金属硫化物及铁、锰氧化物纳米结构的水热合成与表征
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摘要
金属硫化物、氧化物都是重要的且具有广泛应用背景的材料。金属硫化物纳米材料是一类重要的半导体材料。比如硫化锌是重要的宽禁带半导体材料(Eg=3.72 eV)，广泛应用于半导体、颜料、光致发光、太阳能电池、红外探测器、气敏感传感器等领域。硫化锰也是一种宽禁带半导体材料，可以用作太阳能电池的缓冲层，掺入少量的其它离子比如Cd或者Zn时，显示了良好的磁性能。金属氧化物纳米材料不但拥有体相材料时的压电、化学传感、光感应等优异的性能，而且由于几何和尺寸效应表现出许多特有的属性，是一类名副其实的多功能材料，在透明电子元件、压电换能器、发光二极管等方面有着广泛地潜在应用。尽管当前金属硫化物、氧化物的制备已取得了较大的发展，但其形貌的控制合成仍没有很好的解决。因此，大量、低成本和有效地合成与组装各种形貌的金属硫化物、氧化物纳米材料无论从基础研究，还是从性能和应用的角度来看，都有着特殊重要的意义。
本文采用简单的水热法在有机物分子或表面活性剂的辅助下制备出多种不同形貌的金属硫化物、氧化物纳米材料，包括树枝状、球状、立方状、空心立方状及花状的PbS，还有球状的ZnS、SnS、CdS，纺锤形的α-Fe_2O_3、分枝状的γ-MnOOH等，并考察了反应时间、温度、反应物浓度及表面活性剂的种类等对生成产物形貌的影响。最后，对各种形貌产物的形成机制进行了初探。
以醋酸铅为铅源、硫代乙酰胺(TAA)为硫源，在十二烷基磺酸钠(SDS)的辅助下80℃下低温水热反应制备出了树枝状的PbS，观察发现制备的树枝状PbS由纳米颗粒粘连而成。反应物中再加入表面活性剂十六烷基三甲基溴化铵(CTAB)，由于其形成微胶束的限制作用，反应产物不再是颗粒粘连的树枝状纳米结构，而是颗粒粘连的球状PbS。反应温度提高到120℃时生成产物为空心立方状PbS。反应温度继续提高到160℃时生成产物为实心立方状PbS。在120℃下反应时，将硫源替换为硫脲，反应产物也随之变化为PbS纳米棒。此外，将表面活性剂柠檬酸或CTAB替换SDS，可合成花状的PbS。
根据上述球状PbS的合成原理，将其推广到其它硫化物，成功的制备出球状ZnS、SnS、CdS等硫化物。这说明低温反应时表面活性剂CTAB所形成的微胶束在球状产物的合成上起到了主要的软模板限制作用，而合成产物的晶体结构影响不大。提高反应温度，特别是到160℃时，球状ZnS产物已不能形成，而是生成三角的ZnS颗粒，SnS产物中也主要是片状的SnS，CdS产物虽然还有颗粒粘连成球的趋势，但是外观已不再是球形。这说明高温下合成产物的晶体结构对产物的形貌起主要作用，CTAB所形成的微胶束的软模板限制作用相对较弱。
以乙二醇(EG)作为辅助剂，NH_4Cl作为矿化剂水热制备出了纺锤形的α-Fe_2O_3纳米颗粒，其长轴与短轴之比约为2：1。在考察反应物浓度对产物形貌影响时发现，Fe~(3+)起始反应浓度对α-Fe_2O_3纳米颗粒的形貌影响很大。随着Fe~(3+)起始反应浓度的增加，纺锤形的α-Fe_2O_3的短轴越来越长，α-Fe_2O_3纳米颗粒的形貌从纺锤形向球形过渡。采用磁强样品振动器(VSM)对长、短轴比不一的α-Fe_2O_3纳米颗粒的磁性能进行了表征，发现不同轴比的α-Fe_2O_3纳米颗粒表现出两种磁性：顺磁性和反磁性。
利用即具有长链结构，又具有还原性的聚乙二醇(PEG)与高锰酸钾在120℃下低温水热反应，合成了多枝状的γ-MnOOH。合成时通过控制PEG的量或者加入一定量的表面活性剂CTAB作为反应物，反应产物只生成γ-MnOOH纳米线，从而实现γ-MnOOH多枝状纳米结构和一维纳米线的选择性生长。提高水热反应的温度(160℃)，发现多枝状的γ-MnOOH产物的分枝数变得更单一，主要以五分枝的γ-MnOOH为主(约60％)，这可能是温度提高，PEG的还原性增强，有利于晶体多核生长的结果。
Metal sulfides and oxides are important materials with a wide range of application. Metal sulfides nanomaterials are a group of important semiconductors. For example, ZnS is one of the most important semiconducts with a wide bandgap of 3.72 eV, which was widely used in the fields of semiconductors, pigments, photoluminescence, solar cells, infrared windows, gas sensors. MnS is also a semiconduct with a wide bandgap, which was usually used as the buffer layers of solar cells. When a small quantity of ions, such as Cd~(2+), Zn~(2+), was doped, the doped MnS shows excellent magnetic property. Metal oxides nanomaterials are really a group of functional materials, which not only have excellent properties such as piezoelectricity, chemical sensors, light sensors as well as the corresponding blocks, but also have a wide range of potential application in transparent electronics, piezoelectric transducers, light-emitting devices, etc. for the shape and size effect. At present, the preparation of metal sulfides and oxides has made a great progress, but their shape-controlled synthesis is not solved still. Therefore, large-scale, cost-effective, simple and practical synthesis and assembly of metal sulfides and oxides with different shapes is of importance for the fundamental research and application.
