CN104692349A - Method for performing CO2-enriched hydrothermal synthesis to gadolinium phosphate nanorod - Google Patents
Method for performing CO2-enriched hydrothermal synthesis to gadolinium phosphate nanorod Download PDFInfo
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- CN104692349A CN104692349A CN201410810264.3A CN201410810264A CN104692349A CN 104692349 A CN104692349 A CN 104692349A CN 201410810264 A CN201410810264 A CN 201410810264A CN 104692349 A CN104692349 A CN 104692349A
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- salt
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- gadolinium
- hydrothermal synthesis
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- JAOZQVJVXQKQAD-UHFFFAOYSA-K gadolinium(3+);phosphate Chemical compound [Gd+3].[O-]P([O-])([O-])=O JAOZQVJVXQKQAD-UHFFFAOYSA-K 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 11
- 239000002073 nanorod Substances 0.000 title abstract 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 235000011089 carbon dioxide Nutrition 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 150000003839 salts Chemical class 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000000243 solution Substances 0.000 abstract description 11
- 229910019142 PO4 Inorganic materials 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract 1
- 230000002045 lasting effect Effects 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 7
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- -1 rare earth phosphate Chemical class 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910052688 Gadolinium Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- VWDWKYIASSYTQR-YTBWXGASSA-N sodium;dioxido(oxo)azanium Chemical compound [Na+].[O-][15N+]([O-])=O VWDWKYIASSYTQR-YTBWXGASSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical group [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for performing CO2-enriched hydrothermal synthesis to a gadolinium phosphate nanorod. The method is characterized by comprising the following steps: respectively preparing a Gd<3+> salt solution and a PO4<3+> solution at room temperature; adding the two solutions into the reaction kettle according to the volume ratio of 1:1, stirring while adding, continuously stirring for 30min to 1h; introducing CO2 gas or dry ice into the reaction kettle, controlling the pressure in the kettle to be 1-10Mpa, and sealing and heating the high-pressure reaction kettle, setting the reaction temperature to be 100-200DEG C and the lasting time to be 12h-2d, then naturally cooling the high-pressure reaction kettle to room temperature; filtering the reacted product, washing sequentially with deionized water and anhydrous ethanol and centrifuging for twice; and drying the dried and centrifuged product for more than 6h at 50-100DEG C, thus obtaining a final pure product.
Description
Technical field
The present invention relates to a kind of preparation method of rare earth phosphate nanometer material, belong to functional materials synthesis technical field.
Background technology
In the periodic table of elements, gadolinium (Gd) is positioned at IIIB race, and ordination number is 64, belongs to light rare earths, and the content of gadolinium in the earth's crust is 0.000636%.In addition, the element of ordination number 57 to 71, they are called as lanthanon together with gadolinium.Lanthanon and yttrium of the same clan (Y) and scandium (Sc) are referred to as rare earth element.Rare earth element has special electron structure (4f
0-145d
0-16s
2), their out-shell electron is substantially identical, internal layer 4f electronic level is very close again, and 4f is the shell of a underfilling, electronic orbit is complete empty, be partly full of and be entirely full of the ion of electronics has optics inertia, for stable state, because of the feature of its outer electronic structure, make it have special physicochemical property.
RE phosphate material, because having the advantages such as specific refraction that in good thermostability, water, solubleness is minimum and high, is widely used in the fields such as luminescent material, stupalith, catalyzer, alloy material and lubricant.Gadolinium phosphate (GdPO
4), be often used as the good matrix of other rare earth ion of doping.The luminescent material being matrix with nanometer Gadolinium phosphate have good stability, thermal capacitance large, there is high efficiency feature under the exciting of vacuum-ultraviolet light, excite because material particle size is less than or launches optical wavelength simultaneously, therefore light field can be approximately even in particle range, can significantly improve cathode tube and plasma display sharpness.Meanwhile, Gadolinium phosphate fusing point is high, with some oxide compound compounds, as Al
2o
3, high temperature resistant, anti-oxidant, that electrical insulating property the is good composite ceramics processed can be prepared.In addition, Gadolinium phosphate is also widely used in alloy material, catalytic material.Therefore the Gadolinium phosphate studying controlled monazite structure has great importance.
