CN106497553B - A kind of Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material and preparation method - Google Patents
A kind of Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material and preparation method Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 41
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011701 zinc Substances 0.000 claims abstract description 15
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 13
- 150000002500 ions Chemical class 0.000 claims abstract description 8
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 6
- 238000005516 engineering process Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 17
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 7
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004246 zinc acetate Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 4
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 3
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims 2
- 150000003751 zinc Chemical class 0.000 claims 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 7
- 238000004020 luminiscence type Methods 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- -1 rare earth ion Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005415 bioluminescence Methods 0.000 description 1
- 230000029918 bioluminescence Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
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- 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
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7767—Chalcogenides
- C09K11/7769—Oxides
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- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The present invention provides a kind of Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material and preparation method, using ZnO as matrix, with rare earth element Ho3+、Yb3+、Gd3+For Doped ions, consisting of, Zn1‑x‑y‑zHoxYbyGdzO.The high zinc oxide up-conversion luminescent material of the rear-earth-doped preparation luminous intensity of the present invention, synthesis technology is simple, and repeatability is high, and material therefor is environmentally friendly, safe and non-toxic, it is easy to accomplish industrialized production.Simultaneously by changing Gd3+Doping concentration can significantly improve the Up-conversion Intensity of zinc oxide so that rare earth doping zinc oxide up-conversion luminescent material luminous intensity is strong, can be used for showing, illuminate, laser anti-counterfeit etc..
Description
Technical field
The invention belongs to up-conversion luminescent material technical field, it is related to converting on a kind of rare earth doped zinc oxide material
Luminescent material.
Background technique
In recent years, rear-earth-doped up-conversion luminescent material is since it shows in 3 D stereo, laser anti-counterfeit, bioluminescence mark
The extensive use in the fields such as note and short wavelength laser, arouses great concern.But for entirety, up-conversion luminescence effect
Rate is also relatively low.Current some common preferable materials of luminescent properties thermally and chemically stability, in terms of also
There are some problems not solve, this just brings difficulty to practical application.So it is all to find high conversion efficiency, physical and chemical performance
Good New-type matrix material becomes one of the research hotspot of current up-conversion luminescent material.
Zinc oxide (ZnO) the direct wide bandgap semiconductor materials novel as one kind, forbidden bandwidth at room temperature are
3.37eV, exciton binding energy (60meV) with higher have stronger absorption in ultra-violet (UV) band, and its physics and chemical property are steady
It is fixed, there is lower phonon energy (437cm-1), this makes it possible to become ideal up-conversion luminescence host material.But it arrives
So far, the up-conversion luminescence efficiency of rear-earth-doped ZnO material is also relatively low.Wherein reason first is that rare earth ion generally very
It is difficult to replace Zn2+The form of lattice point enters ZnO lattice.This is because the radius ratio Zn of trivalent rare earth ions2+Ion is much bigger,
And the charge of the two mismatches.
Summary of the invention
In view of the deficienciess of the prior art, the present invention provides a kind of Ho3+/Yb3+/Gd3+Hair is converted on codope zinc oxide
Luminescent material and preparation method solve prior art zinc oxide up-conversion luminescent material preparation process complexity, and luminous intensity is low, can not
The technical issues of carrying out high-concentration dopant.
The technical solution adopted in the present invention is as follows:
Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material, using ZnO as matrix, with rare earth element Ho3+、Yb3 +、Gd3+For Doped ions, consisting of Zn1-x-y-zHoxYbyGdzO, wherein 6mol%≤x+y+z≤9mol%.
Preferably, Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material, using ZnO as matrix, with rare earth element
Ho3+、Yb3+、Gd3+For Doped ions, consisting of Zn1-x-y-zHoxYbyGdzO, wherein x=1mol%, y=5mol%, z≤
3mol%.
Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material preparation method, comprising the following steps:
Zinc acetate or zinc nitrate are dissolved in deionized water by step 1, stirring, until zinc acetate or zinc nitrate sufficiently dissolve
Obtain zinc solution；
Step 2, by Ho2O3、Yb2O3And Gd2O3It is dissolved in after mixing in dust technology or dilute hydrochloric acid solution, 40 DEG C~60 DEG C add
Solution is evaporated to obtain powdered rubber 50 DEG C~70 DEG C after thermal agitation to abundant reaction；
Powdered rubber obtained by step 2 is dissolved in the water, stirs to clarify, dropwise one gained zinc of a dropping step by step 3
Salting liquid stirs to clarify to obtain solution；
Triethanolamine or monoethanolamine are added dropwise in step 3 acquired solution step 4, until what is occurred when initial is white
After color flocculent deposit dissolution, colourless transparent solution is obtained；
- 600 polyethylene glycol-400 of polyethylene glycol is added in step 4 acquired solution, is stirred by step 5；
Step 6, it is anti-to high pressure after step 5 acquired solution is transferred to 140 DEG C~180 DEG C 2~6h of reaction of autoclave
It answers kettle to be cooled to room temperature, obtains sediment；
Step 6 gained sediment is centrifuged, cleans, after 60 DEG C~80 DEG C dry 2~4h and grinding by step 7
White powder is obtained, 550 DEG C~750 DEG C 2~4h of annealing of white powder are made annealing treatment.
The beneficial effects of the present invention are:
1, the high zinc oxide up-conversion luminescent material of the rear-earth-doped preparation luminous intensity of the present invention, synthesis technology is simple, can
Repeated high, material therefor is environmentally friendly, safe and non-toxic, it is easy to accomplish industrialized production.
2, the zinc oxide up-conversion luminescent material luminous intensity that the present invention prepares is strong, can be used for showing, illuminate, laser is prevented
Puppet etc..
3, the preparation method of rare earth doping zinc oxide up-conversion luminescent material provided by the invention, Ho3+/Yb3+/Gd3+'s
Doping concentration maintains higher level, by changing Gd3+Doping concentration can significantly improve zinc oxide up-conversion luminescence it is strong
Degree.
Detailed description of the invention
Fig. 1 is Ho3+/Yb3+/Gd3+The XRD spectrum of co-doped nano ZnO；
Fig. 2 is Ho3+/Yb3+/Gd3+The SEM of co-doped nano ZnO schemes.
Fig. 3 (a) is different Gd3+The Up-conversion emission spectrum of sample under doping concentration is (b) red-green glow integrated emission intensity
With Gd3+The variation relation of doping concentration；
Specific embodiment
Yb3+As sensitized ions, it is greatly improved active ions Ho3+To the absorption efficiency of pump light, therefore use Ho3+/
Yb3+The mode of codope, Gd3+The reason of enhancing up-conversion luminescence may be Gd3+And Ho3+Between there are energy transmissions and reversed
Energy transfer process has eventually led to the enhancing of feux rouges and green emission, it is also necessary to further verifying.
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments, it should be noted that the present invention is not
Following specific embodiments are confined to, all equivalent transformations made on the basis of the technical solutions of the present application each falls within protection model of the invention
It encloses.
Embodiment 1
To achieve the above object, the present invention provides a kind of Ho3+/Yb3+/Gd3+Codope ZnO up-conversion luminescent material, chemistry
Composition are as follows: Zn1-x-y-zHoxYbyGdzO, wherein Ho3+For active ions, Yb3+For sensitizer, x Ho3+The Mole percent of doping
Number, y Yb3+The mole percent of doping, z Gd3+The mole percent of doping, and x+y+z=9mol%, i.e. x=
1mol%, y=5mol%, z=3mol%, preparation step are as follows:
Step 1 prepares acetic acid zinc solution, takes the Zn (Ac) of 6.585g2, it is dissolved in 30ml deionized water, stirs, until
1. it is sufficiently dissolved into colourless transparent solution.
Step 2 prepares rare earth nitrades.Zn:Ho:Yb:Gd=0.91:0.01:0.05:0.03 is weighed accordingly in proportion
Rare earth oxide Ho2O3、Yb2O3And Gd2O3, it is dissolved in dilute nitric acid solution after mixing, in 40 DEG C of -60 DEG C of heating stirrings,
After sufficiently reacting, solution is evaporated in 50 DEG C -70 DEG C.
