CN113087946A - 一种基于应力发光材料的可重复记忆型应力薄膜的制备方法 - Google Patents
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Abstract
本发明涉及一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，属于应力发光材料技术领域。本发明将高纯的CaCO3、Ga2O3、Bi2O3和Tm2O3进行研磨混匀得到混合粉料A；混合粉料A置于温度为1200～1250℃、氧化气氛中高温烧结10～12h，研磨得到CaGa2O4:Bi3+,Tm3+应力发光粉；CaGa2O4:Bi3+,Tm3+应力发光粉与PMMA胶体混合均匀得到混合液体，混合液体置于模具中，保鲜膜包覆后加热固化模具中的胶体，得到可重复记忆型应力薄膜。本发明可重复记忆型应力薄膜具有较高的应力发光强度，可在长期重复使用过程中保持原有的应力发光强度，且可实时记录每次施力的痕迹；具有高应力发光亮度、高稳定性、高灵敏度和可重复性等特点。
Description
技术领域
本发明涉及一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，属于应力发光材料技术领域。
背景技术
应力发光材料的机械刺激的光子为特征，这在医疗健康诊断、生物力学传感、建筑结构探伤、激活光源的应用至关重要。目前，发现的应力发光材料方面的应用(CaAl2Si2O8:Eu2+、CaNb2O7:Pr3+等)存在以下缺点：(1)所施加的机械刺激转换成光能的效率较低，不能有效的产生亮度较高的应力发光，极大的限制了其在分析受力应用方面的精准度；(2)应力发光材料与胶体混合封装后，应力发光等光学性能严重下降，成为了其在涂层成膜领域的瓶颈；(3)由于传统的应力发光材料大多属于分形发光材料，应力发光由原子键和化学键的断裂产生，导致其可重复性极差，制约了应用潜力。
因此，急需稳定的高亮度、高灵敏度、可重复记忆型应力薄膜，以解决传统应力发光材料存在亮度低、封装后粉末在胶体中分散不均匀、可重复性差等问题。
发明内容
本发明针对现有技术应力发光材料的机械刺激问题，提供一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，本发明利用高温固相烧结和成膜处理，制备可均匀分散在PMMA薄膜中并具有高灵敏度、高亮度应力发光以及可重复记忆型的CaGa2O4:Bi3+,Tm3 +应力薄膜，该可重复记忆型应力薄膜具有较强的应力发光强度，可长期重复使用过程中保持原有的应力发光强度，且可实时记录每次施力的痕迹。
一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，具体步骤如下：
(1)将高纯的CaCO3、Ga2O3、Bi2O3和Tm2O3进行研磨混匀得到混合粉料A；
(2)将步骤(1)混合粉料A置于温度为1200～1250℃、氧化气氛中高温焙烧10～12h，研磨得到CaGa2O4:Bi3+,Tm3+应力发光粉；
(3)将步骤(2)CaGa2O4:Bi3+,Tm3+应力发光粉与PMMA胶体混合均匀得到混合液体，混合液体置于模具中，保鲜膜包覆后加热固化模具中的胶体，得到可重复记忆型应力薄膜；
以混合粉料A的摩尔分数为100％计，步骤(1)混合粉料A中CaCO3占30～35％、Ga2O3占60～65％、Bi2O3占1～5％和Tm2O3占1～5％；
所述步骤(2)氧化气氛为空气或O2/N2混合还原气氛，以体积分数计，O2/N2混合还原气氛中O2占90～95％；
所述步骤(3)CaGa2O4:Bi3+,Tm3+应力发光粉与PDMS胶体的质量比为1:1.8～2.0；
所述步骤(3)加热固化温度为80～100℃，固化时间为24～36h。
所述可重复记忆型应力薄膜可用于力学分析、损伤检测等领域。
本发明应力发光原理：在给与可重复记忆型CaGa2O4:Bi3+,Tm3+应力薄膜在施力过程中，可重复记忆型施力处的受力大小和范围均有所不同，应力发光材料CaGa2O4:Bi3+,Tm3+可以有效地将机械受力刺激转化为应力发光，将应力发光粉末材料CaGa2O4:Bi3+,Tm3+均匀分散在PMMA胶体封装成膜，即可赋予薄膜应力发光特性，实时的记录和施力的力度大小及范围，进行有效的受力分析。
本发明的有益效果是：
