纳米稀土氧化物的控制制备及其催化性能研究
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摘要
由于稀土元素特殊的电子结构，稀土材料具有独特的性质，在许多催化领域有着广泛的应用，但是在复合固体推进剂燃烧催化方面的研究却很少。稀土材料的催化活性除与其电子结构有关外，还与其组成、尺寸、物相、分散性、比表面积和表面状态等有密切关系，因此，稀土催化材料的控制制备引起全世界范围内科学家的研究兴趣。本论文在纳米稀土氧化物的控制制备新方法及其催化固体推进剂燃烧性能方面的进行了一些有益的探索。
在第二章中，首次以乙二醇为燃料采用溶液燃烧法一步合成了CeO_2基纳米晶，通过由相关热力学数据计算得到的溶液燃烧的绝热火焰温度研究了乙二醇和硝酸根摩尔比(EG／NO_3~-)对燃烧产物性质的影响。乙二醇无毒、廉价易得、燃烧反应缓和，在溶液燃烧法合成中具有一定的推广应用价值。
为了解决溶液燃烧合成纳米粒子中普遍存在的团聚问题，提高产物比表面积，提出了一种快速制备高比表面氧化铈基纳米粉体的新方法——盐助溶液燃烧法(SSCS)。研究发现在传统溶液燃烧合成(CSCS)的混合液中加入可溶性惰性盐导致产物比表面积剧增十多倍，得到4～6 nm高分散性的纳米氧化铈粒子。该法应用于Ce_(0.75)Zr_(0.25)O_2固溶体的制备发现Ce_(0.75)Zr_(0.25)O_2比表面积由不加NaCl时的17.34m~2／g剧增至208.17m~2／g，产物为球形粒子之间松软团聚形成的介孔结构。第二章还研究了乙二醇量和盐量对产物性质的影响，初步讨论了盐助燃烧合成高分散性的CeO_2基纳米粒子的可能机理，考察了合成的CeO_2基纳米粉对高氯酸铵(AP)热分解的催化效果。
基于第二章的工作，第三章首先研究了以乙二醇为燃料采用SSCS法直接制备高分散性的钙钛矿型LaMnO_3纳米粒子。产物粒子的物相、分散性和形貌可以通过调节乙二醇量和NaCl量进行控制。非常有意义的是在适当的条件下，可以得到立方相和斜方相的LaMnO_3纳米晶以及大小均匀的钙钛矿型LaMnO_3立方形纳米粒子。
以甘氨酸为燃料采用SSCS法得到的含NaCl的前驱体经一定温度煅烧处理制备了高分散性的钙钛矿型NdCoO_3纳米粒子。NaCl的引入抑制了粒子的烧结和团聚，使产物比表面积由CSCS法的1.7m~2／g增至43.2m~2／g，团聚的大颗粒变成了粒径约10nm分散粒子。除提高煅烧温度外，NaCl的加入及其量的增加在煅烧过程促进钙钛矿相的形成和晶粒度的增大。
TG-DSC结果表明SSCS法合成的纳米LaMnO_3和NdCoO_3对AP的热分解有强烈的催化活性，前者最多使AP的高温分解峰温降低103.9℃，表观分解热增加838 J／g；后者最多使得AP的高温分解峰温降低116.7℃，表观分解热增加947 J／g，其催化性能与合成ABO_3粒子的大小、分散性和物相有关，但是很大程度上决定于其比表面积大小，最后初步探讨了纳米ABO_3催化AP热分解的机理。
在第四章中，首次通过非水相体系的乙二醇凝胶燃烧法制备了纳米Y_2O_3和Nd_2O_3及其掺杂产物。制备的Y_2O_3粒子呈球形，粒径约20 nm；Nd_2O_3粒子呈球形，分散性好，粒径在30～40nm。另外研究了乙二醇与金属离子的摩尔比和煅烧温度对产物性质的影响，该制备方法条件控制简单，成胶时间较短，避免了掺杂时偏析的出现。
催化性能研究表明2wt.％的纳米Y_2O_3和Nd_2O_3可分别使AP的高温分解峰温降低106.7℃和96.2℃，表观分解热增加645 J／g和625 J／g；在Y_2O_3和Nd_2O_3中分别掺入3.4％的Fe~(3+)，Co~(2+)，Ni~(2+)，Cu~(2+)和Mn~(2+)，可使AP的高温分解峰温进一步降低1～10℃，表观分解热增加；随着Co~(2+)掺入量的增加，掺杂后Y_2O_3和Nd_2O_3使AP的表观分解热增加，高温分解峰温度变化不大或有所降低。
为了便于放大制备，第五章首先研究了以NdCl_3·6H_2O+CoCl_2·6H_2O+6NaOH为原料，机械化学法制备钙钛矿型NdCoO_3纳米粒子。通过利用球磨过程原位生成的和外加的NaCl在煅烧过程的阻聚作用，可以改善产物粒子的分散性和形貌。随着外加NaCl量的增加，产物的分散性提高，比表面积增大，还能促进NdCoO_3成相。当外加的NaCl量和煅烧温度合适时，可以得到高分散性的NdCoO_3立方形纳米粒子和纳米方棒。该法的特点是原料易得，操作方便，工艺简单，产率高和易于工业化制备。
然后以Nd_2O_3和Co_3O_4为原料，采用湿固相机械化学法通过在球磨过程中添加稀释剂ZnO制备了粒径在10～23 nm的椭球状NdCoO_3。随着ZnO量的增加，产物比表面积由原来7.39 m~2／g增至36.11 m~2／g；随着煅烧温度的提高，产物晶粒度增大，比表面积减小，但是该法制备时间长，能耗较大，稀释剂ZnO完全分离较为困难。
最后考察了分别以氯化物和氧化物为原料机械化学法制备的纳米NdCoO_3对AP的热分解的催化性能，前者最多使AP的高温分解峰温降低144.3℃，表观分解热增加632 J／g；后者最多使得AP的高温分解峰温降至321.6℃，表观分解热增至1210 J／g。就同一方法制备的纳米NdCoO_3而言，比表面积大，催化活性高。在AP／HTPB复合固体推进剂中添加3％纳米NdCoO_3后，推进剂样品的低温和高温放热峰重叠，放热峰温度降低了33℃。
燃烧性能试验表明添加3wt.％纳米NdCoO_3后，AP／HTPB复合固体推进剂在4MPa，7PMa和10MPa三个压力左右燃烧速度分别提高约40.0％，40.6％和23.7％；在4～7 MPa，7～10MPa和4～10 MPa压力范围的压力指数分别降低了16.05％，44.4％和32.1％。总之，无定形纳米NdCoO_3能大幅度提高AP／HTPB复合固体推进剂的燃速，明显降低燃烧压力指数，是一种很有希望应用于AP／HTPB复合固体推进剂的性能优良的燃烧调节剂。
