CN107556998A - A kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion - Google Patents
A kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion Download PDFInfo
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- CN107556998A CN107556998A CN201710808638.1A CN201710808638A CN107556998A CN 107556998 A CN107556998 A CN 107556998A CN 201710808638 A CN201710808638 A CN 201710808638A CN 107556998 A CN107556998 A CN 107556998A
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Abstract
The invention discloses a kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion, belong to chemical industry, material and photonic propulsion crossing domain, be related to a kind of method for preparing rare-earth-doped fluoride up-conversion luminescence Nanodispersion using hypergravity reaction reinforcement technique i.e. rotating packed-bed reactor.Realize above-mentioned is included with source chemicals needed for the synthetic method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion：Rare Earths salt, sodium hydroxide, ammonium fluoride, surfactant, deionized water and absolute ethyl alcohol, Rare Earths salt includes yttrium chloride, ytterbium chloride and erbium chloride, surfactant is respectively oleic acid, oleyl amine and sodium citrate, and dispersion solvent includes ethanol, tetrahydrofuran, hexamethylene, chloroform and toluene.This method introduces rotating packed-bed reactor, and reaction precursor liquid is premixed, realizes that molecular level uniformly mixes, so as to synthesize the rare-earth-doped fluoride up-conversion luminescence Nanodispersion that particle size is small and particle diameter distribution is narrow.
Description
Technical field
The invention belongs to chemical industry, material and photonic propulsion crossing domain, more particularly to one kind to utilize high-gravity technology with rare earth
The method of doped fluoride up-conversion luminescence Nanodispersion.
Background technology
Up-conversion luminescent material is a kind of luminescent material that visible ray is excited by near infrared light, is to be based on anti-Stokes principles
Luminescent material.Up-conversion luminescent material has widely at bioluminescence imaging, three dimensional display and false proof aspect at present
Using.Up-conversion luminescent material is typically to be made up of two parts：Crystalline host material and the rare earth ion of doping.Host material has
Fluoride (composite fluoride), rare earth oxide (composite oxides), oxyfluoride, halide (oxyhalide), and sulfur-bearing
Compound.The phonon energy of wherein fluoride and halide (oxyhalide) is relatively low, has higher up-conversion luminescence performance, is
Most common up-conversion luminescent material matrix.At present for preparing with the side of conversion nano luminescent material on rare-earth-doped fluoride
Method includes following several：(a) thermal decomposition method, (b) high temperature solid-state method, (c) molte-salt synthesis, the hot method of (d) hydrothermal/solvent.First three
Method is required to higher reaction temperature, in addition, thermal decomposition method preparation process is to sky compared to the hot method of hydrothermal/solvent
Air-sensitive sense, it is desirable to have inert gas of a relatively high as protection gas, synthesis cost；High temperature solid-state method preparation process requires that high temperature is high
Pressure processing raw material, is unfavorable for volume production.The equipment and condition of the hot method of hydrothermal/solvent are simple, and building-up process is easy to operate, is most common
The method for preparing nano material, but the sample topography of this method synthesis is difficult to control, therefore based on the simple of hydrothermal/solvent heat
Method, propose a kind of its product morphology can be overcome uncontrollable and method the shortcomings that particle diameter distribution is uneven is extremely important.
Hypergravity refers in (the 9.8m/s accelerated than terrestrial gravitation2) under much bigger environment, the power suffered by material.
Under Elevated Gravity molecule diffusion and interphase mass transfer process ratio normal condition under it is much faster, huge shearing force can tear liquid
The film, silk and drop of micron to nano grade are cleaved into, produces boundary that is huge and quickly updating, microcosmic mixing and mass transport process obtain
Strengthen to great.High-gravity technology can realize that typical hypergravity equipment is RPB by hypergravity equipment.
High gravity rotating packed bed can produce Elevated Gravity so that and concentration, temperature and degree of supersaturation in bed are evenly distributed,
Be advantageous to nucleation and the growth of single-size.High gravity rotating packed bed provides industrial platform for production nano material simultaneously.
