CN110066173A - A kind of BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, preparation method and applications - Google Patents
A kind of BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, preparation method and applications Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 59
- 229910052771 Terbium Inorganic materials 0.000 title claims abstract description 56
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 50
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 30
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000004061 bleaching Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 6
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 6
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005242 forging Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000002845 discoloration Methods 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 6
- 230000002441 reversible effect Effects 0.000 description 5
- 230000005284 excitation Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003760 hair shine Effects 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 230000002929 anti-fatigue Effects 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- -1 terbium ion Chemical class 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/20—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in magnesium oxide, e.g. forsterite
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- 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
- C09K11/7774—Aluminates
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The present invention relates to a kind of BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, preparation method and applications belong to photochromism anti-forging and identification technology field.The BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, chemical constitution formula BaMgSiO4: x%Yb, y%Tb, wherein x=0.01 ~ 2, y=0.01 ~ 2.First by BaCO3、Tb4O7、Yb2O3, MgO and SiO2Grinding is uniformly mixed according to the molar ratio of chemical constitution formula and obtains mixed material, and mixed material is pressed into disk；Under the conditions of restoring atmosphere, by obtained disk temperature be 1000 ~ 1300 DEG C of 5 ~ 10 h of heat preservation, obtain BaMgSiO after being cooled to room temperature4: Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd.The BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd can be applied by the luminous power of the controllable upper conversion of coloring-bleaching process in anti-counterfeit field.
Description
Technical field
The present invention relates to a kind of BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, preparation method and applications,
Belong to photochromism anti-forging and identification technology field.
Background technique
Photochromic material is a kind of in external electrical field, and magnetic field, the material of reversible change occurs for color under the stimulation of light and heat
Material.Variation based on material color, the conductivity of material, absorption spectrum, refractive index etc. is with changing.Therefore, light-induced variable
Color material light open the light information storage, carbon paper, molecular switch, imaging, anti-fake mark, bio-sensing, logic gate, molecular line,
The fields such as optics/electronic device have important utilization.Off-color material includes organic off-color material, inorganic off-color material and organic-
Inorganic hybridization off-color material.Traditional organic off-color material has furans, pyridine, two fragrant alkene etc., but high temperatures are bad,
Heating can cause irreversible breaking to material structure, and chemical stability is bad, and the environmental requirement used is harsh；Further, since having
Machine class material is volatile, has very big damage to human body, encapsulation is improper to be easy to pollute the environment.Compared to the organic material of tradition
Material, inorganic off-color material have colour developing thermal stability is good, anti-fatigue performance is good, synthesis cost is low, environmental pollution is small, it can be achieved that big
Area such as shows at the advantages, compensates for the deficiency of organic off-color material.With the development of inorganic off-color material, outfield such as electricity is used
, magnetic field, heating etc. realize material discoloration or bleaching research had very much, but there is also change colour the response time it is slow,
The problems such as discoloration or bleaching protocols are single.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of BaMgSiO4: hair is converted on Yb, Tb
Light Anti-false ceramic material, preparation method and applications.BaMgSiO of the invention4: Yb, Tb up-conversion luminescence Anti-false ceramic material,
With the pure BaMgSiO adulterated without Yb and Tb4Ceramic material is compared, BaMgSiO4: Yb, Tb ceramic material discoloration property are good, become
The colour response time is fast, and thermal stability is good, and anti-fatigue performance is good, and changing colour and bleach can be with light stimulus come the advantages that realization.
The BaMgSiO in practice4: Yb, Tb up-conversion luminescence Anti-false ceramic material only need to be using uv light irradiations i.e. it can be seen that spoke
According to place become pink, 473nm irradiation under again can be restored to original light gray, in addition, with pure BaMgSiO4Pottery
Ceramic material is compared, BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material generate under the excitation of 980nm near-infrared laser
Visible upper conversion shines, and is shone by the reversible regulation of color shifting properties energy conversion thereon, has widely in anti-counterfeit field
Application prospect.The invention is realized by the following technical scheme.
A kind of BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, chemical constitution formula BaMgSiO4: x%Yb, y%
Tb, wherein x=0.01 ~ 2, y=0.01 ~ 2.
A kind of BaMgSiO4: the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material, the specific steps of which are as follows:
Step 1, first by BaCO3、Tb4O7、Yb2O3, MgO and SiO2It is uniformly mixed and grinds according to the molar ratio of chemical constitution formula
To mixed material, mixed material is pressed into disk；
Step 2, under the conditions of restoring atmosphere, disk that step 1 is obtained is 1000 ~ 1300 DEG C of 5 ~ 10 h of heat preservation in temperature, is cooled down
BaMgSiO is obtained after to room temperature4: Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd.