Above-mentioned gained powder is dissolved in 10ml deionized water, stirs to clarify, 1. solution is added dropwise dropwise by step 3,
Stir to clarify solution 2..
Step 4 weighs 20ml triethanolamine, is added dropwise in 2. solution, occurs white flock precipitate when initial, continues
It is added dropwise, until white precipitate is completely dissolved, finally obtains colourless transparent solution 3..
Step 5 measures the polyethylene glycol -600 of 5ml, is added in 3. solution, is sufficiently stirred, and is uniformly mixed it.
Above-mentioned gained mixture solution is transferred in 50ml autoclave by step 6, anti-under the conditions of 140 DEG C -180 DEG C
Answer 2-6h.
Step 7 is taken out reaction kettle and is cooled to room temperature after reaction.Gained sediment is centrifugated, is cleaned repeatedly
The dry 2-4h at 60 DEG C -80 DEG C afterwards, takes out grinding, finally by above-mentioned gained white powder at 550 DEG C -750 DEG C after drying
Anneal 2-4h.
Embodiment 2
The present embodiment Ho3+/Yb3+/Gd3+Chemical composition of codope ZnO up-conversion luminescent material and preparation method thereof with
Embodiment 1 is identical, the difference is that x+y+z=6mol%, z=0.
Embodiment 3
The present embodiment Ho3+/Yb3+/Gd3+Chemical composition of codope ZnO up-conversion luminescent material and preparation method thereof with
Embodiment 1 is identical, the difference is that x+y+z=7mol%, z=1mol%.
X-ray powder diffraction pattern analysis, SEM figure and sample is carried out to sample made from above embodiments to exist
The Up-conversion emission spectrum obtained under 980nmLD excitation is analyzed, as a result as follows:
Fig. 1 is 1 sample Zn of embodiment0.91Ho0.01Yb0.05Gd0.03The X-ray powder diffraction pattern of O.It can be seen that oikocryst
It is mutually ZnO, individual Yb occurs2O3Peak.Table 1 is enumerated the lattice constant of rear-earth-doped ZnO Yu pure ZnO.The number from table
According to, it is evident that with rare earth ion incorporation, lattice constant becomes larger, this may be the crystalline substance that rare earth ion part enters ZnO
Lattice, instead of caused by Zn atom.
The rear-earth-doped ZnO of table 1 and pure ZnO lattice constant compare
Fig. 2 is 1 sample Zn of embodiment0.91Ho0.01Yb0.05Gd0.03The SEM of O schemes, it can be seen from Fig. 2 that sample shape is not very
Completely, loose chondritic is partially showed, size is uneven, and rough exquisiteness has partial particulate shape substance, hinders ZnO
The growth of certain crystal faces.It therefore is not that the rare earth element concentration mixed is the bigger the better.
Fig. 3 (a) is under 980nm LD excitation, according to the 1mol%Ho of present case scheme preparation3+, 5mol%Yb3+And z
Mol%Gd3+The Up-conversion emission of (z=0,1,3, i.e. x+y+z=6mol%, 7mol%, 9mol%) codope ZnO nano crystalline substance
Spectrum.As can be seen that the material mainly shines in green light and red spectral band.With Gd3+The increase of incorporation, fluorescence intensity are obvious
Enhancing, but red-green glow variation is slightly different, and green intensity increases always, and red light intensity first reduces increase, from whole angle
See that feux rouges enhancing ratio is greater than green light.In x=1mol%, y=5mol%, z=3mol% effect is preferable, Fig. 3 (b) display
It is upper conversion red-green glow intensity ratio under different ratio, value is with Gd3+The increase of doping concentration first reduces to increase afterwards.
