CN106967411A - 一种GdAP:Tb3+绿色荧光粉的助熔剂 - Google Patents

一种GdAP:Tb3+绿色荧光粉的助熔剂 Download PDF

Info

Publication number
CN106967411A
CN106967411A CN201710235212.1A CN201710235212A CN106967411A CN 106967411 A CN106967411 A CN 106967411A CN 201710235212 A CN201710235212 A CN 201710235212A CN 106967411 A CN106967411 A CN 106967411A
Authority
CN
China
Prior art keywords
fluxing agent
gdap
emitting phosphor
green emitting
nacl
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710235212.1A
Other languages
English (en)
Other versions
CN106967411B (zh
Inventor
张正阳
李金凯
刘宗明
段广彬
操振涛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Jinan
Original Assignee
University of Jinan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Jinan filed Critical University of Jinan
Priority to CN201710235212.1A priority Critical patent/CN106967411B/zh
Publication of CN106967411A publication Critical patent/CN106967411A/zh
Application granted granted Critical
Publication of CN106967411B publication Critical patent/CN106967411B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7774Aluminates
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7781Sulfates

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Luminescent Compositions (AREA)

Abstract

本发明涉及一种GdAP:Tb3+绿色荧光粉的助熔剂,属于稀土发光材料领域。本发明所涉及助熔剂其主要成分包含NaCl、Na2SO4、NaCl和Na2SO4的混合物,通过调整NaCl和Na2SO4的混合物的配比,找到了一组最适宜于GdAP:Tb3+绿色荧光粉的助熔剂,通过添加本发明所涉及的助熔剂后,所制备出的绿色荧光粉具有颗粒大小均匀、分散性良好且荧光性能优异等优点。

Description

一种GdAP:Tb3+绿色荧光粉的助熔剂
技术领域
本发明涉及一种应用于照明领域的绿色荧光粉,尤其涉及到一种GdAP:Tb3+绿色荧光粉的助熔剂。
背景技术
钙钛矿相(GdAlO3)荧光粉因其具有结构稳定、成相温度低且性能优异等优点而广泛应用于照明、显示等领域。随着社会的需求的不断增加,制造出荧光性能优异的钙钛矿相荧光粉也显得尤为重要。
在合成高品质的发光材料时,往往需要添加适量的助熔剂以控制晶粒的生产,使其结晶性更加完美,而不同配比和种类的助熔剂对荧光粉的性能也会产生不同的影响,因此选择适合的助熔剂对荧光粉具有重要的意义。
发明内容
本发明主要涉及一种GdAP:Tb3+绿色荧光粉的助熔剂,通过不断调整其配比和组合,找到了一组最适宜于GdAP:Tb3+绿色荧光粉的助熔剂组合。选用本发明所选的助熔剂制得的荧光粉具有颗粒大小均匀、分散性良好、荧光性能优异等优点。
一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于:
(1)所加入的助熔剂种类为NaCl、Na2SO4、NaCl和Na2SO4的混合物;
(2)所加入的助熔剂的量为:助熔剂/前驱体质量比为1:1~3:1;
(3)运用碳酸氢铵共沉淀技术制备得到前驱体后加入助熔剂与之混合,经煅烧后得到荧光性能优异的绿色荧光粉。
附图说明
图1为本发明的实施例1所得的荧光粉的X射线衍射图。
图2为本发明的实施例1-3所得的荧光粉的发射光谱图,激发波长为275nm。
图3为本发明的实施例1、4、5、6所得的荧光粉的发射光谱图,激发波长为275nm。
具体实施方式
实施例1
(1)将稀土氧化物Gd2O3、Tb4O7溶于热硝酸配制成稀土硝酸盐溶液(其浓度分别为0.5mol/L和0.1mol/L),将Al(NO3)3·9H2O溶解在去离子水中制成Al(NO3)3溶液(浓度为0.5mol/L);
(2)按Gd:Tb:Al=0.9:0.1:1称取步骤(1)的溶液(其中Gd(NO3)3所用量为8.1mM),加去离子水到100ml,搅拌均匀得母盐溶液;
(3)称取适量碳酸氢铵溶于去离子水(所得溶液浓度为1.125mol/L,所用量为160ml),并在25℃恒温下将母盐溶液滴加到沉淀剂中,待滴加结束后时效处理30min得到前驱体溶液;
(4)将步骤(3)中溶液进行离心、水洗并在80℃下烘干6 h得到荧光粉的前驱体;
(5)将步骤(4)中的前驱体均匀分散在适量的无水乙醇中,然后加入5%NaCl和95%Na2SO4,超声分散,待溶液均匀后放入80℃烘箱中烘干;
(6)将步骤(5)中得到的前驱体粉末在600℃空气气氛下进行煅烧,去除粉体里面所含的碳酸根等杂质离子,接着在1300℃通混合气体煅烧还原4 h得到最终的产物。
实施例1所得的荧光粉的X射线衍射图如图1所示。
实施例2
为了和实施例1形成对比,本实施把实施例1步骤(5)助熔剂换成7%NaCl和93%Na2SO4其余步骤与实施例1相同。
实施例3
为了和实施例1形成对比,本实施把实施例1步骤(5)助熔剂换成3%NaCl和97%Na2SO4其余步骤与实施例1相同。
实施例1-3所得的荧光粉的发射光谱图如图2所示。
实施例4
为了和实施例1形成对比,本实施把实施例1步骤(5)添加助熔剂这一步去掉其余步骤与实施例1相同。
实施例5
为了和实施例1形成对比,本实施把实施例1步骤(5)助熔剂换成NaCl其余步骤与实施例1相同。
实施例6
为了和实施例1形成对比,本实施把实施例1步骤(5)助熔剂换成Na2SO4其余步骤与实施例1相同。
实施例1、4、5、6所得的荧光粉的发射光谱图如图3所示。