Rare earth materials have found wide applications in many catalytic areas due to theirunique properties depending on the peculiar electronic structures of rare earth elements,however, there are few studies on rare earth materials in catalytic combustion of compositesolid propellants. Besides their electronic structures, the catalytic properties of rare earthmaterials are intimately related to their composition, size, phase, dispersibility, specificsurface areas and surface state, et al. Therefore, controlled synthesis of rare earth materialshas drawn continuous and worldwide research attention. In this dissertation, valuableexplorations have been carried out on the new chemical synthetic strategies ofnanostructured rare earth oxides and their catalytic properties for combustion of compositesolid propellants.
In chapter 2, one-step synthesis of nanocrystalline ceria-based powders via a solutioncombustion route using ethylene glycol as a novel fuel is described. An interpretationbased on an adiabatic flame temperature for different fuel-to-oxidant ratios(EG/NO_3~-) hasbeen proposed for the nature of combustion and its correlation with the powdercharacteristics. Ethylene glycol is nontoxic, cheap, easily available, mild duringcombustion reaction and has broad and potentiao applications in solution combustionsynthesis.
To solve the problem of particle agglomeration widely existing in solutioncombustion synthesis and enhance specific surface area of the combustion resultants, Wehave come up with a facile and novel salt-assisted solution combustion synthesis (SSCS)route to high surface area ceria-based nanopowders. It is revealed that the introduction ofsoluble and inert salt in the conventional combustion synthesis process was found to resultin the formation of 4～6 nm well-dispersed ceria nanoparticles and a more than ten-foldincrease in the specific surface area of the products from 14.10 to 156.74 m~2/g. In the caseof SSCS of Ce_(0.75)Zr_(0.25)O_2 solid solution, the addition of NaCl enhanced the specific surfacearea of the products from 17.34 to 208.17 m~2/g and led to the mesoporous structure formedby the loose agglomeration of monodisperse nanoparticles. The effects of such influencingfactors as the fuel-to-oxidant ratio, and the nature and amount of added salt on thecharacteristics of the products were investigated. A mechanism scheme was proposed toillustrate the possible formation processes of highly dispersed ceria-based nanoparticles. Finally, the influnce of nanocrystalline ceria-based powders on thermal decomposition ofammonium perchlorate(AP) was studied.
