固体推进剂用无机纳米材料的合成及催化性能的研究
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摘要
首先,我们通过液相还原的方法,在磁场作用下采用水合肼为还原剂合成出了由纳米片和纳米球组装成的花状Ni纳米金属粒子。研究发现在未添加任何表面活性剂的情况下合成出的样品没有发生任何氧化和团聚,长时间存放也未发生氧化,并探讨了磁场作用对粒子形成的作用机理。采用相似的路径,在液相的开放体系中,依然以水合肼作为还原剂合成出了尺寸均一的Cu纳米金属粒子；我们最大的成功就是不加入表面活性剂,而是采用引入痕量Ni的方法改变了此类金属还原过程为了避免氧化必须引入表面活性剂的问题,为Cu纳米金属粒子的合成提供了新的方法。通过对实验条件的考察,择优出反应的最佳条件,提出反应的可能进程,并研究了制备出的Ni、Cu纳米金属粒子样品的对固体推进剂的高能组分高氯酸铵(NH4ClO4, AP)的催化性能研究,证明二者均具有较好的正催化性能。
其次,在Ni、Cu纳米金属粒子的研究基础之上,我们也合成出了Ni-Cu双金属纳米材料,择优出反应的最佳条件,通过研究反应机理,研究出此双金属材料的形成过程及形成机理；我们且把制备出的Ni-Cu双金属纳米材料进行了对高氯酸铵(NH4ClO4, AP)的催化性能研究,研究发现Ni-Cu双金属纳米材料对高氯酸铵(NH_4ClO_4,AP)分子的高温、低温热分解放热峰温度降低的幅度比单一金属而言更大,这说明制备的双金属纳米材料比混合的粉末更有利于Ni与Cu之间发生协同作用,更能对高氯酸按的热分解起到催化作用。且Ni-Cu双金属纳米材料结合了两种金属的特性或优点,弥补单一金属性能的不足。
最后,我们对CaCO3和BaCO3纳米粒子制备和催化性能进行了研究。采用碳化方法制备出了CaCO3纳米粒子,发现Mg~2+的引入可以起到控制晶型的作用,并对各类反应条件进行逐一分析；采用室温固相研磨方法制备出了BaCO3纳米粒子,发现EDTA的引入可以起到控制晶型的作用,并对各类反应条件进行逐一分析。通过反应机理研究发现,CaCO3和BaCO3纳米粒子对高氯酸铵(NH4ClO4,AP)分子燃烧的催化作用趋势完全相似,且其对高氯酸铵燃烧的催化机理基本完全相似,在高氯酸铵的燃烧中二者均属于负催化剂。可以起到调燃的作用。
本论文详细的阐述了Ni纳米金属粒子、Cu纳米金属粒子、Ni-Cu双金属纳米材料、CaCO3纳米粒子以及BaCO3纳米粒子的合成方法以及最优条件的考察,并考察了这一系列纳米材料在固体推进剂中的高能组分高氯酸铵(NH4ClO4,AP)的燃烧过程中催化性能应用,为固体推进剂中催化剂的使用在理论和实践中的应用提供了有利的依据,具有实际的研究意义。
We synthesised Ni, Cu nanometallic l and Ni-Cu doublemetallic nanomaterial without surfactant, studied the morphology and formation mechanism of samples. Meanwhile we also studied the synthesis process of CaCO3 nanoparticles and BaCO3 nanoparticles, the morphology and formation mechanism. Studying the two part of system was in order to investigate the catalytic application of these nanomaterials for ammonium perchlorate, which was one of important rocket propellent.
Firstly, this work focused on a synthetic method to produce flower-like nickel nanostructures under the induction of magnetic field. Flower-like nickel nano-structures were obtained by using nontoxic reactants, nontoxic solvents, and low reaction temperature. It was improved that t amples matained better stability.We also found the samples did not oxide after a long time. We studied the reaction condition, the purity of samples and the morphology and formation mechanism of samples.And we synthesized high purity Cu nanometallic material by addition of trace Ni. And this trace Ni used as seeds to accelerate the reduction of Cu and keep Cu nanometallic pure and stable. We studied the reaction condition, the purity of samples and the morphology and formation mechanism of samples.