Current synthesizing rare-earth phosphoric acid salt mainly contains the methods such as sol-gel method, hydrothermal method, the precipitator method, solid phase method, combustion method and microwave method, wherein commonplace with hydrothermal synthesis method.Existing large quantity research shows that pH controls one of most important factor of the brilliant looks of rare earth phosphate nanometer material crystalline form, but adopt the method for Syntheses in water RE phosphate at present, all just in initial aqueous solution, have adjusted pH, there is no buffer pH, lacked the control of gradual change physical and chemical condition to the brilliant looks of its crystalline form, to there is crystallization degree be not very high, size be not very evenly, problem that controllability is not strong.At occurring in nature, the geologic fluids that the Ree-phospeate Minerals of hydrothermal origin is formed has certain CO usually
2dividing potential drop, CO in hydrothermal solution
2can the pH of buffered soln.The present invention is by making full use of CO
2the feature of dividing potential drop buffered soln pH, the Gadolinium phosphate nanometer rod that Hydrothermal Synthesis purity is high, size uniform, crystallization degree are good, controllability is strong.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of feature making full use of CO2 dividing potential drop buffered soln pH, the method for the Gadolinium phosphate nanometer rod that Hydrothermal Synthesis purity is high, size uniform, crystallization degree are good, controllability is strong.
Technical scheme of the present invention is: a kind of rich CO
2the method of Hydrothermal Synthesis Gadolinium phosphate nanometer rod, under room temperature, prepares Gd respectively
3+salt and PO
4 3+salts solution; Be that 1:1 adds in reactor by above-mentioned two kinds of solution according to volume ratio, add and stir, and Keep agitation 30 min to 1 h; Logical CO in reactor
2gas or add dry ice, controlling still internal pressure is 1-10 Mpa, sealed high pressure reactor; Heating high-pressure reactor, setting temperature of reaction is 100-200 DEG C, time length 12 h-2 d, and then naturally cooling autoclave is to room temperature; Reacted product is filtered, and priority deionized water and dehydrated alcohol respectively wash, centrifugal twice; By washing, centrifugal after product at 50 DEG C ~ 100 DEG C drying 6 more than h; Final clean product can be obtained.
Described Gd
3+salt and PO
4 3+salt is respectively conventional soluble g d
3+salt and solubility PO
4 3+salt.
Beneficial effect of the present invention:
(1) the present invention makes full use of CO
2the pH of dividing potential drop buffered soln, the Gadolinium phosphate nanometer rod purity of Hydrothermal Synthesis is high, size uniform, crystallization degree are good, controllability is strong.
(2) organism that tensio-active agent, dispersion agent, coating etc. not can be recycled is not added in preparation process of the present invention, environmental friendliness.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the Gadolinium phosphate that embodiment 3 is synthesized;
Fig. 2 is the SEM figure of the Gadolinium phosphate that embodiment 3 is synthesized.
Embodiment
Embodiment 1
Take the Gadolinium trinitrate [Gd (NO of certain mass
3)
3 6H
2o] and Secondary ammonium phosphate [(NH
4)
2hPO
4], being made into concentration with deionized water is respectively the aqueous solution of the Gadolinium trinitrate of 0.36mol/L and the aqueous solution of Secondary ammonium phosphate.Be that 1:1 adds in reactor by Gadolinium trinitrate solution and ammonium dibasic phosphate solution according to volume ratio, add and stir, the initial compactedness controlling reactor is 70%, and Keep agitation 30 min to 1 h.Be filled with 1 MPa carbon dioxide to autoclave, close autoclave.Heating high-pressure reactor, controlling temperature of reaction is 180 DEG C, and 2 days time length, then autoclave naturally cools to room temperature.After reactor pressure release, product is filtered, centrifugal, and successively alternately respectively to wash twice with deionized water and dehydrated alcohol respectively, most relief product dry 12 h under 70 DEG C of environment.
Embodiment 2
Take the Gadolinium trinitrate [Gd (NO of certain mass
3)
3 6H
2o] and Secondary ammonium phosphate [(NH4)
2hPO
4], being made into concentration with deionized water is respectively the aqueous solution of the Gadolinium trinitrate of 0.36mol/L and the aqueous solution of Secondary ammonium phosphate.Be that 1:1 adds in reactor by Gadolinium trinitrate solution and ammonium dibasic phosphate solution according to volume ratio, add and stir, the initial compactedness controlling reactor is 70%, and Keep agitation 30 min to 1 h.Be filled with 5 MPa carbon dioxides to autoclave, close autoclave.Heating high-pressure reactor, controlling temperature of reaction is 180 DEG C, and 2 days time length, then autoclave naturally cools to room temperature.After reactor pressure release, product is filtered, centrifugal, and successively alternately respectively to wash twice with deionized water and dehydrated alcohol respectively, most relief product dry 12 h under 70 DEG C of environment.
