CN115557780A - 一种颜色可调蓄光陶瓷及其制备方法 - Google Patents
一种颜色可调蓄光陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明适用于蓄光陶瓷领域，提供了一种颜色可调蓄光陶瓷及其制备方法，所述方法包括：S01：称量，以原料粉体总质量为100％计，分别称取质量百分比为35％～44％的10～30目的石英原料、35％～40％的50～100目的石英原料、5％～15％的150～250目的石英原料，1％～9％的光色转换剂原料，1％～3％的硅烷偶联剂，其余为长余辉材料的原料粉体；S02：制粉，利用高温固相法制备所需的长余辉材料，即SrAl2O4:Eu2+,Dy3+或Sr2MgSi2O7:Eu2+,Dy3+，并通过过筛网过筛，得到所需要的长余辉基质材料，本发明内容的有益效果在于：实现了颜色可调的蓄光陶瓷的制备。
Description
技术领域
本发明属于蓄光陶瓷领域，尤其涉及一种颜色可调蓄光陶瓷及其制备方法。
背景技术
蓄光材料又称长余辉材料，是一种在激发光(可见光、紫外光)撤去以后仍可以长效发光的一种发光材料，其中典型代表包括SrAl2O4:Eu2+,Dy3+(黄绿色)、Sr2MgSi2O7:Eu2+,Dy3+(蓝色)等，因其具有稳定的持久自发光特点，近年来基于该材料的应用领域也在不断地拓展。基于蓄光材料的蓄光陶瓷及其制备方法正在成为研究热点。石英陶瓷由于具有较高的耐酸碱侵蚀性能和抗热震性，此外热膨胀系数低，体积稳定性好等优势，常常被选作复合材料的基质相。近年来研究人员也在不断地尝试将蓄光材料与陶瓷基体复合开发出一种蓄光陶瓷，该类陶瓷在保证陶瓷体本身硬度高、耐磨性强、使用寿命长的同时也拓宽了其功能性，可适用于消防救援，应急通道等。
然而目前已有的蓄光类陶瓷并没有全色域制备技术和特性，如中国专利文献“一种具有超高亮度的蓄光型复相陶瓷材料及其制备方法”(CN201910587392.9)中仅仅提出了一种单色性的高亮度的蓄光型陶瓷，并没有提到基于蓄光陶瓷实现全色域，再如：“一种消防指示用多色系蓄光陶瓷及其制备方法”(CN201910587345.4)中虽有提到采用不同基质的蓄光材料开发出一种蓄光陶瓷，但所需用的蓄光材料基质过于分散，不能实现基于单一蓄光材料下的多色蓄光陶瓷。
发明内容
本发明实施例的目的在于提供一种颜色可调蓄光陶瓷及其制备方法，旨在解决背景技术中确定的现有技术存在的问题。
本发明实施例是这样实现的，一种颜色可调蓄光陶瓷的其制备方法，所述方法包括：
S01：称量，以原料粉体总质量为100％计，分别称取质量百分比为35％～44％的10～30目的石英原料、35％～40％的50～100目的石英原料、5％～15％的150～250目的石英原料，1％～9％的光色转换剂原料，1％～3％的硅烷偶联剂，其余为长余辉材料的原料粉体；
S02：制粉，利用高温固相法制备所需的长余辉材料，即SrAl2O4:Eu2+,Dy3+或Sr2MgSi2O7:Eu2+,Dy3+，并通过过筛网过筛，得到所需要的长余辉基质材料；
S03：包覆，首先将S02所得到的长余辉材料，与硅烷偶联剂混合经过水热法包裹有机物层，然后再利用溶胶凝胶法再包裹一层光色转换剂得到，然后再对该材料进行煅烧除去有机物，最终得到光色转换剂包覆的长余辉材料；
S04：混料，将S03称量的粉体原料置于球磨罐内，同时加入磨球和去离子水进行球磨混合；
S05：成型，将S04球磨后的浆料进行真空除泡处理，然后将除泡后的浆料注入模具中成型，得到素坯；
S06：干燥，将S05得到的素坯静置6～13小时后进行脱模，然后置于干燥箱内干燥；
