CN106756788B - 一种负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法 - Google Patents
一种负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法 Download PDFInfo
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Abstract
本发明公开了一种负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法,步骤是:首先,将白色二氧化钛粉末压片,得到压强为140~200Mpa的靶材;然后,将靶材置于真空罐,抽真空使真空罐内压力达到1×10‑6‑1×104Pa;调节脉冲激光器的入射激光束与靶材之间的角度为10~45°,激光器的基片基底与靶材的距离为15~50mm;开启脉冲激光器,调节激光脉宽、激光能量、激光波长和频率,激光聚焦辐照真空罐中的靶材,处理一定时间,在基片上得到黑色二氧化钛薄膜,将黑色二氧化钛薄膜上的黑色二氧化钛刮下即得到黑色二氧化钛粉末。本发明制备过程简单快速,原材料费用低,反应时间短。
Description
技术领域
本发明属于无机材料制备的技术领域,具体涉及一种真空环境下通过脉冲激光溅射沉积法制备黑色二氧化钛粉末或薄膜的方法。
背景技术
二氧化钛作为一种应用广泛的半导体催化剂,目前可以应用于太阳能电池,光催化裂解水释放氢气和氧气,也可以用来降解环境污染物。由于二氧化钛属于宽带隙半导体(3.0-3.2eV),所以其只能吸收太阳光谱内的紫外线区域,而这一部分只有整个太阳能的3%~5%,这就大大降低了二氧化钛的应用范围和催化效率。因此,要想提高二氧化钛的光催化活性,就需要增强其对可见光的吸收,拓宽其光响应范围。
为了提高二氧化钛对可见光的吸收,提高其光催化效率,研究者们尝试了很多方法对二氧化钛进行改性(如离子掺杂、贵金属沉积、半导体复合、染料敏化等)。然而,改进后的二氧化钛对可见光的吸收仍然不足。2011年,Chen等通过高压下氢化处理二氧化钛5天得到了氢掺杂的核壳结构的黑色二氧化钛,大大提高了二氧化钛对可见光的吸收及其光催化性能,为二氧化钛的改性提供了另一条途径(Chen,X.,Liu,L.,Yu,P.Y.&Mao,S.S.Increasing solar absorption for photocatalysis with black hydrogenatedtitanium dioxide nanocrystals.Science 331,746-750)。此后,研究者们还探索出了氢等离子体辅助氢化法、化学还原法、化学氧化法等来制备黑色二氧化钛。其中,氢还原法涉及到了高温高压,存在易燃易爆等不安全因素且对设备要求比较高;氢等离子体辅助氢化法有氢气的加入,与此同时还需要加热,同样增加了实验的风险;化学法制备过程复杂,耗时比较长。这些方法涉及的还原、高温高压等制备原理,限制了黑色二氧化钛的制备效率。
发明内容
针对黑色二氧化钛制备方法复杂且制备效率较低的问题,本发明提出了一种真空环境下通过脉冲激光溅射沉积法制备黑色二氧化钛的方法。该方法操作简单、成本低、反应时间短,能够高效快速的合成黑色二氧化钛。所得黑色二氧化钛大大提高了对可见光的吸收,拓宽了光响应范围。
为了解决上述技术问题,本发明提出的一种负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法,步骤是:首先,将白色二氧化钛粉末压片,得到压强为140~200Mpa的白色二氧化钛靶材;然后,将制得的白色二氧化钛靶材置于真空罐,抽真空使真空罐内压力达到1×10-6-1×104Pa;调节脉冲激光器的入射激光束与所述白色二氧化钛靶材之间的角度为10~45°,激光器的基片基底与所述白色二氧化钛靶材的距离为15~50mm;开启脉冲激光器,调节激光脉宽、激光能量、激光波长和频率,激光聚焦辐照真空罐中的白色二氧化钛靶材,处理一定时间,在基片上得到黑色二氧化钛薄膜,将黑色二氧化钛薄膜上的黑色二氧化钛刮下即得到黑色二氧化钛粉末。
