CN107418565B - 长余辉转光剂及其制备方法和长余辉转光膜及其制备方法 - Google Patents
长余辉转光剂及其制备方法和长余辉转光膜及其制备方法 Download PDFInfo
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- CN107418565B CN107418565B CN201710495268.0A CN201710495268A CN107418565B CN 107418565 B CN107418565 B CN 107418565B CN 201710495268 A CN201710495268 A CN 201710495268A CN 107418565 B CN107418565 B CN 107418565B
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Abstract
本发明属于转光剂和转光膜领域。长余辉转光剂，化学组成通式为：SrAl2O4‑3x/2Nx:Eu2+，RE3+，其中Re3+是Dy3+、Nd3+、La3+、Ho3+、Pr3+、Er3+稀土元素中的一种或几种的组合，x的取值范围为2/3≤x≤2。该长余辉转光剂的优点是长余辉转光剂能够充分吸收太阳光中的紫光和近紫外光，通过创造性地引入N3‑离子，重新构造发光中心周围的晶体场环境，使发射波长红移至红光区域。
Description
技术领域
本发明属于转光剂和转光膜领域，特别是涉及一种长余辉转光剂和长余辉转光膜。
背景技术
光照是植物生长发育的重要生态因子，对植物的健康生长具有重大影响。但是，由于地球自转的原因，我们的地球存在白天和黑夜，尤其是对于纬度较高的地区，植物的光照时间短，直接导致植物生长速度缓慢。为了改善这一自然条件的限制，我们可以通过人为地延长光照时间的方法来进行改进。长余辉材料是一种非常友好的发光材料，它能够在白天吸收太阳光能量，当太阳下山进入夜晚之后，它还能够持续发光，促进植物的生长。在众多长余辉材料中，最具代表性而且性能最好的是铝酸盐基长余辉发光材料，比如稀土离子掺杂的MAl2O4:Eu2+，RE3+，其中，M是碱土金属元素，Eu2+是发光中心，RE是稀土元素且会导致缺陷能级的形成，从而形成长余辉。在该类荧光粉中，不同的M会使得Eu2+所处的晶体场强度发生明显的变化，从而产生不同的发光和余辉颜色。但是，该类荧光粉通常只发射蓝绿色长余辉，例如，用不同方法合成的CaAl2O4:Eu2+,Nd3+,La3+、SrAl2O4:Eu2+,Dy3+和BaAl2O4:Eu2+,Dy3+发射光谱的峰值一般约为438-445nm、512-530nm、495-500nm。除此以外，在铝酸盐基发光材料中4SrO·7Al2O3:Eu2+,Dy3+和2SrO·3Al2O3:Eu2+,Dy3+等也具有优良的蓝绿色长余辉发光。然而植物更需要的是红光成分，因此，现有的材料不太适合植物照明。
为了获得一种发射红光的长余辉材料，必须对现有荧光粉进行全新的设计与合成。对于长余辉发光材料而言，基质的选择是非常重要的，基质必须提供合适的晶体环境，即使对于同样的激活剂和敏化剂，也并不是所有的基质材料都能有长余辉发光现象。对于合适的基质材料，不同的激活剂及浓度和不同价态的激活离子对发光材料的性能影响也各不相同。另外，并不是所有的激活剂都能产生长余辉现象。一般来说，作为长余辉发光特性的激活剂离子主要是那些具有相对较低的4f-5d跃迁能量或具有很高电荷迁移带能量的稀土离子，如Eu2+、Tm3+、Yb3+、Ce3+、Tb3+、Pr3+等稀土离子。Eu2+在碱土铝酸盐体系中主要表现为d-f宽带跃迁发射，因而发射波长随基质组成和结构的变化而变化。Eu2+的发射波长主要集中在蓝绿色波段，有时也可以延伸到紫色和红色波段，但是此时的亮度和余辉都较弱。由于Eu2+在紫外区到可见区比较宽的波段内具有较强的吸收能力，所以通过改变基质材料和共掺杂剂等方法，可以使得Eu2+激活的材料在太阳光、日光灯或白炽灯等光源的激发下产生由紫色到红色的长余辉发光。