We prepared a few kinds of metal sulfides and oxides with different shapes using a simple hydrothermal method assisted by organic molecules or surfactants, including dendritic, spheric, cubic, hollow cubic and flower-like PbS, spheric ZnS, SnS and CdS, spindle-type α-Fe_2O_3, multi-armed γ-MnOOH, ect. The reation time, temperature, reactant concentration and surfactants were investigated in order to learn about how they affect the shape of the products. Finally, we made a primary study of the formation mechanism of the synthesized nanomaterials with different shapes.
We synthesized dendritic PbS nanostructure, which was conglutinated by the nanoparticles, via a low temperature (80℃) hydrothermal method assisted by the surfactant, SDS. We used Pb(Ac)2 as the lead source and TAA as the sulphur source. When another surfactant, CTAB, was added as a reactant, the obtained PbS nanostructure was not dendritic nanostructure but spheric PbS, which was also conglutinated by the nanoparticles. Maybe the formed micelles of CTAB in the solution played the role of soft template, which confined the conglutianted nanoparticles to form the spheric structure. When the reaction temperature was
increased, the shape of the obtained products was changed. The hollow cubic PbS was obtained when the reaction temperature increased to 120℃. When it was increased to 160 ℃, the obtained product was cubic PbS. When the reaction temperature is 120 ℃ and the sulphur source was replaced by (NH_2)_2CS, the obtained product was 1D PbS nanorod. In addition, When the surfactant, SDS, was replaced by CA or CTAB, we can obtain the flower-like PbS nanostracture.
According to the synthesized principle of spheric PbS nanostructure metioned above, we prepared other spheric metal sulfides successfully,such as ZnS, SnS, CdS, etc. This further proved that It is the formed micelles of CTAB in the solution play more important roles in forming the spheric nanostructure as a soft template, not the crystalline structure of the obtained products at low synthesized temperature. When the reaction temperature was increased, especially to 160 ℃, We can not obtain the spheric ZnS nanostructure again, but the triangle ZnS nanoparticles. The obtained SnS products were mainly the plate-like structure. Although the CdS products still have the trend to form spheric structures, which was conglutinated by the nanoparticles, the shape is not spheric again. This proved that the crystalline structure of the obtained products plays more important roles in deciding the shape of products at high reaction temperature than the formed micelle of CTAB as a soft template.
We prepared a kind of spindle-type α-Fe_2O_3 via a facile hydrothermal method using glycol as the assisted agent and NH_4Cl as the mineralized agent. The ratio of major axis and minor axis of the synthesized spindle-type α-Fe_2O_3 is about 2/1. We found that the starting reaction concentration of Fe~(3+) has great effect on the shape of the products. When it increased, the length of the minor axis of the α-Fe_2O_3 was elongated and the shape of α-Fe_2O_3 nanoparticles was transformed into sphere from spindle-type. The magnetic property of the α-Fe_2O_3 nanoparticles with different ratio of major axis and minor axis were investigated by the vibrating sample magnetometer(VSM). The results show that they have two kinds of magnetic properties, diamagnetism and paramagnetism.
