CN110079315A - A kind of thermochromism MoO3: Yb, Er up-conversion phosphor, preparation method and its reversible regulation method of up-conversion luminescence - Google Patents
A kind of thermochromism MoO3: Yb, Er up-conversion phosphor, preparation method and its reversible regulation method of up-conversion luminescence Download PDFInfo
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 82
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 230000002441 reversible effect Effects 0.000 title claims abstract description 26
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 32
- 230000004913 activation Effects 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 230000009466 transformation Effects 0.000 claims abstract description 7
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 25
- 238000000227 grinding Methods 0.000 claims description 10
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 5
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 5
- 230000008859 change Effects 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 206010026865 Mass Diseases 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001815 biotherapy Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- 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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Abstract
The present invention relates to a kind of thermochromism MoO3: Yb, Er up-conversion phosphor, preparation method and its reversible regulation method of up-conversion luminescence belong to thermochromism fluorescent powder application and preparation technical field.Thermochromism MoO3: Yb, Er up-conversion phosphor, chemical formula MoO3: Yb, Er.By light yellow MoO3: Yb, Er up-conversion phosphor are in H2And N2Reducing atmosphere is 300 DEG C ~ 700 DEG C heat preservation 2h in temperature, obtains blue MoO after being cooled to room temperature3: Yb, Er fluorescent powder, again by blue MoO3: Yb, Er fluorescent powder heat in air atmosphere, are cooled to after room temperature and are transformed into light yellow MoO3: Yb, Er up-conversion phosphor;Under 980nm light source activation, yellow MoO3: the fluorescence of Yb, Er up-conversion phosphor sending green, and blue MoO3: Yb, Er light-emitting phosphor weaken or until do not shine, by realizing MoO3: the multiplicating transformation of Yb, Er fluorescent powder color " light yellow-blue " carries out the reversible regulation of up-conversion luminescence.
Description
Technical field
The present invention relates to a kind of thermochromism MoO3: Yb, Er up-conversion phosphor, preparation method and its up-conversion luminescence can
Inverse regulation method, belongs to thermochromism fluorescent powder application and preparation technical field.
Background technique
Thermochromic material refers to that some compounds or mixture have when undergoing extraneous thermostimulation, absorption spectrum
Middle visible light part is changed, thus the changed characteristic of color sample.This off-color material is widely used in light and deposits
Each neck such as storage, molecular switch, thermometric, imaging, anti-fake mark, bio-sensing, industry, weaving, military affairs, printing, aerospace
Domain.Developing history of the thermochromic material in external existing decades, has developed thermally indicating material early in Germany in 1938 first,
And affecting beauty, day, English, the former Soviet Union etc., lead in the development of science and technology country steps up to research and develop, and has had developed inorganic, organic, liquid so far
All kinds of materials with property such as brilliant, polymer and large biological molecule;And research of the China for thermochromic material
It is later, start from the 1960s, product also develop it is less, it is many also all to draw in terms of practical application and masss production
Into external technology, and have reversible thermochromatic material less, therefore the preparation research of realization thermochromic material is
Significantly, potential great economic benefit and social benefit are shown.Off-color material includes organic and inorganic two at present
Class, wherein organic thermochromic material quantity is more, but before and after colour generation body heat stability, fatigue durability, discoloration sample knot
Structure change etc. exist it is obvious insufficient;And inorganic thermochromatic material can avoid these deficiencies, and with excellent resistance to
Warm nature, durability, light shine etc., but invertibity and sensitivity are poor, when temperature reduction is too fast, may there is also face
Color " rigid " phenomenon.Therefore it is good that invertibity, temperature sensitivity are developed, color change and temperature change linear relationship are good, make
Standby inorganic off-color material at low cost has very big meaning.On the other hand, rare earth doped up-conversion luminescent material
Have good application in numerous areas such as solid state laser, Three-dimensional Display, bio-imaging, biological therapies, but at present for
The regulation effective ways of up-conversion luminescence are all the conventional methods such as change excitation light power, the rear-earth-doped concentration of adjustment mostly, but
These conventional methods are " reversible regulation " difficult to realize, and reversible, repeatable regulation can assign up-conversion just
Therefore more huge application such as lossless data storage, photoswitch, optical memory equipment invent a kind of new reversible weigh
Multiple up-conversion luminescence adjusting method is extremely important.
