CN110066173B - BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material, preparation method and application thereof - Google Patents
BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to BaMgSiO4Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material, a preparation method and application thereof, belonging to the technical field of photochromic anti-counterfeiting and identification. The BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material with chemical composition formula of BaMgSiO4X% Yb, y% Tb, wherein x = 0.01-2, y = 0.01-2. Firstly, BaCO is added3、Tb4O7、Yb2O3MgO and SiO2Uniformly mixing and grinding the materials according to the molar ratio of the chemical composition formula to obtain a mixed material, and pressing the mixed material into a wafer; under the condition of reducing atmosphere, keeping the temperature of the obtained wafer at 1000-1300 ℃ for 5-10 h, and cooling to room temperature to obtain BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material. The BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material ceramic wafer can regulate up-conversion luminescence intensity through coloring-bleaching process, and can be applied to the anti-counterfeiting field.
Description
Technical Field
The invention relates to BaMgSiO4Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material, a preparation method and application thereof, belonging to the technical field of photochromic anti-counterfeiting and identification.
Background
Photochromic materials are materials whose color reversibly changes under the stimulation of an external electric field, a magnetic field, heat and light. The conductivity, absorption spectrum, refractive index, etc. of the material change with the change of the material color. Therefore, the photochromic material has important application in the fields of photonics information storage, carbon paper, molecular switches, imaging, anti-counterfeiting marks, biosensing, logic gates, molecular lines, optical/electronic devices and the like. The color-changing material comprises an organic color-changing material, an inorganic color-changing material and an organic-inorganic hybrid color-changing material. The traditional organic color-changing materials comprise furan, pyridine, diarylene and the like, but the stability at high temperature is poor, heating can cause irreversible damage to the material structure, the chemical stability is poor, and the environmental requirements for use are strict; in addition, organic materials are volatile, so that the organic materials have great damage to human bodies, and the environment is easily polluted due to improper packaging. Compared with the traditional organic material, the inorganic color-changing material has the advantages of good color-developing thermal stability, good fatigue resistance, low synthesis cost, small environmental pollution, large-area display and the like, and makes up for the defects of the organic color-changing material. With the development of inorganic color-changing materials, there have been many researches on the color change or bleaching of materials using external fields such as electric fields, magnetic fields, heating, etc., but there have been problems of slow response time of color change, single means of color change or bleaching, etc.
Disclosure of Invention
Aiming at the problems and the defects in the prior art, the invention provides BaMgSiO4Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material, and a preparation method and application thereof. BaMgSiO of the invention4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material and pure BaMgSiO without doping Yb and Tb4Compared with ceramic material, BaMgSiO4Yb and Tb ceramic materials have the advantages of good color change property, fast color change response time, good thermal stability, good fatigue resistance, realization of color change and bleaching by light stimulation, and the like. In practical application, BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material can be seen to turn pink in the irradiated place only by ultraviolet lamp irradiation, and can be restored to original light gray under 473nm irradiation, and in addition, the Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material can be mixed with pure BaMgSiO4Compared with ceramic material, BaMgSiO4Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material can generate visible up-conversion luminescence under the excitation of 980nm near-infrared laser, and the up-conversion luminescence can be reversibly regulated and controlled through color-changing characteristics, so that the Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material has wide application prospect in the anti-counterfeiting field. The invention is realized by the following technical scheme.
BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material with chemical composition formula of BaMgSiO4:x%Yb，y% Tb, wherein x =0.01~2, and y =0.01~ 2.
BaMgSiO4The Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material preparation method comprises the following specific steps:
step 1, firstly, BaCO is mixed3、Tb4O7、Yb2O3MgO and SiO2Uniformly mixing and grinding the materials according to the molar ratio of the chemical composition formula to obtain a mixed material, and pressing the mixed material into a wafer;
step 2, under the condition of reducing atmosphere, keeping the temperature of the wafer obtained in the step 1 at 1000-1300 ℃ for 5-10 h, and cooling to room temperature to obtain BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material.
The above BaMgSiO4BaMgSiO prepared by the method for preparing Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material ceramic wafer can regulate up-conversion luminescence intensity through coloring-bleaching process, and can be applied to the anti-counterfeiting field. BaMgSiO prepared by the invention4Under the irradiation of ultraviolet 254nm, the ceramic chip can be changed from original light gray into pink and can be clearly seen by naked eyes; the sample can be bleached by irradiating with visible light 473nm after the ceramic is colored by the ultraviolet ray, and the reversibility is good. BaMgSiO prepared by the invention4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material can generate up-conversion luminescence under the excitation of 980nm laser, and BaMgSiO is irradiated by ultraviolet rays of 254nm4Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material is reduced after being colored, and then BaMgSiO is irradiated by visible light at 473nm4The up-conversion luminescence of Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material is recovered, the intensity of up-conversion luminescence can be regulated and controlled through the coloring-bleaching process, and the Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material has application prospect in the anti-counterfeiting field.
