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利用乳糖酸的钝化效应提升K2SiF6∶Mn4+的耐湿性
发光产业及技术前沿 | 更新时间：2022-10-19
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利用乳糖酸的钝化效应提升K2SiF6∶Mn4+的耐湿性 增强出版
- Improving Moisture Resistance of K2SiF6∶Mn4+
via Passivation Effect of Lactobionic Acid - 发光学报 2022年 43卷 第8期 (2022)
- 作者机构：湖南师范大学 化学化工学院,湖南,长沙,410081;湖南普斯赛特光电科技有限公司,湖南,长沙,410116
- 作者简介：
- 基金信息：长沙市自然科学基金(kq2202235);化学生物学及中药分析教育部重点实验室开放基金（KLCBTCMR20‐23）资助项目
- DOI：10.37188/CJL.20220127 中图分类号： O611.3
纸质出版日期：2022-08-05，
收稿日期：2022-04-09，
修回日期：2022-04-23，
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引用本文
万萍萍,杨静,刘红秀等.利用乳糖酸的钝化效应提升K2SiF6∶Mn4+的耐湿性[J].发光学报,2022,43(08):1300-1308.
WAN Ping-ping,YANG Jing,LIU Hong-xiu,et al.Improving Moisture Resistance of K2SiF6∶Mn4+via Passivation Effect of Lactobionic Acid[J].Chinese Journal of Luminescence,2022,43(08):1300-1308.
万萍萍,杨静,刘红秀等.利用乳糖酸的钝化效应提升K2SiF6∶Mn4+的耐湿性[J].发光学报,2022,43(08):1300-1308. DOI： 10.37188/CJL.20220127.
WAN Ping-ping,YANG Jing,LIU Hong-xiu,et al.Improving Moisture Resistance of K2SiF6∶Mn4+via Passivation Effect of Lactobionic Acid[J].Chinese Journal of Luminescence,2022,43(08):1300-1308. DOI： 10.37188/CJL.20220127.
利用乳糖酸的钝化效应提升K2SiF6∶Mn4+的耐湿性 增强出版
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"data": "的氟化物惰性壳层，以提升其耐湿性。结果表明，经乳糖酸钝化后的氟化物的晶相、形貌及发光强度几乎不变。水浸360 h后，钝化的氟化物的内量子效率为96.9%，远高于未处理的氟化物的59.8%。经乳糖酸处理，水解后的氟化物的内量子产率可以恢复到98.8%。在60 mA驱动电流下，将钝化后的氟化物作为红光成分，封装了相关色温为3 518 K、显色指数为88.5、发光效率为130.61 lm·W"
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"data": "-free fluoride inert shell to improve its moisture resistance. The results show that the crystal phase， morphology and luminescence intensity of the passivated fluoride are almost unchanged. After 360 h of water immersion， the internal quantum efficiency of the passivated fluoride is 96.9%， which is much higher than that（59.8%） of the untreated fluoride. After treatment with lactobionic acid， the internal quantum yield of hydrolyzed fluoride can be recovered to 98.8%. At a driving current of 60 mA， a warm white LED with a correlated color temperature of 3 518 K， a color rendering index of 88.5， and a luminous efficiency of 130.61 lm·W"
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"data": " was encapsulated by using the passivated fluoride as the red-light component. After aging in a high temperature（85 ℃） and high humidity（85%） environment for 500 h， the LED device has high stability， and the luminous efficiency can maintain at 90.5% of the initial value， which is higher than that（82.3%） of white LED encapsulated with the untreated fluoride. Therefore， the simple lactobionic acid treatment can effectively improve the moisture resistance of Mn"
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"data": "掺杂的氟化物红色荧光粉可被蓝光高效激发、红光发射带超窄、量子效率高以及发光热猝灭温度高，已成为当前半导体照明（WLED）和广色域液晶显示LED背光用核心发光材料之一"
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"data": {
"data": [
{
"name": "xref",
"data": {
"text": "5",
"type": "bibr",
"rid": "R5",
"data": [
{
"name": "text",
"data": "5"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "11",
"type": "bibr",
"rid": "R11",
"data": [
{
"name": "text",
"data": "11"
}
]
}
}
],
"rid": [
"R5",
"R6",
"R7",
"R8",
"R9",
"R10",
"R11"
],
"text": "5-11",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。然而，氟化物的研究与应用仍然存在一些亟待解决的问题，主要包括：合成方法不环保、衰减寿命长、形貌控制难、耐湿性差。其中，耐湿性差易导致器件的发光颜色不稳定。因此，耐湿性差是氟化物荧光粉在高稳定性器件应用的一个瓶颈问题。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "氟化物红粉耐湿性差的关键原因在于表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "易被水解成不发光的氧化物和氢氧化物，体色变成棕色，量子效率显著降低"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "12",
"type": "bibr",
"rid": "R12",
"data": [
{
"name": "text",
"data": "12"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "13",
"type": "bibr",
"rid": "R13",
"data": [
{
"name": "text",
"data": "13"
}
]
}
}
],
"rid": [
"R12",
"R13"
],
"text": "12-13",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。沸水浸泡导致氟化物表面出现大量的细孔，归因于[MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "]"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2-"
}
]
},
{
"name": "text",
"data": "溶出所致"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "2",
"type": "bibr",
"rid": "R2",
"data": [
{
"name": "text",
"data": "2"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。比利时根特大学Smet教授课题组深入研究了K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "受温度和水解的影响"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "14",
"type": "bibr",
"rid": "R14",
"data": [
{
"name": "text",
"data": "14"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "15",
"type": "bibr",
"rid": "R15",
"data": [