On the basis of the research of chapter 2, chapter 3 deals firstly with preparation ofthe well-dispersed perovskite LaMnO_3 nanoparticles by a solution salt-assisted combustionprocess, using ethylene glycol as a fuel and nitrates as oxidants. By tuning thefuel-to-oxidant ratio and the amount of added NaCl, the phase, dipersibility andmorphology of the resultants can be controlled. It is very significant that the cubic orrehombic LaMnO_3 nanorystal and perovskite nanocubes with narrow size distribution canbe obtained under the proper conditions.
In the second part of chapter 3, highly dispersed perovskite NdCoO_3 nanoparticleshave been successfully prepared by calcining the NaCl-containing precursor derived fromsalt-assisted solution combustion process employing glycine as a fuel. The facileintroduction of NaCl in the conventional combustion synthesis process was found toprevent particles from sintering and agglomerating and increase specific surface area of theresultants from 1.70 to 43.22 m~2/g. Besides enhancing calcination temperature, thepresence and increase of salt promotes formation of peroskite phase and growth ofcrystallite size in the process of calcination.
The TG-DSC results indicate that the combustion-derived nano-sized LaMnO_3 andNdCoO_3 show the intense catalytic activity on thermal decomposition of AP. The formerdecreases the temperature of AP high temperature decomposition peak by 103.9℃andincreases the apparent decomposition heat of AP by 838 J/g at most while the latterdecreases the temperature of AP high temperature decomposition peak by 116.7℃andincreases the apparent decomposition heat of AP by 947 J/g at most. Their catalytic activityis related to their particle size, dispersibility and phase, but is to large degree dependent ontheir specific surface area in the last analysis. Finally, the possible mechanism of catalyticdecomposition of AP by nano-sized ABO_3 was preliminarily discussed.
In chapter 4, we discuss preparation of nano-sized Y_2O_3 and Nd_2O_3 as well as theirdoped resultants via none-aqueous sol-gel process based on hydrated nitrate and ethyleneglycol, auto-propagating combustion and subsequent calcinations (gel combustionmethod).The as-prepared Y_2O_3 particles are spherical in shape and 20 nm in particle sizewhile the resultant Nd_2O_3 crystallites are spherical, well-dispersedand range from 30 nm to40 nm in size. Further, the effects of the molar ratio of ethylene glycol to yttrium ion,calcination temperature on crystallite size of the products were also studied. In summary,the synthetic method is easy to control, shortens the time to form xerogel and avoids segregation when doping.
The results in catalysis show that the 2wt.％Y_2O_3 and Nd_2O_3 respectively reduce thetemperature ofAP exothermic peak by 106.7℃and 96.2℃as well as enhance the apparentdecomposition heat by 645 J/g and 625 J/g. When doping 3.4％Fe~(3+), Co~(2+), Ni~(2+), Cu~(2+) andMn~(2+) into Y_2O_3 and Nd_2O_3, respectively, the doped resultants further decrease thetemperature of AP high temperature decomposition peak by 1～10℃and increases theapparent decomposition heat of AP. As the amount of doped Co~(2+) increases, the dopedY_2O_3 and Nd_2O_3 increase the apparent decomposition heat of AP, and have no greatinfluence on or reduce the temperature of AP high temperature decomposition peak.
In an effort to synthesize nano-sized NdCoO_3 a on a large scale, chapter 5investigates the preparation of nano-sized perovskite NdCoO_3 via a mechanochemicalprocess of NdCl_3·6H_2O+CoCl_2·6H_2O+6NaOH. It is observed that the NaCl derived in-situduring milling and added NaCl can improve the dispersibility and morphology of theas-synthesized particles owing to inhibiting agglomeration and accelerating mass transfer.Moreover, an increasing addition of NaCl not only improves particle dispersibility,increases specific surface area of the product but also promotes the formation of perovskiteNdCoO_3. It is interesting that highly dispersed NdCoO_3 nanocubes or nanorods can beprepared under the proper conditions. The preparative method is characterized byavailability in raw materials, convenient operation, simple process, high yield and potentialindustrialization.
