CN108059446A - 一种白光荧光陶瓷及其制备方法 - Google Patents
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Abstract
本发明提供一种白光荧光陶瓷及其制备方法,一种白光荧光陶瓷属于CaO‑SiO2‑B2O3‑MnO‑Ce2O3‑Tb2O3体系,其中,一种白光荧光陶瓷制备方法,包括以下步骤:(1)称取原料放入球磨机中混合均匀后,放入高温炉中,在1250℃~1350℃还原气氛条件下煅烧8~12小时,制得粉体;(2)将粉体和预混液混合,并放置于球磨机中球磨2~8小时,制得混合浆料;(3)在混合浆料中加入过硫酸铵,搅拌后,将混合浆料倒入模具中干燥24~48小时,制得生坯;(4)将生坯放入高温炉中,在1250℃~1350℃空气气氛条件下继续煅烧8~12小时,制得陶瓷片;(5)将陶瓷片打磨制得最终的陶瓷片;本方法操作简单,产品形状尺寸可调,并可批量制备,成品率高,所制得的白光荧光陶瓷可广泛用于大功率、远程LED、激光光源等领域。
Description
技术领域
本发明属于陶瓷技术领域,尤其涉及一种白光荧光粉及其制备方法和荧光陶瓷及其制备方法。
背景技术
白光发光二极管(white light emitting diodes,WLEDs)作为新一代固态照明器件,具有节能、环保、响应快、体积小等优点,目前已广泛地应用于道路照明、平板显示等领域。白光LED实现白光发射最成熟的方式是荧光粉转换法,即在LED芯片周围包覆荧光粉,目前商用白光LED普遍采用蓝光LED芯片激发YAG:Ce3+黄色荧光粉的组合方案。但这种组合方案获得的白光中由于缺少红光组分,导致光源的显色指数偏低[1,2]。另一种较为常见的方式是紫外LED芯片结合三色(红+绿+蓝)荧光粉制备的WLEDs,在此***中红光的加入明显改善了显色指数,但同时也引入了其他问题,比如红光和绿光荧光粉对蓝光的强吸收效应导致蓝光荧光粉发光效率变低,三种荧光粉不同的衰变速率会产生色差,此外制备工艺复杂化使成本变高。这些不足在实际应用中都是不容忽视的。与多组分白光荧光粉相比,单相白光发射荧光粉具有更高的发光效率、优良的显色指数、更好的稳定性和色彩表现力,在制备工艺方面也比较简单,所以单相白光荧光粉已成为近年来WLEDs用荧光粉研究的一个热点。
然而在将单相白光荧光粉封装为LED器件后,在使用过程中,在无法将吸收能量尽快通过发射光释放的情况下,荧光粉会通过非辐射放热,这就会使得器件温度不断升高,导致树脂和硅胶老化,裂解,黄变,同时又令荧光粉因为热衰而降低效率,最终陷入恶性循环。因此研制开发满足可被紫外芯片激发并可承受高能量激发和高密度的荧光材料是LED技术发展过程亟需解决的重大问题。
有鉴于此,特提出本发明。
发明内容
针对现有技术中存在的问题,本发明的目的是提供一种白光荧光粉及其制备方法和荧光陶瓷及其制备方法,制备工艺简单,成本低,固含量高,成品率高,采用远程封装的方式,光源散热效果好,提高了光源的可靠性,适用范围广,适合工厂模式化批量生产。
为了实现上述目的,本发明提供的一种白光荧光陶瓷及其制备方法,所述白光荧光陶瓷属于CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系。
优选地,一种白光荧光陶瓷的制备方法,包括以下步骤:
(1)制备白光荧光粉:称取组分比例(以氧化基准的质量计)为:0%≤CaO+SrO+BaO≤77.92%,0%<SiO2≤69.99%,0%<B2O3≤13.69%,0%<CeO2≤17.72%,0%<MnO≤4.04%,且0%<Tb2O3≤7.93%的原料放入球磨机中球磨2~8小时混合均匀后,放入高温炉中,在1250℃~1350℃还原气氛条件(白光荧光粉的还原和烧结是同时进行的,即还原气氛温度等于烧结气氛温度)下煅烧8~12小时,制得白光荧光粉;
(2)凝胶注模:将质量比为1000:173的白光荧光粉和预混液混合,所述的预混液的各组分比例为(以质量百分比计),0%<H2O<88.3%,0%<N,N二甲基丙烯酰胺<59.1%,0%<N,N’-亚甲基双丙酰胺<3.1%,0%<聚丙烯酸铵<30.7%,0%<聚乙二醇<7.1%,并放置于滚筒式球磨机中球磨24~48小时,制得混合浆料;