{
"name": "text",
"data": "15"
}
]
}
}
],
"rid": [
"R14",
"R15"
],
"text": "14-15",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。由于Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的强氧化性，K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "易还原成KMnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "和K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "。Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "3+"
}
]
},
{
"name": "text",
"data": "在400~620 nm有较强的吸收，严重影响氟化物的发光效率。张勤远课题组研究发现，结构刚性高和溶解度低的氟化物基质具有更高的耐水性"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "16",
"type": "bibr",
"rid": "R16",
"data": [
{
"name": "text",
"data": "16"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。显然，这些研究对理解氟化物耐湿性与组分及结构的关系具有重要的科学意义。此外，Wang等利用室温生长法制备了Cs"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "X"
}
]
},
{
"name": "text",
"data": "F"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "（"
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "X"
}
]
},
{
"name": "text",
"data": "=Ge,Si,Ti）单晶。相对于粉末材料，单晶荧光粉具有更高的外量子产率以及稳定性"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "7",
"type": "bibr",
"rid": "R7",
"data": [
{
"name": "text",
"data": "7"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。然而，没有经过后处理的氟化物均有严重的耐湿性问题。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "提高氟化物耐湿性的传统策略是表面包覆一层防水壳以抵御湿气的侵蚀。陈学元课题组通过反向阳离子交换法构筑了K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "TiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "@K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "TiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "核壳结构"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": " ["
},
{
"name": "xref",
"data": {
"text": "17",
"type": "bibr",
"rid": "R17",
"data": [
{
"name": "text",
"data": "17"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，将其作为红色荧光粉封装的WLED具有出色的稳定性。但是由于离子交换具有双向性，K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "TiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "并不能被溶液中的Ti"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "完全替代，说明阳离子交换法只能形成一定厚度的低Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "浓度壳层的氟化物。通过在氟化物表面涂覆一些疏水材料，例如烷基磷酸酯、油酸、Al"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "等"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "18",
"type": "bibr",
"rid": "R18",
"data": [
{
"name": "text",
"data": "18"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "21",
"type": "bibr",
"rid": "R21",
"data": [
{
"name": "text",
"data": "21"
}
]
}
}
],
"rid": [
"R18",
"R19",
"R20",
"R21"
],
"text": "18-21",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，可以有效隔离水分子对荧光粉的水解作用。最近，Li等通过石墨烯量子点和K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "TiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "双涂层策略来制备高稳定性的K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "TiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+[22]"
}
]
},
{
"name": "text",
"data": "。然而，非同质壳层容易脱落，无法维持荧光粉在器件中的长期稳定性。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "提高氟化物耐湿性的根本措施是防止表面Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的水解。还原剂可以有效去除氟化物表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "，从而形成一层无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "基质惰性壳层。目前，H"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "、H"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "C"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "等还原剂已经被用于改良Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "掺杂氟化物的耐湿性"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "13",
"type": "bibr",
"rid": "R13",
"data": [
{
"name": "text",
"data": "13"
}
]
}
},
{
"name": "text",
"data": ","
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "23",
"type": "bibr",
"rid": "R23",
"data": [
{
"name": "text",
"data": "23"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "24",
"type": "bibr",
"rid": "R24",
"data": [
{
"name": "text",
"data": "24"
}
]
}
}
],
"rid": [
"R23",
"R24"
],
"text": "23-24",
"type": "bibr"
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，而还原剂的还原能力强弱、浓度、反应时间等因素直接影响氟化物耐湿性改良的程度。叶信宇课题组利用H"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "C"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "的还原性用于劣化氟化物的荧光恢复，为改良氟化物的耐湿性提供了一种新思路"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "25",
"type": "bibr",
"rid": "R25",
"data": [
{
"name": "text",
"data": "25"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。因此，寻找一种合适的还原剂是制备高耐湿性红色氟化物的关键。从分子结构上看，乳糖酸（C"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "12"
}
]
},
{
"name": "text",
"data": "H"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "22"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "12"