In another effort, the well dispersed elliptical NdCoO_3 with particle size in the rangeof 10～23nm was prepared via wet-solid -phase milling and subsequent calcination ofNd_2O_3 and Co_3O_4 mixture, wherein the ZnO diluent was added after some milling period.The results reveal that an increasing addition of ZnO increases the specific surface area ofthe as-prepared NdCoO_3 from 7.39 m~2/g in the absence of ZnO to 36.11m~2/g and thatincreasing the calcination temperature results in crystallite growth and reduction in specificsurface area However, the synthetic process has such disadvantage as long preparativeperiod, high energy comsumption and difficulty in complete separation of ZnO diluent.
In the last part of chapter 5, we investigates catalytic properties of the nano-sizedNdCoO_3 prepared by a mechanochemical route, respectively using oxide and hydratechloride as raw materials, for the thermal decomposition of AP. The catalytic activityinvestigation demonstrates that the former decreases the temperature of AP hightemperature decomposition peak by 144.3℃and increases the apparent decompositionheat of AP by 632 J/g at most while the latter decreases the temperature of AP high temperature decomposition peak by 144.3℃and increases the apparent decompositionheat of AP by 695 J/g at most. As to the nano-sized NdCoO_3 synthesized by the same route,the larger the specific surface area is, the higher the catalytic activity is. The addition of3wt.％amorphous NdCoO_3 nanoparticles into the AP/HTPB composite solid propellantincorporates two exothermic peaks of the composite solid propellant into one exothermicpeak, decreases the temperature of the exothermic peak by 33℃。
The experiments in combustion characteristics show that the addition of 3wt.％nano-sized NdCoO_3 nanoparticles into the AP/HTPB composite solid propellant,respectively, enhances the burning rate at the pressures of about 4MPa, 7 PMa and 10MPby 40.0％, 40.6％and 23.7％, reduces the pressure exponents in the pressure scopes of4～7 MPa, 7～10MPa and 4～10 MPa by 16.05％, 44.4％and 32.1％. In summary, theamorphous nano-sized NdCoO_3 is expected to be an excellent and promising modifier forcombustion of the AP/HTPB composite solid propellant.
在第二章中，首次以乙二醇为燃料采用溶液燃烧法一步合成了CeO_2基纳米晶，通过由相关热力学数据计算得到的溶液燃烧的绝热火焰温度研究了乙二醇和硝酸根摩尔比(EG／NO_3~-)对燃烧产物性质的影响。乙二醇无毒、廉价易得、燃烧反应缓和，在溶液燃烧法合成中具有一定的推广应用价值。
为了解决溶液燃烧合成纳米粒子中普遍存在的团聚问题，提高产物比表面积，提出了一种快速制备高比表面氧化铈基纳米粉体的新方法——盐助溶液燃烧法(SSCS)。研究发现在传统溶液燃烧合成(CSCS)的混合液中加入可溶性惰性盐导致产物比表面积剧增十多倍，得到4～6 nm高分散性的纳米氧化铈粒子。该法应用于Ce_(0.75)Zr_(0.25)O_2固溶体的制备发现Ce_(0.75)Zr_(0.25)O_2比表面积由不加NaCl时的17.34m~2／g剧增至208.17m~2／g，产物为球形粒子之间松软团聚形成的介孔结构。第二章还研究了乙二醇量和盐量对产物性质的影响，初步讨论了盐助燃烧合成高分散性的CeO_2基纳米粒子的可能机理，考察了合成的CeO_2基纳米粉对高氯酸铵(AP)热分解的催化效果。