(3)在混合浆料中加入引发剂过硫酸铵,所述引发剂的添加量占预混合液的质量百分比为,0%<过硫酸铵<2.3%,搅拌后,将混合浆料倒入模具中干燥24~48小时,制得生坯;
(4)将生坯放入高温炉中,在1250℃-1350℃还原气氛条件下继续煅烧8~12小时,制得陶瓷片;
(5)将陶瓷片打磨制得最终的陶瓷片。
优选地,在所述步骤(2)球磨结束之前30min向浆料中加入催化剂N,N,N,N-四甲基乙二胺。
优选地,催化剂添加量占预混合液的质量百分比为,0%<N,N,N,N-四甲基乙二胺<0.37%。
本发明提供的,具有如下有益效果:
1.采用凝胶注模工艺将白光荧光粉进行陶瓷化,具有更高的发光效率、优良的显色指数、更好的稳定性和色彩表现力,同时制备工艺简单,成本低,固含量高,成品率高,适合于工业模式化大规模、批量化生产,适合广泛应用推广。
2.本发明采用远程荧光粉,使荧光粉制得陶瓷和芯片分离,有利于光源的散热,进而提升光源的可靠性,可承受高密度和高能量激发,不会出现荧光粉通过非辐射放热,器件温度过高导致树脂和硅胶老化等,又令荧光粉因热衰降低效率的恶性循环,可用于大功率照明器件中,如激光光源、大功率远程LED光源。
附图说明
图1为一种本发明提供的一种白光荧光陶瓷的白光荧光粉的激发波长为338nm的发射光谱。
具体实施方式
下面结合具体实施例和附图对本发明做进一步说明,以助于理解本发明的内容。
实施例1:
本发明提供的一种白光荧光陶瓷及其制备方法,一种白光荧光陶瓷属于CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系;
其中,一种白光荧光陶瓷的制备方法,包括以下步骤:
1.白光荧光粉制备:按照CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3=59.78﹕24.91﹕7.22﹕4.04﹕1.96﹕2.09(以氧化物含量计)的组分比例,准确称取总质量为100g的药品,其中CaCO368.86g,SiO2 16.03g,H3BO3 8.25g,MnCO3 4.22g,CeO2 1.26g,Tb4O7 1.37g,置于球磨机中球磨4h后,转入到马弗炉中1250℃保温8h,冷却至室温,得到白光荧光粉。
2.凝胶注模:以质量比计,白光荧光粉:预混液:引发剂:催化剂=1000:173:4:0.64,将白光荧光粉100g和预混液17.3g(其中预混液中各组分分别为:去离子水13g,N,N二甲基丙烯酰胺2.52g,N,N’-亚甲基双丙酰胺0.15g,聚丙烯酸铵1.32g,聚乙二醇0.31g)混合,首次在预混液中加入白光荧光粉质量为60g,球磨24h后分两次各加入20g,并在球磨结束之前30min向浆料中加入催化剂N,N,N,N-四甲基乙二胺0.064g。
3.将球磨之后的浆料倒入烧杯中,向其中加入0.4g引发剂过硫酸铵,并轻轻搅拌,将浆料通过80目的不锈钢筛网过滤浆料中的气泡,然后迅速将浆料倒入预先准备的模具中,之后静置约10h后,放在烘箱中50℃干燥4h,脱模,并继续干燥12h。
4.将干燥后的坯体放在马弗炉在1250℃还原气氛下煅烧12h,冷却取出后即得到CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系的远程白光荧光陶瓷。
5.将荧光陶瓷片进行打磨得到最终的远程白光荧光陶瓷。
本发明使用型号为F-7000的荧光光谱仪,测试该体系荧光陶瓷的光谱性质,如图1所示,该体系荧光陶瓷在338nm光激发下,发射出色坐标位于(.0.289,0.250)的白光,其中,红光波段位于623nm~750nm,中心波长位于673nm,绿光波段位于位于479nm~623nm,中心波长位于544nm,蓝光波段位于350nm~479nm,中心波长位于398nm。
实施例2:
本发明提供的一种白光荧光陶瓷及其制备方法,一种白光荧光陶瓷属于CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系;
其中,一种白光荧光陶瓷的制备方法,包括以下步骤:
1.白光荧光粉制备:按照CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3=58.43﹕24.48﹕7.09﹕3.97﹕1.93﹕4.10(以氧化物含量计)的组分比例,准确称取总质量为100g的药品,其中CaCO367.87g,SiO2 15.85g,H3BO3 8.15,MnCO3 4.17g,CeO21.25g,Tb4O7 2.71g,置于球磨机中球磨2h后,转入到马弗炉中1250℃保温8h,冷却至室温,得到白光荧光粉。
2.凝胶注模:以质量比计,白光荧光粉:预混液:引发剂:催化剂=1000:173:4:0.64,将白光荧光粉100g和预混液17.3g(其中预混液中各组分分别为:去离子水7.82g,N,N二甲基丙烯酰胺5.33g,N,N’-亚甲基双丙酰胺0.47g,聚丙烯酸铵2.87g,聚乙二醇0.81g)混合,首次在预混液中加入白光荧光粉质量为60g,球磨26h后分两次各加入20g,并在球磨结束之前30min向浆料中加入催化剂N,N,N,N-四甲基乙二胺0.064g。
3.将球磨之后的浆料倒入烧杯中,向其中加入0.4g引发剂过硫酸铵,并轻轻搅拌,将浆料通过80目的不锈钢筛网过滤浆料中的气泡,然后迅速将浆料倒入预先准备的模具中,之后静置约10h后,放在烘箱中50℃干燥4h,脱模,并继续干燥12h。
4.将干燥后的坯体放在马弗炉在1250℃还原气氛下煅烧8h,冷却取出后即得到CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系的远程白光荧光陶瓷。
5.将荧光陶瓷片进行打磨得到最终的远程白光荧光陶瓷。
本发明使用型号为F-7000的荧光光谱仪,测试该体系荧光陶瓷的光谱性质,如图1所示,该体系荧光陶瓷在338nm光激发下,发射出色坐标位于(0.288,0.278)的白光,其中,红光波段位于623nm~750nm,中心波长位于673nm,绿光波段位于位于479nm~623nm,中心波长位于544nm,蓝光波段位于350nm~479nm,中心波长位于399nm。
实施例3:本发明提供的一种白光荧光陶瓷及其制备方法,一种白光荧光陶瓷属于CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系;
其中,一种白光荧光陶瓷的制备方法,包括以下步骤:
1.白光荧光粉制备:按照CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3=57.12﹕24.06﹕6.97﹕3.90﹕1.90﹕6.04(以氧化物含量计)的组分比例,准确称取总质量为100g的药品,其中CaCO366.90g,SiO2 15.66g,H3BO3 8.06g,MnCO3 4.12g,CeO2 1.24g,Tb4O7 4.02g,置于球磨机中球磨6h后,转入到马弗炉中1250℃保温10h,冷却至室温,得到白光荧光粉。
2.凝胶注模:以质量比计,白光荧光粉:预混液:引发剂:催化剂=1000:173:4:0.64,将白光荧光粉100g和预混液17.3g(其中预混液中各组分分别为:去离子水15.22g,N,N二甲基丙烯酰胺0.21g,N,N’-亚甲基双丙酰胺0.52g,聚丙烯酸铵0.14g,聚乙二醇1.21g)混合,首次在预混液中加入白光荧光粉质量为60g,球磨36h后分两次各加入20g,并在球磨结束之前30min向浆料中加入催化剂N,N,N,N-四甲基乙二胺0.064g。
3.将球磨之后的浆料倒入烧杯中,向其中加入0.4g引发剂过硫酸铵,并轻轻搅拌,将浆料通过80目的不锈钢筛网过滤浆料中的气泡,然后迅速将浆料倒入预先准备的模具中,之后静置约10h后,放在烘箱中50℃干燥4h,脱模,并继续干燥12h。
4.将干燥后的坯体放在马弗炉在1250℃还原气氛下煅烧10h,冷却取出后即得到CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系的远程白光荧光陶瓷。
5.将荧光陶瓷片进行打磨得到最终的远程白光荧光陶瓷。