}
]
},
{
"name": "text",
"data": "，LA）具有八组羟基和一组羧基，由于α-羧基的强吸电子性，乳糖酸具有较强的还原性。本工作中，通过简单的乳糖酸处理，可以将氟化物表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "还原成Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2+"
}
]
},
{
"name": "text",
"data": "，在荧光粉表面重构一层无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的惰性壳层，以隔绝水分子与内部Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "。与未处理的K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "（KSFM）相比，经过乳糖酸溶液钝化的氟化物的晶相、形貌以及光致发光强度几乎不变，耐湿性得到显著提升。此外，乳糖酸溶液还可以恢复水解后的氟化物的荧光强度至初始值。在高温高湿的苛刻条件下，将乳糖酸钝化的氟化物作为红光组分封装的WLED具有优异的光色稳定性。"
}
]
}
]
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2 实 验"
}
],
"level": "1",
"id": "s2"
}
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2.1 样品制备"
}
],
"level": "2",
"id": "s2a"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "：参考Bode的方法"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "26",
"type": "bibr",
"rid": "R26",
"data": [
{
"name": "text",
"data": "26"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。首先，称量45.00 g KHF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "（99%）和2.25 g KMnO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "（99.9%）置于250 mL塑料烧杯中，再取150 mL HF倒入塑料烧杯中，将塑料烧杯置于冰水浴下搅拌60 min后，再将H"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "（30%）缓慢地滴入紫色溶液中，直到紫色溶液颜色变成浅褐色则停止滴定，再离心倒去上层液体，用丙酮数次洗涤剩余的黄色粉末，再在70 ℃下干燥2 h即可得到K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "粉末。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "荧光粉：按照文献["
},
{
"name": "blockXref",
"data": {
"data": [
{
"name": "xref",
"data": {
"text": "27",
"type": "bibr",
"rid": "R27",
"data": [
{
"name": "text",
"data": "27"
}
]
}
},
{
"name": "text",
"data": "-"
},
{
"name": "xref",
"data": {
"text": "28",
"type": "bibr",
"rid": "R28",
"data": [
{
"name": "text",
"data": "28"
}
]
}
}
],
"rid": [
"R27",
"R28"
],
"text": "27-28",
"type": "bibr"
}
},
{
"name": "text",
"data": "]的共沉淀法合成。首先，向35 mL的49% HF溶液中加入1.60 g SiO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "（99.9%）搅拌并溶解制备溶液A，同时向15 mL的49% HF溶液中加入6.25 g KHF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "（99%）制备溶液B。然后将0.65 g的K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "溶解到溶液A中得到溶液C，再将溶液B缓慢滴入溶液C，将得到的沉淀物离心并用乙醇多次洗涤得到K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "荧光粉。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "乳糖酸钝化的氟化物：首先，将0.1 g 乳糖酸溶解于5 mL去离子水中。然后，加入0.5 g K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "荧光粉，搅拌4 h。最后，通过离心分离，用水洗涤2次和乙醇洗涤1次，70"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": " "
}
]
},
{
"name": "text",
"data": "℃干燥12 h，得到乳糖酸钝化的氟化物产物，记作KSFM-LA。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "WLED的封装：将Y"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "Al"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "12"
}
]
},
{
"name": "text",
"data": "∶Ce"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "3+"
}
]
},
{
"name": "text",
"data": "（YAG∶Ce"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "3+"
}
]
},
{
"name": "text",
"data": "，YAG04）黄粉、氟化物红粉和环氧树脂（8820A/B）按照1∶3.6∶7.6的质量比混合均均，再将其涂覆在蓝光芯片（450 nm）上封装制备WLED。"
}
]
}
]
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "2.2 样品表征"
}
],
"level": "2",
"id": "s2b"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "采用型号为Ultima IV的X射线衍射仪分析样品的晶相，通过型号为Zeiss Sigma 300的扫描电镜（SEM）分析样品的形貌，使用F-4500日式荧光分光光度计记录样品的激发光谱（PLE）和发射（PL）光谱，利用爱丁堡FLS1000荧光光谱仪测试样品的荧光寿命和光致发光量子产率。通过型号为TENSOR27的傅里叶红外光谱仪（FTIR）以及型号为EscaLab Xi+的X射线光电子能谱（XPS）对样品的结构与表面成分进行分析。封装的WLED在恒温恒湿老化箱（HYK-TH-80）中进行老化，使用光谱辐射计（HAAS-1200）测量了所制备器件的光电性能。"
}
]
}
]
}
]
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "3 结果与讨论"
}
],
"level": "1",
"id": "s3"
}
},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "3.1 物相与形貌"
}
],
"level": "2",
"id": "s3a"
}
},
{
"name": "p",
"data": [
{
"name": "xref",
"data": {
"text": "图1",
"type": "fig",
"rid": "F1",
"data": [
{
"name": "text",
"data": "图1"
}
]
}
},
{
"name": "text",
"data": "（a）给出了KSFM和KSFM-LA的XRD图谱。从图中可知，经过LA的处理，荧光粉仍为纯相，衍射峰的位置与标准卡号为75-0694的K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "物相一致。如"
},
{
"name": "xref",
"data": {
"text": "图1",
"type": "fig",
"rid": "F1",
"data": [
{
"name": "text",
"data": "图1"
}
]
}
},
{
"name": "text",
"data": "（b）所示，通过室温共沉淀法合成的KSFM粒径分布均匀（~30 μm），形貌为类立方体，具有光滑的表面以及规整的棱角。LA处理对其形貌无明显影响。"
}
]
},
{
"name": "fig",
"data": {
"id": "F1",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图1"
}
],
"title": [
{
"name": "text",
"data": "KSFM和KSFM-LA的XRD图谱（a）和SEM图（b）"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.1"
}
],
"title": [
{
"name": "text",
"data": "XRD patterns（a）， SEM images （b） of KSFM and KSFM-LA."