基于第二章的工作，第三章首先研究了以乙二醇为燃料采用SSCS法直接制备高分散性的钙钛矿型LaMnO_3纳米粒子。产物粒子的物相、分散性和形貌可以通过调节乙二醇量和NaCl量进行控制。非常有意义的是在适当的条件下，可以得到立方相和斜方相的LaMnO_3纳米晶以及大小均匀的钙钛矿型LaMnO_3立方形纳米粒子。
以甘氨酸为燃料采用SSCS法得到的含NaCl的前驱体经一定温度煅烧处理制备了高分散性的钙钛矿型NdCoO_3纳米粒子。NaCl的引入抑制了粒子的烧结和团聚，使产物比表面积由CSCS法的1.7m~2／g增至43.2m~2／g，团聚的大颗粒变成了粒径约10nm分散粒子。除提高煅烧温度外，NaCl的加入及其量的增加在煅烧过程促进钙钛矿相的形成和晶粒度的增大。
TG-DSC结果表明SSCS法合成的纳米LaMnO_3和NdCoO_3对AP的热分解有强烈的催化活性，前者最多使AP的高温分解峰温降低103.9℃，表观分解热增加838 J／g；后者最多使得AP的高温分解峰温降低116.7℃，表观分解热增加947 J／g，其催化性能与合成ABO_3粒子的大小、分散性和物相有关，但是很大程度上决定于其比表面积大小，最后初步探讨了纳米ABO_3催化AP热分解的机理。
在第四章中，首次通过非水相体系的乙二醇凝胶燃烧法制备了纳米Y_2O_3和Nd_2O_3及其掺杂产物。制备的Y_2O_3粒子呈球形，粒径约20 nm；Nd_2O_3粒子呈球形，分散性好，粒径在30～40nm。另外研究了乙二醇与金属离子的摩尔比和煅烧温度对产物性质的影响，该制备方法条件控制简单，成胶时间较短，避免了掺杂时偏析的出现。
催化性能研究表明2wt.％的纳米Y_2O_3和Nd_2O_3可分别使AP的高温分解峰温降低106.7℃和96.2℃，表观分解热增加645 J／g和625 J／g；在Y_2O_3和Nd_2O_3中分别掺入3.4％的Fe~(3+)，Co~(2+)，Ni~(2+)，Cu~(2+)和Mn~(2+)，可使AP的高温分解峰温进一步降低1～10℃，表观分解热增加；随着Co~(2+)掺入量的增加，掺杂后Y_2O_3和Nd_2O_3使AP的表观分解热增加，高温分解峰温度变化不大或有所降低。
为了便于放大制备，第五章首先研究了以NdCl_3·6H_2O+CoCl_2·6H_2O+6NaOH为原料，机械化学法制备钙钛矿型NdCoO_3纳米粒子。通过利用球磨过程原位生成的和外加的NaCl在煅烧过程的阻聚作用，可以改善产物粒子的分散性和形貌。随着外加NaCl量的增加，产物的分散性提高，比表面积增大，还能促进NdCoO_3成相。当外加的NaCl量和煅烧温度合适时，可以得到高分散性的NdCoO_3立方形纳米粒子和纳米方棒。该法的特点是原料易得，操作方便，工艺简单，产率高和易于工业化制备。
然后以Nd_2O_3和Co_3O_4为原料，采用湿固相机械化学法通过在球磨过程中添加稀释剂ZnO制备了粒径在10～23 nm的椭球状NdCoO_3。随着ZnO量的增加，产物比表面积由原来7.39 m~2／g增至36.11 m~2／g；随着煅烧温度的提高，产物晶粒度增大，比表面积减小，但是该法制备时间长，能耗较大，稀释剂ZnO完全分离较为困难。
最后考察了分别以氯化物和氧化物为原料机械化学法制备的纳米NdCoO_3对AP的热分解的催化性能，前者最多使AP的高温分解峰温降低144.3℃，表观分解热增加632 J／g；后者最多使得AP的高温分解峰温降至321.6℃，表观分解热增至1210 J／g。就同一方法制备的纳米NdCoO_3而言，比表面积大，催化活性高。在AP／HTPB复合固体推进剂中添加3％纳米NdCoO_3后，推进剂样品的低温和高温放热峰重叠，放热峰温度降低了33℃。
燃烧性能试验表明添加3wt.％纳米NdCoO_3后，AP／HTPB复合固体推进剂在4MPa，7PMa和10MPa三个压力左右燃烧速度分别提高约40.0％，40.6％和23.7％；在4～7 MPa，7～10MPa和4～10 MPa压力范围的压力指数分别降低了16.05％，44.4％和32.1％。总之，无定形纳米NdCoO_3能大幅度提高AP／HTPB复合固体推进剂的燃速，明显降低燃烧压力指数，是一种很有希望应用于AP／HTPB复合固体推进剂的性能优良的燃烧调节剂。
Rare earth materials have found wide applications in many catalytic areas due to theirunique properties depending on the peculiar electronic structures of rare earth elements,however, there are few studies on rare earth materials in catalytic combustion of compositesolid propellants. Besides their electronic structures, the catalytic properties of rare earthmaterials are intimately related to their composition, size, phase, dispersibility, specificsurface areas and surface state, et al. Therefore, controlled synthesis of rare earth materialshas drawn continuous and worldwide research attention. In this dissertation, valuableexplorations have been carried out on the new chemical synthetic strategies ofnanostructured rare earth oxides and their catalytic properties for combustion of compositesolid propellants.
