CN106187167B - A kind of composite material and preparation method enhancing rare earth Er ion luminescence generated by light - Google Patents

A kind of composite material and preparation method enhancing rare earth Er ion luminescence generated by light Download PDF

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CN106187167B
CN106187167B CN201610543381.7A CN201610543381A CN106187167B CN 106187167 B CN106187167 B CN 106187167B CN 201610543381 A CN201610543381 A CN 201610543381A CN 106187167 B CN106187167 B CN 106187167B
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bntbt
xer
powder
zno
rare earth
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CN106187167A (en
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张善涛
耿晓玉
张骥
朱学艺
胡斌
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Nanjing University
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Abstract

The invention discloses a kind of composite material and preparation methods for enhancing rare earth Er ion luminescence generated by light.The composite material includes the ferroelectric material and ZnO of Er doping, and wherein the chemical formula of the ferroelectric material of Er doping is xEr:0.94Bi0.5Na0.5TiO3‑0.06BaTiO3(it is abbreviated as xEr:BNTBT), the molar ratio that wherein x is Er and BNTBT, and x=0.0050,0.0075 or 0.0100；The molar ratio of the ferroelectric material of ZnO and Er doping is 0.1,0.2,0.3 or 0.4.By the way that rare earth Er ion doping is formed composite material, under laser irradiation, the luminescence generated by light of observable Er ion significantly increased with ZnO into ferroelectric material, and further.This method compared with other conventional methods has many advantages, such as that rare earth Er ion luminescence generated by light can be significantly increased.