Above-mentioned BaMgSiO4: the BaMgSiO that the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material is prepared4:
Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd pass through the luminous power of the controllable upper conversion of coloring-bleaching process, energy
It applies in anti-counterfeit field.The BaMgSiO that the present invention is prepared4: Yb, Tb up-conversion luminescence Anti-false ceramic material are in ultraviolet light
Under 254nm irradiation, potsherd can be become pink by original light gray, and naked eyes are high-visible；Ultraviolet light makes ceramic coloring
Sample can be made to bleach with visible light 473nm irradiation afterwards, there is good invertibity.The BaMgSiO that the present invention is prepared4:Yb,Tb
Up-conversion luminescence Anti-false ceramic material can produce up-conversion luminescence under the excitation of 980nm laser, be irradiated using ultraviolet light 254nm
Afterwards, BaMgSiO4: up-conversion luminescence weakens after Yb, Tb up-conversion luminescence Anti-false ceramic material colour, then through light-exposed 473nm spoke
According to rear, BaMgSiO4: the up-conversion luminescence of Yb, Tb up-conversion luminescence Anti-false ceramic material restores, can by coloring-bleaching process
Luminous power is converted in regulation, and there is application prospect in anti-counterfeit field.
The beneficial effects of the present invention are:
(1) BaMgSiO prepared by the present invention4: Yb, Tb up-conversion luminescence Anti-false ceramic material are irradiated in 254 ~ 365nm of ultraviolet light
Lower color sample occurs by the light grey variation to pink.
(2) sample of (pink) after the present invention colours, color is restored to original by pink after visible light 473nm irradiation
The light gray of beginning, by the way that ultraviolet-visible light is used alternatingly, which may be implemented the reversible change of itself light grey-pink,
With good invertibity.
(3) under near-infrared 980nm laser excitation, BaMgSiO4: x%Yb, y%Tb (x=0.01 ~ 2, y=0.01 ~ 2) ceramics
It can produce the feature up-conversion luminescence of terbium ion；And luminous upper conversion weakens after becoming pink, luminous intensity is multiple after bleaching
Original is with a wide range of applications by coloring-reversible regulation up-conversion luminescence of bleaching process energy in anti-counterfeit field.
(4) present invention institute ceramics BaMgSiO4: x%Yb, y%Tb (x=0.01 ~ 2, y=0.01 ~ 2) Ceramics Ceramic piece discoloration effect
Fruit and up-conversion luminescence regulation are obvious, visually as it can be seen that there is potential applying value in terms of photochromism anti-forging, are expected to realization industry
Metaplasia produces.
Detailed description of the invention
Fig. 1 is BaMgSiO of the present invention4: the synthetic schemes of Yb, Tb up-conversion luminescence Anti-false ceramic material, raw material pass through
Grinding, tabletting are sintered and cooled to obtain final photochromic potsherd.
Fig. 2 is BaMgSiO prepared by example 14: the color changeable effect figure of 1%Yb, 1%Tb potsherd reversible color potsherd,
Ultraviolet light 254nm irradiates lower sample and becomes pink by original light gray.Again by pink discoloration under visible light 473nm irradiation
At light gray.
Fig. 3 is the corresponding BaMgSiO of present example 14: the up-conversion luminescence spectrogram and hair of 1%Yb, 1%Tb potsherd
Radiograph generates visible up-conversion luminescence under 980nm laser excitation；The luminescent decay after 254nm irradiation discoloration,
It shines after 473nm irradiation bleaching and restores again.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in Figure 1, the BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, chemical constitution formula BaMgSiO4:x%
Yb, y%Tb, wherein x=1, y=1.
The BaMgSiO4: the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material, the specific steps of which are as follows:
Step 1, first by BaCO3、Tb4O7、Yb2O3, MgO and SiO2It is uniformly mixed according to molar ratio 1:0.0025:0.005:1:1
Grinding obtains mixed material, and mixed material is pressed into disk；
Step 2, (H under the conditions of restoring atmosphere2And N2Volume ratio be 1:19, the flow of gas is 50 mL/min), by step 1
Obtained disk is 1300 DEG C of heat preservation 5h in temperature, obtains BaMgSiO after being cooled to room temperature4: the anti-fake pottery of Yb, Tb up-conversion luminescence
Ceramic material potsherd.
The BaMgSiO4: 1%Yb, 1%Tb up-conversion luminescence Anti-false ceramic material can under ultraviolet lamp ultraviolet light 254nm irradiation
Pink is become by original light gray, after ultraviolet light 254nm irradiation discoloration；Using the irradiation of 473nm visible light
Afterwards, pink colour is taken off completely, by naked eyes can tell easily potsherd color be restored to by the pink after changing colour it is original shallow
Gray discoloration effect is as shown in Figure 2.