The invention has the beneficial effects that:
(1) BaMgSiO prepared by the invention4The color of a sample of the Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material is changed from light gray to pink under the irradiation of ultraviolet light 254-365 nm.
(2) The colored (pink) sample of the invention returns the color from pink to the original light gray after being irradiated by 473nm of visible light, and the ceramic can realize the reversible change of light gray-pink by alternately using ultraviolet-visible light, and has good reversibility.
(3) Under the excitation of near-infrared 980nm laser, BaMgSiO4X% Yb, y% Tb (x = 0.01-2, y = 0.01-2) ceramic produces the characteristic up-conversion luminescence of terbium ions; and the luminescence upconversion is weakened after the pink is changed, the luminescence intensity is recovered after bleaching, the upconversion luminescence can be reversibly regulated and controlled through the coloring-bleaching process, and the method has wide application value in the anti-counterfeiting field.
(4) The ceramic BaMgSiO of the invention4The ceramic chip with x% Yb and y% Tb (x = 0.01-2, y = 0.01-2) has obvious color changing effect and up-conversion luminescence modulation control, is visible to the naked eye, has potential application value in the aspect of photochromic anti-counterfeiting, and is expected to realize industrial production.
Drawings
FIG. 1 is a diagram of BaMgSiO of the present invention4The raw materials are ground, pressed into sheets, sintered and cooled to obtain the final photochromic ceramic chip.
FIG. 2 is the BaMgSiO solid prepared in example 14The color change effect graph of the reversible color change ceramic wafer of 1% Yb and 1% Tb shows that the sample is changed from original light gray to pink under the irradiation of ultraviolet rays of 254 nm. Changing from pink to light grey under the irradiation of 473nm visible light.
FIG. 3 shows BaMgSiO corresponding to example 1 of the present invention41% Yb,1% Tb ceramic wafer to generate visible up-conversion luminescence under the excitation of 980nm laser; the luminescence is weakened after the color change by 254nm radiation, and the luminescence is recovered after the bleaching by 473nm radiation.
Detailed Description
The invention is further described with reference to the following drawings and detailed description.
Example 1
As shown in FIG. 1, the BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material with chemical composition formula of BaMgSiO4X% Yb, y% Tb, where x =1，y=1。
The BaMgSiO4The Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material preparation method comprises the following specific steps:
step 1, firstly, BaCO is mixed3、Tb4O7、Yb2O3MgO and SiO2According to a molar ratio of 1: 0.0025: 0.005: 1: 1, uniformly mixing and grinding to obtain a mixed material, and pressing the mixed material into a wafer;
step 2, under the condition of reducing atmosphere (H)2And N2Is 1: 19, the flow rate of gas is 50 mL/min), keeping the temperature of the wafer obtained in the step 1 at 1300 ℃ for 5h, and cooling to room temperature to obtain BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material.
The BaMgSiO41% Yb and 1% Tb up-conversion luminescence anti-counterfeiting ceramic material can change from original light gray into pink under the irradiation of ultraviolet 254nm of an ultraviolet lamp, and changes color after the irradiation of the ultraviolet 254 nm; after 473nm visible light irradiation, the pink color is completely faded, and the effect of color change of the ceramic wafer from the pink color after color change to the original light gray color can be easily distinguished by naked eyes as shown in fig. 2.
BaMgSiO41% Yb and 1% Tb ceramic plate turns pink from light gray after being irradiated by ultraviolet rays of 254 nm; exciting the pink ceramic wafer by using 980nm near-infrared laser to generate up-conversion luminescence at 490nm, 548nm, 590nm and 624 nm; the up-conversion luminescence is weakened, and the luminescence spectrum and the luminescence photo are shown in FIG. 3; BaMgSiO41% Yb and 1% Tb ceramic plate is irradiated by ultraviolet ray at 254nm to change color; after 473nm visible light irradiation, the pink color is completely faded, the faded ceramic piece is excited by 980nm near infrared light, the converted luminescence is recovered, and the spectrogram and the luminescence photo are shown in fig. 3.