At the same time, with the synthesis research foundation of Ni-Cu nanometallic material, we synthesized Ni-Cu doublemetallic nanomaterial by using nontoxic reactants, nontoxic solvents, and nonextra nitrogen gas. We studied the influence of reaction condition, and also proved. Ni-Cu nanometallic material was fcc structure. The average sizer of sphere samples was 50nm, and the dispersivity was good.
Secondly, we prepared fusiformate CaCO3 nanoparticles through carbonating with Mg2+ existence. In the experiment,we studied that the size of CaCO3 nanoparticles changed with the velocity of carbon dioxide, the samples morphology of CaCO3 nanoparticles changed with pH value, the crystal morphology of CaCO3 nanoparticles changed with mixing speed. CaCO3 nanoparticles was hexahedronal calcite structure. The average sizer of was 100nm, and the dispersivity was good.
Finally, we synthesized BaCO3 nanoparticles through a room temperature solid phase method. In the experiment,we discovered that the attrition time, the calcining heat, the reactant proportion, the amount of EDTA seemed to influence the size and and morphology of BaCO3 nanoparticles.We also studied the reaction mechanism. BaCO3 nanoparticles was orthogonal structure. The average sizer of was 500nm, and the dispersivity was good.
The series of preparation process was only one of goal, the final goal was that the nanomaterials could be applicated. We added the synthesized nanomaterials to annonium perchlorater, and carried on the thermal analysis to study the catalyzed performance. The synthesized nanomaterials attributed to two kind:Ni, Cu nanometallic material and Ni-Cu doublemetallic nanomaterial was one kind,which belonged to positive catalytical effect,and the catalytical effect of Ni-Cu doublemetallic nanomaterial was better than Ni and Cu nanometallic material; CaCO3 nanoparticles and BaCO3 nanoparticles was the other kind, which belonged to negative catalytical effect, and the catalytical effect was consistent. In the actual application, we did not use the sole nanomaterials as catalyst in the rocket propellent. We usually used two and avove catalysts, in order to achieve the coordination goal and the synergism.
In this paper, we not only succeedly synthesised Ni, Cu nanometallic material and Ni-Cu doublemetallic nanomaterial, but also synthesised CaCO3 nanoparticles and BaCO3 nanoparticles. And we deeply tudied and induced the reaction mechanism of every system, which provided the theory basis and the application basis of catalytical effect for annonium perchlorater. In the actual research work, limited to the experimental condition and time, still a lot of work waited for further studying and consummating. For example, we should continouly determinate the intensity of the combustion pressure, dynamics analysis and so on.
其次,在Ni、Cu纳米金属粒子的研究基础之上,我们也合成出了Ni-Cu双金属纳米材料,择优出反应的最佳条件,通过研究反应机理,研究出此双金属材料的形成过程及形成机理；我们且把制备出的Ni-Cu双金属纳米材料进行了对高氯酸铵(NH4ClO4, AP)的催化性能研究,研究发现Ni-Cu双金属纳米材料对高氯酸铵(NH_4ClO_4,AP)分子的高温、低温热分解放热峰温度降低的幅度比单一金属而言更大,这说明制备的双金属纳米材料比混合的粉末更有利于Ni与Cu之间发生协同作用,更能对高氯酸按的热分解起到催化作用。且Ni-Cu双金属纳米材料结合了两种金属的特性或优点,弥补单一金属性能的不足。
最后,我们对CaCO3和BaCO3纳米粒子制备和催化性能进行了研究。采用碳化方法制备出了CaCO3纳米粒子,发现Mg~2+的引入可以起到控制晶型的作用,并对各类反应条件进行逐一分析；采用室温固相研磨方法制备出了BaCO3纳米粒子,发现EDTA的引入可以起到控制晶型的作用,并对各类反应条件进行逐一分析。通过反应机理研究发现,CaCO3和BaCO3纳米粒子对高氯酸铵(NH4ClO4,AP)分子燃烧的催化作用趋势完全相似,且其对高氯酸铵燃烧的催化机理基本完全相似,在高氯酸铵的燃烧中二者均属于负催化剂。可以起到调燃的作用。
本论文详细的阐述了Ni纳米金属粒子、Cu纳米金属粒子、Ni-Cu双金属纳米材料、CaCO3纳米粒子以及BaCO3纳米粒子的合成方法以及最优条件的考察,并考察了这一系列纳米材料在固体推进剂中的高能组分高氯酸铵(NH4ClO4,AP)的燃烧过程中催化性能应用,为固体推进剂中催化剂的使用在理论和实践中的应用提供了有利的依据,具有实际的研究意义。
We synthesised Ni, Cu nanometallic l and Ni-Cu doublemetallic nanomaterial without surfactant, studied the morphology and formation mechanism of samples. Meanwhile we also studied the synthesis process of CaCO3 nanoparticles and BaCO3 nanoparticles, the morphology and formation mechanism. Studying the two part of system was in order to investigate the catalytic application of these nanomaterials for ammonium perchlorate, which was one of important rocket propellent.