Embodiment 3
Take the Gadolinium trinitrate [Gd (NO of certain mass
3)
3 6H
2o] and Secondary ammonium phosphate [(NH
4)
2hPO
4], being made into concentration with deionized water is respectively the aqueous solution of the Gadolinium trinitrate of 0.36mol/L and the aqueous solution of Secondary ammonium phosphate.By Gadolinium trinitrate solution and Secondary ammonium phosphate, (solution is that 1:1 adds in reactor according to volume ratio, adds and stirs, and the initial compactedness controlling reactor is 70%, and Keep agitation 30 min to 1 h.Add dry ice (solidified carbon dioxide) to autoclave, controlling reacting kettle inner pressure is 10 Mpa, closes autoclave.Heating high-pressure reactor, controlling temperature of reaction is 180 DEG C, and 2 days time length, then autoclave naturally cools to room temperature.After reactor pressure release, product is filtered, centrifugal, and successively alternately respectively to wash twice with deionized water and dehydrated alcohol respectively, most relief product dry 12 h under 70 DEG C of environment.The product of XRD phenogram display synthesis is pure Gadolinium phosphate.Gadolinium phosphate nanometer rod size uniform, the crystallization degree of SEM phenogram display synthesis are good.
Claims (2)
1. a rich CO
2the method of Hydrothermal Synthesis Gadolinium phosphate nanometer rod, is characterized in that: under room temperature, prepares Gd respectively
3+salt and PO
4 3+salts solution; Be that 1:1 adds in reactor by above-mentioned two kinds of solution according to volume ratio, add and stir, and Keep agitation 30 min to 1 h; Logical CO in reactor
2gas or add dry ice, controlling still internal pressure is 1-10 Mpa, sealed high pressure reactor; Heating high-pressure reactor, setting temperature of reaction is 100-200 DEG C, time length 12 h-2 d, and then naturally cooling autoclave is to room temperature; Reacted product is filtered, and priority deionized water and dehydrated alcohol respectively wash, centrifugal twice; By washing, centrifugal after product at 50 DEG C ~ 100 DEG C drying 6 more than h, final clean product can be obtained.
2. the rich CO of one according to claim 1
2the method of Hydrothermal Synthesis Gadolinium phosphate nanometer rod, is characterized in that: described Gd
3+salt and PO
4 3+salt is respectively conventional soluble g d
3+salt and solubility PO
4 3+salt.
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Cited By (1)
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CN111747392A (en) * | 2020-07-17 | 2020-10-09 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rodlike nanocrystalline |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101757642A (en) * | 2010-03-03 | 2010-06-30 | 天津科技大学 | Method for preparing gadolinium-containing nano particles |
CN102534777A (en) * | 2012-02-24 | 2012-07-04 | 南开大学 | Neodymium-doped potassium gadolinium phosphate laser crystal, and preparation method and application thereof |
CN102849711A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method of gadolinium phosphate nano-wires |
WO2014036506A2 (en) * | 2012-09-02 | 2014-03-06 | Global Tungsten & Powders Corp. | Y203:eu having improved brightness at reduced eu weight percentage |
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2014
- 2014-12-24 CN CN201410810264.3A patent/CN104692349B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101757642A (en) * | 2010-03-03 | 2010-06-30 | 天津科技大学 | Method for preparing gadolinium-containing nano particles |
CN102534777A (en) * | 2012-02-24 | 2012-07-04 | 南开大学 | Neodymium-doped potassium gadolinium phosphate laser crystal, and preparation method and application thereof |
CN102849711A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method of gadolinium phosphate nano-wires |
WO2014036506A2 (en) * | 2012-09-02 | 2014-03-06 | Global Tungsten & Powders Corp. | Y203:eu having improved brightness at reduced eu weight percentage |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111747392A (en) * | 2020-07-17 | 2020-10-09 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rodlike nanocrystalline |
CN111747392B (en) * | 2020-07-17 | 2023-03-14 | 南昌航空大学 | Method for preparing semi-hydrated samarium phosphate rod-shaped nanocrystalline |
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