CN107057692A - There is the CaF2 of good luminous performance under a kind of high pressure:Tb3+ nano materials and preparation method thereof - Google Patents
There is the CaF2 of good luminous performance under a kind of high pressure:Tb3+ nano materials and preparation method thereof Download PDFInfo
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- CN107057692A CN107057692A CN201710303206.5A CN201710303206A CN107057692A CN 107057692 A CN107057692 A CN 107057692A CN 201710303206 A CN201710303206 A CN 201710303206A CN 107057692 A CN107057692 A CN 107057692A
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 23
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910001634 calcium fluoride Inorganic materials 0.000 title claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000004020 luminiscence type Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000010436 fluorite Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000001215 fluorescent labelling Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000007850 fluorescent dye Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 1
- 238000001311 chemical methods and process Methods 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- 239000002159 nanocrystal Substances 0.000 description 9
- 230000003287 optical effect Effects 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 229910003460 diamond Inorganic materials 0.000 description 4
- 239000010432 diamond Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 241000931526 Acer campestre Species 0.000 description 1
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000010979 ruby Substances 0.000 description 1
- 229910001750 ruby Inorganic materials 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7743—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing terbium
- C09K11/7747—Halogenides
- C09K11/7748—Halogenides with alkali or alkaline earth metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Composite Materials (AREA)
- Optics & Photonics (AREA)
- Biophysics (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses the CaF under a kind of high pressure with good luminous performance2:Tb3+Nano material and preparation method thereof, belongs to the technical field of nano material preparation.Solvent-thermal method one-step synthesis CaF is utilized there is provided one kind2:Tb3+The Green Chemistry method of nano material, with Ca (NO3)2With Tb (NO3)3For precursor reagent, NaF is used as Fluorine source, HF regulation solution ph.It is to obtain Emission in Cubic fluorite structure CaF of the crystallite dimension as 25nm after solvent reacts 15~17h using solvent-thermal method at 135~145 DEG C using ethanol2:Tb3+Nano material.The inventive method has the advantages that preparation process is simple, cost is low and energy consumption is low, environmental protection is non-toxic, repeatable high.The CaF prepared2：Tb3+Nano material has excellent green-emitting fluorescent characteristic, and still can keep good luminescent properties under pressure.This luminescent material that can overcome maximum conditions holds out broad prospects in terms of display device, bioprobe and fluorescence labeling.
Description
Technical field
The invention belongs to nano luminescent material and technical field.
Background technology
Rare earth mixing with nano luminescent material is by the features such as specific surface area is big, surface energy is high, size is small, with bulk material phase
Occurs many such as red shift or blue-shifted phenomenon, Absorber Bandwidth, luminous intensity enhancing than showing quantum confined effect raising, spectrum
Characteristic.Due to these unique and excellent optical properties, rare earth mixing with nano luminescent material is in luminescent device, optical imagery and light
The fermentation such as electronic device is widely used.
Rare earth mixing with nano luminescent material species is various, and wherein host material is that the rear-earth-doped characteristics of luminescence of influence is important
One of factor.The selection of matrix depends primarily on phonon energy relatively low in the stability and phonon energy size of material, matrix
One key factor of the high emission efficiency as active ions.With CaF2For the luminescent material of matrix, because it has chemistry steady
Qualitative height, phonon energy is low, good dissolubility and nontoxic, has in fields such as display device, bioprobe and fluorescence labelings
Important application, is received more and more attention.With CaF2It is more and more wider in multiple fields application for the luminescent material of matrix
It is general, to material emission performance requirement also more and more higher, the excellent hair of favorable optical performance is particularly still kept under extreme conditions
Luminescent material attracts the extensive research interest of scholars.
