with melt liquid level, is cooled to 630 ℃;
With the rotating speed of 30rpm rotation seed crystal, with the speed of the 0.1mm/h pulling crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 21mm * 16mm * 11mm with the speed of 50 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 7:
Press reaction formula: 2LiOH+3K2CO 3+ 4H 3PO 4→ 2LiK 3P 2O 7+ 7H 2O ↑+3CO 2↑ preparation compound L iK 3P 2O 7Crystal:
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, slowly is heated to 770 ℃, and constant temperature 24 hours is cooled to 720 ℃, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
At the bath surface growing crystal: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, and seed crystal is contacted with melt liquid level, is cooled to 718 ℃;
With the rotating speed of 10rpm rotation seed crystal, with the speed of the 0.1mm/h pulling crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 19mm * 15mm * 13mm with the speed of 45 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 8:
Press reaction formula: Li 2CO 3+ 6KOH+4H 3PO 4→ 2LiK 3P 2O 7+ 9H 2O ↑+CO 2↑ preparation compound L iK 3P 2O 7Crystal:
With the LiK that makes among the embodiment 1 3P 2O 7Powder places the opening platinum crucible of Ф 80mm * 80mm, slowly is heated to 750 ℃, and constant temperature 24 hours is cooled to 700 ℃, obtains lithium potassium phosphorus oxygen LiK 3P 2O 7Melt;
At the bath surface growing crystal: with LiK 3P 2O 7Seed crystal is fixed on the seed rod lower end with platinum filament, from furnace roof portion aperture seed crystal is imported crucible, and seed crystal is contacted with melt liquid level, is cooled to 698 ℃;
With the rotating speed of 20rpm rotation seed crystal, with the speed of the 0.1mm/h pulling crystal seed crystal that makes progress;
After treating that required yardstick is arrived in single crystal growing, strengthen pull rate, make crystal break away from melt liquid level, reduce to room temperature, from burner hearth, take out crystal then lentamente, can obtain being of a size of the lithium potassium phosphorus oxygen LiK of 22mm * 17mm * 10mm with the speed of 35 ℃/h of temperature 3P 2O 7Crystal.
Embodiment 9:
LiK arbitrarily with embodiment 1-8 gained 3P 2O 7Crystal is by the frequency doubling device of the direction processing certain size that is complementary; By being placed in shown in the accompanying drawing 2 on 3 the position, at room temperature, with transferring Q Nd:YAG laser apparatus to make light source; Incident wavelength is 1064nm, is that the infrared beam 2 of 1064nm is injected LiK by transferring Q Nd:YAG laser apparatus 1 to send wavelength 3P 2O 7Monocrystalline 3, producing wavelength is the green frequency doubled light of 532nm, and output intensity is 1/10 times of equal conditions KDP, and it is the infrared light of 1064nm and the green glow of 532nm that outgoing beam 4 contains wavelength, after filter plate 5 eliminations, obtains the green laser that wavelength is 532nm.

Claims (4)

1. compound lithium potassium phosphorus oxygen, the chemical formula that it is characterized in that this compound is LiK 3P 2O 7, molecular weight 298.18 adopts the solid reaction process synthetic compound.
2. a lithium potassium phosphorus oxygen crystal is characterized in that this crystalline chemical formula is LiK 3P 2O 7, molecular weight 298.18 does not have symmetry centre, and crystal belongs to rhombic system, spacer C222 1, unit cell parameters does
Figure FSA00000656677500011
Figure FSA00000656677500012
Figure FSA00000656677500013
Z=4,
Figure FSA00000656677500014
3. compound lithium potassium phosphorus oxygen crystalline preparation method according to claim 2 is characterized in that adopting solid reaction process synthetic compound and high-temperature fusant method growing crystal, and concrete operations follow these steps to carry out:
A, adopt solid reaction process, raw materials of compound is Li: K: P=1 in molar ratio: take by weighing at 3: 2 and to put into mortar, mix and careful the grinding, in the opening corundum crucible of the Ф 100mm * 100mm that packs into then; Put into retort furnace, slowly be warming up to 400 ℃, constant temperature 24 hours is cooled to room temperature; Fully grind, be warming up to 450 ℃ again, constant temperature 24 hours is cooled to room temperature; Fully grind, be warming up to 520 ℃ again, constant temperature 24 hours; Fully grind, obtain sintering lithium potassium phosphorus oxidation compound single-phase polycrystalline powder completely, again this polycrystal powder is carried out X-ray analysis;
B, with step a lithium potassium phosphorus oxygen LiK 3P 2O 7The powder heat temperature raising is to 680-850 ℃, and constant temperature 24 hours, fast cooling obtain lithium potassium phosphorus oxygen LiK to 633-810 ℃ 3P 2O 7Melt;
C, in bath surface or melt growing crystal: seed crystal is fixed on the seed rod, and seed crystal contacts with step b bath surface under the top, is cooled to 630-808 ℃;
D, with the rotating speed of 10-30rpm rotation seed crystal or crucible, with the speed of the 0.1mm/h pulling crystal that makes progress;
E, treat that required yardstick is arrived in single crystal growing after, strengthen pull rate, make crystal break away from melt liquid level, with the speed cooling of 10-50 ℃/h, slowly from burner hearth, take out then, can obtain lithium potassium phosphorus oxygen LiK 3P 2O 7Crystal.
4. according to the said method of claim 3, it is characterized in that step a raw materials of compound contains the Li that is of lithium 2O, Li 2CO 3, LiNO 3Or LiOH, potassic is K 2CO 3, KNO 3Or KOH, phosphorated is H 3PO 4Or NH 4H 2PO 4
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CN107059123A (en) * 2017-01-18 2017-08-18 南开大学 The preparation method and its usage of four metaphosphoric acid dipotassium strontium crystals

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CN107059123A (en) * 2017-01-18 2017-08-18 南开大学 The preparation method and its usage of four metaphosphoric acid dipotassium strontium crystals

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