The content of the invention
The purpose of the present invention in view of the shortcomings of the prior art, while is preparing nanometer material using hypergravity reaction reinforcement technique
Clear superiority in terms of material, there is provided one kind is prepared using high gravity rotating packed bed reactor to be changed on rare-earth-doped fluoride
The new method of Illuminant nanometer dispersion.
To realize above-mentioned purpose, the technical solution adopted by the present invention is a kind of rare-earth-doped fluoride up-conversion luminescence
The preparation method of Nanodispersion, this preparation method add surface and lived using Rare Earths salt, sodium hydroxide and ammonium fluoride as raw material
Property agent, premixed in outer circulation type high gravity rotating packed bed, be well mixed laggard water-filling thermal response, washing, centrifugation, dry
After dry, solvent disperses, obtain with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.Realize with rare-earth-doped fluoride
Source chemicals needed for changing the synthetic method of Illuminant nanometer dispersion include：Rare Earths salt, sodium hydroxide, ammonium fluoride, surface
Activating agent, deionized water and absolute ethyl alcohol, Rare Earths salt include yttrium chloride, ytterbium chloride and erbium chloride, surfactant difference
For oleic acid, oleyl amine and sodium citrate, dispersion solvent includes ethanol, tetrahydrofuran, hexamethylene, chloroform and toluene.
Specific preparation method is as follows：
S1. ammonium fluoride solution is prepared：Compound concentration is 1mol/L ammonium fluoride solution, measures 15mL~20mL.
S2. the sodium hydrate solid for weighing 2g~2.5g is dissolved in 5mL~10mL deionized waters, is poured into after being completely dissolved
In the mixed solution of 40mL oleic acid and 40mL ethanol, stir.
S3. according to erbium chloride：Ytterbium chloride：The molar ratio of yttrium chloride is (2~20):18:(98~62) weigh rare earth chlorine
Hydrochlorate solid, is dissolved in 20mL~30mL deionized water.
S4. the mixed solution obtained in S2 is squeezed into outer circulation type high gravity rotating packed bed by peristaltic pump, and pressed
According to the solution obtained in S3 and the solution obtained in S1 sequentially are squeezed into outer circulation type from another charging aperture by peristaltic pump successively
In high gravity rotating packed bed.The solution obtained in the solution and S1 that are obtained in the mixed solution that is obtained in S2, S3 is molten for raw material
Liquid, material solution circulate 1min~5min. after all adding in high gravity rotating packed bed
S5. the mixed solution handled by S4 hypergravity is placed in 200mL polytetrafluoroethylene (PTFE) water heating kettle inner bags,
1h~2h is reacted under the conditions of 180 DEG C~200 DEG C.Be cooled to centrifugation after room temperature and obtain product powder, centrifugal speed be 8000rpm~
10000rpm, it is washed with deionized after 4 times and is washed 4 times with absolute ethyl alcohol again.
S6. the product for S5 centrifuge washings being handled to obtain dries 5h~10h, is cooled to room temperature as in 60 DEG C of drying boxes
After grind, obtain rare-earth-doped fluoride up-conversion luminescence nano-powder material.
S7. powder S6 obtained is added in dispersion solvent, sonicated to obtain changing hair on rare-earth-doped fluoride
Light Nanodispersion.
Rare earth fluoride is yttrium fluoride natrium or lithium yttrium fluoride.
Oleic acid in S2 can be replaced as surfactant, oleic acid with oleyl amine, sodium citrate.
The solution feed flow ratio obtained in S2 is obtained in S4 mixed solution and S3 is 3:1, S2 obtained mixing is molten
The solution feed flow ratio obtained in liquid and S1 is 3:1；The rotating speed of outer circulation type high gravity rotating packed bed be 1000rpm~
2500rpm, preferably rotating speed are more than 1000rpm, usually less than 2500rpm.
Dispersion solvent in S7 includes ethanol, tetrahydrofuran, hexamethylene, chloroform and toluene.