Summary of the invention
The purpose of the present invention is being directed in existing thermochromic material, colour generation body heat stability, the endurance of organic material
Property and the service life it is poor, the invertibity of most of inorganic off-color material and the reversible regulation side of less reproducible and up-conversion luminescence
The single deficiency of method, the present invention provide a kind of thermochromism MoO3: Yb, Er up-conversion phosphor and preparation method thereof.The MoO3:
Yb, Er up-conversion phosphor have efficient response characteristic to sintering atmosphere and 980nm light source, firstly, it is in air atmosphere and also
After being sintered in Primordial Qi atmosphere, sample can show light yellow and blue;Secondly, 520- can be emitted under the light source activation of 980nm
The green fluorescence of 560nm wave band.In addition, the up-conversion luminescence regulation of the fluorescent powder may be implemented by the color of regulation sample.
The invention is realized by the following technical scheme.
A kind of thermochromism MoO3: Yb, Er up-conversion phosphor, chemical formula MoO3: Yb, Er.
A kind of thermochromism MoO3: the preparation method of Yb, Er up-conversion phosphor, the specific steps of which are as follows:
Step 1, first by (NH4)6Mo7O24·4H2O、Er2O3、Yb2O3It is uniformly mixed, adds according to the molar ratio of chemical constitution formula
Enter dehydrated alcohol, grinding obtains mixed material;
The mixed material that step 1 obtains is heated to 500 DEG C by step 2 in air atmosphere, keeps the temperature after 2h furnace cooling to room
Temperature obtains light yellow MoO after grinding3: Yb, Er up-conversion phosphor.
A kind of thermochromism MoO3: the reversible regulation method of the up-conversion luminescence of Yb, Er up-conversion phosphor:
By light yellow MoO3: Yb, Er up-conversion phosphor are in H2And N2Reducing atmosphere is 300 DEG C ~ 700 DEG C heat preservation 2h in temperature,
Blue MoO is obtained after being cooled to room temperature3: Yb, Er fluorescent powder, again by blue MoO3: Yb, Er fluorescent powder add in air atmosphere
Heat is cooled to after room temperature and is transformed into light yellow MoO3: Yb, Er up-conversion phosphor;Under 980nm light source activation, yellow
MoO3: the fluorescence of Yb, Er up-conversion phosphor sending green, and blue MoO3: Yb, Er light-emitting phosphor weaken or until do not send out
Light, by realizing MoO3: it is reversible that the multiplicating transformation of Yb, Er fluorescent powder color " light yellow-blue " carries out up-conversion luminescence
Regulation.
The beneficial effects of the present invention are:
(1) fluorescent powder synthesized by the present invention is in air atmosphere and H2And N2It is sintered in mixed atmosphere, sample can present light yellow
With blue two kinds of different colours;
(2) under 980nm light source activation, light yellow sample issues the fluorescence of green, and Blue samples do not shine then, pass through change
Up-conversion luminescence regulation may be implemented in color sample;
(3) color sample of the invention variation and up-conversion luminescence regulation are reversible, and are recycled and are repeated as many times;
(4) by adjusting sintering temperature, color sample variation degree formula can change in gradient;
(5) preparation process of the present invention is simple and efficient, at low cost, is advantageously implemented industrialization.
Detailed description of the invention
Fig. 1 is invention embodiment 1,2,3 resulting thermochromism MoO3: Yb, Er up-conversion phosphor shine
Spectrogram;
Fig. 2 is the embodiment of the present invention 1,2,3 resulting thermochromism MoO3: Yb, Er up-conversion phosphor color gradient photo figure;
Fig. 3 is the resulting thermochromism MoO of the embodiment of the present invention 23: Yb, Er up-conversion phosphor luminous intensity are reversible, recyclable
The intensity distribution of regulation;
Fig. 4 is the resulting thermochromism MoO of the embodiment of the present invention 23: the color sample of Yb, Er up-conversion phosphor is reversible, can follow
The photo of ring regulation.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
Thermochromism MoO3: Yb, Er up-conversion phosphor, chemical formula MoO3: Yb, Er.
