CN111389428B - 一种SiP2量子点/光催化材料及其制备方法 - Google Patents
一种SiP2量子点/光催化材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及光催化半导体材料技术领域，具体为一种SiP2量子点/光催化材料及其制备方法。通过机械剥离的的方法将大颗粒的SiP2单晶超声成小尺寸的SiP2量子点，然后通过滴加、旋涂或者浸渍的方法将SiP2量子点均匀的覆盖在光催化材料的表面得到SiP2/光催化材料复合材料。本发明中SiP2量子点能够拓宽吸光范围、加快电子分离与传输、降低光催化能垒、提高效率，此外用量少，价格低，不会对TiO2等光催化剂材料的稳定性等造成影响。另外通过机械剥离获得纳米级SiP2是高度可行的并且表现出优异的光催化性能，其制备方法简单，因此将SiP2量子点与半导体光催化剂进行复合提高催化效率将有很大的应用前景及意义。
Description
技术领域
本发明涉及光催化半导体材料技术领域，具体为一种SiP2量子点/光催化材料及其制备方法。
背景技术
二十一世纪，环境污染与能源危机依然是人类社会发展过程中亟待解决的难题。因此，开发和利用清洁的可再生资源(如：太阳能、水能、风能、生物质能等)至关重要。20世纪 70年代，随着“氢能经济”的提出，氢能作为一种理想的清洁能源日益受到重视。但是，氢能的制取须由消耗一次能源进行，传统制法面临着化石能源消耗及CO2排放问题，不能有效缓解上述两大危机。太阳能是取之不尽的一次能源，而占地球表面面积70％的水资源里蕴藏着充足的氢源，经过太阳光的照射，可将水分解产生氢气，而氢气作为燃料燃烧之后又生成了水，该过程清洁无污染，是一个良性循环。因此，使用太阳能从水中产生氢(H2)被认为是解决全球能源问题的一种有前途的策略，尤其是通过利用半导体光催化剂进行光催化水分解已显示出巨大的潜力。然而，尽管在过去的几十年中在该领域取得了巨大的成就，但是通过太阳能进行光催化的技术还存在一些改进的空间，光催化反应还存在着可见光利用效率不高、光催化剂制备过程复杂、催化效率低等不足，开发由太阳光驱动的高效具有成本效益且稳定的光催化剂仍然是一个巨大的挑战。
上世纪八十年代至九十年代中期，ZnS、ZnO、CdS、SrTiO3等一系列半导体金属氧化物、硫化物以及复合金属氧化物的光催化性能均被研究。随着半导体能带理论的完善和相关测量技术的进步，人们对光催化现象及机理的认识逐渐加深。但是由于紫外光仅占太阳光的 4％左右，且已知的光催化剂量子效率不高，利用太阳光催化分解水制氢一直未能投入实际应用。而且氢存储、氢输运等一系列安全技术问题有待解决，使得氢能的应用研究始终停留在理论阶段。但人们对TiO2光催化剂的研究却不断发展，且其在环保等方面的应用优势逐步显现了出来。因此，大量的方法被用于提高光催化剂的性能，主要包括与金属/非金属离子掺杂、窄禁带半导体耦合、贵金属沉积以及金属化合物表面敏化等。
目前对于非金属元素掺杂的研究主要有N,P,S等元素,例如N掺杂的TiO2，N原子与O 原子半径差不多，具有较小的电离能和高稳定性，因而可以比较容易掺杂到TiO2的晶格中，改变TiO2的电子结构。除了掺杂非金属杂原子外，掺杂金属杂原子也能够改变半导体的禁带宽度。例如采用W对TiO2进行掺杂不仅能够减小TiO2的禁带宽度，还能够抑制锐钛矿相的 TiO2发生相转移为金红石结构的TiO2。同时W掺杂到TiO2的晶格中还能产生氧缺陷，而氧缺陷的形成有利于捕获光生电荷，促进了光生电子和空穴的分离。
