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CN106187167A - A kind of composite strengthening rare earth Er ionic light photoluminescence and preparation method thereof - Google Patents

A kind of composite strengthening rare earth Er ionic light photoluminescence and preparation method thereof Download PDF

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CN106187167A
CN106187167A CN201610543381.7A CN201610543381A CN106187167A CN 106187167 A CN106187167 A CN 106187167A CN 201610543381 A CN201610543381 A CN 201610543381A CN 106187167 A CN106187167 A CN 106187167A
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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

本发明公开了一种增强稀土Er离子光致发光的复合材料及其制备方法。该复合材料包括Er掺杂的铁电材料以及ZnO，其中Er掺杂的铁电材料的化学式为xEr:0.94Bi0.5Na0.5TiO3‑0.06BaTiO3(简写为xEr:BNTBT)，其中x为Er与BNTBT的摩尔比，且x＝0.0050、0.0075或0.0100；ZnO与Er掺杂的铁电材料的摩尔比为0.1、0.2、0.3或0.4。通过把稀土Er离子掺杂到铁电材料中，并进一步与ZnO形成复合材料，在激光照射下，可观察Er离子的显著增强的光致发光。本方法与其他传统方法相比，具有能显著增强稀土Er离子光致发光等优点。

The invention discloses a composite material for enhancing the photoluminescence of rare earth Er ions and a preparation method thereof. The composite material includes Er-doped ferroelectric material and ZnO, wherein the chemical formula of Er-doped ferroelectric material is xEr:0.94Bi 0.5 Na 0.5 TiO 3 ‑0.06BaTiO 3 (abbreviated as xEr:BNTBT), where x is Er Molar ratio to BNTBT, and x=0.0050, 0.0075 or 0.0100; molar ratio of ZnO to Er-doped ferroelectric material is 0.1, 0.2, 0.3 or 0.4. By doping rare earth Er ions into ferroelectric materials and further forming composite materials with ZnO, under laser irradiation, significantly enhanced photoluminescence of Er ions can be observed. Compared with other traditional methods, the method has the advantages of significantly enhancing the photoluminescence of rare earth Er ions and the like.

