CN103525423B - A kind of preparation method of rare earth lutetium phosphate nano-material - Google Patents
A kind of preparation method of rare earth lutetium phosphate nano-material Download PDFInfo
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- CN103525423B CN103525423B CN201310514222.0A CN201310514222A CN103525423B CN 103525423 B CN103525423 B CN 103525423B CN 201310514222 A CN201310514222 A CN 201310514222A CN 103525423 B CN103525423 B CN 103525423B
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Abstract
The invention belongs to functional materials synthesis technical field, relate to a kind of preparation method of rare earth lutetium phosphate nano-material, first lutecium oxide is dissolved in nitric acid reaction and generates lutecium nitrate solution; Again Secondary ammonium phosphate is dissolved in redistilled water and obtains ammonium dibasic phosphate solution; Then dilute lutecium nitrate solution and after heating, instill the continuous stirred solution of ammonium dibasic phosphate solution and obtain white suspension solution; The white suspension solution obtained is carried out centrifugal, after pouring out supernatant liquid, obtains white precipitate, then to use after redistilled water washing and precipitating repeated centrifugation 3-5 time, wash the ion that deposit seeds adheres to, obtain the precipitation after purifying; Then the precipitation after purification is placed in platinum crucible, puts into chamber type electric resistance furnace and dry the powder burning and obtain drying, be rare earth lutetium phosphate nano-material; Its preparation process is simple, and reaction conditions is gentle, simple to operate, is easy to realize and amplify, and cost is low, less energy consumption, and the nano material chemical property of preparation is good, and purity is high.
Description
Technical field:
The invention belongs to functional materials synthesis technical field, relate to a kind of preparation technology of luminous host material, particularly a kind of preparation method of rare earth lutetium phosphate nano-material.
Background technology:
The physical chemistry of RE phosphate excellence makes it at fluorescent material, coating and dense sintering has potential application widely, rare earth ion has the 4f shell of underfilling, the internal layer 4f shell of rare earth ion is many to electronics, electronic level enriches, magnetic moment of atom is high, 1-3 the order of magnitude more than the number of other element transition of electronic energy in the periodic table of elements, thus there is the magnetic of many excellences, electricity, the characteristic such as light and core, nearly 30000 the observable spectral lines of its spectrum, they can be launched from UV-light, visible ray is to the radiation of the various wavelength in infrared light district, therefore, RE phosphate is the luminous host material that a class is excellent.At present, the method preparing rare earth phosphate nanometer material mainly comprises hydrothermal method, microwave method, high-temperature solid phase reaction method, supersonic method, sol-gel method, coprecipitation method and combustion method, but these method complicated operations, reaction conditions requires high, energy consumption is high, therefore, needs to seek to design a kind of mild condition, simple to operate, be easy to realize and amplify, do not need the preparation method of the rare earth lutetium phosphate nano-material that the condition such as High Temperature High Pressure or high vacuum, energy consumption are low.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art existence, seeking to design provides a kind of method adopting chemical precipitation method to prepare rare earth lutetium phosphate nano-material, and reaction conditions is gentle, and easy and simple to handle, the rare earth lutetium phosphate nano-material purity of preparation is high.
To achieve these goals, the rare earth lutetium preparation that the present invention relates to comprises synthesis and two steps of purifying, and its concrete preparation technology is:
(1) synthesize: first by lutecium oxide (Lu
2o
3) be dissolved in nitric acid, wherein the mol ratio of lutecium oxide and nitric acid is 1:70, lutecium oxide (Lu
2o
3) generate lutecium nitrate (Lu (NO with nitric acid reaction
3)
3) solution; Again 400g Secondary ammonium phosphate is dissolved in 700ml redistilled water, obtains ammonium dibasic phosphate solution; Then after adding redistilled water dilution lutecium nitrate solution to pH=1, heated solution is to slowly instilling 100ml ammonium dibasic phosphate solution during close boiling and continuous stirred solution, stop after obtaining white suspension liquid heating and continuing stirred solution, make solution be cooled to room temperature, obtain white suspension solution;
(2) purify: the white suspension solution that step (1) is obtained with 5000r/min carry out 10 minutes centrifugal, white precipitate is obtained after pouring out supernatant liquid, use redistilled water washing and precipitating again, again with 5000r/min carry out 10 minutes centrifugal, repeated centrifugation 3-5 time is until after supernatant liquid pH=7, wash the ion soluble in water that deposit seeds adheres to, obtain the precipitation after purifying; Then the precipitation after purification is placed in conventional platinum crucible, puts into chamber type electric resistance furnace and at 1000 DEG C, dry burning 5 hours, obtain dry powder, be rare earth lutetium phosphate nano-material.
The fusing point of rare earth lutetium phosphate nano-material prepared by the present invention is higher than 2000 DEG C, and Mohs' hardness is 4-7.5, and RE phosphate crystal is the tetragonal system of body-centered cubic structure, and spacer is I4
1/ amd,
α=β=γ=90 °, Z=4; The stable chemical nature of rare earth lutetium phosphate nano-material, is not included most of pharmaceutical chemicals corrosion of nitric acid and hydrochloric acid.