(1)本发明利用高温固相烧结和成膜处理，制备可均匀分散在PMMA薄膜中并具有高灵敏度、高亮度应力发光以及可重复记忆型的CaGa2O4:Bi3+,Tm3+应力薄膜，该可重复记忆型应力薄膜具有较强的应力发光强度，可长期重复使用过程中保持原有的应力发光强度，且可实时记录每次施力的痕迹；
(2)本发明可重复记忆型的CaGa2O4:Bi3+,Tm3+应力薄膜具有高应力发光亮度、高稳定性、高灵敏度和可重复性等特点，可作为记忆型材料应用于力学分析、损伤检测等领域；
(3)本发明可重复记忆型的CaGa2O4:Bi3+,Tm3+应力薄膜解决了传统应力发光材料存在亮度低、封装后粉末在胶体中分散不均匀、可重复性差等问题。
附图说明
图1为实施例1CaGa2O4基质、CaGa2O4:0.02Bi3+、CaGa2O4:0.02Bi3+,0.01Tm3+应力发光材料的XRD图；
图2为实施例1CaGa2O4:0.02Bi3+,0.01Tm3+的激发和发射光谱；
图3为实施例1CaGa2O4:0.02Bi3+的热释光光谱；
图4为实施例1CaGa2O4:0.02Bi3+在日光填充下不同时间后的热释光光谱；
图5为实施例1CaGa2O4:0.02Bi3+,0.01Tm3+粉末封装成膜后产生的应力发光现象；
图6为实施例1可重复记忆型应力薄膜内部结构图；
图7为实施例1可重复记忆型应力薄膜的示意图。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明，但本发明的保护范围并不限于所述内容。
实施例1：一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，具体步骤如下：
(1)将高纯的CaCO3、Ga2O3、Bi2O3和Tm2O3进行研磨混匀得到混合粉料A；以混合粉料A的摩尔分数为100％计，混合粉料A中CaCO3占30-35％、Ga2O3占60～65％、Bi2O3占1～5％和Tm2O3占1～5％；
(2)将步骤(1)混合粉料A置于温度为1200～1250℃、氧化气氛中高温焙烧10～12h，研磨得到CaGa2O4:Bi3+,Tm3+应力发光粉；其中氧化气氛为空气或O2/N2混合还原气氛，以体积分数计，O2/N2混合还原气氛中O2占90～95％；
(3)将步骤(2)CaGa2O4:Bi3+,Tm3+应力发光粉与PMMA胶体混合均匀得到混合液体，混合液体置于模具中，保鲜膜包覆后加热固化模具中的胶体，得到可重复记忆型应力薄膜；其中CaGa2O4:Bi3+,Tm3+应力发光粉与PDMS胶体的质量比为1:1.8～1:2；加热固化温度为80～100℃，固化时间为24～36h；
样品的具体工艺参数见表1，
表1样品的具体工艺参数
本实施例CaGa2O4基质、CaGa2O4:0.02Bi3+、CaGa2O4:0.02Bi3+,0.01Tm3+应力发光材料的XRD图见图1，从图1可知，样品掺杂Bi3+和Tm3+后的衍射峰均与CaGa2O4标准卡片PDFNO.160593匹配，均保持CaGa2O4纯相；
本实施例CaGa2O4:0.02Bi3+,0.01Tm3+的激发和发射光谱见图2，图中显示367nm的光能够有效的激发该样品，并且样品在367nm的最佳激发下可显示出523nm的绿光发射；
本实施例CaGa2O4:0.02Bi3+的热释光光谱见图3；CaGa2O4:0.02Bi3+热释光峰位强度随Tm3+掺杂浓度的变化趋势，当Tm3+浓度为0.01时热释光峰值达到最高，可重复记忆型应力薄膜在具有陷阱深度较深和浓度较高的陷阱；
本实施例CaGa2O4:0.02Bi3+在日光填充下不同时间后的热释光光谱见图4；表明该可重复记忆型应力薄膜随着日光填充时间的延长，热释光陷阱浓度逐渐上升，证实了该应力发光薄膜可被日光有效地填充；在使用前无需额外光源进行填充，更便于其使用和应用；
本实施例CaGa2O4:0.02Bi3+,0.01Tm3+粉末封装成膜后产生的应力发光现象见图5；CaGa2O4:0.02Bi3+,0.01Tm3+粉末在胶体中封装的十分均匀，并且能够产生明显的应力发光和应力磷光拖尾现象，证实了该薄膜具有良好的应力发光特性；
本实施例可重复记忆型应力薄膜内部结构图见图6；外层框架为固化之后的PMMA胶体，可使薄膜保持优异的柔韧性，CaGa2O4:0.02Bi3+,0.01Tm3+应力发光粉体均匀分散于PMMA胶体中，能够保持CaGa2O4:0.02Bi3+,0.01Tm3+应力发光粉体的应力发光特性；