半导体复合是一种有效提高光催化效率的手段。按组分性质的不同,复合半导体可分为半导体-TiO2复合物和绝缘体-TiO2复合物。Bessekhouad等通过直接混合法分别制得了Bi2S3-TiO2和CdS-TiO2复合光催化剂,通过Uv-vis光谱分析可知,两者均能大量吸收可见光,它们的吸收波长分别达到800nm和600nm。一般来说,可通过提高电荷分离效率和延伸光激发的波长范围来提高半导体与复合的光催化活性。而绝缘体与的复合主要受催化剂的粒径、比表面积、表面酸性、光吸收性能等物理性质所影响。而在复合半导体中主要考虑不同半导体的禁带宽度、价带能级、导带能级及晶型的匹配等因素。
贵金属沉积是TiO2光催化剂修饰的另外一种方法。贵金属包括Os、Pd、Ru、Rh、Ag、Ir、Pt和Au等，它们具有较高的耐腐蚀性和在潮湿空气中耐氧化。以往的研究表明贵金属(包括Pt、Ag、Au、Pd、Ni、Rh和Cu)沉积可以有效的提高TiO2的光催化活性，因为贵金属的费米能级比TiO2的要低，光生电子可以从TiO2的导带传递到沉积在TiO2表面的金属颗粒上，而价带上的光生空穴仍然在TiO2上。这就很大程度上降低了电子-空穴的复合几率，从而有效的提高光催化活性。大量的研究表明，这类复合材料的性质主要取决于金属颗粒的大小、分散和组成，当金属颗粒的尺寸小于2nm时，复合材料显示出优异的催化行为。当金属颗粒浓度太高时，TiO2对光的吸收降低，从而使得金属颗粒成为电子-空穴复合中心，降低催化效率。
Li等报道了用呫吨染料作为敏化剂敏化TiO2在可见光下光催化降解2,4-二氯苯酚。用不同染料敏化的TiO2对2,4-二氯苯酚的光催化降解效率的顺序是：伊红≈玫瑰红>赤藓红>罗丹明B。Shang等用水热法制备了二萘嵌苯四甲酸二酰亚胺和四磺酸酞菁铜敏化的TiO2复合物。通过在可见光下光催化降解罗丹明B的实验结果表明，二萘嵌苯四甲酸二酰亚胺和四磺酸酞菁铜敏化的TiO2复合物与单纯的TiO2相比具有更高的光催化效率。两种染料敏化的 TiO2复合物与一种染料敏化的TiO2复合物相比，具有有效电子收集的两种染料敏化的TiO2复合物显示出更高的光催化活性。除此之外，目前通过负载窄带隙量子点敏化半导体材料的也越来越多，Sang等利用CdS量子点敏化TiO2纳米管发现光电化学性能以及光催化产氢都得到了有效提高。
针对现有的技术比如金属掺杂，在阳离子的植入过程中会产生大量的缺陷，这些缺陷可以作为复合中心，从而降低光催化活性；通过直接混合的方法进行半导体复合，存在稳定性低，易脱落，利用效率不高的问题；采用贵金属作为助催化剂，例如Pt，Ru，Rh和Pd，这会增加产生氢能的成本，从而限制了大规模的商业化；通过物理或者化学吸附染料进行染料敏化或者量子的负载都存在稳定性差，易脱落还可能存在一定的毒性等问题。此外从目前报道的一系列提高光催化的方法来看，合成的路线越来越繁琐，结构越来越复杂，但光催化性能提高并不大。所以亟需寻找一种合成简单，催化性能优异的的非贵金属助催化剂来提高半导体材料光生载流子的分离效率。
发明内容
本发明要解决的技术问题是光催化对于解决能源问题有着重要的作用，在半个世纪以来得到了快速的发展,但是光催化半导体材料普遍存在禁带宽度较大、光响应范围窄以及高的光生载流子复合率的问题，这些缺点大大的影响了半导体材料的光电性能。