The inventive method prepares rare-earth-doped fluoride up-conversion luminescence using outer circulation type high gravity rotating packed bed and received
Rice dispersion, by transmission electron microscope (TEM), X-ray diffraction (XRD) analysis shows：Product purity is high, particle size
Small and particle diameter distribution is narrow, has good up-conversion luminescence performance.
Brief description of the drawings
Fig. 1 is product X-x ray diffraction (XRD) spectrogram of embodiment 1~4.
Fig. 2 is product transmission electron microscope (TEM) photo of embodiment 1.
Fig. 3 is product transmission electron microscope (TEM) photo of embodiment 2.
Fig. 4 is the dispersion luminous photo of embodiment 1.
Fig. 5 is the dispersion luminous photo of embodiment 2.
Fig. 6 is the dispersion luminous photo of embodiment 3.
Fig. 7 is the dispersion luminous photo of embodiment 4.
Fig. 8 is the dispersion luminous photo of embodiment 6.
Fig. 9 is the up-conversion luminescence spectrum of the product of embodiment 4.
Figure 10 is the transmission electron microscope and dispersion luminous photo figure of the present invention.
Embodiment
It is that the present invention is prepared with rare-earth-doped fluoride up-conversion luminescence using outer circulation high gravity rotating packed bed below
The non-limiting example of Nanodispersion.These embodiments have further described and demonstrated the embodiment in the scope of the invention.
The embodiment provided is merely to illustrate the present invention and not limited the scope of the invention, in bar without departing from the spirit and scope of the present invention
Under part, those skilled in the art can carry out various changes or modification to it, and these equivalent form of values are equally fallen within appended by the application
Claims limited range.
Embodiment 1
Weigh 2.4g sodium hydrate solids to be dissolved in 6mL deionized waters, by solution and 40mL oleic acid, 40mL after being completely dissolved
The mixed solution mixing of absolute ethyl alcohol, as solution A；It is 24.8mg to measure erbium chloride, ytterbium chloride and yttrium chloride solid respectively,
223.2mg it is dissolved in 776.8mg in 22mL deionized water, as B solution；The ammonium fluoride solution 16mL of quantitative preparation is measured,
As C solution.It is 1000rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through by peristaltic pump
In outer circulation type high gravity rotating packed bed, B solution and C solution are led to from another charging aperture by peristaltic pump successively in sequence
Enter in outer circulation type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, material solution is whole
After being passed through in outer circulation type high gravity rotating packed bed, 5min is circulated, the solution that discharges is placed in 200mL polytetrafluoroethylene (PTFE) hydro-thermal
In kettle inner bag, 200 DEG C of hydro-thermal reaction 2h, be cooled to after room temperature the centrifuge for being 8000rpm with rotating speed, and spend respectively from
Respectively washing 4 times of sub- water and absolute ethyl alcohol, are placed in 60 DEG C of dry 8h in drying box by resulting product powder, are cooled to room temperature and grind
Mill, is dispersed in alcohol solvent, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Embodiment 2
Weigh 2.4g sodium hydrate solids to be dissolved in 6mL deionized waters, by solution and 40mL oleic acid, 40mL after being completely dissolved
The mixed solution mixing of absolute ethyl alcohol, as solution A；It is 24.8mg to measure erbium chloride, ytterbium chloride and yttrium chloride solid respectively,
223.2mg and 776.8mg are dissolved in 22mL deionized water, as B solution；The ammonium fluoride solution 16mL of quantitative preparation is measured,
As C solution.It is 1500rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through by peristaltic pump
In outer circulation type high gravity rotating packed bed, B solution and C solution are led to from another charging aperture by peristaltic pump successively in sequence
Enter in outer circulation type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, material solution is whole