Firstly, this work focused on a synthetic method to produce flower-like nickel nanostructures under the induction of magnetic field. Flower-like nickel nano-structures were obtained by using nontoxic reactants, nontoxic solvents, and low reaction temperature. It was improved that t amples matained better stability.We also found the samples did not oxide after a long time. We studied the reaction condition, the purity of samples and the morphology and formation mechanism of samples.And we synthesized high purity Cu nanometallic material by addition of trace Ni. And this trace Ni used as seeds to accelerate the reduction of Cu and keep Cu nanometallic pure and stable. We studied the reaction condition, the purity of samples and the morphology and formation mechanism of samples.
At the same time, with the synthesis research foundation of Ni-Cu nanometallic material, we synthesized Ni-Cu doublemetallic nanomaterial by using nontoxic reactants, nontoxic solvents, and nonextra nitrogen gas. We studied the influence of reaction condition, and also proved. Ni-Cu nanometallic material was fcc structure. The average sizer of sphere samples was 50nm, and the dispersivity was good.
Secondly, we prepared fusiformate CaCO3 nanoparticles through carbonating with Mg2+ existence. In the experiment,we studied that the size of CaCO3 nanoparticles changed with the velocity of carbon dioxide, the samples morphology of CaCO3 nanoparticles changed with pH value, the crystal morphology of CaCO3 nanoparticles changed with mixing speed. CaCO3 nanoparticles was hexahedronal calcite structure. The average sizer of was 100nm, and the dispersivity was good.
Finally, we synthesized BaCO3 nanoparticles through a room temperature solid phase method. In the experiment,we discovered that the attrition time, the calcining heat, the reactant proportion, the amount of EDTA seemed to influence the size and and morphology of BaCO3 nanoparticles.We also studied the reaction mechanism. BaCO3 nanoparticles was orthogonal structure. The average sizer of was 500nm, and the dispersivity was good.
The series of preparation process was only one of goal, the final goal was that the nanomaterials could be applicated. We added the synthesized nanomaterials to annonium perchlorater, and carried on the thermal analysis to study the catalyzed performance. The synthesized nanomaterials attributed to two kind:Ni, Cu nanometallic material and Ni-Cu doublemetallic nanomaterial was one kind,which belonged to positive catalytical effect,and the catalytical effect of Ni-Cu doublemetallic nanomaterial was better than Ni and Cu nanometallic material; CaCO3 nanoparticles and BaCO3 nanoparticles was the other kind, which belonged to negative catalytical effect, and the catalytical effect was consistent. In the actual application, we did not use the sole nanomaterials as catalyst in the rocket propellent. We usually used two and avove catalysts, in order to achieve the coordination goal and the synergism.
In this paper, we not only succeedly synthesised Ni, Cu nanometallic material and Ni-Cu doublemetallic nanomaterial, but also synthesised CaCO3 nanoparticles and BaCO3 nanoparticles. And we deeply tudied and induced the reaction mechanism of every system, which provided the theory basis and the application basis of catalytical effect for annonium perchlorater. In the actual research work, limited to the experimental condition and time, still a lot of work waited for further studying and consummating. For example, we should continouly determinate the intensity of the combustion pressure, dynamics analysis and so on.
引文
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