We synthesized a kind of multipods γ-MnOOH via a low temperature hydrothermal method based on the reaction of polyglycol, which has a long chain structure and reductive property, and KMnO_4. When the volume of PEG was controlled or an appropriate mount of surfactant, CTAB, was added as the starting reactant, the obtained product will be 1D γ-MnOOH nanorod or nanowire only. It can easily realize the selective growth of γ-MnOOH multipods and 1D nanowire. When the reaction temperature was increased to 160 ℃, the
number of the arms of the obtained y-MnOOH multipods were more uniform. They are mainly five-armed γ-MnOOH, 60%. Maybe the stronger reductive property of polyglycol led to the multiple growth centers of γ-MnOOH, When the reaction temperature was increased.
本文采用简单的水热法在有机物分子或表面活性剂的辅助下制备出多种不同形貌的金属硫化物、氧化物纳米材料，包括树枝状、球状、立方状、空心立方状及花状的PbS，还有球状的ZnS、SnS、CdS，纺锤形的α-Fe_2O_3、分枝状的γ-MnOOH等，并考察了反应时间、温度、反应物浓度及表面活性剂的种类等对生成产物形貌的影响。最后，对各种形貌产物的形成机制进行了初探。
以醋酸铅为铅源、硫代乙酰胺(TAA)为硫源，在十二烷基磺酸钠(SDS)的辅助下80℃下低温水热反应制备出了树枝状的PbS，观察发现制备的树枝状PbS由纳米颗粒粘连而成。反应物中再加入表面活性剂十六烷基三甲基溴化铵(CTAB)，由于其形成微胶束的限制作用，反应产物不再是颗粒粘连的树枝状纳米结构，而是颗粒粘连的球状PbS。反应温度提高到120℃时生成产物为空心立方状PbS。反应温度继续提高到160℃时生成产物为实心立方状PbS。在120℃下反应时，将硫源替换为硫脲，反应产物也随之变化为PbS纳米棒。此外，将表面活性剂柠檬酸或CTAB替换SDS，可合成花状的PbS。
根据上述球状PbS的合成原理，将其推广到其它硫化物，成功的制备出球状ZnS、SnS、CdS等硫化物。这说明低温反应时表面活性剂CTAB所形成的微胶束在球状产物的合成上起到了主要的软模板限制作用，而合成产物的晶体结构影响不大。提高反应温度，特别是到160℃时，球状ZnS产物已不能形成，而是生成三角的ZnS颗粒，SnS产物中也主要是片状的SnS，CdS产物虽然还有颗粒粘连成球的趋势，但是外观已不再是球形。这说明高温下合成产物的晶体结构对产物的形貌起主要作用，CTAB所形成的微胶束的软模板限制作用相对较弱。
以乙二醇(EG)作为辅助剂，NH_4Cl作为矿化剂水热制备出了纺锤形的α-Fe_2O_3纳米颗粒，其长轴与短轴之比约为2：1。在考察反应物浓度对产物形貌影响时发现，Fe~(3+)起始反应浓度对α-Fe_2O_3纳米颗粒的形貌影响很大。随着Fe~(3+)起始反应浓度的增加，纺锤形的α-Fe_2O_3的短轴越来越长，α-Fe_2O_3纳米颗粒的形貌从纺锤形向球形过渡。采用磁强样品振动器(VSM)对长、短轴比不一的α-Fe_2O_3纳米颗粒的磁性能进行了表征，发现不同轴比的α-Fe_2O_3纳米颗粒表现出两种磁性：顺磁性和反磁性。
利用即具有长链结构，又具有还原性的聚乙二醇(PEG)与高锰酸钾在120℃下低温水热反应，合成了多枝状的γ-MnOOH。合成时通过控制PEG的量或者加入一定量的表面活性剂CTAB作为反应物，反应产物只生成γ-MnOOH纳米线，从而实现γ-MnOOH多枝状纳米结构和一维纳米线的选择性生长。提高水热反应的温度(160℃)，发现多枝状的γ-MnOOH产物的分枝数变得更单一，主要以五分枝的γ-MnOOH为主(约60％)，这可能是温度提高，PEG的还原性增强，有利于晶体多核生长的结果。
Metal sulfides and oxides are important materials with a wide range of application. Metal sulfides nanomaterials are a group of important semiconductors. For example, ZnS is one of the most important semiconducts with a wide bandgap of 3.72 eV, which was widely used in the fields of semiconductors, pigments, photoluminescence, solar cells, infrared windows, gas sensors. MnS is also a semiconduct with a wide bandgap, which was usually used as the buffer layers of solar cells. When a small quantity of ions, such as Cd~(2+), Zn~(2+), was doped, the doped MnS shows excellent magnetic property. Metal oxides nanomaterials are really a group of functional materials, which not only have excellent properties such as piezoelectricity, chemical sensors, light sensors as well as the corresponding blocks, but also have a wide range of potential application in transparent electronics, piezoelectric transducers, light-emitting devices, etc. for the shape and size effect. At present, the preparation of metal sulfides and oxides has made a great progress, but their shape-controlled synthesis is not solved still. Therefore, large-scale, cost-effective, simple and practical synthesis and assembly of metal sulfides and oxides with different shapes is of importance for the fundamental research and application.