}
]
}
],
"subcaption": [],
"note": [],
"graphics": [
{
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},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "3.2 发光性质"
}
],
"level": "2",
"id": "s3b"
}
},
{
"name": "p",
"data": [
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "（a）显示了KSFM和KSFM-LA的光致发光图。KSFM-LA和KSFM荧光粉的光谱形状与强度几乎保持不变。365 nm和469 nm处具有双宽带激发峰，分别来自Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "自旋允许的"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "A"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "→"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "T"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "1"
}
]
},
{
"name": "text",
"data": "和"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "A"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "→"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "T"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "跃迁，在631 nm处的窄带发射峰属于"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "E"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "g"
}
]
},
{
"name": "text",
"data": " →"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "A"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "宇称-自旋禁阻跃迁。"
},
{
"name": "xref",
"data": {
"text": "图2",
"type": "fig",
"rid": "F2",
"data": [
{
"name": "text",
"data": "图2"
}
]
}
},
{
"name": "text",
"data": "（b）显示，Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "掺杂氟化物的发光强度呈现单指数衰减趋势。KSFM和KSFM-LA的荧光寿命分别为8.54 ms和8.51 ms，说明LA处理只是钝化了氟化物表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "，不影响Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的衰减性质。"
}
]
},
{
"name": "fig",
"data": {
"id": "F2",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图2"
}
],
"title": [
{
"name": "text",
"data": "KSFM和KSFM-LA的PLE光谱和PL光谱（a）及衰减曲线（b）"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.2"
}
],
"title": [
{
"name": "text",
"data": "PLE and PL spectrum（a）， decay curves（b） of KSFM and KSFM-LA"
}
]
}
],
"subcaption": [],
"note": [],
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"data": {
"title": [
{
"name": "text",
"data": "3.3 耐湿性和热稳定性"
}
],
"level": "2",
"id": "s3c"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "氟化物荧光粉在潮湿环境中的不稳定性是由于表面Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的水解，而不是氟化物基质的分解。虽然 K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "的溶度积常数（"
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "K"
}
]
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "sp"
}
]
},
{
"name": "text",
"data": "）非常小（8.7 × 10"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-7"
}
]
},
{
"name": "text",
"data": "），但K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "∶Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "仍然缓慢溶解在水中（方程"
},
{
"name": "xref",
"data": {
"text": "式（1）",
"type": "disp-formula",
"rid": "DF1",
"data": [
{
"name": "text",
"data": "式（1）"
}
]
}
},
{
"name": "text",
"data": "），释放出[MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "]"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2-"
}
]
},
{
"name": "text",
"data": "，与水分子进一步反应形成固体Mn（OH）"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "4"
}
]
},
{
"name": "text",
"data": "（方程"
},
{
"name": "xref",
"data": {
"text": "式（2）",
"type": "disp-formula",
"rid": "DF2",
"data": [
{
"name": "text",
"data": "式（2）"
}
]
}
},
{
"name": "text",
"data": "），最后变成棕黑色的MnO"
},
{
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"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "（方程"
},
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"data": {
"text": "式（3）",
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"data": [
{
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"name": "sub",
"data": [
{
"name": "text",
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},
{
"name": "text",
"data": "Si"
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"data": [
{
"name": "text",
"data": "1-"
}
]
},
{
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"data": [
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"name": "sub",
"data": [
{
"name": "text",
"data": "x"
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"data": "Mn"
},
{
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"data": [
{
"name": "sub",
"data": [
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"name": "text",
"data": "x"
}
]
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},
{
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"data": "F"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": " ↔2K"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "+"