Claims (6)

1.一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于:所加入的助熔剂种类为NaCl、Na2SO4、NaCl和Na2SO4的混合物。
2.一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于:所加入的助熔剂的量为:助熔剂/前驱体质量比为1:1~3:1。
3.一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于:运用碳酸氢铵共沉淀技术制备得到前驱体后加入助熔剂与之混合,经煅烧后得到荧光性能优异的绿色荧光粉。
4.如权利要求1所述的一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于,最适合GdAP:Tb3+荧光粉的种类为NaCl和Na2SO4的混合物,其最佳配比为5wt%NaCl和95wt%Na2SO4
5.如权利要求2所述的一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于,所加入的助熔剂的量最佳配比为:助熔剂/前驱体质量比为2:1。
6.如权利要求3所述的一种GdAP:Tb3+绿色荧光粉的助熔剂,其特征在于,将前驱体均匀分散在适量的无水乙醇中,然后加入适量配比的不同种类的助熔剂,超声分散,待溶液均匀后放入80℃烘箱中烘干,然后经煅烧得到荧光粉。
CN201710235212.1A 2017-04-12 2017-04-12 一种GdAP:Tb3+绿色荧光粉的助熔剂 Active CN106967411B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710235212.1A CN106967411B (zh) 2017-04-12 2017-04-12 一种GdAP:Tb3+绿色荧光粉的助熔剂

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710235212.1A CN106967411B (zh) 2017-04-12 2017-04-12 一种GdAP:Tb3+绿色荧光粉的助熔剂

Publications (2)

Publication Number Publication Date
CN106967411A true CN106967411A (zh) 2017-07-21
CN106967411B CN106967411B (zh) 2019-08-06

Family

ID=59336699

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710235212.1A Active CN106967411B (zh) 2017-04-12 2017-04-12 一种GdAP:Tb3+绿色荧光粉的助熔剂

Country Status (1)

Country Link
CN (1) CN106967411B (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108330541A (zh) * 2018-01-19 2018-07-27 暨南大学 一种gyap激光晶体及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1528859A (zh) * 2003-10-09 2004-09-15 中国科学院上海硅酸盐研究所 钙钛矿型铝酸钆基荧光粉体及制备方法
CN1900216A (zh) * 2005-07-22 2007-01-24 北京大学 一种制备稀土激活的铝酸锶长余辉荧光粉的方法
CN105062482A (zh) * 2015-08-28 2015-11-18 东南大学 一种制备小粒径铈激活钇铝石榴石荧光粉的方法
CN106554033A (zh) * 2015-09-24 2017-04-05 中国科学院上海硅酸盐研究所 采用熔盐法制备铝酸镧粉体的方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1528859A (zh) * 2003-10-09 2004-09-15 中国科学院上海硅酸盐研究所 钙钛矿型铝酸钆基荧光粉体及制备方法
CN1900216A (zh) * 2005-07-22 2007-01-24 北京大学 一种制备稀土激活的铝酸锶长余辉荧光粉的方法
CN105062482A (zh) * 2015-08-28 2015-11-18 东南大学 一种制备小粒径铈激活钇铝石榴石荧光粉的方法
CN106554033A (zh) * 2015-09-24 2017-04-05 中国科学院上海硅酸盐研究所 采用熔盐法制备铝酸镧粉体的方法

Non-Patent Citations (10)