In recent years, people are to rear-earth-doped CaF2The preparation of nano material and luminescent properties carry out substantial amounts of research, still
It is concentrated mainly on Yb3+/Er3+、Yb3+/Tm3+Deng changing CaF on codope2Nano luminescent material, and to Tb3+Single doping CaF2Receive
The preparation of rice green fluorescent material and optical property research report are less, and particularly the stable luminescent property of material is ground under high pressure
Study carefully and have not been reported.Existing synthetic method is preparing CaF2：Tb3+All there are some shortcomings in nano material.Such as：Method is simple
A step hydrothermal synthesis method prepare CaF2：Tb3+Nano material, crystallite dimension is larger, it is impossible to realize below 50nm nanocrystals
Preparation.And want to prepare the less CaF of crystallite dimension2：Tb3+Nano material generally require by oleyl amine and oleic acid be with
Body, or need addition surfactant etc. to be aided in, preparation technology is complicated, and cost is higher；Prepared using oleyl amine and oleic acid
During also need to, by a large amount of poisonous organic solvents, have a strong impact on for producing then cause environment.
The content of the invention
In view of the above-mentioned problems, a kind of simple and environmentally-friendly green method synthesis crystallite dimension is small, photism under extreme conditions
The stable CaF of energy2:Tb3+Nano material is very necessary.For this, the invention provides have good luminous performance under a kind of high pressure
CaF2:Tb3+Nano material and preparation method thereof.
The technical solution adopted in the present invention is specific as follows：
1), by Ca (NO3)2With Tb (NO3)3Dissolving obtains mixed solution, wherein Tb in 10mL deionized waters3+Account for metal
The molar percentage of cation is 10%, and metal cation concentration is 0.0120~0.0130mol/L in mixed solution；
2) NaF stirrings, are added in mixed solution, the mol ratio for making metal cation and fluorine ion is 1:2,
3) it is 1 that, mixed solution, which adds hydrofluoric acid regulation pH, is sufficiently mixed after stirring and moves into reactor sealing,
4) CaF, is prepared using solvent thermal reaction2:Tb3+, solvent is ethanol, and reactor compactedness is 80~90%, temperature
For 135~145 DEG C of 15~17h of reaction, taken out after furnace cooling.
5) after, washing away impurity through deionized water, absolute ethyl alcohol, through being dried to obtain CaF2:Tb3+Nano material.
Gained CaF2:Tb3+Nano material is fluorite cube phase structure, and particle size is 25nm, under 8.9GPa pressure most
216% is added during the luminous intensity contrast 0GPa at strong green luminescence peak.
Beneficial effects of the present invention：
1st, the inventive method is using solvent-thermal method one-step synthesis crystallite dimension is small, the uniform Tb of pattern3+Adulterate CaF2Nanometer
Fluorescent material, with simple to operate, energy consumption is low, environmental protection, it is repeatable high the advantages of；
2nd, Tb of the invention3+Adulterate CaF2Nano material, with excellent fluorescent characteristic.Using using diamond anvil cell
The luminescent properties of sample under press in site measurement high pressure, sample has remained in that the good characteristics of luminescence under 8.9GPa high pressures.
CaF needed for being applied to large-scale production under maximum conditions2：Tb3+The potentiality of nano material.
3rd, this luminescent material that can overcome maximum conditions has extensively in terms of display device, bioprobe and fluorescence labeling
Wealthy prospect.
Brief description of the drawings
Fig. 1 is CaF2：Tb3+The transmission electron microscope picture of nanocrystal.
Fig. 2 is CaF2：Tb3+The X-ray diffraction spectrogram of nanocrystal.
Fig. 3 is CaF2：Tb3+Photoluminescence spectra under nanocrystal normal pressure.
Fig. 4 is CaF2：Tb3+The photoluminescence spectra of nanocrystal under high pressure.
Embodiment
Technical solution of the present invention is further explained and illustrated with reference to embodiment, unless otherwise specified, examination used
Agent is commercially available obtainable product, purifies not plus further and uses.