}
]
},
{
"name": "text",
"data": "+ （1-"
},
{
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"data": [
{
"name": "text",
"data": "x"
}
]
},
{
"name": "text",
"data": "）[SiF"
},
{
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"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "]"
},
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"name": "sup",
"data": [
{
"name": "text",
"data": "2-"
}
]
},
{
"name": "text",
"data": " + "
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "x"
}
]
},
{
"name": "text",
"data": "[MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "]"
},
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"data": [
{
"name": "text",
"data": "2-"
}
]
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"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "］"
},
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"data": [
{
"name": "text",
"data": "2- "
}
]
},
{
"name": "text",
"data": "+ 4H"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "O → Mn（OH）"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "4 "
}
]
},
{
"name": "text",
"data": "+ 4H"
},
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"name": "sup",
"data": [
{
"name": "text",
"data": "+ "
}
]
},
{
"name": "text",
"data": "+ 6F"
},
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"data": [
{
"name": "text",
"data": "-"
}
]
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},
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"name": "sub",
"data": [
{
"name": "text",
"data": "4 "
}
]
},
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"name": "text",
"data": "→ MnO"
},
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{
"name": "text",
"data": "2 "
}
]
},
{
"name": "text",
"data": "+ 2H"
},
{
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{
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"data": "2"
}
]
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"data": "O，"
}
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}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "这些锰氧化物吸附在氟化物表面，导致PL强度降低。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "水浸实验结果表明，随着水浸时间延长，未经处理的KSFM荧光粉的发光强度迅速降低（"
},
{
"name": "xref",
"data": {
"text": "图 3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图 3"
}
]
}
},
{
"name": "text",
"data": "（a）），而KSFM-LA荧光粉发光强度缓慢下降（"
},
{
"name": "xref",
"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（b））。水中浸泡360 h后，KSFM-LA的体色仍然保持亮黄色（"
},
{
"name": "xref",
"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（c）插图），发光强度维持为初始值的87.5%，未经改性的KSFM变成棕褐色（锰的氧化物），发光强度仅维持初始值的63%（"
},
{
"name": "xref",
"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（c））。"
}
]
},
{
"name": "fig",
"data": {
"id": "F3",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图3"
}
],
"title": [
{
"name": "text",
"data": "不同水浸时间的KSFM（a）和KSFM-LA（b）的发光光谱；（c）KSFM和KSFM-LA的相对发光强度与水浸时间的关系， 插图：水中KSFM（左边）和KSFM-LA（右边）在日光和蓝光灯下的照片；KSFM（d）和KSFM-LA（e）发光光谱的热稳定性；（f）KSFM和KSFM-LA相对发光强度随温度的变化。"
}
]
},
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"label": [
{
"name": "text",
"data": "Fig.3"
}
],
"title": [
{
"name": "text",
"data": "PL spectra of KSFM（a） and KSFM-LA（b） under different water immersion time. （c）Relative luminescence intensity of KSFM and KSFM-LA "
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "versus"
}
]
},
{
"name": "text",
"data": " water immersion time， insert： photos of KSFM（left） and KSFM-LA（right） in water under natural and blue light. Thermal stability of PL spectra of KSFM（d） and KSFM-LA（e）. （f）Relative luminescence intensity of KSFM and KSFM-LA as a function of temperature."
}
]
}
],
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"data": [
{
"name": "text",
"data": "KSFM和KSFM-LA的量子效率（表S1，补充文件）也进一步支撑了上述结果。KSFM的内、外量子产率（IQE和EQE）分别为94.7%和57%。水浸360 h后，KSFM的IQE和EQE分别降到59.8%和37.9%，吸收率（AE）从60.0%升高到63.4%，这归因于氟化物表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "水解为强可见光吸收的黑色MnO"
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{
"name": "text",
"data": "2"
}
]
},
{
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"data": [
{
"name": "text",
"data": "["
},
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"data": {
"text": "29",
"type": "bibr",
"rid": "R29",
"data": [
{
"name": "text",
"data": "29"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。然而，经表面钝化的KSFM-LA的AE、IQE和EQE水浸前后几乎没有差异，这一现象暗示了氟化物表面可形成耐湿的保护层。"
}
]
},
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"data": [
{
"name": "xref",