BaMgSiO4: 1%Yb, 1%Tb potsherd color after ultraviolet light 254nm irradiation by original light gray become pink
Color；Pink colour potsherd is excited with 980nm near-infrared laser, generates the upper conversion being located at 490nm, 548nm, 590nm and 624nm
It shines；Luminescent decay is converted thereon, and luminescent spectrum and luminous photo are as shown in Figure 3；BaMgSiO4: 1%Yb, 1%Tb potsherd
After ultraviolet light 254nm irradiation discoloration；After irradiation using 473nm visible light, pink colour is taken off completely, the ceramics of colour fading
Piece is excited in 980nm near infrared light, and up-conversion luminescence restores, and spectrogram and luminous photo are as shown in Figure 3.
The resulting BaMgSiO of present example 14: the potsherd of 1%Yb, 1%Tb can become under ultraviolet light 254nm irradiation
Pink；Original color can be restored to again under visible light 473nm irradiation, reversible discoloration is kept very after being repeated several times
Good stability；This up-conversion luminescence based on metachromasia regulation has good potential applying value at anti-fake aspect.
Embodiment 2
The BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, chemical constitution formula BaMgSiO4: x%Yb, y%Tb,
Middle x=0.01, y=0.01.
The BaMgSiO4: the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material, the specific steps of which are as follows:
Step 1, first by BaCO3、Tb4O7、Yb2O3, MgO and SiO2It is mixed according to molar ratio 1:0.000025:0.00005:1:1
Uniformly grinding obtains mixed material, and mixed material is pressed into disk；
Step 2, (H under the conditions of restoring atmosphere2And N2Volume ratio be 1:19, the flow of gas is 50 mL/min), by step 1
Obtained disk is 1000 DEG C of 10 h of heat preservation in temperature, obtains BaMgSiO after being cooled to room temperature4: Yb, Tb up-conversion luminescence are anti-
Pseudo- ceramic material potsherd.
Above-mentioned BaMgSiO4: the BaMgSiO that the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material is prepared4:
Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd pass through the luminous power of the controllable upper conversion of coloring-bleaching process, energy
It applies in anti-counterfeit field.
Embodiment 3
The BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, chemical constitution formula BaMgSiO4: x%Yb, y%Tb,
Middle x=2, y=2.
The BaMgSiO4: the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material, the specific steps of which are as follows:
Step 1, first by BaCO3、Tb4O7、Yb2O3, MgO and SiO2It is uniformly mixed and grinds according to molar ratio 1:0.005:0.01:1:1
Mill obtains mixed material, and mixed material is pressed into disk；
Step 2, (H under the conditions of restoring atmosphere2And N2Volume ratio be 1:19, the flow of gas is 50 mL/min), by step 1
Obtained disk is 1150 DEG C of 8 h of heat preservation in temperature, obtains BaMgSiO after being cooled to room temperature4: Yb, Tb up-conversion luminescence are anti-fake
Ceramic material potsherd.
Above-mentioned BaMgSiO4: the BaMgSiO that the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material is prepared4:
Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd pass through the luminous power of the controllable upper conversion of coloring-bleaching process, energy
It applies in anti-counterfeit field.
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 BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material, it is characterised in that: chemical constitution formula is
BaMgSiO4: x%Yb, y%Tb, wherein x=0.01 ~ 2, y=0.01 ~ 2.
2. a kind of BaMgSiO according to claim 14: the preparation method of Yb, Tb up-conversion luminescence Anti-false ceramic material,
It is characterized in that specific step is as follows:
Step 1, first by BaCO3、Tb4O7、Yb2O3, MgO and SiO2It is uniformly mixed and grinds according to the molar ratio of chemical constitution formula
To mixed material, mixed material is pressed into disk；
Step 2, under the conditions of restoring atmosphere, disk that step 1 is obtained is 1000 ~ 1300 DEG C of 5 ~ 10h of heat preservation in temperature, is cooled to
BaMgSiO is obtained after room temperature4: Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd.
3. a kind of BaMgSiO according to claim 24: the preparation method system of Yb, Tb up-conversion luminescence Anti-false ceramic material
Standby obtained BaMgSiO4: Yb, Tb up-conversion luminescence Anti-false ceramic material potsherd, by coloring-bleaching process it is controllable on
The luminous power of conversion, can apply in anti-counterfeit field.
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| CN115215641A (en) * | 2022-08-10 | 2022-10-21 | 松山湖材料实验室 | Photochromic ceramic, preparation method thereof and optical device |
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| CN101928139A (en) * | 2010-09-02 | 2010-12-29 | 同济大学 | Bismuth calcium titanate-based luminous piezoelectric ceramic material and preparation method |
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| 段倩倩: "Tb3+-Yb3+体系的量子剪切及上转换荧光特性研究", 《中国博士学位论文全文数据库基础科学辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115215641A (en) * | 2022-08-10 | 2022-10-21 | 松山湖材料实验室 | Photochromic ceramic, preparation method thereof and optical device |
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