Description

A kind of composite material and preparation method enhancing rare earth Er ion luminescence generated by light
Technical field
The present invention relates to a kind of composite material of rare earth Er ion luminescence generated by light that can enhance and be adulterated in ferroelectric material and its Preparation method belongs to material science/optical field.
Background technique
Rare earth embedded photoluminescent material has very important in fields such as optical fiber technology, display technology, laser, biomedicines Using.Under normal circumstances, rare earth ion need to be doped in other materials and form luminescent material.The host material generallyd use Crystal structure is unable to real-time monitoring, this is unfavorable for studying the physical process that crystal structure regulates and controls luminosity.
Since inorganic perovskite oxide ferroelectric material can generate structural phase transition under external electric field, rare earth ion It is doped in ferroelectric material, it, can be rare earth luminous with real-time monitoring by the structure of extra electric field real-time monitoring host's ferroelectric material Property, this will be helpful to deep understand crystal structure to the regulatory mechanism of rare earth luminous property.Therefore, in recent years, rare earth is mixed Miscellaneous ferroelectric material has obtained extensive research.Then, compared with other rear-earth-doped hosts, rear-earth-doped ferroelectric material It is small to the enhancement effect of rare earth luminous property, it is difficult to meet real requirement.This to enhance rare earth ion in ferroelectricity host material In luminosity seem especially urgent.
Summary of the invention
It is an object of the invention to the weak problems of the photoluminescence performance for existing rear-earth-doped ferroelectric material, provide one Composite material and preparation method of the kind based on rear-earth-doped ferroelectric material.By rare earth Er ion doping to ferroelectric material 0.94Bi0.5Na0.5TiO3-0.06BaTiO3(xEr:BNTBT in), and composite material (xEr further is formed with ZnO:BNTBT/ YZnO), under laser irradiation, the luminescence generated by light of observable Er ion significantly increased.
The technical solution adopted by the present invention is as follows：
A kind of composite material enhancing rare earth Er ion luminescence generated by light, ferroelectric material and ZnO including Er doping, Er mix The chemical formula of miscellaneous ferroelectric material is xEr:0.94Bi0.5Na0.5TiO3-0.06BaTiO3, it is abbreviated as xEr:BNTBT, wherein x be The molar ratio of Er and BNTBT, and x=0.0050,0.0075 or 0.0100；Mole of the ferroelectric material of ZnO and Er doping Than being 0.1,0.2,0.3 or 0.4.
The preparation method of above-mentioned composite material, includes the following steps：
(1) xEr of Er doping is prepared:BNTBT：Er2O3、Bi2O3、NaCO3、TiO2And BaCO3Starting powder is according to change Proportion is learned, ball grinder is put into and dehydrated alcohol is added, is uniformly mixed by ball-milling method；It is after drying that mixed-powder is Celsius 900 Degree pre-burning 3 hours；After being uniformly mixed and dry again by ball-milling method, powder is sintered 3 hours at 1100 degrees Celsius, is obtained single The xEr of phase:BNTBT powder；
(2) by step (1) preparation-obtained xEr:BNTBT powder is uniformly mixed with ZnO powder by ball-milling method, wherein ZnO and xEr:The molar ratio y of BNTBT is 0.1,0.2,0.3 or 0.4；30- is sintered under 950-1150 degrees Celsius after pressed powder 90 minutes, obtain fine and close xEr:BNTBT/yZnO composite ceramics.
The present invention uses Ferroelectric Composites as parent, regulates and controls the photoluminescent property of rare earth Er ion, beneficial to effect Fruit is：
1, sample preparation methods are easy, high-efficient, compared with the way of traditional replacement doping host, method of the invention Cost is relatively low, high-efficient；
2, compared with not introducing ZnO and forming the method for composite ceramics, the method for the present invention uses Er:BNTBT and ZnO constitutes multiple Ceramics are closed, composite ceramics can more effectively improve luminous intensity.Excitation of the composite material prepared by the present invention in laser light source Under, the xEr with not ZnO:BNTBT one-component ceramic is compared, and rare earth Er ion luminescence generated by light is significantly increased in composite ceramics, Intensification factor is up to 4.5 times.
Detailed description of the invention
Fig. 1 is the xEr being prepared in the method for the present invention:BNTBT/yZnO composite ceramics sample (x=0.0100, y= 0.4) scanning electron microscope image.
Fig. 2 (a) is the xEr being prepared:BNTBT/yZnO composite ceramics sample (x=0.0050, y=0.1,0.2, 0.3,0.4 luminescence generated by light figure).
Fig. 2 (b) is the xEr being prepared:BNTBT/yZnO composite ceramics sample (x=0.0075, y=0.1,0.2, 0.3,0.4 luminescence generated by light figure).
Fig. 2 (c) is the xEr being prepared:BNTBT/yZnO composite ceramics sample (x=0.0100, y=0,0.1,0.2, 0.3,0.4 luminescence generated by light figure).
Specific embodiment
Embodiment 1：By xEr:BNTBT (x=0.0050,0.0075,0.0100) powder is mixed with ZnO (y=0.1) powder Tabletting after uniformly obtains xEr after 1150 degrees Celsius are sintered 90 minutes:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Under light excitation, luminosity is measured.
Embodiment 2：By xEr:BNTBT (x=0.0050,0.0075,0.0100) powder is mixed with ZnO (y=0.2) powder Tabletting after uniformly obtains xEr after 1050 degrees Celsius are sintered 90 minutes:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Under light excitation, luminosity is measured.
Embodiment 3：By xEr:BNTBT (x=0.0050,0.0075,0.010) powder is mixed with ZnO (y=0.3) powder Tabletting after uniformly is sintered after sixty minutes at 1000 degrees Celsius, obtains xEr:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Under light excitation, luminosity is measured.
Embodiment 4：By xEr:BNTBT (x=0.0050,0.0075,0.010) powder is mixed with ZnO (y=0.4) powder Tabletting after uniformly obtains xEr after 950 degrees Celsius are sintered 30 minutes:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Under light excitation, luminosity is measured.
Test result：
Fig. 1 is the xEr being prepared:The scanning electron of BNTBT/yZnO composite ceramics sample (x=0.0100, y=0.4) MIcrosope image.As can be seen that the mutual independence of ZnO particle and being present in Er:In BNTBT substrate, 0-3 type composite ceramic is constituted Porcelain.The ingredient of other y ≠ 0 all has this microstructure features.
Fig. 2 (a) is the xEr being prepared:BNTBT/yZnO composite ceramics sample (x=0.0050, y=0.1,0.2, 0.3,0.4) luminescence generated by light figure, Fig. 2 (b) are the xEr being prepared:BNTBT/yZnO composite ceramics sample (x=0.0075, y =0.1,0.2,0.3,0.4) luminescence generated by light figure, Fig. 2 (c) are the xEr being prepared:BNTBT/yZnO composite ceramics sample (x =0.0100, y=0,0.1,0.2,0.3,0.4) luminescence generated by light figure.It can be seen that with the increase of ZnO content (y value), pottery The luminous intensity of porcelain sample all dramatically increases, and compared with no ZnO (y=0), the increase multiple of luminous intensity is up to 4.5 times.
As described above, the method for the present invention uses Er:BNTBT and ZnO constitutes the composite ceramics of 0-3 type, in laser light source XEr under excitation, with not ZnO:BNTBT one-component ceramic is compared, and the luminescence generated by light of rare earth Er ion obtains in composite ceramics It significantly increases, intensification factor is up to 4.5 times, this is to the rear-earth-doped ferroelectric material of realization using most important.Sample of the invention Product preparation method is easy, high-efficient.