但是，如果单纯掺杂Eu2+，余辉性能仍然较差，在这种情况下，一般需要添加辅助激活剂。最常用的辅助激活剂是三价稀土离子Re3+。当将三价稀土离子掺入含有二价铕的材料如碱土铝酸盐形成MAl2O4:Eu2+,Re3+时，三价稀土离子Re3+不等价取代二价的碱土离子M2+(M2 +为Sr2+、Ca2+、Ba2+、Mg2+等)，从而产生不同深度的陷阱，该陷阱可用于存储电子和空穴。为了产生超长余辉的发光，首先要求陷阱具有合适的深度。若陷阱太深，则存储其内的电子和空穴就不能释放出来，在室温下就观察不到超长余辉发光现象；若陷阱太浅，则存储其内的电子和空穴很快就全部释放出来而使得余辉时间不长。除此之外，还要求掺入的三价稀土离子对陷阱中的电子、空穴具有合适的亲和力，亲和力太强或太弱都起不到延长余辉时间的作用。对于不同的基质材料，可以有不同的三价稀土离子(如La3+、Ce3+、Pr3+、Nd3+、Sm3+、Tb3+、Dy3+、Ho3+、Er3+、Tm3+、Yb3+、Y3+等)作为辅助激活剂。每一种材料都对应有一种最合适的辅助激活剂，例如，对于SrAl2O4:Eu2+和Sr4Al14O25:Eu2+以Dy3+为最好，而对于CaAl2O4:Eu2+则以Nd3 +和La3+按一定比例共同掺杂为最好。三价稀土辅助激活剂Dy3+、Nd3+、Ho3+、Pr3+、Er3+具有合适的光学电负性(1.09-1.21)，对电子、空穴具有合适的亲和力，可缓慢地把存储在陷阱内的电子和空穴释放至Eu2+，从而可以产生Eu2+的超长余辉发光现象。尤其是Dy3+，可以显著地延长余辉时间，而易还原的稀土离子Sm3+、Tm3+和Yb3+的光学电负性较大，易氧化的稀土离子Ce3+和Tb3+的光学电负性则较小，当这些离子作为辅助激活剂时，对陷阱中的电子、空穴的亲和力或是太强或是太弱，因而对延长余辉时间的作用并不明显。
发明内容
为了克服上述现有技术中长余辉材料在红光区域发光较弱，余辉时间太短的缺点，本发明的一个目的是提供一种在红光区域具有较强的长余辉发光的转光剂及其制备方法。本发明的另一个目的是提供一种利用在红光区域具有较强的长余辉发光的转光剂和薄膜树脂合成了一种新型的转光膜。
为解决上述现有技术的不足，本发明所采用的技术方案如下：长余辉转光剂，化学组成通式为：SrAl2O4-3x/2Nx:Eu2+，RE3+，其中Re3+是Dy3+、Nd3+、La3+、Ho3+、Pr3+、Er3+稀土元素中的一种或几种的组合，x的取值范围为2/3≤x≤2。
作为优选，制备方法包括以下步骤：(1)以SrCO3、Al2O3、AlN、Eu2O3及其它稀土氧化物为原料，按照化学式SrAl2O4-3x/2Nx:Eu2+，RE3+的化学计量比称取各原料；(2)将步骤(1)获得的原料在玛瑙研钵中充分研磨后混合均匀；(3)将步骤(2)获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1300-1500℃，灼烧时间为6-10小时，灼烧完成后样品随炉降温至室温，最后取出获得烧结体；(4)将步骤(3)获得的烧结体进行球磨粉碎，然后用蒸馏水洗涤烘干，即得所述长余辉转光剂。
作为优选，烧结气氛为5％的氢气和95％的氮气混合气。
一种长余辉转光膜，包括薄膜树脂、改性助剂和权利要求1所述的长余辉转光剂；按重量百分比计，长余辉转光剂为0.1-2.0％，所述改性助剂为0.1％-5.0％，其余为薄膜树脂。
作为优选，所述薄膜树脂的成分为聚乙烯、聚苯乙烯、聚氯乙烯、乙烯-醋酸乙烯共聚物、聚丙烯、聚酰胺中的一种或几种。
作为优选，改性助剂为光稳定剂、抗氧化剂、润滑剂中的一种或几种。
作为优选，光稳定剂为2-(2-羟基-5-甲基苯基)苯并三唑或丁二酸，抗氧化剂为2,6-二叔丁基对甲酚或2,4,6三叔丁基苯酚水杨酸苯酯、润滑剂为聚乙烯蜡或硬脂酸锌。
一种长余辉转光膜制备方法，制备方法包括以下步骤：(1)按重量百分比称取薄膜树脂50-80份、长余辉转光剂10-40份、改性助剂3-30份；(2)在塑炼机将上述材料均匀混合，加热温度为150-200℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒1-10份、薄膜树脂90-99份，混合均匀后在吹膜机上吹制薄膜，加热温度为150-200℃。
作为优选，改性助剂是光稳定剂1-10份、抗氧化剂1-10份、润滑剂1-10份。