"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（d）、（e）分别展示了KSFM和KSFM-LA温度依赖的发光光谱。随着温度升高，两种氟化物的发光强度都出现了缓慢降低的趋势。150"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": " "
}
]
},
{
"name": "text",
"data": "℃以后，热猝灭效应显著。从归一化的积分发光强度变化来看（"
},
{
"name": "xref",
"data": {
"text": "图3",
"type": "fig",
"rid": "F3",
"data": [
{
"name": "text",
"data": "图3"
}
]
}
},
{
"name": "text",
"data": "（f）），两种氟化物显示了相同的高热稳定性。"
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]
}
]
},
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"title": [
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"data": "3.4 耐湿性改善机理"
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}
},
{
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"data": [
{
"name": "text",
"data": "红外光谱用来验证KSFM-LA表面是否存在LA。"
},
{
"name": "xref",
"data": {
"text": "图4",
"type": "fig",
"rid": "F4",
"data": [
{
"name": "text",
"data": "图4"
}
]
}
},
{
"name": "text",
"data": "显示，LA分子在3 100 ~ 3 700 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "范围内有一个宽带吸收，属于分子中O—H键的伸缩振动，1 743 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "处的吸收带归因于LA分子中C=O键引起的振动"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "30",
"type": "bibr",
"rid": "R30",
"data": [
{
"name": "text",
"data": "30"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。KSFM和KSFM-LA的吸收峰强度一致，483 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "和745 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "处的尖峰是Si—F键的振动所致"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "["
},
{
"name": "xref",
"data": {
"text": "31",
"type": "bibr",
"rid": "R31",
"data": [
{
"name": "text",
"data": "31"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "，3 438 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "和1 629 cm"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "-1"
}
]
},
{
"name": "text",
"data": "的吸收峰分别来自氟化物表面O—H的拉伸和弯曲振动。红外光谱中无C=O特征峰，说明KSFM-LA表面无LA包覆层。"
}
]
},
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"lang": "zh",
"label": [
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"data": "图4"
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"name": "text",
"data": "KSFM、KSFM-LA和LA的红外光谱。"
}
]
},
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"label": [
{
"name": "text",
"data": "Fig.4"
}
],
"title": [
{
"name": "text",
"data": "Infrared spectra of KSFM， KSFM-LA and LA."
}
]
}
],
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"data": {
"text": "图5",
"type": "fig",
"rid": "F5",
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"data": "图5"
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]
}
},
{
"name": "text",
"data": "（a）描述了20%Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "掺杂的KSFM以及经过表面改性的KSFM-LA的XPS全谱图。结合能为686，293，531，104 eV处的吸收峰分别归属于F1s、K2p、O1s和Si2p的特征峰。相对而言，在KSFM的XPS全谱上能观察到明显的Mn2p信号。"
},
{
"name": "xref",
"data": {
"text": "图5",
"type": "fig",
"rid": "F5",
"data": [
{
"name": "text",
"data": "图5"
}
]
}
},
{
"name": "text",
"data": "（b）中Mn2p的精细XPS谱清晰地表明了氟化物表面Mn元素的相对含量。相对于未处理的KSFM，KSFM-LA的Mn2p的吸收强度明显更低，表面Mn的含量从0.7%降低到0.34%（表S2，补充文件），说明强还原能力的LA可以有效清除表面Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "，形成惰性壳层。"
}
]
},
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"caption": [
{
"lang": "zh",
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"title": [
{
"name": "text",
"data": "（a）KSFM和KSFM-LA的全谱XPS图，插图为670 ~ 615 eV范围内的Mn2p信号；（b）Mn2p谱图。"
}
]
},
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"label": [
{
"name": "text",
"data": "Fig.5"
}
],
"title": [
{
"name": "text",
"data": "（a）Full XPS spectra， the inset is the Mn2p signal in the 670-615 eV range. （b）Mn2p spectra of KSFM and KSFM-LA."
}
]
}
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"data": [
{
"name": "text",
"data": "LA分子因其—COOH较为活泼表现出较强的还原性"
},
{
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"data": [
{
"name": "text",
"data": "["
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"data": {
"text": "32",
"type": "bibr",
"rid": "R32",
"data": [
{
"name": "text",
"data": "32"
}
]
}
},
{
"name": "text",
"data": "]"
}
]
},
{
"name": "text",
"data": "。当遇到氧化剂时，LA分子会被氧化成醛和CO"
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"data": "2"
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]
},
{
"name": "text",
"data": "。Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "还原为Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2+"
}
]
},
{
"name": "text",
"data": "的标准电极电位（"
},
{
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"data": [
{