S07：烧结，将S06干燥后的素坯在还原气氛下进行高温煅烧，煅烧温度为750～1150℃，保温时间为2.5～5.5h，随后随炉冷却至室温，即得到蓄光陶瓷基体。
优选地，在S01中的光色转换剂为香豆素类光色转换剂，包括红色转换剂、蓝色转换剂和绿色转换剂中的一种或者几种。
优选地，在S02中过筛网的目数为200-500目，过筛时间为3-7小时。
优选地，在S02中，所述球磨的转速为150～320r/min，球磨时间为7～14h。
优选地，所述真空除泡的真空度为-10～-30kpa，除泡时间为30～50min。
优选地，所述SrAl2O4:Eu2+,Dy3+的原料粉体为SrCO3、Al2O3、Eu2O3和Dy2O3，所述Sr2MgSi2O7:Eu2+,Dy3+的原料粉体为SrCO3、H2SiO3、4MgCO3Mg(OH)25H2O、Eu2O3和Dy2O3，根据化学式SrAl2O4:Eu2+,Dy3+中各元素的化学计量比称量、混合再经高温固相法烧汁而成得到。
优选地，一种颜色可调蓄光陶瓷，采用如前述任一所述制备方法所制得。
本发明实施例提供的颜色可调蓄光陶瓷及其制备方法，采用了光色转换剂包覆长余辉材料进而制备颜色可调的蓄光陶瓷，有效解决了现有技术中蓄光陶瓷颜色单一的问题，进而实现了低成本制备高品质颜色可调的蓄光陶瓷；由于采用了多种光色转换剂与长余辉材料高效组合进而制备出颜色可控可调的蓄光陶瓷用基材，有效解决了现有技术中蓄光陶瓷无法实现颜色可调可控的问题，进而实现了低成本制备高品质颜色可调的蓄光陶瓷。
附图说明
图1为本发明实施例提供的长余辉材料与光色转换剂结合后微观结构图；
图2为本发明实施例提供的蓄光陶瓷色坐标图；
图3为本发明实施例提供的长余辉材料与光色转换剂结合后XRD图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
以下结合具体实施例对本发明的具体实现进行详细描述。
为本发明的一个实施例提供的一种颜色可调蓄光陶瓷的制备方法，包括：
S01：称量，以原料粉体总质量为100％计，分别称取质量百分比为35％～44％的10～30目的石英原料、35％～40％的50～100目的石英原料、5％～15％的150～250目的石英原料，1％～9％的光色转换剂原料，1％～3％的硅烷偶联剂，其余为长余辉材料的原料粉体；
S02：制粉，利用高温固相法制备所需的长余辉材料，即SrAl2O4:Eu2+,Dy3+或Sr2MgSi2O7:Eu2+,Dy3+，并通过过筛网过筛，得到所需要的长余辉基质材料；即将稀土离子掺杂入SrAl2O4或Sr2MgSi2O7中；
S03：包覆，首先将S02所得到的长余辉材料，与硅烷偶联剂混合经过水热法包裹有机物层，然后再利用溶胶凝胶法再包裹一层光色转换剂得到，然后再对该材料进行煅烧除去有机物，最终得到光色转换剂包覆的长余辉材料；
S04：混料，将S03称量的粉体原料置于球磨罐内，同时加入磨球和去离子水进行球磨混合；
S05：成型，将S04球磨后的浆料进行真空除泡处理，然后将除泡后的浆料注入模具中成型，得到素坯；
S06：干燥，将S05得到的素坯静置6～13小时后进行脱模，然后置于干燥箱内干燥；
S07：烧结，将S06干燥后的素坯在还原气氛下进行高温煅烧，煅烧温度为750～1150℃，保温时间为2.5～5.5h，随后随炉冷却至室温，即得到蓄光陶瓷基体。
作为本发明的一种优选实施例，在S01中的光色转换剂为香豆素类光色转换剂，包括红色转换剂、蓝色转换剂和绿色转换剂中的一种或者几种。
作为本发明的另一种优选实施例，在S02中过筛网的目数为200-500目，过筛时间为3-7小时。
所述球磨的转速为150～320r/min，球磨时间为7～14h。
作为本发明的另一种优选实施例，所述真空除泡的真空度为-10～-30kpa，除泡时间为30～50min。