* Cited by examiner, † Cited by third party
Title
CHIEN-TUNG LIU 等: "THE STRUCTURE AND HIGH TEMPERATURE CORROSION PROPERTIES OF CHROMIZED COATINGS", 《SURFACE AND COATINGS TECHNOLOGY》 *
H.H.S. OLIVEIRA 等: "Structural and optical properties of GdAlO3:RE3+ (RE = Eu or Tb) prepared by the Pechini method for application as X-ray phosphors", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
JOO-SIN LEE: "Molten salt synthesis of gadolinium aluminate powders", 《JOURNAL OF CERAMIC PROCESSING RESEARCH》 *
JOO-SIN LEE: "Molten salt synthesis of YAlO3 powders", 《MATERIALS SCIENCE-POLAND》 *
王瑞萍 等: "LnAlO3中Ce3+,Tb3+,Dy3+的发光及Ce-Tb,Ce-Dy的敏化发光(Ln=La,Gd,Y)", 《发光学报》 *
罗岚 等: "GdAlO3:Tb,RE中Tb,RE 的能量传递研究", 《影像科学与光化学》 *
虞文奇: "熔盐法制备小粒径高光效YAG:Ce荧光粉", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
邓陶丽 等: "GdAlO3:Er3+,Yb3+荧光粉的制备与上转换发光性能", 《物理化学学报》 *
黄燕: "熔盐法制备Y2O3:Eu3+及YAG:Ce3+荧光粉新工艺研究", 《中国博士学位论文全文数据库 工程科技I辑》 *
黄燕: "熔盐法对红粉Y2O3:Eu3+表面性能改进的探讨", 《湖南理工学院学报(自然科学版)》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108330541A (zh) * 2018-01-19 2018-07-27 暨南大学 一种gyap激光晶体及其制备方法

Also Published As

Publication number Publication date
CN106967411B (zh) 2019-08-06

Similar Documents

Publication Publication Date Title
CN1318540C (zh) 一种蓝光激发的白色led用荧光粉及其制造方法
JP5932934B2 (ja) ミョウバン法によるアルミン酸塩発光体、bam,yag、及びcatを製造する方法
CN101338188B (zh) 一种具有高初始荧光强度的长余辉发光材料的制备方法
CN109021973A (zh) 一种双钙钛矿型钼酸盐红色荧光粉及其制备方法
CN105441079B (zh) 一种高强度uvb荧光粉及其制备方法
Han et al. Sol-gel synthesis of single phase, high quantum efficiency LiCaPO4: Eu2+ phosphors
CN106967411A (zh) 一种GdAP:Tb3+绿色荧光粉的助熔剂
CN109135744A (zh) 一种新型钨酸盐NaLaW2O7(OH)2(H2O)及其制备方法
CN107686730A (zh) 一种Tb3+掺杂钨酸盐新型绿色荧光粉
WO2014067113A1 (zh) 硅酸盐发光材料及其制备方法
CN105754596B (zh) 一种稀土掺杂的氟锆酸盐发光材料及其制备方法
CN104610965A (zh) 一种球形荧光粉的制备方法
Popovici et al. Synthesis and characterisation of europium activated yttrium oxide fine powders
US9416308B2 (en) Core-shell structured silicate luminescent material and preparation method therefor
Ji et al. Preparation and luminescent properties of nanocrystals of Ce3+-activated SrHfO3
CN104073252B (zh) ZnB2O4:Eu3+发光材料的制备方法
CN108559504A (zh) 一种高灵敏度荧光测温材料及其制备方法
CN102337122B (zh) 一种硅酸盐绿色荧光粉及其制备方法
CN104927856B (zh) 基于溶胶‑凝胶燃烧法制备钨酸盐红色荧光粉的方法
CN100503775C (zh) 一种CaSiO3:Eu3+纳米球形红色荧光粉的制备
CN103725283B (zh) 一种硅酸盐橙红色荧光粉的制备方法
CN106010528A (zh) 一种铋、锰掺杂的蓝色荧光粉及其制备方法和应用
CN107794042B (zh) 一种掺杂稀土元素Sm的磷钨酸盐发光材料及其制备方法
US8936733B2 (en) Borate luminescent materials, preparation methods and uses thereof
RU2567305C1 (ru) Способ получения сложного алюмината кальция-магния

Legal Events

Date Code Title Description
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB03 Change of inventor or designer information

Inventor after: Li Jinkai

Inventor after: Zhang Zhengyang

Inventor after: Liu Zongming

Inventor after: Duan Guangbin

Inventor after: Cao Zhentao

Inventor before: Zhang Zhengyang

Inventor before: Li Jinkai

Inventor before: Liu Zongming

Inventor before: Duan Guangbin

Inventor before: Cao Zhentao

CB03 Change of inventor or designer information
GR01 Patent grant
GR01 Patent grant