本实施例可重复记忆型应力薄膜的示意图见图7，在给与薄膜施力后能够保存明显的受力痕迹，且在施力后保持一段时间；薄膜采用PMMA胶体封装具有足够的柔性和韧性，在施力过程中可以对人体施力部位起到有效地保护作用。该薄膜具有良好的可重复性，可在重复施力后保持原有的应力发光强度，便于该产品能够长时间反复使用。
实施例2：一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，具体步骤如下：
(1)将高纯的CaCO3、Ga2O3、Bi2O3和Tm2O3进行研磨混匀得到混合粉料A；以混合粉料A的摩尔分数为100％计，混合粉料A中CaCO3占30-35％、Ga2O3占60～65％、Bi2O3占1～5％和Tm2O3占1～5％；
(2)将步骤(1)混合粉料A置于温度为1200～1250℃、氧化气氛中高温焙烧10～12h，研磨得到CaGa2O4:Bi3+,Tm3+应力发光粉；其中氧化气氛为空气或O2/N2混合还原气氛，以体积分数计，O2/N2混合还原气氛中O2占90～95％；
(3)将步骤(2)CaGa2O4:Bi3+,Tm3+应力发光粉与PMMA胶体混合均匀得到混合液体，混合液体置于模具中，保鲜膜包覆后加热固化模具中的胶体，得到可重复记忆型应力薄膜；其中CaGa2O4:Bi3+,Tm3+应力发光粉与PDMS胶体的质量比为1:1.8～1:2；加热固化温度为80～100℃，固化时间为24～36h；
样品的具体工艺参数见表2，
表2样品的具体工艺参数
本实施例CaGa2O4基质、CaGa2O4:0.02Bi3+、CaGa2O4:0.02Bi3+,0.01Tm3+应力发光材料的XRD图可知，样品掺杂Bi3+和Tm3+后的衍射峰均与CaGa2O4标准卡片PDF NO.160593匹配，均保持CaGa2O4纯相；
本实施例CaGa2O4:0.02Bi3+,0.01Tm3+的激发和发射光谱图中显示367nm的光能够有效的激发该样品，并且样品在367nm的最佳激发下可显示出523nm的绿光发射；
本实施例CaGa2O4:0.02Bi3+的热释光光谱中，CaGa2O4:0.02Bi3+热释光峰位强度随Tm3+掺杂浓度的变化趋势，当Tm3+浓度为0.01时热释光峰值达到最高，可重复记忆型应力薄膜在具有陷阱深度较深和浓度较高的陷阱；
本实施例CaGa2O4:0.02Bi3+在日光填充下不同时间后的热释光光谱表明该可重复记忆型应力薄膜随着日光填充时间的延长，热释光陷阱浓度逐渐上升，证实了该应力发光薄膜可被日光有效地填充；在使用前无需额外光源进行填充，更便于其使用和应用；
本实施例CaGa2O4:0.02Bi3+,0.01Tm3+粉末封装成膜后能够产生明显的应力发光和应力磷光拖尾现象，证实了该薄膜具有良好的应力发光特性；
本实施例可重复记忆型应力薄膜的外层框架为固化之后的PMMA胶体，可使薄膜保持优异的柔韧性，CaGa2O4:0.02Bi3+,0.01Tm3+应力发光粉体均匀分散于PMMA胶体中，能够保持CaGa2O4:0.02Bi3+,0.01Tm3+应力发光粉体的应力发光特性；
本实施例可重复记忆型应力薄膜，在给与薄膜施力后能够保存明显的受力痕迹，且在施力后保持一段时间；薄膜采用PMMA胶体封装具有足够的柔性和韧性，在施力过程中可以对人体施力部位起到有效地保护作用。该薄膜具有良好的可重复性，可在重复施力后保持原有的应力发光强度，便于该产品能够长时间反复使用。
实施例3：一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，具体步骤如下：
(1)将高纯的CaCO3、Ga2O3、Bi2O3和Tm2O3进行研磨混匀得到混合粉料A；以混合粉料A的摩尔分数为100％计，混合粉料A中CaCO3占30-35％、Ga2O3占60～65％、Bi2O3占1～5％和Tm2O3占1～5％；
(2)将步骤(1)混合粉料A置于温度为1200～1250℃、氧化气氛中高温焙烧10～12h，研磨得到CaGa2O4:Bi3+,Tm3+应力发光粉；其中氧化气氛为空气或O2/N2混合还原气氛，以体积分数计，O2/N2混合还原气氛中O2占90～95％；