After being passed through in outer circulation type high gravity rotating packed bed, 5min is circulated, the solution that discharges is placed in 200mL polytetrafluoroethylene (PTFE) hydro-thermal
In kettle inner bag, 200 DEG C of hydro-thermal reaction 2h, be cooled to after room temperature the centrifuge for being 8000rpm with rotating speed, and spend respectively from
Respectively washing 4 times of sub- water and absolute ethyl alcohol, are placed in 60 DEG C of dry 8h in drying box by resulting product powder, are cooled to room temperature and grind
Mill, is dispersed in tetrahydrofuran solvent, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Embodiment 3
Weigh 2.4g sodium hydrate solids to be dissolved in 6mL deionized waters, by solution and 40mL oleic acid, 40mL after being completely dissolved
The mixed solution mixing of absolute ethyl alcohol, as solution A；It is 24.8mg to measure erbium chloride, ytterbium chloride and yttrium chloride solid respectively,
223.2mg and 776.8mg are dissolved in 22mL deionized water, as B solution；The ammonium fluoride solution 16mL of quantitative preparation is measured,
As C solution.It is 2000rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through by peristaltic pump
In outer circulation type high gravity rotating packed bed, B solution and C solution are led to from another charging aperture by peristaltic pump successively in sequence
Enter in outer circulation type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, material solution is whole
After being passed through in outer circulation type high gravity rotating packed bed, 5min is circulated, the solution that discharges is placed in 200mL polytetrafluoroethylene (PTFE) hydro-thermal
In kettle inner bag, 200 DEG C of hydro-thermal reaction 2h, be cooled to after room temperature the centrifuge for being 8000rpm with rotating speed, and spend respectively from
Respectively washing 4 times of sub- water and absolute ethyl alcohol, are placed in 60 DEG C of dry 8h in drying box by resulting product powder, are cooled to room temperature and grind
Mill, is dispersed in chloroform solvent, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Embodiment 4
Weigh 2.4g sodium hydrate solids to be dissolved in 6mL deionized waters, by solution and 40mL oleic acid, 40mL after being completely dissolved
The mixed solution mixing of absolute ethyl alcohol, as solution A；It is 24.8mg to measure erbium chloride, ytterbium chloride and yttrium chloride solid respectively,
223.2mg and 776.8mg are dissolved in 22mL deionized water, as B solution；The ammonium fluoride solution 16mL of quantitative preparation is measured,
As C solution.It is 2500rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through by peristaltic pump
In outer circulation type high gravity rotating packed bed, B solution and C solution are led to from another charging aperture by peristaltic pump successively in sequence
Enter in outer circulation type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, material solution is whole
After being passed through in outer circulation type high gravity rotating packed bed, 5min is circulated, the solution that discharges is placed in 200mL polytetrafluoroethylene (PTFE) hydro-thermal
In kettle inner bag, 200 DEG C of hydro-thermal reaction 2h, be cooled to after room temperature the centrifuge for being 8000rpm with rotating speed, and spend respectively from
Respectively washing 4 times of sub- water and absolute ethyl alcohol, are placed in 60 DEG C of dry 8h in drying box by resulting product powder, are cooled to room temperature and grind
Mill, is dispersed in cyclohexane solvent, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Embodiment 5
Weigh 2.4g sodium hydrate solids to be dissolved in 6mL deionized waters, by solution and 40mL oleic acid, 40mL after being completely dissolved
The mixed solution mixing of absolute ethyl alcohol, as solution A；It is 24.8mg to measure erbium chloride, ytterbium chloride and yttrium chloride solid respectively,
223.2mg and 776.8mg are dissolved in 22mL deionized water, as B solution；The ammonium fluoride solution 16mL of quantitative preparation is measured,