上述负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法中,所述激光器的基片为耐高温基片,耐温不低于550℃;可以选用石英基或是K9玻璃基片。
所述激光脉宽为10ns-50ps,激光能量为450-1500mJ,激光波长为532-1064nm,频率为5~20Hz。激光聚焦辐照白色二氧化钛靶材每点处理时间为30~120s。
与现有技术相比,本发明的有益效果是:
(1)本发明中,只需要激光器和真空系统即可,真空环境下,利用激光聚焦辐照白色二氧化钛靶材,靶材吸收激光能量迅速升温气化产生高温等离子体,提高了常规热处理的热力学和动力学,从而快速制得黑色二氧化钛粉末,提高了黑色二氧化钛的制备效率;(2)室温条件下,激光溅射沉积过程中,粒子沉积到基底上迅速冷却,限制了晶体的长大;(3)调节激光电压(能量),能够控制产物中锐钛矿相和金红石相的比例;(4)与原有制备黑色二氧化钛的的方法相比,本发明操作简单,对设备要求低,反应时间短,避免了氢气等危险气体的使用,降低了实验的危险性;(5)本发明制备的黑色二氧化钛粉末大大提高了对可见光的吸收,拓宽了光响应范围,为其光催化效率的提高奠定了基础。
附图说明
图1为实施例1制备的黑色二氧化钛粉末与原始的白色二氧化钛粉末的实物对比图;
图2为实施例1制备的黑色二氧化钛粉末与原始的白色二氧化钛的X射线衍射谱图;
图3(a)为实施例1制备的黑色二氧化钛粉末的透射电镜照片;
图3(b)为原始的白色二氧化钛的透射电镜照片;
图4(a)为实施例1制备的黑色二氧化钛粉末的高分辨透射电镜照片及选区电子衍射图;
图4(b)为原始的白色二氧化钛的高分辨透射电镜照片及选区电子衍射图;
图5为实施例1制备的黑色二氧化钛粉末与原始的白色二氧化钛的紫外-可见-近红外的吸收谱图。
具体实施方式
下面结合附图和具体实施例对本发明技术方案作进一步详细描述,所描述的具体实施例仅对本发明进行解释说明,并不用以限制本发明。
实施例1:黑色二氧化钛粉末的制备,步骤是:
用压片机将购买的锐钛矿型的白色二氧化钛压成直径为2cm厚度为2mm的圆形靶材,压强为200MPa;将该圆形靶材置于真空罐中,抽真空使真空罐中的内压力为1×103Pa;调节脉冲激光器的入射激光束与圆形靶材之间的角度为10°,脉冲激光器的基片选用为耐高温的石英基片或是K9玻璃基片,调整基片基底与圆形靶材的距离为25mm,以确保产物可以溅射沉积到基片上;开启脉冲激光器,调节脉冲激光器的激光脉宽为8ns,波长为1064nm,能量为950mJ,频率为10Hz;激光聚焦为直径为2mm的光斑辐照真空罐中的白色二氧化钛的圆形靶材,聚焦点辐照时间每点30s,则在基片基底上得到黑色二氧化钛薄膜;关闭脉冲激光器,取出基片,将基片基底上的黑色二氧化钛轻轻刮下即得到黑色二氧化钛粉末。
图1为实施例1制备的黑色二氧化钛粉末与原始的白色二氧化钛粉末的实物对比照片;图2为实施例1制备的黑色二氧化钛粉末与原始的白色二氧化钛的X射线衍射谱图;图3(a)示出了实施例1制备的黑色二氧化钛粉末的透射电镜照片;图3(b)为原始的白色二氧化钛的透射电镜照片;图4(a)为实施例1制备的黑色二氧化钛粉末的高分辨透射电镜照片及选区电子衍射图;图4(b)为原始的白色二氧化钛的高分辨透射电镜照片及选区电子衍射图;图5为实施例1制备的黑色二氧化钛粉末与原始的白色二氧化钛的紫外-可见-近红外的吸收谱图。
实施例2:黑色二氧化钛粉末的制备,步骤是:
用压片机将购买的锐钛矿型的白色二氧化钛压成直径为2cm厚度为1mm的圆形靶材,压强为160MPa;将该圆形靶材置于真空罐中,抽真空使真空罐中的内压力为1×10-3Pa;调节脉冲激光器的入射激光束与圆形靶材之间的角度为45°,脉冲激光器的基片选用为耐高温的石英基片或是K9玻璃基片,调整基片基底与圆形靶材的距离为40mm,以确保产物可以溅射沉积到基片上;开启脉冲激光器,调节脉冲激光器的激光脉宽为10ns,波长为1064nm,能量为500mJ,频率为15Hz;激光聚焦为直径为1mm的光斑辐照真空罐中的白色二氧化钛的圆形靶材,聚焦点辐照时间每点60s,则在基片基底上得到黑色二氧化钛薄膜;关闭脉冲激光器,取出基片,将基片基底上的黑色二氧化钛轻轻刮下即得到黑色二氧化钛粉末。
实施例3:黑色二氧化钛粉末的制备,步骤是:
用压片机将购买的锐钛矿型的白色二氧化钛压成直径为3cm厚度为3mm的圆形靶材,压强为140MPa;将该圆形靶材置于真空罐中,抽真空使真空罐中的内压力为1×10-6Pa;调节脉冲激光器的入射激光束与圆形靶材之间的角度为15°,脉冲激光器的基片选用石英基片,调整基片基底与圆形靶材的距离为15mm,以确保产物可以溅射沉积到基片上;开启脉冲激光器,调节脉冲激光器的激光脉宽为50ns,波长为532nm,能量为450mJ,频率为10Hz;激光聚焦为直径为1mm的光斑辐照真空罐中的白色二氧化钛的圆形靶材,聚焦点辐照时间每点90s,则在基片基底上得到黑色二氧化钛薄膜;关闭脉冲激光器,取出基片,将基片基底上的黑色二氧化钛轻轻刮下即得到黑色二氧化钛粉末。
实施例4:黑色二氧化钛粉末的制备,步骤是:
用压片机将购买的锐钛矿型的白色二氧化钛压成直径为4cm厚度为3mm的圆形靶材,压强为140MPa;将该圆形靶材置于真空罐中,抽真空使真空罐中的内压力为1×104Pa;调节脉冲激光器的入射激光束与圆形靶材之间的角度为30°,脉冲激光器的基片选用石英基片,调整基片基底与圆形靶材的距离为50mm,以确保产物可以溅射沉积到基片上;开启脉冲激光器,调节脉冲激光器的激光脉宽为10ns,波长为1064nm,能量为1500mJ,频率为5Hz;激光聚焦为直径为2mm的光斑辐照真空罐中的白色二氧化钛的圆形靶材,聚焦点辐照时间每点120s,则在基片基底上得到黑色二氧化钛薄膜;关闭脉冲激光器,取出基片,将基片基底上的黑色二氧化钛轻轻刮下即得到黑色二氧化钛粉末。
本发明中黑色二氧化钛的制作过程简单快速,原材料费用低,反应时间短,是一种高效经济的合成方法。
尽管上面结合附图对本发明进行了描述,但是本发明并不局限于上述的具体实施方式,上述的具体实施方式仅仅是示意性的,而不是限制性的,本领域的普通技术人员在本发明的启示下,在不脱离本发明宗旨的情况下,还可以做出很多变形,这些均属于本发明的保护之内。
Claims (3)
1.一种负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法,其特征在于,包括以下步骤:
步骤一、将原始的白色二氧化钛粉末压片,得到压强为140~200Mpa的白色二氧化钛靶材;
步骤二、将步骤一制得的白色二氧化钛靶材置于真空罐,抽真空使真空罐内压力达到1×10-6-1×104Pa;调节脉冲激光器的入射激光束与所述白色二氧化钛靶材之间的角度为10~45°,激光器的基片基底与所述白色二氧化钛靶材的距离为15~50mm;开启脉冲激光器,调节激光脉宽、激光能量、激光波长和频率,激光聚焦辐照真空罐中的白色二氧化钛靶材,靶材吸收激光能量迅速升温气化产生高温等离子体,处理一定时间,在基片上得到黑色二氧化钛薄膜,将黑色二氧化钛薄膜上的黑色二氧化钛刮下即得到黑色二氧化钛粉末。
2.根据权利要求1所述负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法,其特征在于,所述激光器的基片为耐高温基片,耐温不低于550℃。
3.根据权利要求1所述负压环境下脉冲激光溅射沉积制备黑色二氧化钛粉末的方法,其特征在于,所述激光脉宽为10ns-50ps,激光能量为450-1500mJ,激光波长为532-1064nm,频率为5~20Hz;激光聚焦辐照白色二氧化钛靶材每点处理时间为30~120s。
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