CN105967162A - Preparation method of micron-sized spherical gallium phosphate - Google Patents
Preparation method of micron-sized spherical gallium phosphate Download PDFInfo
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- CN105967162A CN105967162A CN201610571110.2A CN201610571110A CN105967162A CN 105967162 A CN105967162 A CN 105967162A CN 201610571110 A CN201610571110 A CN 201610571110A CN 105967162 A CN105967162 A CN 105967162A
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- phosphoric acid
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- reactor
- size spherical
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910000154 gallium phosphate Inorganic materials 0.000 title abstract description 5
- LWFNJDOYCSNXDO-UHFFFAOYSA-K gallium;phosphate Chemical compound [Ga+3].[O-]P([O-])([O-])=O LWFNJDOYCSNXDO-UHFFFAOYSA-K 0.000 title abstract description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 48
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 10
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 33
- 229910052733 gallium Inorganic materials 0.000 claims description 33
- 239000000376 reactant Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 2
- 238000005352 clarification Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 7
- 238000001704 evaporation Methods 0.000 abstract description 6
- 230000008020 evaporation Effects 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000010790 dilution Methods 0.000 abstract description 4
- 239000012895 dilution Substances 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229950000845 politef Drugs 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000005237 high-frequency sound signal Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 phosphate anion Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of micron-sized spherical gallium phosphate. The method comprises the following steps: adding Ga2O3 and a phosphoric acid solution into a closed reaction kettle, and heating and stirring to react until the reaction solution is clear; opening the reaction kettle, heating until the reaction solution is boiled, carrying out evaporation until the reaction solution is viscous, adding pure water into the reaction kettle for dilution, closing the reaction kettle, heating to react, introducing argon, naturally cooling, filtering, and drying to obtain the high-purity micron-sized spherical gallium phosphate powder. The method is simple to operate and low in cost, and does not need any additive, thereby avoiding the introduction of impurities and enhancing the product purity.
Description
Technical field
The present invention relates to the preparation method of a kind of phosphoric acid gallium, particularly relate to the preparation of a kind of micron-size spherical phosphoric acid gallium
Method, belongs to piezoelectric preparation field.
Background technology
The crystalline material of voltage can occur when piezoelectric is affected by pressure effect between both ends of the surface, 1880,
French physician P. Curie and J. Curie brother find, weight are placed on quartz crystal, some table of crystal
Face can produce electric charge, the quantity of electric charge and proportional pressure.This phenomenon is referred to as piezoelectric effect, piezoelectric effect former
Reason is, if piezoelectric is applied pressure, it will produce potential difference (referred to as direct piezoelectric effect), otherwise
Apply voltage, then produce mechanical stress (referred to as inverse piezoelectric effect).If pressure is a kind of high-frequency vibration, then produce
Raw is exactly high frequency electric.And high frequency electrical signal is when being added on piezoelectric ceramics, then produce high frequency sound signal (machinery
Vibrations), here it is the ultrasonic signal described in we are usual.Piezoelectric is a kind of energy-saving environment-friendly materials,
Green safety, will not produce poisonous and hazardous residuals, and its application is not limited by place, it is not required that ad hoc
Place, retractility and the activeness of its application are strong.Utilize the piezoelectric generating device structure that piezoelectric makes simultaneously
Simply, it is easy to accomplish, low cost, can be mass-produced.Quartz is the representative of piezoquartz, utilizes quartz
Piezoelectric effect can make agitator and wave filter equifrequency control element, but quartz piezoelectric is more weak, and dielectric constant is very
Low, limited by cut type and be there is size limitations, phosphoric acid gallium is as a kind of quartz-like crystal, and it almost has quartzy institute
Some advantages, i.e. do not have single order pyroelectricity, there is the temperature-compensating cut type required for piezoelectric oscillator and wave filter,
And there is the highest resistivity, but its electromechanical coupling factor is more much higher, when up to 933 DEG C than quartz
Physical characteristic also only has the least change, therefore has an excellent thermal power characteristic with its device made, the highest and
The most highly stable sensitivity and extraordinary linearly, all substantially exceed in terms of certainty of measurement and reliability
The device that quartz makes.
At present, the production method of phosphoric acid gallium mainly has hydrothermal/solvent heat, pyrosol growth method, makes
During by adding additive reaction and the impurity that introduces easily affects the purity of final products, high temperature
Manufacture method be difficult to again to reach to make the purpose of small size phosphoric acid man, existing hydrothermal/solvent by the use of thermal means
All introduce the impurity elements such as Cl, N, and glomerate phosphoric acid gallium can not be given birth to, and ultimately generate phosphorus
Purifying after acid gallium product, this greatly reduces the purity of product, directly affects follow-up piezoelectricity again
The using effect of device.
Summary of the invention
The defect existed for the preparation method of phosphoric acid gallium in prior art, it is an object of the invention to be to provide
A kind of purity is high and has the preparation method of phosphoric acid gallium of micron-size spherical pattern.