Thermochromism MoO3: the preparation method of Yb, Er up-conversion phosphor, the specific steps of which are as follows:
Step 1, first by 0.01mol (NH4)6Mo7O24·4H2O、Er2O3、Yb2O3It is 1/7:0.5:0.5 mixing according to molar ratio
Uniformly, 5mL dehydrated alcohol is added, grinding obtains mixed material;
The mixed material that step 1 obtains is heated to 500 DEG C by step 2 in air atmosphere, keeps the temperature after 2h furnace cooling to room
Temperature obtains light yellow MoO after grinding3: Yb, Er up-conversion phosphor.Light yellow MoO3: Yb, Er up-conversion phosphor practical photograph
As shown in original in Fig. 2, color is light yellow.
Thermochromism MoO3: the reversible regulation method of the up-conversion luminescence of Yb, Er up-conversion phosphor:
By light yellow MoO3: Yb, Er up-conversion phosphor are in H2And N2Reducing atmosphere (H2And N2Volume ratio be 1:19, gas
Flow is 50 mL/min), it is 300 DEG C of heat preservation 2h in temperature, obtains blue MoO after being cooled to room temperature3: Yb, Er fluorescent powder, then
It is secondary by blue MoO3: Yb, Er fluorescent powder are heated to 300 DEG C in air atmosphere, keep the temperature 2h, are cooled to after room temperature and are transformed into shallow
Yellow MoO3: Yb, Er up-conversion phosphor;Under 980nm light source activation, yellow MoO3: Yb, Er up-conversion phosphor issue green
The fluorescence of color, and blue MoO3: Yb, Er light-emitting phosphor weaken or until do not shine, by realizing MoO3: Yb, Er fluorescent powder face
The multiplicating transformation of color " light yellow-blue " carries out the reversible regulation of up-conversion luminescence.
In H2And N2In reducing atmosphere, temperature is the blue MoO restored at 300 DEG C3: Yb, Er fluorescent powder practical photograph
As shown in 300 reduction in Fig. 2, color is light blue.
Light yellow MoO3: Yb, Er up-conversion phosphor switch illumination spectra are as shown in Figure 1, as can be seen from Figure 1 sample
Luminous intensity is about 66.The blue MoO restored at 300 DEG C3: Yb, Er fluorescent powder switch illumination spectra are as shown in Figure 1, can
To find out that sample luminous intensity is about 45.Color from it is light yellow fade to it is light blue during, luminous intensity is changed, therefore
By realizing MoO3: up-conversion luminescence regulation may be implemented in the transformation of Yb, Er fluorescent powder color " light yellow-blue ".
Embodiment 2
Thermochromism MoO3: Yb, Er up-conversion phosphor, chemical formula MoO3: Yb, Er.
Thermochromism MoO3: the preparation method of Yb, Er up-conversion phosphor, the specific steps of which are as follows:
Step 1, first by 0.01mol (NH4)6Mo7O24·4H2O、Er2O3、Yb2O3It is 1/7:0.5:0.5 mixing according to molar ratio
Uniformly, 5mL dehydrated alcohol is added, grinding obtains mixed material;
The mixed material that step 1 obtains is heated to 500 DEG C by step 2 in air atmosphere, keeps the temperature after 2h furnace cooling to room
Temperature obtains light yellow MoO after grinding3: Yb, Er up-conversion phosphor.Light yellow MoO3: Yb, Er up-conversion phosphor practical photograph
As shown in original in Fig. 2, color is light yellow.
