CN103525423A - Preparation method of rare earth lutetium phosphate nano-material - Google Patents
Preparation method of rare earth lutetium phosphate nano-material Download PDFInfo
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Abstract
Belonging to the technical field of functional material synthesis, the invention relates to a preparation method of a rare earth lutetium phosphate nano-material. The method consists of: firstly dissolving lutetium oxide in nitric acid to react so as to generate a lutetium nitrate solution; then dissolving diammonium phosphate in re-distilled water to obtain a diammonium phosphate solution; then diluting the lutetium nitrate solution and conducting heating, adding the diammonium phosphate solution dropwisely, and performing stirring continuously to obtain a white suspended solution; centrifuging the obtained white suspended solution, pouring out the supernatant to obtain white precipitates, then employing the re-distilled water to clean the precipitates, and repeating centrifugation 3-5 times to wash off ions attached to precipitated particles, thus obtaining the purified precipitates; then placing the purified precipitates in a platinum crucible, and putting the platinum crucible into a box type resistance furnace to carry out baking, thus obtaining dry powder, i.e. the rare earth lutetium phosphate nano-material. The method has the advantages of simple preparation process, mild reaction conditions, simple operation, easy realization and amplification, low cost and less energy consumption, and the prepared nano-material has good chemical properties and high purity.
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 phosphoric acid lutetium nano material.
Background technology:
The physical chemistry of RE phosphate excellence makes it at fluorescent material, on coating and dense sintering, there is 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 is abundant, magnetic moment of atom is high, than the many 1-3 of a number order of magnitude of other element transition of electronic energy in the periodic table of elements, thereby 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 good.At present, the method of preparing rare earth phosphate nano 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, need to seek to design a kind of mild condition, simple to operate, be easy to realize and amplify, not needing the preparation method of the conditions such as High Temperature High Pressure or high vacuum, rare earth phosphoric acid lutetium nano material that energy consumption is low.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seek design a kind of method that adopts chemical precipitation method to prepare rare earth phosphoric acid lutetium nano material is provided, reaction conditions is gentle, and easy and simple to handle, the rare earth phosphoric acid lutetium nano material purity of preparation is high.
To achieve these goals, the rare earth phosphoric acid lutetium preparation the present invention relates to comprises synthetic and two steps of purifying, and its concrete preparation technology is:
(1) synthetic: 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 add redistilled water dilution lutecium nitrate solution to pH=1, heated solution slowly splashes into 100ml ammonium dibasic phosphate solution continuous stirred solution while extremely approaching boiling, obtain stopping heating and continuing stirred solution after white suspension liquid, 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, after pouring out supernatant liquid, obtain white precipitate, use again redistilled water washing and precipitating, 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 adhering on deposit seeds, the precipitation after being purified; Then the precipitation after purifying is placed in to conventional platinum crucible, puts into chamber type electric resistance furnace and at 1000 ℃, dry burning 5 hours, obtain dry powder, be rare earth phosphoric acid lutetium nano material.
The fusing point of rare earth phosphoric acid lutetium nano material prepared by the present invention is higher than 2000 ℃, and Mohs' hardness is 4-7.5, the tetragonal system that RE phosphate crystal is body-centered cubic structure, and spacer is I4
1/ amd,
α=β=γ=90 °, Z=4; The stable chemical nature of rare earth phosphoric acid lutetium 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, is easy to realize and amplify, and cost is low, less energy consumption, and the rare earth phosphoric acid lutetium nano material chemical property of preparation is good, and purity is high.
Accompanying drawing explanation:
Fig. 1 is the rare earth phosphoric acid lutetium 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 the rare earth phosphoric acid lutetium nano material prepared of the present invention.
Embodiment:
Below by embodiment, be also described further by reference to the accompanying drawings.
Embodiment:
The present embodiment is prepared phosphoric acid salt LuPO
4the concrete steps of nano material comprise synthetic and two steps of purifying:
(1) synthetic: the lutecium oxide (Lu that is 99.99% by 3.98g purity
2o
3) be dissolved in the nitric acid that 30ml concentration is 65-68w% and react and obtain lutecium nitrate solution, then add redistilled water diluting soln to pH=1; The Secondary ammonium phosphate that is 99.5% by 400g purity is again dissolved in 700ml redistilled water, filters after one time, then use the membrane filtration twice of 0.22 μ m with qualitative filter paper, obtains pure ammonium dibasic phosphate solution; Then the lutecium nitrate solution after dilution is transferred on digital display heating magnetic stirring apparatus 6, putting into length is magneton 5 stirred solutions of 5cm, and be heated to approach and get ammonium dibasic phosphate solution that 100ml prepares after boiling in drop-burette, slowly splash in lutecium nitrate solution to pH=3, obtain stopping heating and continuing stirred solution after white suspension liquid, make solution be cooled to room temperature;
(2) purify: the white suspension liquid obtaining in step (1) is poured in centrifuge tube, put into supercentrifuge with 5000r/min centrifugal 10 minutes, pour out after supernatant liquid, to the centrifugal precipitation going out, repeatedly wash centrifugal, the supernatant liquid pH=7 going out until centrifugal, wash the ion soluble in water adhering on deposit seeds, the precipitation after being purified; Then the precipitation after purifying is placed in to platinum crucible, puts into chamber type electric resistance furnace and at 1000 ℃, dry burning 5 hours, obtain dry powder and be rare earth phosphoric acid lutetium nano material.
The theoretical yield of rare earth phosphoric acid lutetium 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 phosphoric acid lutetium (LuPO prepared by the present embodiment
4) diffraction peak is consistent with standard JCPDS card (No.43-0003) in the XRD figure spectrum of nano material, the LuPO that each diffraction peak all can index is body-centered cubic structure
4(I4
1/ amd), illustrate that the powder that adopts the present embodiment to prepare is LuPO
4powder; In diffraction peak, there is not non-LuPO
4peak, the LuPO preparing is described
4powder is comparatively pure.
Claims (2)
1. a preparation method for rare earth phosphoric acid lutetium nano material, is characterized in that comprising synthetic and two steps of purifying, and its concrete preparation technology is:
(1) synthetic: first lutecium oxide is dissolved in nitric acid, wherein the mol ratio of lutecium oxide and nitric acid is 1:70, 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 add redistilled water dilution lutecium nitrate solution to pH=1, heated solution slowly splashes into 100ml ammonium dibasic phosphate solution continuous stirred solution while extremely approaching boiling, obtain stopping heating and continuing stirred solution after white suspension liquid, 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, after pouring out supernatant liquid, obtain white precipitate, use again redistilled water washing and precipitating, 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 adhering on deposit seeds, the precipitation after being purified; Then the precipitation after purifying is placed in to conventional platinum crucible, puts into chamber type electric resistance furnace and at 1000 ℃, dry burning 5 hours, obtain dry powder, be rare earth phosphoric acid lutetium nano material.
2. the preparation method of rare earth phosphoric acid lutetium nano material according to claim 1, it is characterized in that the fusing point of rare earth phosphoric acid lutetium nano material of preparation is higher than 2000 ℃, Mohs' hardness is 4-7.5, the tetragonal system that RE phosphate crystal is body-centered cubic structure, and spacer is I4
1/ amd,
α=β=γ=90 °, Z=4; Rare earth phosphoric acid lutetium nano material not with nitric acid and hydrochloric acid reaction.
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Granted publication date: 20160217 Termination date: 20191025 |