BaMgSiO obtained in example 1 of the invention4Ceramic sheets of 1% Yb and 1% Tb can turn pink under the irradiation of ultraviolet rays of 254 nm; the original color can be recovered under the irradiation of 473nm visible light, and the reversible color change can keep good stability after repeated times; the up-conversion luminescence based on the color-changing reaction regulation and control is used in an anti-counterfeiting methodThe noodle has good potential application value.
Example 2
The BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material with chemical composition formula of BaMgSiO4X% Yb, y% Tb, where x =0.01 and y = 0.01.
The BaMgSiO4The Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material preparation method comprises the following specific steps:
step 1, firstly, BaCO is mixed3、Tb4O7、Yb2O3MgO and SiO2According to a molar ratio of 1: 0.000025: 0.00005: 1: 1, uniformly mixing and grinding to obtain a mixed material, and pressing the mixed material into a wafer;
step 2, under the condition of reducing atmosphere (H)2And N2Is 1: 19, the flow rate of gas is 50 mL/min), keeping the temperature of the wafer obtained in the step 1 at 1000 ℃ for 10h, and cooling to room temperature to obtain BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material.
The above BaMgSiO4BaMgSiO prepared by the method for preparing Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material ceramic wafer can regulate up-conversion luminescence intensity through coloring-bleaching process, and can be applied to the anti-counterfeiting field.
Example 3
The BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material with chemical composition formula of BaMgSiO4X% Yb, y% Tb, where x =2 and y = 2.
The BaMgSiO4The Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material preparation method comprises the following specific steps:
step 1, firstly, BaCO is mixed3、Tb4O7、Yb2O3MgO and SiO2According to a molar ratio of 1: 0.005: 0.01: 1: 1, uniformly mixing and grinding to obtain a mixed material, and pressing the mixed material into a wafer;
step 2, under the condition of reducing atmosphere (H)2And N2Is 1: 19, flow rate of gas 50 mL/min), the step (B)1, preserving the heat of the wafer at 1150 ℃ for 8 h, and cooling to room temperature to obtain BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material.
The above BaMgSiO4BaMgSiO prepared by the method for preparing Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material ceramic wafer can regulate up-conversion luminescence intensity through coloring-bleaching process, and can be applied to the anti-counterfeiting field.
While the present invention has been described in detail with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit and scope of the present invention.
Claims (3)
1. BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material, which is characterized in that: the chemical composition formula is BaMgSiO4X% Yb, y% Tb, wherein x = 0.01-2, y = 0.01-2.
2. BaMgSiO of claim 14The preparation method of the Yb and Tb up-conversion luminescence anti-counterfeiting ceramic material is characterized by comprising the following specific steps:
step 1, firstly, BaCO is mixed3 、Tb4O7、Yb2O3MgO and SiO2Uniformly mixing and grinding the materials according to the molar ratio of the chemical composition formula to obtain a mixed material, and pressing the mixed material into a wafer;
step 2, under the condition of reducing atmosphere, keeping the temperature of the wafer obtained in the step 1 at 1000-1300 ℃ for 5-10 h, and cooling to room temperature to obtain BaMgSiO4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material.
3. BaMgSiO of claim 24BaMgSiO prepared by the method for preparing Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material4Yb, Tb up-conversion luminescence anti-counterfeiting ceramic material ceramic sheet can regulate up-conversion luminescence intensity through coloring-bleaching processThe method is used in the anti-counterfeiting field.
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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 |
| CN106916581A (en) * | 2017-04-13 | 2017-07-04 | 广东工业大学 | A kind of silicate ability of reverse photochromism material and preparation method thereof |
| US20180246084A1 (en) * | 2017-02-27 | 2018-08-30 | The Hong Kong Polytechnic University | Heterogeneous microarray based hybrid upconversion nanoprobe/nanoporous membrane system |
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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 |
| US20180246084A1 (en) * | 2017-02-27 | 2018-08-30 | The Hong Kong Polytechnic University | Heterogeneous microarray based hybrid upconversion nanoprobe/nanoporous membrane system |
| CN106916581A (en) * | 2017-04-13 | 2017-07-04 | 广东工业大学 | A kind of silicate ability of reverse photochromism material and preparation method thereof |
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| Photochromism enhancement in reduced tridymite BaMgSiO4 by Fe-doping;Morito Akiyama et al.;《Journal of the Ceramic Society of Japan》;20110228;第119卷(第5期);第338-341页 * |
| Tb3+-Yb3+体系的量子剪切及上转换荧光特性研究;段倩倩;《中国博士学位论文全文数据库基础科学辑》;20140115(第01期);第A005-31页 * |
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