As C solution.It is 1000rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through by peristaltic pump
In outer circulation type high gravity rotating packed bed, B solution and C solution are led to from another charging aperture by peristaltic pump successively in sequence
Enter in outer circulation type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, material solution is whole
After being passed through in outer circulation type high gravity rotating packed bed, 5min is circulated, the solution that discharges is placed in 200mL polytetrafluoroethylene (PTFE) hydro-thermal
In kettle inner bag, 180 DEG C of hydro-thermal reaction 1h, be cooled to after room temperature the centrifuge for being 8000rpm with rotating speed, and spend respectively from
Respectively washing 4 times of sub- water and absolute ethyl alcohol, are placed in 60 DEG C of dry 8h in drying box by resulting product powder, are cooled to room temperature and grind
Mill, is dispersed in alcohol solvent, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Embodiment 6
Weigh 2.4g sodium hydrate solids to be dissolved in 6mL deionized waters, by solution and 20mL oleic acid, 20mL after being completely dissolved
The mixed solution of oleyl amine and 40mL absolute ethyl alcohols mixes, as solution A；Erbium chloride, ytterbium chloride and yttrium chloride solid are measured respectively
It is dissolved in for 24.8mg, 223.2mg and 776.8mg in 22mL deionized water, as B solution；Measure the ammonium fluoride of quantitative preparation
Solution 16mL, as C solution.It is 2000rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through
Peristaltic pump is passed through in outer circulation type high gravity rotating packed bed, is in sequence successively passed through B solution and C solution from another charging aperture
Cross peristaltic pump to be passed through in outer circulation type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, by original
After material solution is all passed through in outer circulation type high gravity rotating packed bed, 5min is circulated, discharging solution is placed in poly- the four of 200mL
In PVF water heating kettle inner bag, 200 DEG C of hydro-thermal reaction 2h, the centrifuge for being 8000rpm with rotating speed is cooled to after room temperature, and
Respectively with respectively washing 4 times of deionized water and absolute ethyl alcohol, resulting product powder is placed in 60 DEG C of dry 8h in drying box, it is cold
But to grinding at room temperature, it is dispersed in toluene solvant, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Embodiment 7
Weigh 941.12mg sodium citrate solids to be dissolved in 32mL deionized waters, solution A is used as after being completely dissolved；Measure respectively
It is that 24.8mg, 223.2mg and 776.8mg are dissolved in 16mL deionized water to take erbium chloride, ytterbium chloride and yttrium chloride solid, as
B solution；The sodium hydrate solid and 1.4816g ammonium fluoride solids for measuring 1.6g are dissolved in 48mL deionized water, molten as C
Liquid.It is 2000rpm by the rotational speed regulation of outer circulation type high gravity rotating packed bed, solution A is passed through outer circulation by peristaltic pump
In formula high gravity rotating packed bed, B solution and C solution are passed through outer follow from another charging aperture by peristaltic pump successively in sequence
In ring type high gravity rotating packed bed, it is 3 to set solution A and B, the feed flow rates of C solution:1, material solution is all passed through outer
After in circulating high gravity rotating packed bed, 5min is circulated, the solution that discharges is placed in 200mL polytetrafluoroethylene (PTFE) water heating kettle inner bag
In, 200 DEG C of hydro-thermal reaction 2h are cooled to after room temperature the centrifuge for being 8000rpm with rotating speed, and respectively with deionized water and
Absolute ethyl alcohol respectively washing 4 times, are placed in 60 DEG C of dry 8h in drying box by resulting product powder, are cooled to grinding at room temperature, point
It is dissipated in tetrahydrofuran solvent, obtains with rare-earth-doped fluoride up-conversion luminescence Nanodispersion.