Claims (4)

1. a kind of composite material for enhancing rare earth Er ion luminescence generated by light, ferroelectric material and ZnO including Er doping, feature It is, the chemical formula of the ferroelectric material of Er doping is xEr:0.94Bi0.5Na0.5TiO3-0.06BaTiO3, it is abbreviated as xEr: BNTBT, wherein x is the molar ratio of Er and BNTBT, and x=0.0050,0.0075 or 0.0100；The iron of ZnO and Er doping The molar ratio of electric material is 0.1,0.2,0.3 or 0.4.
2. a kind of preparation method for the composite material for enhancing rare earth Er ion luminescence generated by light, feature exist as described in claim 1 In including the following steps：
(1) xEr of Er doping is prepared:BNTBT：Er2O3、Bi2O3、NaCO3、TiO2And BaCO3Starting powder is matched according to chemistry Than being uniformly mixed；After drying by mixed-powder 900 degrees Celsius pre-burning 3 hours；It is uniformly mixed and dries again by ball-milling method Afterwards, powder is sintered 3 hours at 1100 degrees Celsius, obtains single-phase xEr:BNTBT powder；
(2) by step (1) preparation-obtained xEr:BNTBT powder is uniformly mixed with ZnO powder, wherein ZnO and xEr:BNTBT Molar ratio y be 0.1,0.2,0.3 or 0.4；It is sintered 30-90 minutes, is caused under 950-1150 degrees Celsius after pressed powder Close xEr:BNTBT/yZnO composite ceramics.
3. preparation method according to claim 2, which is characterized in that in the step (1), starting powder is put into ball milling Simultaneously dehydrated alcohol is added in tank, is uniformly mixed by ball-milling method.
4. preparation method according to claim 2, which is characterized in that in the step (2), xEr:BNTBT powder and ZnO Powder is uniformly mixed by ball-milling method.
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CN108341667B (en) * 2018-03-30 2020-10-02 常州大学 Preparation method of nano cubic ferroelectric material
CN110357616A (en) * 2019-07-22 2019-10-22 福州大学 A kind of preparation method of Er ions bismuth sodium titanate-barium titanate flexibility ferroelectricity light-emitting film

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Photoluminescence and Temperature Dependent Electrical Properties of Er-Doped 0.94 Bi0.5N0.5TiO3-0.06BaTiO3 Ceramics;Bin Hue et al.;《J.Am.Ceram.Soc》;20141231;第97卷(第12期);第3877-3882页 *
Semiconductor/relaxor 0-3 type composites without thermal depolarization in Bi0.5Na0.5TiO3-based lead-free piezoceramics;Ji Zhang et al.;《NATURE COMMUNICATIONS》;20150319;第1-10页 *
Temperature dependent structures and properties of Bi0.5Na0.5TiO3-based lead free piezoelectric composite;Ji Zhang et al.;《Dalton Transactions》;20160615(第45期);第10891-10896页 *

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