"name": "text",
"data": "φ"
}
]
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "Θ"
}
]
},
{
"name": "text",
"data": "）为1.64 eV，表明Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "很容易还原。在此，GA和表面Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "之间可能发生的氧化还原反应如下式所示："
}
]
},
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"title": []
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{
"name": "text",
"data": "为了进一步说明LA的还原性，我们设计了一个验证实验。首先，将氟化物加入到水中，使其充分水解，得到体色为暗棕色的氟化物（KSFM-W）；然后在水溶液中加入少量LA，30 min后观察到KSFM-W荧光粉的体色从暗棕色变为亮黄色，在蓝光照射下发出明亮的红光。如"
},
{
"name": "xref",
"data": {
"text": "图6",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图6"
}
]
}
},
{
"name": "text",
"data": "（a）的量子产率数据所示，经LA处理的KSFM-W（KSFM-W-LA）的AE从66.7%下降到54.7%，IQE从35.8%上升到98.8%，这表明LA能有效清除表面暗棕色的锰氧化物，形成一层无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的惰性层。该验证实验过程中涉及的氟化物的物相保持不变（"
},
{
"name": "xref",
"data": {
"text": "图6",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图6"
}
]
}
},
{
"name": "text",
"data": "（b））。KSFM-W荧光粉的XRD图中也未观察到锰氧化物（如MnO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "）的存在，说明KSFM荧光粉只有表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "发生水解。从KSFM-W的SEM图（"
},
{
"name": "xref",
"data": {
"text": "图6",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图6"
}
]
}
},
{
"name": "text",
"data": "（c））来看，水解后的氟化物表面出现一些坑洼，而KSFM-W-LA表面变得更加粗糙（"
},
{
"name": "xref",
"data": {
"text": "图6",
"type": "fig",
"rid": "F7",
"data": [
{
"name": "text",
"data": "图6"
}
]
}
},
{
"name": "text",
"data": "（d））。"
}
]
},
{
"name": "fig",
"data": {
"id": "F7",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图6"
}
],
"title": [
{
"name": "text",
"data": "（a）样品1（KSFM）、2（KSFM-W）、3（KSFM-W-LA）的吸收率（AE）和内量子产率（IQE）；（b）KSFM、KSFM-W和KSFM-W-LA的XRD图；KSFM-W（c）和KSFM-W-LA（d）的SEM图。"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.6"
}
],
"title": [
{
"name": "text",
"data": "（a）Absorptivity（AE） and internal quantum yield（IQE） of samples 1（KSFM）， 2（KSFM-W）， 3（KSFM-W-LA）. （b）XRD patterns of KSFM， KSFM-W and KSFM-W-LA. SEM images of KSFM-W（c） and KSFM-W-LA（d）."
}
]
}
],
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"note": [],
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{
"name": "p",
"data": [
{
"name": "text",
"data": "LA钝化KSFM表面Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的过程如"
},
{
"name": "xref",
"data": {
"text": "图7",
"type": "fig",
"rid": "F8",
"data": [
{
"name": "text",
"data": "图7"
}
]
}
},
{
"name": "text",
"data": "所示。无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "惰性壳层的重构有两种途径。一种是LA直接将KSFM氟化物表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "还原成可溶的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2+"
}
]
},
{
"name": "text",
"data": "，由于K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "晶体在水中溶解度很低，在去除Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "后氟化物表面的K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "可作为防水层保护内部的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "。另一种是KSFM表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "首先水解成MnO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "，LA将黑色的MnO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "还原成Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2+"
}
]
},
{
"name": "text",
"data": "，剩下的K"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "SiF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "text",
"data": "壳同样可以阻止内部Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的水解。在乳糖酸水溶液钝化KSFM的制备过程中，由于酸性环境抑制了KSFM的水解，KSFM表面的Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "以[MnF"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "6"
}
]
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "2-"
}
]
},
{
"name": "text",
"data": "]形式存在，无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "惰性壳层的重构将以途径一进行；当氟化物的表面被完全水解并形成MnO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "，乳糖酸主要还原其表面的MnO"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "2"
}
]
},
{
"name": "text",
"data": "，此时无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "惰性壳层的重构将以途径二方式进行。"
}
]
},
{
"name": "fig",
"data": {
"id": "F8",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图7"
}
],
"title": [
{
"name": "text",
"data": "乳糖酸的钝化效应以及氟化物表面惰性壳层重构示意图"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.7"
}
],
"title": [
{
"name": "text",
"data": "Schematic illustration of the passivation effect of lactobionic acid and the reconstruction of the inert shell on the surface of fluoride"
}
]
}
],
"subcaption": [],
"note": [],