Claims (5)
- A kind of 1. preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion, it is characterised in that：This preparation method Using Rare Earths salt, sodium hydroxide and ammonium fluoride as raw material, surfactant is added, in outer circulation type high gravity rotating packed bed In premixed, be well mixed laggard water-filling thermal response, washing, centrifugation, drying, solvent it is scattered after, obtain with rear-earth-doped fluorine Compound up-conversion luminescence Nanodispersion；Realize with the synthetic method institute of rare-earth-doped fluoride up-conversion luminescence Nanodispersion Source chemicals are needed to include：Rare Earths salt, sodium hydroxide, ammonium fluoride, surfactant, deionized water and absolute ethyl alcohol, rare earth Chlorate includes yttrium chloride, ytterbium chloride and erbium chloride, and surfactant is respectively oleic acid, oleyl amine and sodium citrate, dispersion solvent Including ethanol, tetrahydrofuran, hexamethylene, chloroform and toluene；Specific preparation method is as follows：S1. ammonium fluoride solution is prepared：Compound concentration is 1mol/L ammonium fluoride solution, measures 15mL~20mL；S2. the sodium hydrate solid for weighing 2g~2.5g is dissolved in 5mL~10mL deionized waters, and 40mL oil is poured into after being completely dissolved In the mixed solution of acid and 40mL ethanol, stir；S3. according to erbium chloride：Ytterbium chloride：The molar ratio of yttrium chloride is (2~20):18:(98~62) weigh rare earth chlorate Solid, it is dissolved in 20mL~30mL deionized water；S4. the mixed solution obtained in S2 is squeezed into outer circulation type high gravity rotating packed bed by peristaltic pump, and according to suitable It is overweight that the solution obtained in S3 and the solution obtained in S1 are squeezed into outer circulation type by sequence by peristaltic pump from another charging aperture successively In power RPB；The solution obtained in the solution and S1 that are obtained in the mixed solution that is obtained in S2, S3 is material solution, former Expect that solution circulates 1min~5min. after all adding in high gravity rotating packed bedS5. the mixed solution handled by S4 hypergravity is placed in 200mL polytetrafluoroethylene (PTFE) water heating kettle inner bags, at 180 DEG C 1h~2h is reacted under the conditions of~200 DEG C；Be cooled to centrifugation after room temperature and obtain product powder, centrifugal speed be 8000rpm~ 10000rpm, it is washed with deionized after 4 times and is washed 4 times with absolute ethyl alcohol again；S6. the product for S5 centrifuge washings being handled to obtain is dried 5h~10h, ground after being cooled to room temperature as in 60 DEG C of drying boxes Mill, obtains rare-earth-doped fluoride up-conversion luminescence nano-powder material；S7. powder S6 obtained is added in dispersion solvent, sonicated to obtain rare-earth-doped fluoride up-conversion luminescence and receive Rice dispersion.
- 2. a kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion according to claim 1, its It is characterised by：Rare earth fluoride is yttrium fluoride natrium or lithium yttrium fluoride.
- 3. a kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion according to claim 1, its It is characterised by：Oleic acid in S2 can be replaced as surfactant, oleic acid with oleyl amine, sodium citrate.
- 4. a kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion according to claim 1, its It is characterised by：The solution feed flow ratio obtained in S2 is obtained in S4 mixed solution and S3 is 3:1, S2 obtained mixing is molten The solution feed flow ratio obtained in liquid and S1 is 3:1；The rotating speed of outer circulation type high gravity rotating packed bed be 500rpm~ 2500rpm。
- 5. a kind of preparation method of rare-earth-doped fluoride up-conversion luminescence Nanodispersion according to claim 1, its It is characterised by：Dispersion solvent in S7 includes ethanol, tetrahydrofuran, hexamethylene, chloroform and toluene.
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| CN109666482A (en) * | 2018-12-17 | 2019-04-23 | 达州职业技术学院 | A kind of preparation method of rare-earth-doped fluoride up-conversion luminescence nano-powder |
| CN109929203A (en) * | 2019-02-27 | 2019-06-25 | 南京航空航天大学 | A kind of preparation method of wavelength convert light-emitting film |
| CN110079372A (en) * | 2019-05-30 | 2019-08-02 | 中国科学院兰州化学物理研究所 | A kind of Nanoparticles As Lubricating Oil Additives and preparation method thereof with oil temperature monitoring function |
| CN111071991A (en) * | 2020-01-03 | 2020-04-28 | 大连民族大学 | Environment-friendly fluoride nano-material large-scale preparation method |
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| CN111071991B (en) * | 2020-01-03 | 2021-07-20 | 大连民族大学 | Environment-friendly fluoride nano-material large-scale preparation method |
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