Compared with prior art, its preparation process is simple in the present invention, and reaction conditions is gentle, simple to operate, and be easy to realize and amplify, cost is low, less energy consumption, and the rare earth lutetium phosphate nano-material chemical property of preparation is good, and purity is high.
Accompanying drawing illustrates:
Fig. 1 is the rare earth lutetium phosphate nano-material synthesizer structural principle schematic diagram that the present invention uses, comprising drop-burette 1, ammonium dibasic phosphate solution 2, beaker 3, lutecium nitrate solution 4, magneton 5, digital display heating magnetic stirring apparatus 6 and thermopair 7.
Fig. 2 is the XRD figure spectrum of rare earth lutetium phosphate nano-material prepared by the present invention.
Embodiment:
Also be described further by reference to the accompanying drawings below by embodiment.
Embodiment:
The present embodiment prepares phosphoric acid salt LuPO
4the concrete steps of nano material comprise synthesis and two steps of purifying:
(1) synthesize: be the lutecium oxide (Lu of 99.99% by 3.98g purity
2o
3) to be dissolved in 30ml concentration be carry out in the nitric acid of 65-68w% being obtained by reacting lutecium nitrate solution, then adds redistilled water diluting soln to pH=1; By 400g purity be again 99.5% Secondary ammonium phosphate be dissolved in 700ml redistilled water, after filtering one time with qualitative filter paper, then use the membrane filtration twice of 0.22 μm, obtain pure ammonium dibasic phosphate solution; Then the lutecium nitrate solution after dilution is transferred on digital display heating magnetic stirring apparatus 6, put into magneton 5 stirred solution that length is 5cm, and be heated to close to getting ammonium dibasic phosphate solution that 100ml prepares after boiling in drop-burette, slowly be added dropwise in lutecium nitrate solution to pH=3, stop after obtaining white suspension liquid heating and continuing stirred solution, make solution be cooled to room temperature;
(2) purify: the white suspension liquid obtained in step (1) is poured in centrifuge tube, put into supercentrifuge with 5000r/min centrifugal 10 minutes, after pouring out supernatant liquid, to centrifugal go out precipitation repeatedly wash centrifugal, until centrifugal go out supernatant liquid pH=7, wash the ion soluble in water that deposit seeds adheres to, obtain the precipitation after purifying; Then the precipitation after purification is placed in platinum crucible, puts into chamber type electric resistance furnace and at 1000 DEG C, dry burning 5 hours, obtain dry powder and be rare earth lutetium phosphate nano-material.
The theoretical yield of rare earth lutetium phosphate nano-material prepared by the present embodiment is 5.4g, and after purification process, output is 5.02g, and productive rate is 93%.
The present embodiment adopts D8Advance type X-ray diffractometer to record the RE phosphate LuPO of preparation
4the XRD figure of powder is composed as shown in Figure 2, as can be seen from Figure 2, and rare earth lutetium (LuPO prepared by the present embodiment
4) nano material XRD figure spectrum in diffraction peak consistent with standard JCPDS card (No.43-0003), each diffraction peak can index be all the LuPO of body-centered cubic structure
4(I4
1/ amd), illustrate that the powder adopting the present embodiment to prepare is LuPO
4powder; Non-LuPO is there is not in diffraction peak
4peak, the LuPO prepared is described
4powder is comparatively pure.
Claims (1)
1. a preparation method for rare earth lutetium phosphate nano-material, it is characterized in that comprising synthesis and two steps of purifying, its concrete preparation technology is:
(1) synthesize: be first dissolved in nitric acid by lutecium oxide, wherein the mol ratio of lutecium oxide and nitric acid is 1:70, and lutecium oxide and nitric acid reaction generate lutecium nitrate solution; Again 400g Secondary ammonium phosphate is dissolved in 700ml redistilled water, obtains ammonium dibasic phosphate solution; Then after adding redistilled water dilution lutecium nitrate solution to pH=1, heated solution is to slowly instilling 100ml ammonium dibasic phosphate solution during close boiling and continuous stirred solution, stop after obtaining white suspension liquid heating and continuing stirred solution, make solution be cooled to room temperature, obtain white suspension solution;
(2) purify: the white suspension solution that step (1) is obtained with 5000r/min carry out 10 minutes centrifugal, white precipitate is obtained after pouring out supernatant liquid, use redistilled water washing and precipitating again, again with 5000r/min carry out 10 minutes centrifugal, repeated centrifugation 3-5 time is until after supernatant liquid pH=7, wash the ion soluble in water that deposit seeds adheres to, obtain the precipitation after purifying; Then the precipitation after purification is placed in conventional platinum crucible, puts into chamber type electric resistance furnace and at 1000 DEG C, dry burning 5 hours, obtain dry powder, be rare earth lutetium phosphate nano-material; The fusing point of the rare earth lutetium phosphate nano-material of preparation is higher than 2000 DEG C, and Mohs' hardness is 4-7.5, and rare earth lutetium is the tetragonal system of body-centered cubic structure, and spacer is I4
1/ amd,
α=β=γ=90 °, Z=4; Rare earth lutetium phosphate nano-material not with nitric acid and hydrochloric acid reaction.
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|---|---|---|---|---|
| CN102849714A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method for rare earth phosphate nanometer material |
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