In order to realize above-mentioned technical purpose, the invention provides the preparation method of a kind of micron-size spherical phosphoric acid gallium,
The method comprises the following steps:
1) by Ga2O3Join in reactor with phosphoric acid solution, closed reactor, it is heated to 80～90 DEG C and stirs
Mix reaction, until reactant liquor clarification；
2) open wide reactor, be heated to reactant liquor boiling and be evaporated, until after thickness, adding in reactor
Enter pure water dilution, then closed reactor, be heated to 90～110 DEG C, be incubated 40～80 minutes；Further add
Heat, to 120～180 DEG C, is passed through argon to reacting kettle inner pressure simultaneously in reactor and reaches 3～5MPa, maintain
After 60～180 minutes, natural cooling, filters, dries, obtain micron-size spherical phosphoric acid gallium powder.
Preferably scheme, phosphoric acid solution mass percent concentration is 10～80%；It is more preferably 40～60%.
Preferably scheme, Ga2O3Purity is 99.999%.
More preferably scheme, phosphoric acid solution and Ga2O3Mass ratio be 7～3:1, be more preferably 3:1.
Preferably scheme, water typically uses pure water, it is to avoid the introducing of impurity.
The inventive method is obtained in that high-purity spherical phosphoric acid gallium, and its committed step is: 1, initially with phosphorus
G is dissolved in acid2O3After, remove unnecessary phosphoric acid by heating direct evaporation, it is not necessary to add in alkali and unnecessary acid, and
Avoid basic ion to follow-up phosphoric acid gallium pattern and the impact of purity；2, stepwise reaction is used to prepare standard ball
The phosphoric acid gallium of shape pattern, is first heated to 90～110 DEG C, is incubated 40～80 minutes；Further it is heated to 120～180
DEG C, being passed through argon to reacting kettle inner pressure in reactor reaches 3～5MPa simultaneously, and its purpose makes first to exist
Spherical phosphoric acid gallium seed crystal is grown, further in following temperature 120～180 DEG C and pressure at a temperature of 90～110 DEG C
Under the conditions of power 3～5MP, under the High Temperature High Pressure hydrothermal condition of the present invention, in solution, phosphate anion can press down
Gallium phosphate crystal processed, at unidirectional unidirectional growth, allows crystal grow in XYZ direction simultaneously, thus phosphoric acid
The growth of gallium crystalchecked obtains micron-size spherical gallium phosphate crystal.
Hinge structure, the Advantageous Effects that technical scheme is brought:
1, Ga prepared by the present invention2O3Purity is high, and up to 99.999%.
2, the phosphoric acid gallium powder size that prepared by the present invention is micron order, and pattern is spherical.
3, the preparation method of the present invention is simple to operate, low cost, it is not necessary to use any additive, it is to avoid miscellaneous
The introducing of matter, improves product purity.
Accompanying drawing explanation
[Fig. 1] is the micron-size spherical phosphoric acid gallium powder X-ray diffraction pattern of embodiment 1 preparation；
[Fig. 2] is the scanning electron microscope (SEM) photograph of the micron-size spherical phosphoric acid gallium powder of embodiment 1 preparation；A sweeps for × 500
Retouch Electronic Speculum figure；B is × 5000 scanning electron microscope (SEM) photographs；C is × 10000 scanning electron microscope (SEM) photographs；
[Fig. 3] is the micron-size spherical phosphoric acid gallium powder diameter scattergram of embodiment 1 preparation.
Detailed description of the invention
Following example are intended to further illustrate present invention rather than limit the protection of the claims in the present invention
Scope.
The phosphoric acid related in following example is UP level；Ga2O3For 5N level (99.999%), it is city
Sell conventional products.
Embodiment 1
1) adding 0.3kg mass percent concentration in politef reactor is the phosphoric acid of 50%, and
The Ga of 0.1kg purity 99.999%2O3, closed reactor, heated and stirred to solution is clarified.
2) open wide sealed reactor, by clear liquor heating evaporation to thick (evaporation water and excess phosphoric acid), add
Enter the pure water dilution of 3 times of liquor capacities of dope, then closed reactor, be warming up to 80 DEG C, be incubated 60 minutes,
Then it is warmed up to 120 DEG C, is passed through 99.999% argon simultaneously, maintain pressure at 3 MPas, hold time 160
Minute, the then near room temperature of natural cooling, i.e. obtain micron-size spherical phosphoric acid gallium powder after product filtering drying.
Preparation micron-size spherical phosphoric acid gallium powder XRD figure as it is shown in figure 1, from figure 1 it appears that
Compared with the phosphoric acid gallium of standard, its substantially free of impurities peak occurs, shows that its purity is high.Micron-size spherical phosphoric acid gallium
The pattern of powder and particle diameter distribution can be found out from Fig. 2 and Fig. 3, and its pattern is the spherical of standard, and particle diameter
It is evenly distributed, there is micron-scale.