与现有技术相比，本发明的有益效果是：(1)长余辉转光剂能够充分吸收太阳光中的紫光和近紫外光，将其引入农用薄膜之后，由于其余辉时间长，发光可以一直持续到夜晚，因此可以有效促进植物在夜间的生长；(2)现有的铝酸盐基长余辉发光材料只发射蓝绿光，本发明通过创造性地引入N3-离子，重新构造发光中心周围的晶体场环境，使发射波长红移至红光区域，在长余辉转光膜上使用，非常有利于植物的生长。
附图说明
图1为实施例1制备的转光剂激发光谱图。
图2为实施例1-4的发射光谱图。
图3为实施例5-8的发射光谱图。
图4为实施例1制备的转光剂发光强度衰减曲线图。
具体实施方式
下面结合说明书附图1-4和具体实施例对本发明作进一步详细说明。
实施例1
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Dy2O3为原料，按照化学式SrAl2O3N2/3:0.02Eu2+，0.02Dy3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1300℃，灼烧时间为10小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚苯乙烯树脂80份、长余辉转光剂10份、2-(2-羟基-5-甲基苯基)苯并三唑4份、2,6-二叔丁基对甲酚4份、硬脂酸锌2份；(2)在塑炼机将上述材料均匀混合，加热温度为150℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒10份、聚苯乙烯树脂90份，混合均匀后在吹膜机上吹制薄膜，加热温度为200℃。
不使用膜种植的生菜A、使用市售膜种植的生菜B和使用实施例1制备的长余辉转光膜种植的生菜C进行生菜生长指标试验。生菜生长指标动态测定说明：随机选取20株样本参数接近的生菜，重复3次，测量生菜株高、株幅、叶长、叶宽。取样后先称量地上和地下部的鲜重，然后在60℃烘箱中烘至恒重后测其干重；叶绿素和类胡萝卜素含量测定采用分光光度法；粗蛋白含量测定采用考马斯亮蓝G-250染色法；Vc含量测定采用分光光度法；可溶性糖含量测定采用蒽酮比色法；硝酸盐含量测定采用紫外分光光度法。试验是单因素实验设计方案，意味除了膜的不同或者有无膜，别的条件基本一致，所以这些指标如果有显著差异，都是由膜的不同所造成的，天数是播种后40天，试验数据下表1。
表1：
| 生菜A | 生菜B | 生菜C | |
| 光合速率[μmol/(m2*s)] | 7.66±0.23 | 8.77±0.17 | 9.36±0.11 |
| 蒸腾速率[mol/(m2*s)] | 3.96±0.21 | 4.17±0.1 | 4.47±0.17 |
| 维生素(mg/kg) | 238.33±4.41 | 279.67±3.18 | 314.34±11.02 |
| 硝酸盐(g/kg) | 535.67±28.75 | 442.33±10.84 | 439.56±13.08 |
| 总糖(mg/g) | 22.33±0.88 | 25.67±0.88 | 28.35±1.1 |
| 地上部分鲜重(g) | 105.67±4.1 | 112±2.52 | 118±3.01 |
| 根鲜重(g) | 7.65±0.13 | 8.3±0.12 | 8.9±0.22 |
| 地上部分干重(g) | 4.33±0.03 | 4.76±0.04 | 4.89±0.17 |
| 根干重(g) | 0.589±0.0072 | 0.556±0.0084 | 0.514±0.009 |
| 叶片数(片) | 9.9±0.15 | 10.1±0.23 | 10.35±0.11 |
| 叶面积(cm2) | 194±2.89 | 201.67±3.38 | 216.8±4.02 |
| 叶宽(mm) | 152±2.89 | 163.67±2.85 | 168.02±2.01 |
| 叶长(mm) | 177±3.61 | 177.67±2.33 | 181.2±3.42 |
| 株高(mm) | 15.8±2.89 | 16.87±3.38 | 17.3±4.11 |
| 株幅 | 172.33±3.18 | 174.33±3.18 | 183.25±1.37 |