作为本发明的另一种优选实施例，所述SrAl2O4:Eu2+,Dy3+的原料粉体为SrCO3、Al2O3、Eu2O3和Dy2O3，所述Sr2MgSi2O7:Eu2+,Dy3+的原料粉体为SrCO3、H2SiO3、4MgCO3Mg(OH)25H2O、Eu2O3和Dy2O3，根据化学式SrAl2O4:Eu2+,Dy3+中各元素的化学计量比称量、混合再经高温固相法烧汁而成得到。
一种颜色可调蓄光陶瓷，采用上述任一所述制备方法所制得。
下面结合具体的实施例来进行说明。
实施例1
一种颜色可调蓄光陶瓷及其制备方法，方法如下：
(1)称量：以原料粉体总质量为100％计，分别称取质量百分比为35％的10～30目的石英原料、40％的50～100目的石英原料、5％％的150～250目的石英原料，1％～4％的红色光色转换剂原料，1％的硅烷偶联剂，其余为长余辉材料的原料粉体；
(2)制粉：利用高温固相法制备所需的长余辉材料，SrAl2O4:Eu2+,Dy3+(黄绿色)，并通过过筛网过筛，得到所需要的长余辉基质材料；
(3)包覆：首先将步骤(2)所得到的长余辉材料，与硅烷偶联剂混合经过水热法包裹有机物层，然后再利用溶胶凝胶法再包裹一层光色转换剂得到，然后再对该材料进行煅烧除去有机物，最终得到光色转换剂包覆的长余辉材料。
(4)混料：将步骤(3)称量的粉体原料置于球磨罐内，同时加入磨球和去离子水进行球磨混合；
(5)成型：将步骤(4)球磨后的浆料进行真空除泡处理，然后将除泡后的浆料注入模具中成型，得到素坯；
(6)干燥：将步骤(5)得到的素坯静置6～13小时后进行脱模，然后置于干燥箱内干燥；
(7)烧结：将步骤(6)干燥后的素坯在还原气氛下进行高温煅烧，煅烧温度为750～1150℃，保温时间为2.5～5.5h，随后随炉冷却至室温，即得到蓄光陶瓷基体。
上述本申请实施例中的技术方案，至少具有如下的技术效果或优点：
见附图1，本实施例制备的红色转换剂与绿色长余辉材SrAl2O4:Eu2+,Dy3+进行有机结合后的SEM图以及EDS元素分析，其中随着掺杂的红色转换剂的浓度越大，绿色长余辉材料SrAl2O4:Eu2+,Dy3+颗粒表面吸附的红色转换剂的密度也随之增大。
见附图2，本实施例制备的颜色可调的蓄光陶瓷的发光颜色，随着掺杂的红色转换剂的浓度越大，蓄光陶瓷表现为从发绿色光到红色光的逐渐变化，表现在CIE图中便如图2所示。
见附图3，本实施例制备的红色转换剂与绿色长余辉材SrAl2O4:Eu2+,Dy3+进行有机结合后的XRD图，由于掺杂的光色转换剂的含量相对较小，并未对SrAl2O4:Eu2+,Dy3+物相结构产生重大改变，因此蓄光陶瓷的发光效果较好。
实施例2
一种颜色可调的蓄光陶瓷的制备方法，方法如下：
(1)称量：以原料粉体总质量为100％计，分别称取质量百分比为36的10～30目的石英原料、39％的50～100目的石英原料、6％％的150～250目的石英原料，1％～4％的红色光色转换剂原料，1％～3％的硅烷偶联剂，其余为长余辉材料的原料粉体；
(2)制粉：利用高温固相法制备所需的长余辉材料，Sr2MgSi2O7:Eu2+,Dy3+(蓝色)等，并通过过筛网过筛，得到所需要的长余辉基质材料；
(3)包覆：首先将步骤(2)所得到的长余辉材料，与硅烷偶联剂混合经过水热法包裹有机物层，然后再利用溶胶凝胶法再包裹一层光色转换剂得到，然后再对该材料进行煅烧除去有机物，最终得到光色转换剂包覆的长余辉材料；
(4)混料：将步骤(3)称量的粉体原料置于球磨罐内，同时加入磨球和去离子水进行球磨混合；
(5)成型：将步骤(4)球磨后的浆料进行真空除泡处理，然后将除泡后的浆料注入模具中成型，得到素坯；