Embodiment 2
1) adding 0.9kg in politef reactor, mass percent concentration is the UP level phosphoric acid of 50%,
And the Ga of 0.3kg purity 99.999%2O3, closed reactor, heated and stirred to solution is clarified.
2) sealed reactor is opened wide, by clear liquor heating evaporation to thick (evaporation water and excess phosphoric acid),
Add the pure water dilution of 4 times of liquor capacities of dope, then closed reactor, be warming up to 100 DEG C, be incubated 60
Minute, be then warmed up to 180 DEG C, be passed through 99.999% argon simultaneously, maintain pressure at 5 MPas, the time 80
Minute, the then near room temperature of natural cooling, i.e. obtain micron-size spherical phosphoric acid gallium powder after product filtering drying；
The phosphoric acid gallium powder purity obtained and pattern are close with embodiment 1.
Claims (6)
1. the preparation method of a micron-size spherical phosphoric acid gallium, it is characterised in that: comprise the following steps:
1) by Ga2O3Join in reactor with phosphoric acid solution, closed reactor, it is heated to 80～90 DEG C of stirrings anti-
Should, until reactant liquor clarification；
2) open wide reactor, be heated to reactant liquor boiling and be evaporated, until after thickness, adding pure in reactor
Water dilutes, then closed reactor, is heated to 90～110 DEG C, is incubated 40～80 minutes；Further it is heated to
120～180 DEG C, in reactor, it is passed through argon to reacting kettle inner pressure simultaneously reaches 3～5MPa, maintain 60～180
After minute, natural cooling, filters, dries, obtain micron-size spherical phosphoric acid gallium powder.
The preparation method of micron-size spherical phosphoric acid gallium the most according to claim 1, it is characterised in that: described
Phosphoric acid solution mass percent concentration is 10～80%.
The preparation method of micron-size spherical phosphoric acid gallium the most according to claim 2, it is characterised in that: described
Phosphoric acid solution mass percent concentration is 40～60%.
The preparation method of micron-size spherical phosphoric acid gallium the most according to claim 2, it is characterised in that: described
Ga2O3Purity is 99.999%.
5. according to the preparation method of the micron-size spherical phosphoric acid gallium described in any one of Claims 1 to 4, it is characterised in that:
Described phosphoric acid solution and Ga2O3Mass ratio be 7～3:1.
The preparation method of micron-size spherical phosphoric acid gallium the most according to claim 5, it is characterised in that: described
Phosphoric acid solution and Ga2O3Mass ratio be 3:1.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108965A (en) * | 1985-12-20 | 1987-12-09 | 联合碳化公司 | Crystalline gallophosphate compositions |
| CN1311355A (en) * | 1999-12-28 | 2001-09-05 | Avl里斯脱有限公司 | Method for single-crystal growth |
| CN1763264A (en) * | 2005-10-08 | 2006-04-26 | 山东大学 | Flux Growth Method of Gallium Phosphate Crystal |
| CN101104950A (en) * | 2007-08-07 | 2008-01-16 | 山东大学 | Flux Growth Method of TriGallium Phosphate Crystal |
| CN104495778A (en) * | 2015-01-06 | 2015-04-08 | 青岛大学 | Preparation method of gallophosphate microporous material |
| CN105018089A (en) * | 2015-07-06 | 2015-11-04 | 河北大学 | Phosphate or metaphosphate based visible-ultraviolet up-conversion luminescence material doped with rare earth ions, and preparation method and application thereof |
-
2016
- 2016-07-19 CN CN201610571110.2A patent/CN105967162B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108965A (en) * | 1985-12-20 | 1987-12-09 | 联合碳化公司 | Crystalline gallophosphate compositions |
| CN1311355A (en) * | 1999-12-28 | 2001-09-05 | Avl里斯脱有限公司 | Method for single-crystal growth |
| CN1763264A (en) * | 2005-10-08 | 2006-04-26 | 山东大学 | Flux Growth Method of Gallium Phosphate Crystal |
| CN101104950A (en) * | 2007-08-07 | 2008-01-16 | 山东大学 | Flux Growth Method of TriGallium Phosphate Crystal |
| CN104495778A (en) * | 2015-01-06 | 2015-04-08 | 青岛大学 | Preparation method of gallophosphate microporous material |
| CN105018089A (en) * | 2015-07-06 | 2015-11-04 | 河北大学 | Phosphate or metaphosphate based visible-ultraviolet up-conversion luminescence material doped with rare earth ions, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| SHIN-ICHI HIRANO, ET AL.: ""Hydrothermal Synthesis of Gallium Orthophosphate Crystals"", 《BULL. CHEM. SOC. JPN》 * |
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Address after: 412000 Jinshan private science and Technology Park, Hetang District, Zhuzhou City, Hunan Province Patentee after: Zhuzhou Keneng New Material Co.,Ltd. Address before: 412000 Jinshan private science and Technology Park, Hetang District, Zhuzhou City, Hunan Province Patentee before: ZHUZHOU KENENG NEW MATERIAL Co.,Ltd. |