Thermochromism MoO3: the reversible regulation method of the up-conversion luminescence of Yb, Er up-conversion phosphor:
By light yellow MoO3: Yb, Er up-conversion phosphor are in H2And N2Reducing atmosphere (H2And N2Volume ratio be 1:19, gas
Flow is 50 mL/min), it is 450 DEG C of heat preservation 2h in temperature, obtains blue MoO after being cooled to room temperature3: Yb, Er fluorescent powder, then
It is secondary by blue MoO3: Yb, Er fluorescent powder are heated to 450 DEG C in air atmosphere, keep the temperature 2h, are cooled to after room temperature and are transformed into shallow
Yellow MoO3: Yb, Er up-conversion phosphor;Under 980nm light source activation, yellow MoO3: Yb, Er up-conversion phosphor issue green
The fluorescence of color, and blue MoO3: Yb, Er light-emitting phosphor weaken or until do not shine, repeatedly in air atmosphere and H2And N2Mixing
With 450 DEG C of respectively sintering 5 times in atmosphere, passes through and realize MoO3: the multiplicating of Yb, Er fluorescent powder color " light yellow-blue " becomes
The reversible regulation of swap-in row up-conversion luminescence.
In H2And N2In reducing atmosphere, temperature is the blue MoO restored at 450 DEG C3: Yb, Er fluorescent powder practical photograph
As shown in 450 reduction in Fig. 2, color is blue.
Light yellow MoO3: Yb, Er up-conversion phosphor switch illumination spectra are as shown in Figure 1, as can be seen from Figure 1 sample
Luminous intensity is about 66.The blue MoO restored at 450 DEG C3: Yb, Er fluorescent powder switch illumination spectra are as shown in Figure 1, can
To find out that sample luminous intensity is about 16.Color from it is light yellow fade to blue during, luminous intensity is changed, therefore logical
Cross realization MoO3: up-conversion luminescence regulation may be implemented in the transformation of Yb, Er fluorescent powder color " light yellow-blue ".The present embodiment
In MoO3: Yb, Er fluorescent powder are repeatedly in air atmosphere and H2And N2With 450 DEG C of respectively sintering 5 times, thermochromism in mixed atmosphere
MoO3: the intensity distribution of reversible, the recyclable regulation of Yb, Er up-conversion phosphor luminous intensity is as shown in figure 3, can from Fig. 3
To find out that luminous intensity can be realized multiple circulating and reversible regulation, and intensity is undamped;Each sintering 5 times, thermochromism MoO3:
The color sample of Yb, Er up-conversion phosphor is reversible, the photo of recyclable regulation is as shown in figure 4, as can be seen from Figure 4 sample
Color can realize multiple circulating and reversible regulation, and colour stable is without decrease.
Embodiment 3
Thermochromism MoO3: Yb, Er up-conversion phosphor, chemical formula MoO3: Yb, Er.
Thermochromism MoO3: the preparation method of Yb, Er up-conversion phosphor, the specific steps of which are as follows:
Step 1, first by 0.01mol (NH4)6Mo7O24·4H2O、Er2O3、Yb2O3It is 1/7:0.5:0.5 mixing according to molar ratio
Uniformly, 5mL dehydrated alcohol is added, grinding obtains mixed material;
The mixed material that step 1 obtains is heated to 500 DEG C by step 2 in air atmosphere, keeps the temperature after 2h furnace cooling to room
Temperature obtains light yellow MoO after grinding3: Yb, Er up-conversion phosphor.Light yellow MoO3: Yb, Er up-conversion phosphor practical photograph
As shown in original in Fig. 2, color is light yellow.