不使用膜种植的黄瓜A、使用市售膜种植的黄瓜B和使用实施例1制备的长余辉转光膜种植的黄瓜C进行黄瓜生长指标试验。生菜生长指标动态测定说明：随机选取20株样本参数接近的生菜，重复3次。育苗后65天，试验数据下表2。
表2：
| 黄瓜A | 黄瓜B | 黄瓜C | |
| 总产量(kg/pot) | 0.77±0.0208 | 0.82±0.0208 | 0.88±0.0037 |
| 单果重(g) | 90.23±1.1 | 93.5±1.18 | 97.85±1.21 |
| 直径(mm) | 27.07±0.88 | 27.97±0.24 | 29.85±0.54 |
| 瓜长(cm) | 16.3±0.52 | 17.47±0.35 | 17.67±0.52 |
| 含水率(％) | 95.82±0.14 | 96.11±0.52 | 95.88±0.22 |
| 维生素(mg/kg) | 134.33±7.01 | 137.23±3.17 | 129.85±6.24 |
| 硝酸盐(mg/kg) | 227.59±9.24 | 186.32±5.29 | 182.12±2.9 |
| 可溶性糖(mg/g) | 8.64±0.06 | 9.26±0.09 | 9.68±0.06 |
| 有机酸(mg/g) | 7.6±0.32 | 8.1±0.17 | 7.78±0.19 |
实施例2
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Nd2O3为原料，按照化学式SrAl2O5/2N:0.03Eu2+，0.03Nd3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1350℃，灼烧时间为9小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚乙烯树脂50份、长余辉转光剂40份、2-(2-羟基-5-甲基苯基)苯并三唑3份、2,6-二叔丁基对甲酚3份、聚乙烯蜡4份；(2)在塑炼机将上述材料均匀混合，加热温度为200℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒1份、聚乙烯树脂99份，混合均匀后在吹膜机上吹制薄膜，加热温度为150℃。
实施例3
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及La2O3为原料，按照化学式SrAl2O2N4/3:0.02Eu2+，0.02La3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1400℃，灼烧时间为8小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚丙烯树脂75份、长余辉转光剂10份、2-(2-丁二酸5份、2,6-二叔丁基对甲酚5份、聚乙烯蜡5份；(2)在塑炼机将上述材料均匀混合，加热温度为160℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒6份、聚丙烯树脂94份，混合均匀后在吹膜机上吹制薄膜，加热温度为170℃。
实施例4
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Ho2O3为原料，按照化学式SrAl2O3/2N5/3:0.04Eu2+，0.04Ho3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1450℃，灼烧时间为7小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取乙烯-醋酸乙烯共聚物树脂70份、长余辉转光剂20份、2-(2-羟基-5-甲基苯基)苯并三唑2份、2,4,6三叔丁基苯酚水杨酸苯酯3份、硬脂酸锌5份；(2)在塑炼机将上述材料均匀混合，加热温度为180℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒8份、乙烯-醋酸乙烯共聚物树脂92份，混合均匀后在吹膜机上吹制薄膜，加热温度为180℃。
实施例5