(6)干燥：将步骤(5)得到的素坯静置6小时后进行脱模，然后置于干燥箱内干燥；
(7)烧结：将步骤(6)干燥后的素坯在还原气氛下进行高温煅烧，煅烧温度为850℃，保温时间为3.5h，随后随炉冷却至室温，即得到蓄光陶瓷基体。
经过观测，本实施例2中所制备得到的一种颜色可调低成本蓄光陶瓷主要结构性能，色坐标、微观结构与实施例1相似。
本发明上述实施例中提供了一种颜色可调蓄光陶瓷的制备方法，采用了光色转换剂包覆长余辉材料进而制备颜色可调的蓄光陶瓷，有效解决了现有技术中蓄光陶瓷颜色单一的问题，进而实现了低成本制备高品质颜色可调的蓄光陶瓷；由于采用了多种光色转换剂与长余辉材料高效组合进而制备出颜色可控可调的蓄光陶瓷用基材，有效解决了现有技术中蓄光陶瓷无法实现颜色可调可控的问题，进而实现了低成本制备高品质颜色可调的蓄光陶瓷。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (7)
1.一种颜色可调蓄光陶瓷的制备方法，其特征在于，所述方法包括：
S01：称量，以原料粉体总质量为100％计，分别称取质量百分比为35％～44％的10～30目的石英原料、35％～40％的50～100目的石英原料、5％～15％的150～250目的石英原料，1％～9％的光色转换剂原料，1％～3％的硅烷偶联剂，其余为长余辉材料的原料粉体；
S02：制粉，利用高温固相法制备所需的长余辉材料，即SrAl2O4:Eu2+,Dy3+或Sr2MgSi2O7:Eu2+,Dy3+，并通过过筛网过筛，得到所需要的长余辉基质材料；
S03：包覆，首先将S02所得到的长余辉材料，与硅烷偶联剂混合经过水热法包裹有机物层，然后再利用溶胶凝胶法再包裹一层光色转换剂得到，然后再对该材料进行煅烧除去有机物，最终得到光色转换剂包覆的长余辉材料；
S04：混料，将S03称量的粉体原料置于球磨罐内，同时加入磨球和去离子水进行球磨混合；
S05：成型，将S04球磨后的浆料进行真空除泡处理，然后将除泡后的浆料注入模具中成型，得到素坯；
S06：干燥，将S05得到的素坯静置6～13小时后进行脱模，然后置于干燥箱内干燥；
S07：烧结，将S06干燥后的素坯在还原气氛下进行高温煅烧，煅烧温度为750～1150℃，保温时间为2.5～5.5h，随后随炉冷却至室温，即得到蓄光陶瓷基体。
2.根据权利要求1所述的颜色可调蓄光陶瓷的制备方法，其特征在于，在S01中的光色转换剂为香豆素类光色转换剂，包括红色转换剂、蓝色转换剂和绿色转换剂中的一种或者几种。
3.根据权利要求2所述的颜色可调蓄光陶瓷的制备方法，其特征在于，在S02中过筛网的目数为200-500目，过筛时间为3-7小时。
4.根据权利要求1所述的颜色可调蓄光陶瓷的制备方法，其特征在于，在S02中，所述球磨的转速为150～320r/min，球磨时间为7～14h。
5.根据权利要求2所述的颜色可调蓄光陶瓷的制备方法，其特征在于，所述真空除泡的真空度为-10～-30kpa，除泡时间为30～50min。
6.根据权利要求1所述的颜色可调蓄光陶瓷的制备方法，其特征在于，所述SrAl2O4:Eu2+,Dy3+的原料粉体为SrCO3、Al2O3、Eu2O3和Dy2O3，所述Sr2MgSi2O7:Eu2+,Dy3+的原料粉体为SrCO3、H2SiO3、4MgCO3Mg(OH)25H2O、Eu2O3和Dy2O3，根据化学式SrAl2O4:Eu2+,Dy3+中各元素的化学计量比称量、混合再经高温固相法烧汁而成得到。
7.一种颜色可调蓄光陶瓷，其特征在于，采用如权利要求1-6任一所述制备方法所制得。
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