(3)将步骤(2)CaGa2O4:Bi3+,Tm3+应力发光粉与PMMA胶体混合均匀得到混合液体，混合液体置于模具中，保鲜膜包覆后加热固化模具中的胶体，得到可重复记忆型应力薄膜；其中CaGa2O4:Bi3+,Tm3+应力发光粉与PDMS胶体的质量比为1:1.8～1:2；加热固化温度为80～100℃，固化时间为24～36h；
样品的具体工艺参数见表3，
表3样品的具体工艺参数
本实施例CaGa2O4基质、CaGa2O4:0.02Bi3+、CaGa2O4:0.02Bi3+,0.01Tm3+应力发光材料的XRD图可知，样品掺杂Bi3+和Tm3+后的衍射峰均与CaGa2O4标准卡片PDF NO.160593匹配，均保持CaGa2O4纯相；
本实施例CaGa2O4:0.02Bi3+,0.01Tm3+的激发和发射光谱图中显示367nm的光能够有效的激发该样品，并且样品在367nm的最佳激发下可显示出523nm的绿光发射；
本实施例CaGa2O4:0.02Bi3+的热释光光谱中，CaGa2O4:0.02Bi3+热释光峰位强度随Tm3+掺杂浓度的变化趋势，当Tm3+浓度为0.01时热释光峰值达到最高，可重复记忆型应力薄膜在具有陷阱深度较深和浓度较高的陷阱；
本实施例CaGa2O4:0.02Bi3+在日光填充下不同时间后的热释光光谱表明该可重复记忆型应力薄膜随着日光填充时间的延长，热释光陷阱浓度逐渐上升，证实了该应力发光薄膜可被日光有效地填充；在使用前无需额外光源进行填充，更便于其使用和应用；
本实施例CaGa2O4:0.02Bi3+,0.01Tm3+粉末封装成膜后能够产生明显的应力发光和应力磷光拖尾现象，证实了该薄膜具有良好的应力发光特性；
本实施例可重复记忆型应力薄膜的外层框架为固化之后的PMMA胶体，可使薄膜保持优异的柔韧性，CaGa2O4:0.02Bi3+,0.01Tm3+应力发光粉体均匀分散于PMMA胶体中，能够保持CaGa2O4:0.02Bi3+,0.01Tm3+应力发光粉体的应力发光特性；
本实施例可重复记忆型应力薄膜，在给与薄膜施力后能够保存明显的受力痕迹，且在施力后保持一段时间；薄膜采用PMMA胶体封装具有足够的柔性和韧性，在施力过程中可以对人体施力部位起到有效地保护作用。该薄膜具有良好的可重复性，可在重复施力后保持原有的应力发光强度，便于该产品能够长时间反复使用。
上面对本发明的具体实施例作了详细说明，但是本发明并不限于上述实施例，在本领域普通技术人员所具备的知识范围内，还可以在不脱离本发明宗旨的前提下作出各种变化。
Claims (6)
1.一种基于应力发光材料的可重复记忆型应力薄膜的制备方法，其特征在于，具体步骤如下：
(1)将高纯的CaCO3、Ga2O3、Bi2O3和Tm2O3进行研磨混匀得到混合粉料A；
(2)将步骤(1)混合粉料A置于温度为1200～1250℃、氧化气氛中高温烧结10～12h，研磨得到CaGa2O4:Bi3+,Tm3+应力发光粉；
(3)将步骤(2)CaGa2O4:Bi3+,Tm3+应力发光粉与PMMA胶体混合均匀得到混合液体，混合液体置于模具中，保鲜膜包覆后加热固化模具中的胶体，得到可重复记忆型应力薄膜。
2.根据权利要求1所述基于应力发光材料的可重复记忆型应力薄膜的制备方法，其特征在于：以混合粉料A的摩尔分数为100％计，步骤(1)混合粉料A中CaCO3占30～35％、Ga2O3占60～65％、Bi2O3占1～5％和Tm2O3占1～5％。
3.根据权利要求1所述基于应力发光材料的可重复记忆型应力薄膜的制备方法，其特征在于：步骤(2)氧化气氛为空气或O2/N2混合还原气氛，以体积分数计，O2/N2混合还原气氛中O2占90～95％。
4.根据权利要求1所述基于应力发光材料的可重复记忆型应力薄膜的制备方法，其特征在于：步骤(3)CaGa2O4:Bi3+,Tm3+应力发光粉与PDMS胶体的质量比为1:1.8～2.0。
5.根据权利要求1所述基于应力发光材料的可重复记忆型应力薄膜的制备方法，其特征在于：步骤(3)加热固化温度为80～100℃，固化时间为24～36h。
6.权利要求1-5任一项所述制备方法所制备的可重复记忆型应力薄膜。
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| CN111148816A (zh) * | 2017-06-02 | 2020-05-12 | 奈科斯多特股份公司 | 包括经封裝之纳米颗粒之发光粒子及其用途 |
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