Thermochromism MoO3: the reversible regulation method of the up-conversion luminescence of Yb, Er up-conversion phosphor:
By light yellow MoO3: Yb, Er up-conversion phosphor are in H2And N2Reducing atmosphere (H2And N2Volume ratio be 1:19, gas
Flow is 50 mL/min), it is 700 DEG C of heat preservation 2h in temperature, obtains blue MoO after being cooled to room temperature3: Yb, Er fluorescent powder, then
It is secondary by blue MoO3: Yb, Er fluorescent powder are heated to 700 DEG C in air atmosphere, keep the temperature 2h, are cooled to after room temperature and are transformed into shallow
Yellow MoO3: Yb, Er up-conversion phosphor;Under 980nm light source activation, yellow MoO3: Yb, Er up-conversion phosphor issue green
The fluorescence of color, and blue MoO3: Yb, Er light-emitting phosphor weaken or until do not shine, repeatedly in air atmosphere and H2And N2Mixing
With 450 DEG C of respectively sintering 5 times in atmosphere, passes through and realize MoO3: the multiplicating of Yb, Er fluorescent powder color " light yellow-blue " becomes
The reversible regulation of swap-in row up-conversion luminescence.
In H2And N2In reducing atmosphere, temperature is the blue MoO restored at 700 DEG C3: Yb, Er fluorescent powder practical photograph
As shown in 700 reduction in Fig. 2, color is navy blue.
Light yellow MoO3: Yb, Er up-conversion phosphor switch illumination spectra are as shown in Figure 1, as can be seen from Figure 1 sample
Luminous intensity is about 66.The blue MoO restored at 450 DEG C3: Yb, Er fluorescent powder switch illumination spectra are as shown in Figure 1, can
To find out that sample luminous intensity is about 0.Color from it is light yellow fade to navy blue during, luminous intensity is changed, therefore
By realizing MoO3: up-conversion luminescence regulation may be implemented in the transformation of Yb, Er fluorescent powder color " light yellow-blue ".
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (3)
1. a kind of thermochromism MoO3: Yb, Er up-conversion phosphor, it is characterised in that: chemical formula MoO3: Yb, Er.
2. a kind of thermochromism MoO according to claim 13: the preparation method of Yb, Er up-conversion phosphor, feature exist
In specific step is as follows:
Step 1, first by (NH4)6Mo7O24·4H2O、Er2O3、Yb2O3It is uniformly mixed, is added according to the molar ratio of chemical constitution formula
Dehydrated alcohol, grinding obtain mixed material;
The mixed material that step 1 obtains is heated to 500 DEG C by step 2 in air atmosphere, keeps the temperature after 2h furnace cooling to room
Temperature obtains light yellow MoO after grinding3: Yb, Er up-conversion phosphor.
3. a kind of thermochromism MoO according to claim 13: the reversible tune of the up-conversion luminescence of Yb, Er up-conversion phosphor
Prosecutor method, it is characterised in that:
By light yellow MoO3: Yb, Er up-conversion phosphor are in H2And N2Reducing atmosphere is 300 DEG C ~ 700 DEG C heat preservation 2h in temperature,
Blue MoO is obtained after being cooled to room temperature3: Yb, Er fluorescent powder, again by blue MoO3: Yb, Er fluorescent powder add in air atmosphere
Heat is cooled to after room temperature and is transformed into light yellow MoO3: Yb, Er up-conversion phosphor;Under 980nm light source activation, yellow
MoO3: the fluorescence of Yb, Er up-conversion phosphor sending green, and blue MoO3: Yb, Er light-emitting phosphor weaken or until do not send out
Light, by realizing MoO3: it is reversible that the multiplicating transformation of Yb, Er fluorescent powder color " light yellow-blue " carries out up-conversion luminescence
Regulation.
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CN110511024A (en) * | 2019-09-05 | 2019-11-29 | 昆明理工大学 | A kind of MoO based on thermo-chromic effects3The application of ceramics |
CN110818411A (en) * | 2019-09-05 | 2020-02-21 | 昆明理工大学 | MoO based on photochromic effect3Method for producing ceramic and use thereof |
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CN104371715A (en) * | 2014-11-28 | 2015-02-25 | 赵兵 | Water-soluble molybdenum trioxide up-conversion nanometer material and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110511024A (en) * | 2019-09-05 | 2019-11-29 | 昆明理工大学 | A kind of MoO based on thermo-chromic effects3The application of ceramics |
CN110818411A (en) * | 2019-09-05 | 2020-02-21 | 昆明理工大学 | MoO based on photochromic effect3Method for producing ceramic and use thereof |
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