Description

A kind of composite strengthening rare earth Er ionic light photoluminescence and preparation method thereof
Technical field
The present invention relates to a kind of rare earth Er ionic light photoluminescence that can strengthen in ferroelectric material doping composite and Preparation method, belongs to material science/optical field.
Background technology
Rare earth embedded photoluminescent material has very important in fields such as optical fiber technology, Display Technique, laser, biomedicines Application.Generally, rare earth ion need to be doped in other materials be formed luminescent material.The host material generally used Crystal structure can not real-time monitoring, this is unfavorable for studying the crystal structure physical process that regulates and controls luminosity.
Owing to inorganic calcium titanium ore oxide ferroelectric material can produce structural phase transition, therefore rare earth ion under external electric field It is doped in ferroelectric material, by the structure of extra electric field real-time monitoring host's ferroelectric material, can be rare earth luminous with real-time monitoring Character, this will assist in and deep understands the crystal structure regulatory mechanism to rare earth luminous character.Therefore, in recent years, rare earth is mixed Miscellaneous ferroelectric material has obtained studying widely.Then, compared with the host that other are rear-earth-doped, rear-earth-doped ferroelectric material Little to the enhancement effect of rare earth luminous character, it is difficult to meet real requirement.This makes to strengthen rare earth ion at ferroelectricity host material In luminosity seem the most urgent.
Summary of the invention
Present invention aims to the problem that the photoluminescence performance of existing rear-earth-doped ferroelectric material is weak, it is provided that one Plant composite based on rear-earth-doped ferroelectric material and preparation method thereof.By rare earth Er ion doping to ferroelectric material 0.94Bi0.5Na0.5TiO3-0.06BaTiO3(xEr:BNTBT) in, and composite (xEr:BNTBT/ is formed with ZnO further YZnO), under laser irradiates, the luminescence generated by light being obviously enhanced of observable Er ion.
The technical solution used in the present invention is as follows:
A kind of composite strengthening rare earth Er ionic light photoluminescence, ferroelectric material and ZnO, Er including Er doping are mixed The chemical formula of miscellaneous ferroelectric material is xEr:0.94Bi0.5Na0.5TiO3-0.06BaTiO3, it is abbreviated as xEr:BNTBT, wherein x is The mol ratio of Er Yu BNTBT, and x=0.0050,0.0075 or 0.0100；The ferroelectric material of ZnO and described Er doping mole Ratio is 0.1,0.2,0.3 or 0.4.
The preparation method of above-mentioned composite, comprises the following steps:
(1) xEr:BNTBT of Er doping is prepared: Er2O3、Bi2O3、NaCO3、TiO2And BaCO3Starting powder is according to change Learn proportioning, put into ball grinder and add dehydrated alcohol, by ball-milling method mix homogeneously；After drying mixed-powder is Celsius 900 Degree pre-burning 3 hours；After ball-milling method mix homogeneously drying, powder is sintered 3 hours at 1100 degrees Celsius, it is thus achieved that single The xEr:BNTBT powder of phase；
(2) step (1) preparation-obtained xEr:BNTBT powder is mixed homogeneously by ball-milling method with ZnO powder, wherein Mol ratio y of ZnO Yu xEr:BNTBT is 0.1,0.2,0.3 or 0.4；Under 950-1150 degree Celsius, 30-is sintered after pressed powder 90 minutes, it is thus achieved that fine and close xEr:BNTBT/yZnO composite ceramics.
The present invention uses Ferroelectric Composites as parent, the photoluminescent property of regulation and control rare earth Er ion, its useful effect Fruit is:
1, sample preparation methods is easy, efficiency is high, compared with traditional way changing doping host, and the method for the present invention Cost is relatively low, efficiency is high；
2, compared with the method not introducing ZnO formation composite ceramics, it is multiple that the inventive method uses Er:BNTBT and ZnO to constitute Closing pottery, composite ceramics can more effectively improve luminous intensity.Composite exciting at LASER Light Source prepared by the present invention Under, compared with the xEr:BNTBT one-component ceramic not having ZnO, composite ceramics middle rare earth Er ionic light photoluminescence obtains and is obviously enhanced, Intensification factor is up to 4.5 times.
Accompanying drawing explanation
Fig. 1 is xEr:BNTBT/yZnO composite ceramics sample (x=0.0100, the y=prepared in the inventive method 0.4) scanning electron microscope image.
Fig. 2 (a) for prepare xEr: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) for prepare xEr: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) for prepare xEr:BNTBT/yZnO composite ceramics sample (x=0.0100, y=0,0.1,0.2, 0.3,0.4) luminescence generated by light figure.
Detailed description of the invention
Embodiment 1: xEr:BNTBT (x=0.0050,0.0075,0.0100) powder is mixed with ZnO (y=0.1) powder Tabletting after uniformly, after 1150 degrees Celsius of sintering 90 minutes, it is thus achieved that xEr:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Light excites down, measures luminosity.
Embodiment 2: xEr:BNTBT (x=0.0050,0.0075,0.0100) powder is mixed with ZnO (y=0.2) powder Tabletting after uniformly, after 1050 degrees Celsius of sintering 90 minutes, it is thus achieved that xEr:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Light excites down, measures luminosity.
Embodiment 3: xEr:BNTBT (x=0.0050,0.0075,0.010) powder is mixed with ZnO (y=0.3) powder Tabletting after uniformly, after 1000 degrees Celsius of sintering 60 minutes, it is thus achieved that xEr:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Light excites down, measures luminosity.
Embodiment 4: xEr:BNTBT (x=0.0050,0.0075,0.010) powder is mixed with ZnO (y=0.4) powder Tabletting after uniformly, after 950 degrees Celsius of sintering 30 minutes, it is thus achieved that xEr:BNTBT/yZnO composite ceramics；Above-mentioned sample is being swashed Light excites down, measures luminosity.
Test result:
Fig. 1 is the scanning electron of xEr:BNTBT/yZnO composite ceramics sample (x=0.0100, y=0.4) prepared MIcrosope image.It can be seen that ZnO particle independence mutually and being present in Er:BNTBT substrate, constitute 0-3 type composite ceramic Porcelain.The composition of other y ≠ 0 all has this microstructure features.
Fig. 2 (a) for prepare xEr: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 xEr:BNTBT/yZnO composite ceramics sample (x=0.0075, the y prepared =0.1,0.2,0.3,0.4) luminescence generated by light figure, Fig. 2 (c) is the xEr:BNTBT/yZnO composite ceramics sample (x prepared =0.0100, y=0,0.1,0.2,0.3,0.4) luminescence generated by light figure.It will be seen that along with the increase of ZnO content (y value), pottery The luminous intensity of porcelain sample all dramatically increases, and compared with not having ZnO (y=0), the increase multiple of luminous intensity is up to 4.5 times.
As it has been described above, the inventive method uses Er:BNTBT and ZnO to constitute the composite ceramics of 0-3 type, at LASER Light Source Exciting down, compared with the xEr:BNTBT one-component ceramic not having ZnO, the luminescence generated by light of composite ceramics middle rare earth Er ion obtains Being obviously enhanced, intensification factor is up to 4.5 times, and this is most important to the application realizing rear-earth-doped ferroelectric material.The sample of the present invention Product preparation method is easy, efficiency is high.