1. Ca (NO are selected3)2、Tb(NO3)3, NaF be precursor reagent, by 0.01125mol/L Ca (NO3)2With
0.00125mol/L Tb (NO3)3Add in 10mL deionized waters and dissolve together；0.025mol/L NaF is added into mixed solution
In stirred on magnetic stirring apparatus, while instill concentration dropwise drips (often drop be about 0.05mL) for 40% hydrofluoric acid 5, adjust pH
=1,60min is sufficiently stirred for, the sealing of 40mL reactors is moved into, solvent is ethanol, and compactedness is 85%.It is heat-treated at 140 DEG C
16h, takes out after furnace cooling.By the product utilization deionized water of taking-up ultrasound, centrifuge washing 2 times, then with absolute ethyl alcohol ultrasound,
Centrifuge washing 3 times.Sample is through 80 DEG C, and 10h drying process obtains Emission in Cubic Tb3+Adulterate CaF2Nanocrystal initial sample.
As can be seen from Figure 1 the sample size prepared is uniform, and particle diameter distribution is narrow, and its average-size is 25nm.Fig. 2 is
Tb3+Adulterate CaF2The XRD spectra of nanocrystal, it is not miscellaneous from spectrogram it can be seen that the sample prepared is fluorite cube phase structure
Matter diffraction maximum, illustrates to mix Tb3+The crystal structure of matrix is not changed afterwards.Fig. 3 is Tb3+Adulterate CaF2The photic hair of nanocrystal
Light spectrum, it can be seen that the sample of preparation has good fluorescent characteristic, wherein most strong glow peak is green luminescence peak, it is a kind of
Promising green-emitting fluorescent material.
②CaF2:Tb3+Baroluminescence performance study be in symmetrical expression diamond anvil cell carry out, utilize symmetrical expression gold
Hard rock opposed anvils is pressurizeed, and diamond anvil face size is 400 μm, and sealing gasket uses T301 stainless steel substrates, and precompressed thickness is 60 μ
m.A diameter of 120 μm of apertures are bored on the pad of precompressed, as high pressure sample chamber, selection silicone oil is transmission medium, pressure
Demarcation is the technology using standard ruby fluorescence mark pressure.By step 1. in obtained CaF2:Tb3+Nanocrystal is put into diamond
In opposed anvils press, sample is carried out to be forced into maximum pressure 8.9GPa, baroluminescence test optical maser wavelength used is 325nm.
Fig. 4 can be seen that with the increase of pressure in sample pressure process, and luminous intensity gradually strengthens.Wherein, it is located at during 0GPa
The luminous intensity at most strong green luminescence peak adds 216% when pressure adds to 8.9GPa at 545nm, illustrates that sample has good
Optical property, still there is the stable characteristics of luminescence under conditions of high voltage limit.
Claims (5)
1. there is the CaF of good luminous performance under a kind of high pressure2:Tb3+Nano material, it is characterised in that fluorite cube phase structure,
Particle size is 25nm, Tb3+Doping ratio be 10%, under 8.9GPa pressure most strong green luminescence peak luminous intensity contrast
216% is added during 0GPa, its preparation process is specific as follows：
1), by Ca (NO3)2With Tb (NO3)3Dissolving obtains mixed solution, wherein Tb in 10mL deionized waters3+Account for metal sun from
The molar percentage of son is 10%, and metal cation concentration is 0.0120~0.0130mol/L in mixed solution；
2) NaF stirrings, are added in mixed solution, the mol ratio for making metal cation and fluorine ion is 1:2；
3) it is 1 that, mixed solution, which adds hydrofluoric acid regulation pH, is sufficiently mixed after stirring and moves into reactor sealing；
4) CaF, is prepared using solvent thermal reaction2:Tb3+, solvent is ethanol, and reactor compactedness is 80~90%, and temperature is 135
~145 DEG C of 15~17h of reaction, take out after furnace cooling.
5) after, washing away impurity through deionized water, absolute ethyl alcohol, through being dried to obtain CaF2:Tb3+Nano material.