本发明使用型号为F-7000的荧光光谱仪,测试该体系荧光陶瓷的光谱性质,如图1所示,该体系荧光陶瓷在338nm光激发下,发射出色坐标位于(0.303,0.309)的白光,其中,红光波段位于623nm~750nm,中心波长位于673nm,绿光波段位于位于477nm~623nm,中心波长位于544nm,蓝光波段位于350nm~477nm,中心波长位于397nm。
实施例4:本发明提供的一种白光荧光陶瓷及其制备方法,一种白光荧光陶瓷属于CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系;
其中,一种白光荧光陶瓷的制备方法,包括以下步骤:
1.白光荧光粉制备:按照CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3=55.86﹕23.66﹕6.85﹕3.84﹕1.86﹕7.93(以氧化物含量计)的组分比例,准确称取总质量为100g的药品,其中CaCO365.96g,SiO2 15.48g,H3BO3 7.97g,MnCO3 4.07g,CeO2 1.22g,Tb4O7 5.30g,置于球磨机中球磨8h后,转入到马弗炉中1250℃保温12h,冷却至室温,得到白光荧光粉。
2.凝胶注模:以质量比计,白光荧光粉:预混液:引发剂:催化剂=1000:173:4:0.64,将白光荧光粉100g和预混液17.3g(其中预混液中各组分分别为:去离子水1.38g,N,N二甲基丙烯酰胺10.16g,N,N’-亚甲基双丙酰胺0.12g,聚丙烯酸铵5.29g,聚乙二醇0.35g)混合,首次在预混液中加入白光荧光粉质量为60g,球磨48h后分两次各加入20g,并在球磨结束之前30min向浆料中加入催化剂N,N,N,N-四甲基乙二胺0.064g。
3.将球磨之后的浆料倒入烧杯中,向其中加入0.4g引发剂过硫酸铵,并轻轻搅拌,将浆料通过80目的不锈钢筛网过滤浆料中的气泡,然后迅速将浆料倒入预先准备的模具中,之后静置约10h后,放在烘箱中50℃干燥4h,脱模,并继续干燥12h。
4.将干燥后的坯体放在马弗炉在1250℃还原气氛下煅烧12h,冷却取出后即得到CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系的远程白光荧光陶瓷。
5.将荧光陶瓷片进行打磨得到最终的远程白光荧光陶瓷。
本发明使用型号为F-7000的荧光光谱仪,测试该体系荧光陶瓷的光谱性质,如图1所示,该体系荧光陶瓷在338nm光激发下,发射出色坐标位于(0.317,0.316)的白光,其中,红光波段位于623nm~750nm,中心波长位于673nm,绿光波段位于位于478nm~623nm,中心波长位于544nm,蓝光波段位于350nm~478nm,中心波长位于397nm。
本发明提供的一种白光荧光陶瓷及其制备方法,荧光陶瓷可用于大功率照明器件中,如激光光源、大功率远程LED光源。采用远程封装方式,使荧光粉材料和芯片分离,有利于光源的散热,进而提升光源的可靠性。
本文中应用了具体个例对发明构思进行了详细阐述,以上实施例的说明只是用于帮助理解本发明的核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离该发明构思的前提下,所做的任何显而易见的修改、等同替换或其他改进,均应包含在本发明的保护范围之内。
Claims (4)
1.一种白光荧光陶瓷,其特征在于,所述白光荧光陶瓷属于CaO-SiO2-B2O3-MnO-Ce2O3-Tb2O3体系。
2.根据权利要求1所述的一种白光荧光陶瓷的制备方法,其特征在于,包括以下步骤:
(1)制备白光荧光粉:称取组分比例(以氧化基准的质量计)为:0%≤CaO+SrO+BaO≤77.92%,0%<SiO2≤69.99%,0%<B2O3≤13.69%,0%<CeO2≤17.72%,0%<MnO≤4.04%,且0%<Tb2O3≤7.93%的原料放入球磨机中球磨2-~8小时混合均匀后,放入高温炉中,在1250℃~1350℃还原气氛条件下煅烧8~12小时,制得白光荧光粉;