为解决上述问题，本发明通过对光催化半导体材料负载二维量子点SiP2来增加光生电子与空穴的数量，扩宽太阳光吸收范围，从而提高光催化水分解产氢性能。本发明中SiP2量子点能够拓宽吸光范围、加快电子分离与传输、降低光催化能垒、提高效率，此外用量少，价格低，不会对TiO2等光催化剂材料的稳定性等造成影响。另外我们发现通过机械剥离获得纳米级SiP2是高度可行的并且表现出优异的光催化性能，其制备方法简单，因此将SiP2量子点与半导体光催化剂进行复合提高催化效率将有很大的应用前景及意义。
为实现上述目的，本发明提供如下技术方案：一种SiP2量子点/光催化复合材料的制备方法，通过机械剥离的的方法将大颗粒的SiP2单晶超声成小尺寸的SiP2量子点，然后通过滴加、旋涂或者浸渍的方法将SiP2量子点均匀的覆盖在光催化材料的表面得到SiP2/光催化复合材料。结果表明，SiP2量子点不仅可以显着提高复合材料的稳定性，而且可以通过增强电荷转移，电荷传输，载流子密度，光吸收以及减小能带弯曲边缘和电荷复合来显着提高其光催化性能。
进一步的，将SiP2量子点均匀的覆盖在光催化材料的表面时，调节SiP2的浓度从0.1mg/ml～0.5mg/ml。浓度过低导致负载量太少SiP2没有作用浓度太高负载量过高影响基底材料的光吸收，所以0.1mg/ml～0.5mg/ml是最佳浓度。
进一步的，所述光催化材料为TiO2纳米材料。通过机械剥离获得尺寸较小的SiP2量子点，然后通过浸渍的方法负载到光催化材料、特别是半导体材料上，能够增强了复合材料的光吸收，提高电子空穴的分离效率。
进一步的，SiP2量子点的制备步骤如下：
将原料按照Si:P:Sn:Gd＝1:6:5:0.03的摩尔比例进行配料并充分混合均匀，转移到石英管中，将石英管用分子泵抽真空至5×10-3Pa后，采用氢氧焰进行封结，将石英管置于合成炉中，采用FP23控温表进行控温，控温程序如下：初始温度为室温，缓慢升温至723K，并恒温36h，然后经36h升温到973K，最终再经过48h升温到1123K，接下来，经25h缓慢降温到1073K，然后经50h降温到873K，再经25h降温到673K，然后关闭炉子，冷却至室温。将烧结后的样品置于1:1的稀盐酸中浸泡，除掉样品中的Sn，然后采用乙醇清洗干净并在333K下烘干，得到SiP2单晶。将上述获得的SiP2乙醇溶液放入240W大功率超声机中超声10小时，然后离心取上清液，得到小尺寸的SiP2量子点。
进一步的，TiO2纳米材料的制备步骤如下：
(1)水热法制备的TiO2纳米棒或者纳米颗粒。将30ml盐酸和30ml去离子水混合搅拌 10min，然后加入1ml钛酸四丁酯继续搅拌10min，最后将混合溶液转移到放有导电玻璃的反应釜中，然后再放入烘箱调节温度170℃水热6h得到TiO2纳米棒。
(2)TiO2纳米颗粒由两相水热合成法制备。首先将0.1mL 3-氯苯胺和10mL蒸馏水加到聚四氟乙烯水热釜内衬中，然后将0.17g钛酸四丁酯和1.0mL油酸加到10m L甲苯中。最后将混合溶液加入到聚四氟乙烯水热釜内衬中。将最终的混合溶液转移到马弗炉中，调节温度160-200℃水热处理12h，将产物离心处理并用甲醇多次清洗得到TiO2纳米颗粒。
(3)阳极氧化法制备TiO2纳米管或者薄膜。首先将钛箔切成5×5cm,然后用丙酮、乙醇、去离子水分别超声10min，然后将钛箔放入到含有0.5wt％NH4F的乙二醇溶液和1％体积的 HF混合溶液中，在60V恒压条件下15℃氧化不同时间得到备TiO2纳米管或者薄膜。
进一步的，SiP2量子点/光催化复合材料的制备步骤如下：