2. there is the CaF of good luminous performance under high pressure as claimed in claim 12:Tb3+The preparation method of nano material, tool
Body is as follows：
1), by Ca (NO3)2With Tb (NO3)3Dissolving obtains mixed solution, wherein Tb in 10mL deionized waters3+Account for metal sun from
The molar percentage of son is 10%, and metal cation concentration is 0.0120~0.0130mol/L in mixed solution；
2) NaF stirrings, are added in mixed solution, the mol ratio for making metal cation and fluorine ion is 1:2；
3) it is less than 1 that, mixed solution, which adds hydrofluoric acid regulation pH, is sufficiently mixed after stirring and moves into reactor sealing；
4) CaF, is prepared using solvent thermal reaction2:Tb3+, solvent is ethanol, and reactor compactedness is 80~90%, and temperature is 135
~145 DEG C of 15~17h of reaction, take out after furnace cooling.
3. there is the CaF of good luminous performance under high pressure according to claim 22:Tb3+The preparation method of nano material,
Characterized in that, step 1) in mixed solution metal cation concentration be 0.0125mol/L.
4. there is the CaF of good luminous performance under high pressure according to claim 22:Tb3+The preparation method of nano material,
Characterized in that, step 4) in reactor compactedness be 85%.
5. there is the CaF of good luminous performance under high pressure according to claim 22:Tb3+The preparation method of nano material,
Characterized in that, temperature is 140 DEG C of reaction 16h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710303206.5A CN107057692B (en) | 2017-05-03 | 2017-05-03 | CaF with good light-emitting performance under high pressure2:Tb3+Nano material and preparation method thereof |
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|---|---|---|---|
| CN201710303206.5A CN107057692B (en) | 2017-05-03 | 2017-05-03 | CaF with good light-emitting performance under high pressure2:Tb3+Nano material and preparation method thereof |
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| CN107057692A true CN107057692A (en) | 2017-08-18 |
| CN107057692B CN107057692B (en) | 2020-05-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403065A (en) * | 2021-04-30 | 2021-09-17 | 河北大学 | Fluoride-based stress luminescent material, preparation method and application thereof |
| CN113956872A (en) * | 2021-11-02 | 2022-01-21 | 西安文理学院 | Terbium-doped calcium fluoride nano particle, sol-gel hybrid material and preparation method |
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|---|---|---|---|---|
| CN1880406A (en) * | 2005-06-03 | 2006-12-20 | 纳幕尔杜邦公司 | Method for preparing rare-earth doped fluoride nanoparticles |
| US20100012898A1 (en) * | 2006-06-02 | 2010-01-21 | E. I. Du Pont De Nemours And Company | Method for controlling the size of rare-earth-doped fluoride nanoparticles |
| US20100019200A1 (en) * | 2006-06-02 | 2010-01-28 | E. I. Du Pont De Nemours And Company | Method for preparing rare-earth-doped fluoride nanoparticles of controlled size |
| CN105295905A (en) * | 2015-11-18 | 2016-02-03 | 湖北工业大学 | Preparation method of water-soluble Eu<3+>-doped calcium fluoride nano particles |
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2017
- 2017-05-03 CN CN201710303206.5A patent/CN107057692B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880406A (en) * | 2005-06-03 | 2006-12-20 | 纳幕尔杜邦公司 | Method for preparing rare-earth doped fluoride nanoparticles |
| US20100012898A1 (en) * | 2006-06-02 | 2010-01-21 | E. I. Du Pont De Nemours And Company | Method for controlling the size of rare-earth-doped fluoride nanoparticles |
| US20100019200A1 (en) * | 2006-06-02 | 2010-01-28 | E. I. Du Pont De Nemours And Company | Method for preparing rare-earth-doped fluoride nanoparticles of controlled size |
| CN105295905A (en) * | 2015-11-18 | 2016-02-03 | 湖北工业大学 | Preparation method of water-soluble Eu<3+>-doped calcium fluoride nano particles |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113403065A (en) * | 2021-04-30 | 2021-09-17 | 河北大学 | Fluoride-based stress luminescent material, preparation method and application thereof |
| CN113403065B (en) * | 2021-04-30 | 2022-11-18 | 河北大学 | Fluoride-based stress luminescent material, preparation method and application thereof |
| CN113956872A (en) * | 2021-11-02 | 2022-01-21 | 西安文理学院 | Terbium-doped calcium fluoride nano particle, sol-gel hybrid material and preparation method |
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