(2)凝胶注模:将质量比为1000:173的白光荧光粉和预混液混合,所述的预混液的各组分比例为(以质量百分比计),0%<H2O<88.3%,0%<N,N二甲基丙烯酰胺<59.1%,0%<N,N’-亚甲基双丙酰胺<3.1%,0%<聚丙烯酸铵<30.7%,0%<聚乙二醇<7.1%,并放置于滚筒式球磨机中球磨24~48小时,制得混合浆料;
(3)在混合浆料中加入引发剂过硫酸铵,所述引发剂的添加量占预混液的质量百分比为,0%<过硫酸铵<2.3%,搅拌后,将混合浆料倒入模具中干燥24~48小时,制得生坯;
(4)将生坯放入高温炉中,在1250℃-1350℃还原气氛条件下继续煅烧8~12小时,制得陶瓷片;
(5)将陶瓷片打磨制得最终的陶瓷片。
3.根据权利要求1所述的一种荧光陶瓷的制备方法,其特征在于,在所述步骤(2)球磨结束之前30min向浆料中加入催化剂N,N,N,N-四甲基乙二胺。
4.根据权利要求1所述的一种荧光陶瓷的制备方法,其特征在于,催化剂添加量占预混合液的质量百分比为,0%<N,N,N,N-四甲基乙二胺<0.37%。
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116161954A (zh) * | 2023-02-28 | 2023-05-26 | 东莞科伏精密制造有限公司 | 一种高强度熔融石英陶瓷的制备方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102807863A (zh) * | 2011-06-03 | 2012-12-05 | 三星电子株式会社 | 硅酸盐磷光体及其制造方法和光产生装置 |
CN103980889A (zh) * | 2014-04-30 | 2014-08-13 | 广东工业大学 | 一种硅酸盐基多色长余辉发光材料及其制备方法 |
CN105038787A (zh) * | 2015-07-01 | 2015-11-11 | 上海应用技术学院 | 一种铈、铽、锰共激活的单基质磷酸盐白光荧光粉及其制备方法 |
CN107266046A (zh) * | 2017-06-26 | 2017-10-20 | 江门市凯昌科技发展有限公司 | 一种氧化铝荧光陶瓷片及其制备方法和应用 |
-
2018
- 2018-01-10 CN CN201810024176.9A patent/CN108059446A/zh active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102807863A (zh) * | 2011-06-03 | 2012-12-05 | 三星电子株式会社 | 硅酸盐磷光体及其制造方法和光产生装置 |
CN103980889A (zh) * | 2014-04-30 | 2014-08-13 | 广东工业大学 | 一种硅酸盐基多色长余辉发光材料及其制备方法 |
CN105038787A (zh) * | 2015-07-01 | 2015-11-11 | 上海应用技术学院 | 一种铈、铽、锰共激活的单基质磷酸盐白光荧光粉及其制备方法 |
CN107266046A (zh) * | 2017-06-26 | 2017-10-20 | 江门市凯昌科技发展有限公司 | 一种氧化铝荧光陶瓷片及其制备方法和应用 |
Non-Patent Citations (2)
Title |
---|
潘裕柏等: "《稀土陶瓷材料》", 31 May 2016, 冶金工业出版社 * |
王锦高著: "《半导体照明LED白光荧光粉论文集:2005-2012》", 31 January 2013, 厦门:厦门大学出版社 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116161954A (zh) * | 2023-02-28 | 2023-05-26 | 东莞科伏精密制造有限公司 | 一种高强度熔融石英陶瓷的制备方法 |
CN116161954B (zh) * | 2023-02-28 | 2023-12-12 | 东莞科伏精密制造有限公司 | 一种高强度熔融石英陶瓷的制备方法 |
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