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Pr2O3为原料，按照化学式SrAl2ON2:0.03Eu2+，0.03Pr3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1500℃，灼烧时间为6小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚氯乙烯树脂60份、长余辉转光剂20份、2-(2-羟基-5-甲基苯基)苯并三唑10份、2,4,6三叔丁基苯酚水杨酸苯酯5份、聚乙烯蜡5份；(2)在塑炼机将上述材料均匀混合，加热温度为180℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒5份、聚氯乙烯树脂95份，混合均匀后在吹膜机上吹制薄膜，加热温度为160℃。
实施例6
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Er2O3为原料，按照化学式SrAl2ON2:0.05Eu2+，0.05Er3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1450℃，灼烧时间为6小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚酰胺树脂65份、长余辉转光剂30份、丁二酸2份、2,6-二叔丁基对甲酚2份、硬脂酸锌1份；(2)在塑炼机将上述材料均匀混合，加热温度为190℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒2份、聚酰胺树脂98份，混合均匀后在吹膜机上吹制薄膜，加热温度为160℃。
实施例7
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Dy2O3、Nd2O3为原料，按照化学式SrAl2O5/2N:0.04Eu2+,0.02Dy3+,0.02Nd3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1400℃，灼烧时间为8小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚苯乙烯树脂80份、长余辉转光剂10份、丁二酸4份、2,4,6三叔丁基苯酚水杨酸苯酯3份、硬脂酸锌3份；(2)在塑炼机将上述材料均匀混合，加热温度为200℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒10份、聚丙烯树脂90份，混合均匀后在吹膜机上吹制薄膜，加热温度为200℃。
实施例8
长余辉转光剂制备：以高纯的SrCO3、Al2O3、AlN、Eu2O3及Dy2O3、La2O3为原料，按照化学式SrAl2O2N4/3:0.02Eu2+,0.01Dy3+,0.01La3+的化学计量比称取各原料；然后将获得的原料在玛瑙研钵中充分研磨后混合均匀，并将获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1300℃，灼烧时间为6.5小时，烧结气氛为5％的氢气和95％的氮气混合气，灼烧完成后样品随炉降温至室温，最后取出获得烧结体进行球磨、粉碎、洗涤、烘干即可获得所述长余辉转光剂。
转光膜吹制：(1)按重量百分比称取聚乙烯树脂55份、长余辉转光剂30份、丁二酸5份、2,4,6三叔丁基苯酚水杨酸苯酯5份、聚乙烯蜡5份；(2)在塑炼机将上述材料均匀混合，加热温度为160℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒8份、聚氯乙烯树脂92份，混合均匀后在吹膜机上吹制薄膜，加热温度为160℃。
图1为实施例1制备的转光剂激发光谱图。从图1中可以发现，其适合的激发光波长覆盖了250-425nm范围的紫光和近紫外光，能够有效吸收太阳光谱中的紫光和近紫外光。图2为实施例1-4的发射光谱图，图3为实施例5-8的发射光谱图，从图2和图3中可以看出，转光剂在紫光激发下可以发出650nm左右的红光，非常有利于植物的生长。图4所示为实施例1制备的转光剂余辉亮度衰减曲线图，从图1中可以看出，该转光剂的余辉时间非常长，即使到了夜间仍然能够持续发出红光，促进植物的生长。