通过滴加、旋涂或者浸渍的方法，调节SiP2的浓度从0.1mg/ml～0.5mg/ml，将SiP2量子点均匀的覆盖在TiO2纳米材料的表面得到SiP2/TiO2复合材料。
一种上述方法制备的SiP2量子点/光催化复合材料及在光催化领域的应用。其优异的光电性能可以提高光电化学水分解的性能。
与现有技术相比，本发明有以下几个方面的优点：
(1)本发明是通过水热法制取TiO2纳米棒，这种一维有序阵列一方面能减少缺陷密度，降低光生电子空穴对的复合率，另一方面，由于一维纳米结构较大的比表面积，有利于SiP2量子点的负载为其负载提供更多的活性位点。SiP2量子点具有较大的比表面积，带隙较窄。 SiP2量子点的负载降低了复合材料的带隙，增强了太阳光的利用率，提高了电子空穴的分离效率，从而使光催化性能得到很大的提高。
(2)本发明中SiP2的负载不会对TiO2光催化剂材料的稳定性造成影响。
(3)本发明制备的复合光催化材料在模拟太阳光下表现出优异的光电化学性能，与纯的氧化钛纳米棒相比，光电流提高了两倍。
(4)光催化反应具有满足低能耗、对环境友好等优点，得到了众多学者的青睐。因此本发明的复合光催化材料存在很多潜在的应用领域:如光解水制氢解决能源问题；在环境治理方面光催化可以降解水体中有机物以及一些有毒物质，用于房屋装修中甲醛等有害有机物的去除；另外在医疗卫生方面纳米TiO2催化剂具有很好的抑制或杀灭细菌﹑真菌﹑病毒和癌细胞等作用，光催化与医疗卫生的结合,可实行不同领域间的合作等。
附图说明
图1为TiO2纳米棒负载SiP2前后复合材料的光电性能图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1：
一种SiP2量子点/二氧化钛高效光催化材料的制备方法，包括以下步骤：
(1)SiP2量子点的制备：
将原料按照Si:P:Sn:Gd＝1:6:5:0.03的摩尔比例进行配料并充分混合均匀，转移到石英管中，将石英管用分子泵抽真空至5×10-3Pa,后，采用氢氧焰进行封结，将石英管置于合成炉中，采用FP23控温表进行控温，控温程序如下：初始温度为室温，缓慢升温至723K，并恒温36h，然后经36h升温到973K，最终再经过48h升温到1123K，接下来，经25h缓慢降温到1073K，然后经50h降温到873K，再经25h降温到673K，然后关闭炉子，冷却至室温。将烧结后的样品置于1:1的稀盐酸中浸泡，除掉样品中的Sn，然后采用乙醇清洗干净并在333K下烘干，得到SiP2单晶。将获得上述SiP2乙醇溶液放入大功率超声机中超声10 小时，然后离心取上清液，得到厚度小尺寸的SiP2量子点。
(2)TiO2纳米材料的制备，水热法制备的TiO2纳米棒或者纳米颗粒：
将30ml盐酸和30ml去离子水混合搅拌10min，然后加入1ml钛酸四丁酯继续搅拌10min，最后将混合溶液转移到放有导电玻璃的反应釜中，然后再放入烘箱170℃水热6h得到TiO2纳米棒。
(3)SiP2量子点/光催化复合材料的制备：
通过滴加、旋涂或者浸渍的方法,调节SiP2的浓度从0.1mg/ml～0.5mg/ml，将SiP2量子点均匀的覆盖在TiO2纳米材料的表面得到SiP2/TiO2复合材料。
实施例2：
步骤(2)TiO2纳米颗粒由两相水热合成法制备。首先将0.1mL 3-氯苯胺和10mL蒸馏水加到聚四氟乙烯水热釜内衬中，然后将0.17g钛酸四丁酯和1.0mL油酸加到10m L甲苯中。最后将混合溶液加入到聚四氟乙烯水热釜内衬中。将最终的混合溶液转移到马弗炉中，调节温度160-200℃水热处理12h，将产物离心处理并用甲醇多次清洗得到TiO2纳米颗粒。