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},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "3.5 WLED性能"
}
],
"level": "2",
"id": "s3e"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "为了评估改性后的KSFM-LA可被应用于WLED照明，我们将Y"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "3"
}
]
},
{
"name": "text",
"data": "Al"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "5"
}
]
},
{
"name": "text",
"data": "O"
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "12"
}
]
},
{
"name": "text",
"data": "∶Ce"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "3+"
}
]
},
{
"name": "text",
"data": "（YAG∶Ce"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "3+"
}
]
},
{
"name": "text",
"data": "）黄粉、氟化物红粉和环氧树脂按照1∶3.6∶7.6的质量比混合均匀，再将其涂覆在蓝光芯片上封装制备WLED。分别将KSFM和KSFM-LA作红光成分封装的WLED记为LED1和LED2。如"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F9",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "（a）所示，在60 mA驱动电流下，制备的LED1和LED2所对应的电致发光谱（EL）形状与峰位一致，并发出耀眼的暖白光（"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F9",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "（a）的内插图）。LED1的光效为126.14 lm/W（CCT=3 092 K，"
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "R"
}
]
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "a"
}
]
},
{
"name": "text",
"data": "=89.8），而LED2的光效高达130.61 lm/W（CCT=3 518 K，"
},
{
"name": "italic",
"data": [
{
"name": "text",
"data": "R"
}
]
},
{
"name": "sub",
"data": [
{
"name": "text",
"data": "a"
}
]
},
{
"name": "text",
"data": "=88.5）。"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F9",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "（b）展示了LED2在不同驱动电流下的EL图，随着驱动电流从20 mA增加到120 mA，EL谱图的形状与位置没有显著差异，发光强度逐渐增加。为了验证KSFM-LA的稳定性，我们将封装的LED1和LED2放置在高温（85 ℃）高湿（85%）老化箱点亮500 h，每隔100 h将WLED装置在60 mA下测试其光色性能。随着老化时间延长，LED2对应的色坐标比LED1分布更集中（"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F9",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "（c）），LED2的光效比LED1下降得更缓慢（"
},
{
"name": "xref",
"data": {
"text": "图8",
"type": "fig",
"rid": "F9",
"data": [
{
"name": "text",
"data": "图8"
}
]
}
},
{
"name": "text",
"data": "（d）），当老化时间为500 h时，LED2和LED1的光效分别维持为初始值的90.5%和82.3%。这些老化数据进一步表明KSFM-LA比KSFM具有更高的稳定性。表S3（补充文件）给出了LED1和LED2在60 mA驱动电流下测试的光电参数。"
}
]
},
{
"name": "fig",
"data": {
"id": "F9",
"caption": [
{
"lang": "zh",
"label": [
{
"name": "text",
"data": "图8"
}
],
"title": [
{
"name": "text",
"data": "（a）LED1和LED2的电致发光光谱；（b）LED2在不同驱动电流（20~120 mA）下的电致发光光谱；（c）色坐标图；（d）LED1和LED2的发光效率随老化时间的变化。"
}
]
},
{
"lang": "en",
"label": [
{
"name": "text",
"data": "Fig.8"
}
],
"title": [
{
"name": "text",
"data": "（a）EL spectra of LED1 and LED2. （b）EL spectra of LED2 under different driving currents（20-120 mA）. （c）CIE. （d）Luminous efficiency of LED1 and LED2 with aging time."
}
]
}
],
"subcaption": [],
"note": [],
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},
{
"name": "sec",
"data": [
{
"name": "sectitle",
"data": {
"title": [
{
"name": "text",
"data": "4 结 论"
}
],
"level": "1",
"id": "s4"
}
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "通过乳糖酸对Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "的钝化效应，本工作在KSFM表面重构了无Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "惰性壳层。经水浸360 h后，KSFM-LA的发光强度仍维持为初始值的87.5%，远高于KSFM的63%。经LA处理，水解的氟化物的体色可由棕褐色恢复为亮黄色，量子产率从35.8%恢复到98.8%。在高温高湿条件下老化500 h后，分别用KSFM-LA和KSFM作为红光组分封装的WLED的流明效率维持为初始值的90.5%和82.3%。由此可见，KSFM-LA封装的WLED比KSFM具有更高的稳定性。因此，简单的乳糖酸处理可以有效提升掺Mn"
},
{
"name": "sup",
"data": [
{
"name": "text",
"data": "4+"
}
]
},
{
"name": "text",
"data": "氟化物的耐湿性。本工作可为高稳定性氟化物红色荧光粉的工业化生产提供借鉴。"
}
]
},
{
"name": "p",
"data": [
{
"name": "text",
"data": "本文补充文件和专家审稿意见及作者回复内容的下载地址："
},
{
"name": "extlink",
"data": {
"text": [
{
"name": "text",
"data": "http://cjl.lightpublishing.cn/thesisDetails#10.37188/CJL.20220127."
}
],
"href": "http://cjl.lightpublishing.cn/thesisDetails#10.37188/CJL.20220127."
}
}
]
}
]
}
],
"footnote": [],
"reflist": {
"title": [
{
"name": "text",
"data": "参考文献"
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"text": "WAN Ping-ping,YANG Jing,LIU Hong-xiu,et al.Improving Moisture Resistance of K2SiF6∶Mn4+via Passivation Effect of Lactobionic Acid[J].Chinese Journal of Luminescence,2022,43(08):1300-1308."
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"text": [
{
"name": "text",
"data": "长沙市自然科学基金（kq2202235）； 化学生物学及中药分析教育部重点实验室开放基金（KLCBTCMR20‐23）资助项目"
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"journalTitle": "发光学报",
"issue": "8",
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}
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