Claims (9)
1.长余辉转光剂，其特征在于化学组成通式为：SrAl2O4-3x/2Nx:Eu2+，RE3+，其中Re3+是Dy3 +、Nd3+、La3+、Ho3+、Pr3+、Er3+稀土元素中的一种或几种的组合，x的取值范围为2/3≤x≤2。
2.长余辉转光剂的制备方法，其特征在于长余辉转光剂如权利要求1所述；制备方法包括以下步骤：(1)以SrCO3、Al2O3、AlN、Eu2O3及其它稀土氧化物为原料，按照化学式SrAl2O4-3x/2Nx:Eu2+，RE3+的化学计量比称取各原料；(2)将步骤(1)获得的原料在玛瑙研钵中充分研磨后混合均匀；(3)将步骤(2)获得的混合物放入刚玉坩埚中，然后将刚玉坩埚和混合物一起放入高温管式炉中进行灼烧，灼烧温度为1300-1500℃，灼烧时间为6-10小时，灼烧完成后样品随炉降温至室温，最后取出获得烧结体；(4)将步骤(3)获得的烧结体进行球磨粉碎，然后用蒸馏水洗涤烘干，即得所述长余辉转光剂。
3.长余辉转光剂的制备方法，其特征在于烧结气氛为5％的氢气和95％的氮气混合气。
4.一种长余辉转光膜，其特征在于包括薄膜树脂、改性助剂和权利要求1所述的长余辉转光剂；按重量百分比计，长余辉转光剂为0.1-2.0％，所述改性助剂为0.1％-5.0％，其余为薄膜树脂。
5.根据权利要求4所述的一种长余辉转光膜，其特征在于所述薄膜树脂的成分为聚乙烯、聚苯乙烯、聚氯乙烯、乙烯-醋酸乙烯共聚物、聚丙烯、聚酰胺中的一种或几种。
6.根据权利要求4所述的一种长余辉转光膜，其特征在于所述改性助剂为光稳定剂、抗氧化剂、润滑剂中的一种或几种。
7.根据权利要求6所述的一种长余辉转光膜，其特征在于所述光稳定剂为2-(2-羟基-5-甲基苯基)苯并三唑或丁二酸，抗氧化剂为2,6-二叔丁基对甲酚或2,4,6三叔丁基苯酚水杨酸苯酯、润滑剂为聚乙烯蜡或硬脂酸锌。
8.一种长余辉转光膜制备方法，其特征在于余辉转光膜如权利要求4所述，制备方法包括以下步骤：(1)按重量百分比称取薄膜树脂50-80份、长余辉转光剂10-40份、改性助剂3-30份；(2)在塑炼机将上述材料均匀混合，加热温度为150-200℃，然后利用造粒挤出机制作成转光母粒；(3)按重量百分比称取转光母粒1-10份、薄膜树脂90-99份，混合均匀后在吹膜机上吹制薄膜，加热温度为150-200℃。
9.根据权利要求8所述的一种长余辉转光膜制备方法，其特征在于改性助剂是光稳定剂1-10份、抗氧化剂1-10份、润滑剂1-10份。
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| CN101613601A (zh) * | 2009-07-23 | 2009-12-30 | 长春理工大学 | 白光LED用Sr-Al-O-N系列荧光粉 |
| WO2011008930A2 (en) * | 2009-07-15 | 2011-01-20 | Performance Indicator Llc | Phosphorescent phosphors |
| KR20120139127A (ko) * | 2011-06-16 | 2012-12-27 | 엘지이노텍 주식회사 | 형광체, 형광체 제조방법 및 발광 소자 |
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| KR20130051718A (ko) * | 2011-11-10 | 2013-05-21 | 금호전기주식회사 | 형광체 및 그 제조방법 |
| CN105400513A (zh) * | 2015-07-21 | 2016-03-16 | 杭州萤鹤光电材料有限公司 | 一种红色荧光粉及其制备方法 |
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| CN101613601A (zh) * | 2009-07-23 | 2009-12-30 | 长春理工大学 | 白光LED用Sr-Al-O-N系列荧光粉 |
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