Claims (4)

1.一种增强稀土Er离子光致发光的复合材料，包括Er掺杂的铁电材料以及ZnO，其特征在于，Er掺杂的铁电材料的化学式为xEr:0.94Bi0.5Na0.5TiO3-0.06BaTiO3，简写为xEr:BNTBT，其中x为Er与BNTBT的摩尔比，且x＝0.0050、0.0075或0.0100；ZnO与所述Er掺杂的铁电材料的摩尔比为0.1、0.2、0.3或0.4。1. A composite material for enhancing the photoluminescence of rare earth Er ions, including Er-doped ferroelectric material and ZnO, characterized in that, the chemical formula of Er-doped ferroelectric material is xEr:0.94Bi 0.5 Na 0.5 TiO 3 - 0.06BaTiO 3 , abbreviated as xEr:BNTBT, wherein x is the molar ratio of Er to BNTBT, and x=0.0050, 0.0075 or 0.0100; the molar ratio of ZnO to the Er-doped ferroelectric material is 0.1, 0.2, 0.3 or 0.4. 2.如权利要求1所述一种增强稀土Er离子光致发光的复合材料的制备方法，其特征在于，包括以下步骤：2. a kind of preparation method that strengthens the composite material of rare earth Er ion photoluminescence as claimed in claim 1, is characterized in that, comprises the following steps: (1)制备Er掺杂的xEr:BNTBT：把Er2O3、Bi2O3、NaCO3、TiO2和BaCO3原始粉末按照化学配比，混合均匀；烘干后将混合粉末在900摄氏度预烧3小时；再次通过球磨法混合均匀并烘干后，将粉末在1100摄氏度烧结3小时，获得单相的xEr:BNTBT粉末；(1) Preparation of Er-doped xEr:BNTBT: Mix the original powders of Er 2 O 3 , Bi 2 O 3 , NaCO 3 , TiO 2 and BaCO 3 according to the stoichiometric ratio; Pre-sintered for 3 hours; after mixing again by ball milling and drying, the powder was sintered at 1100 degrees Celsius for 3 hours to obtain single-phase xEr:BNTBT powder; (2)将步骤(1)所制备得到的xEr:BNTBT粉末与ZnO粉末混合均匀，其中ZnO与xEr:BNTBT的摩尔比y为0.1、0.2、0.3或0.4；粉末压片后在950-1150摄氏度下烧结30-90分钟，获得致密的xEr:BNTBT/yZnO复合陶瓷。(2) Mix the xEr:BNTBT powder prepared in step (1) with ZnO powder evenly, wherein the molar ratio y of ZnO to xEr:BNTBT is 0.1, 0.2, 0.3 or 0.4; Sintering at lower temperature for 30-90 minutes to obtain dense xEr:BNTBT/yZnO composite ceramics. 3.根据权利要求2所述的制备方法，其特征在于，所述步骤(1)中，将原始粉末放入球磨罐并加入无水乙醇，通过球磨法混合均匀。3. The preparation method according to claim 2, characterized in that, in the step (1), the original powder is put into a ball mill jar and added with absolute ethanol, and mixed uniformly by ball milling. 4.根据权利要求2所述的制备方法，其特征在于，所述步骤(2)中，xEr:BNTBT粉末与ZnO粉末通过球磨法混合均匀。4. The preparation method according to claim 2, characterized in that, in the step (2), xEr:BNTBT powder and ZnO powder are mixed uniformly by ball milling.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108341667A (en) * 2018-03-30 2018-07-31 常州大学 A kind of preparation method of nanocube 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
BIN HUE ET AL.: "Photoluminescence and Temperature Dependent Electrical Properties of Er-Doped 0.94 Bi0.5N0.5TiO3-0.06BaTiO3 Ceramics", 《J.AM.CERAM.SOC》 *
JI ZHANG ET AL.: "Semiconductor/relaxor 0-3 type composites without thermal depolarization in Bi0.5Na0.5TiO3-based lead-free piezoceramics", 《NATURE COMMUNICATIONS》 *
JI ZHANG ET AL.: "Temperature dependent structures and properties of Bi0.5Na0.5TiO3-based lead free piezoelectric composite", 《DALTON TRANSACTIONS》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108341667A (en) * 2018-03-30 2018-07-31 常州大学 A kind of preparation method of nanocube ferroelectric material
CN108341667B (en) * 2018-03-30 2020-10-02 常州大学 A kind of preparation method of nano-cube 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

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