其余均与实施例1相同。
实施例3：
步骤(2)用阳极氧化法制备TiO2纳米管或者薄膜。首先将钛箔切成5×5cm,然后用丙酮、乙醇、去离子水超声10min，然后将钛箔放入到含有0.5wt％NH4F的乙二醇溶液和1％体积的 HF混合溶液中，在60V恒压条件下15℃氧化不同时间得到备TiO2纳米管或者薄膜。
其余均与实施例1相同。
由图1可以看出，负载SiP2量子点之后，光催化材料的光电流密度得到了很大的提高。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (9)
1.一种SiP2量子点/光催化复合材料的制备方法，其特征在于：通过机械剥离的的方法将大颗粒的SiP2单晶超声成小尺寸的SiP2量子点，然后通过滴加、旋涂或者浸渍的方法将SiP2量子点均匀的覆盖在光催化材料的表面得到SiP2/光催化材料复合材料；
所述光催化材料为TiO2纳米材料。
2.如权利要求1所述的SiP2量子点/光催化复合材料的制备方法，其特征在于：将SiP2量子点均匀的覆盖在光催化材料的表面时，调节SiP2的浓度从0.1mg/ml～0.5mg/ml。
3.如权利要求1所述的SiP2量子点/光催化复合材料的制备方法，其特征在于：SiP2量子点的制备步骤如下：将原料按照Si、P、Sn、Gd按比例进行配料并充分混合均匀，转移到石英管中，将石英管用分子泵抽真空后，采用氢氧焰进行封结，将石英管置于合成炉中进行烧结，然后关闭炉子，冷却至室温；将烧结后的样品置于稀盐酸中浸泡，然后采用乙醇清洗干净并烘干，得到SiP2单晶；将上述获得的SiP2乙醇溶液超声然后离心取上清液，得到厚度小尺寸的SiP2量子点。
4.如权利要求3所述的SiP2量子点/光催化复合材料的制备方法，其特征在于：烧结过程的控温程序如下：初始温度为室温，缓慢升温至723K，并恒温36h，然后经36h升温到973K，最终再经过48h升温到1123K，接下来，经25h缓慢降温到1073K，然后经50h降温到873K，再经25h降温到673K，然后关闭炉子，冷却至室温。
5.如权利要求1所述的SiP2量子点/光催化复合材料的制备方法，其特征在于：TiO2纳米材料的制备步骤如下：将盐酸和去离子水混合搅拌，然后加入钛酸四丁酯继续搅拌，最后将混合溶液转移到放有导电玻璃的反应釜中，然后再放入烘箱水热处理得到TiO2纳米棒。
6.如权利要求1所述的SiP2量子点/光催化复合材料的制备方法，其特征在于：TiO2纳米材料的制备步骤如下：首先将3-氯苯胺和蒸馏水加到聚四氟乙烯水热釜内衬中，然后将钛酸四丁酯和油酸加到甲苯中；最后将混合溶液加入到聚四氟乙烯水热釜内衬中；将最终的混合溶液转移到马弗炉中，水热处理后将产物离心处理并用甲醇多次清洗得到TiO2纳米颗粒。
7.如权利要求1所述的SiP2量子点/光催化复合材料的制备方法，其特征在于：TiO2纳米材料的制备步骤如下：首先将钛箔切成正方形然后分别用丙酮、乙醇、去离子水超声，然后将钛箔放入到含有NH4F的乙二醇溶液和HF混合溶液中，在恒压条件下氧化得到备TiO2纳米管或者薄膜。
8.一种权利要求1-7任一所述的制备方法制备的SiP2量子点/光催化复合材料。
9.一种权利要求8所述SiP2量子点/光催化复合材料，在光催化领域的应用。
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