Claims (2)
1.Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material, using ZnO as matrix, which is characterized in that with rare earth member
Plain Ho3+、Yb3+、Gd3+Codope is as Doped ions；
The Ho3+/Yb3+/Gd3+Codope zinc oxide up-conversion luminescent material group becomes, Zn1-x-y-zHoxYbyGdzO, wherein x=
1mol%, y=5mol%, z=3mol%；
The Ho3+/Yb3+/Gd3+The preparation method of codope zinc oxide up-conversion luminescent material, comprising the following steps:
Zinc acetate or zinc nitrate are dissolved in deionized water by step 1, stirring, until zinc acetate or zinc nitrate are sufficiently dissolved and obtained
Zinc solution；
Step 2, by Ho2O3、Yb2O3And Gd2O3It is dissolved in after mixing in dust technology or dilute hydrochloric acid solution, heating stirring is to sufficiently instead
Should after solution is evaporated to obtain powdered rubber；
Powdered rubber obtained by step 2 is dissolved in the water, stirs to clarify, one gained zinc salt of a dropping step is molten dropwise by step 3
Liquid stirs to clarify to obtain solution；
Triethanolamine or monoethanolamine are added dropwise in step 3 acquired solution step 4, until the white wadding occurred when initial
After shape precipitating dissolution, colourless transparent solution is obtained；
Polyethylene glycol -600 or polyethylene glycol-400 are added in step 4 acquired solution, are stirred by step 5；
Step 5 acquired solution is transferred to after autoclave reacted, is cooled to room temperature, obtains to autoclave by step 6
To sediment；
Step 7 obtains white powder after step 6 gained sediment is centrifuged, cleans, dries and is ground, will be white
Powder is made annealing treatment；
Heating stirring temperature is 40 DEG C~60 DEG C in the step 2；Stating solution evaporated temperature in step 2 is 50 DEG C~70 DEG C；
The step 6 high pressure reactor reaction condition is 140 DEG C~180 DEG C 2~6h of reaction；The step 7 drying condition is 60 DEG C
~80 DEG C of dry 2~4h；The step 7 annealing conditions are 550 DEG C~750 DEG C 2~4h of annealing.
2. Ho described in claim 13+/Yb3+/Gd3+The preparation method of codope zinc oxide up-conversion luminescent material, including it is following
Step:
Zinc acetate or zinc nitrate are dissolved in deionized water by step 1, stirring, until zinc acetate or zinc nitrate are sufficiently dissolved and obtained
Zinc solution；
It is characterized in that,
Step 2, by Ho2O3、Yb2O3And Gd2O3It is dissolved in after mixing in dust technology or dilute hydrochloric acid solution, heating stirring is to sufficiently instead
Should after solution is evaporated to obtain powdered rubber；
Powdered rubber obtained by step 2 is dissolved in the water, stirs to clarify, one gained zinc salt of a dropping step is molten dropwise by step 3
Liquid stirs to clarify to obtain solution；
Triethanolamine or monoethanolamine are added dropwise in step 3 acquired solution step 4, until the white wadding occurred when initial
After shape precipitating dissolution, colourless transparent solution is obtained；
Polyethylene glycol -600 or polyethylene glycol-400 are added in step 4 acquired solution, are stirred by step 5；
Step 5 acquired solution is transferred to after autoclave reacted, is cooled to room temperature, obtains to autoclave by step 6
To sediment；
Step 7 obtains white powder after step 6 gained sediment is centrifuged, cleans, dries and is ground, will be white
Powder is made annealing treatment；
Heating stirring temperature is 40 DEG C~60 DEG C in the step 2；Solution evaporated temperature is 50 DEG C~70 in the step 2
℃；The step 6 high pressure reactor reaction condition is 140 DEG C~180 DEG C 2~6h of reaction；The step 7 drying condition is 60
DEG C~80 DEG C of dry 2~4h；The step 7 annealing conditions are 550 DEG C~750 DEG C 2~4h of annealing.
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Non-Patent Citations (3)
| Title |
|---|
| Gd3+,Tm3+和Yb3+掺杂的Y2O3微晶中Gd3+离子的紫外上转换发光及其增强的研究;张鹏等;《发光学报》;20151231;893-897 |
| Microstructure and upconversion luminescence in Ho3+ and Yb3+ co-doped ZnO naocrystalline powders;Xiaochen Yu等;《Optics Communications》;20141231;90– 93 |
| ZnO:Er,Yb,Gd Particles Designed for Magnetic-Fluorescent Imaging and Near-Infrared Light Triggered Photodynamic Therapy;Xiaojun Wei等;《J. Phys. Chem. C》;20131231;23716-23729 |
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