We prepared a few kinds of metal sulfides and oxides with different shapes using a simple hydrothermal method assisted by organic molecules or surfactants, including dendritic, spheric, cubic, hollow cubic and flower-like PbS, spheric ZnS, SnS and CdS, spindle-type α-Fe_2O_3, multi-armed γ-MnOOH, ect. The reation time, temperature, reactant concentration and surfactants were investigated in order to learn about how they affect the shape of the products. Finally, we made a primary study of the formation mechanism of the synthesized nanomaterials with different shapes.
We synthesized dendritic PbS nanostructure, which was conglutinated by the nanoparticles, via a low temperature (80℃) hydrothermal method assisted by the surfactant, SDS. We used Pb(Ac)2 as the lead source and TAA as the sulphur source. When another surfactant, CTAB, was added as a reactant, the obtained PbS nanostructure was not dendritic nanostructure but spheric PbS, which was also conglutinated by the nanoparticles. Maybe the formed micelles of CTAB in the solution played the role of soft template, which confined the conglutianted nanoparticles to form the spheric structure. When the reaction temperature was
increased, the shape of the obtained products was changed. The hollow cubic PbS was obtained when the reaction temperature increased to 120℃. When it was increased to 160 ℃, the obtained product was cubic PbS. When the reaction temperature is 120 ℃ and the sulphur source was replaced by (NH_2)_2CS, the obtained product was 1D PbS nanorod. In addition, When the surfactant, SDS, was replaced by CA or CTAB, we can obtain the flower-like PbS nanostracture.
According to the synthesized principle of spheric PbS nanostructure metioned above, we prepared other spheric metal sulfides successfully,such as ZnS, SnS, CdS, etc. This further proved that It is the formed micelles of CTAB in the solution play more important roles in forming the spheric nanostructure as a soft template, not the crystalline structure of the obtained products at low synthesized temperature. When the reaction temperature was increased, especially to 160 ℃, We can not obtain the spheric ZnS nanostructure again, but the triangle ZnS nanoparticles. The obtained SnS products were mainly the plate-like structure. Although the CdS products still have the trend to form spheric structures, which was conglutinated by the nanoparticles, the shape is not spheric again. This proved that the crystalline structure of the obtained products plays more important roles in deciding the shape of products at high reaction temperature than the formed micelle of CTAB as a soft template.
We prepared a kind of spindle-type α-Fe_2O_3 via a facile hydrothermal method using glycol as the assisted agent and NH_4Cl as the mineralized agent. The ratio of major axis and minor axis of the synthesized spindle-type α-Fe_2O_3 is about 2/1. We found that the starting reaction concentration of Fe~(3+) has great effect on the shape of the products. When it increased, the length of the minor axis of the α-Fe_2O_3 was elongated and the shape of α-Fe_2O_3 nanoparticles was transformed into sphere from spindle-type. The magnetic property of the α-Fe_2O_3 nanoparticles with different ratio of major axis and minor axis were investigated by the vibrating sample magnetometer(VSM). The results show that they have two kinds of magnetic properties, diamagnetism and paramagnetism.
We synthesized a kind of multipods γ-MnOOH via a low temperature hydrothermal method based on the reaction of polyglycol, which has a long chain structure and reductive property, and KMnO_4. When the volume of PEG was controlled or an appropriate mount of surfactant, CTAB, was added as the starting reactant, the obtained product will be 1D γ-MnOOH nanorod or nanowire only. It can easily realize the selective growth of γ-MnOOH multipods and 1D nanowire. When the reaction temperature was increased to 160 ℃, the
number of the arms of the obtained y-MnOOH multipods were more uniform. They are mainly five-armed γ-MnOOH, 60%. Maybe the stronger reductive property of polyglycol led to the multiple growth centers of γ-MnOOH, When the reaction temperature was increased.
引文
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