In chapter 2, one-step synthesis of nanocrystalline ceria-based powders via a solutioncombustion route using ethylene glycol as a novel fuel is described. An interpretationbased on an adiabatic flame temperature for different fuel-to-oxidant ratios(EG/NO_3~-) hasbeen proposed for the nature of combustion and its correlation with the powdercharacteristics. Ethylene glycol is nontoxic, cheap, easily available, mild duringcombustion reaction and has broad and potentiao applications in solution combustionsynthesis.
To solve the problem of particle agglomeration widely existing in solutioncombustion synthesis and enhance specific surface area of the combustion resultants, Wehave come up with a facile and novel salt-assisted solution combustion synthesis (SSCS)route to high surface area ceria-based nanopowders. It is revealed that the introduction ofsoluble and inert salt in the conventional combustion synthesis process was found to resultin the formation of 4～6 nm well-dispersed ceria nanoparticles and a more than ten-foldincrease in the specific surface area of the products from 14.10 to 156.74 m~2/g. In the caseof SSCS of Ce_(0.75)Zr_(0.25)O_2 solid solution, the addition of NaCl enhanced the specific surfacearea of the products from 17.34 to 208.17 m~2/g and led to the mesoporous structure formedby the loose agglomeration of monodisperse nanoparticles. The effects of such influencingfactors as the fuel-to-oxidant ratio, and the nature and amount of added salt on thecharacteristics of the products were investigated. A mechanism scheme was proposed toillustrate the possible formation processes of highly dispersed ceria-based nanoparticles. Finally, the influnce of nanocrystalline ceria-based powders on thermal decomposition ofammonium perchlorate(AP) was studied.
On the basis of the research of chapter 2, chapter 3 deals firstly with preparation ofthe well-dispersed perovskite LaMnO_3 nanoparticles by a solution salt-assisted combustionprocess, using ethylene glycol as a fuel and nitrates as oxidants. By tuning thefuel-to-oxidant ratio and the amount of added NaCl, the phase, dipersibility andmorphology of the resultants can be controlled. It is very significant that the cubic orrehombic LaMnO_3 nanorystal and perovskite nanocubes with narrow size distribution canbe obtained under the proper conditions.
In the second part of chapter 3, highly dispersed perovskite NdCoO_3 nanoparticleshave been successfully prepared by calcining the NaCl-containing precursor derived fromsalt-assisted solution combustion process employing glycine as a fuel. The facileintroduction of NaCl in the conventional combustion synthesis process was found toprevent particles from sintering and agglomerating and increase specific surface area of theresultants from 1.70 to 43.22 m~2/g. Besides enhancing calcination temperature, thepresence and increase of salt promotes formation of peroskite phase and growth ofcrystallite size in the process of calcination.
The TG-DSC results indicate that the combustion-derived nano-sized LaMnO_3 andNdCoO_3 show the intense catalytic activity on thermal decomposition of AP. The formerdecreases the temperature of AP high temperature decomposition peak by 103.9℃andincreases the apparent decomposition heat of AP by 838 J/g at most while the latterdecreases the temperature of AP high temperature decomposition peak by 116.7℃andincreases the apparent decomposition heat of AP by 947 J/g at most. Their catalytic activityis related to their particle size, dispersibility and phase, but is to large degree dependent ontheir specific surface area in the last analysis. Finally, the possible mechanism of catalyticdecomposition of AP by nano-sized ABO_3 was preliminarily discussed.
In chapter 4, we discuss preparation of nano-sized Y_2O_3 and Nd_2O_3 as well as theirdoped resultants via none-aqueous sol-gel process based on hydrated nitrate and ethyleneglycol, auto-propagating combustion and subsequent calcinations (gel combustionmethod).The as-prepared Y_2O_3 particles are spherical in shape and 20 nm in particle sizewhile the resultant Nd_2O_3 crystallites are spherical, well-dispersedand range from 30 nm to40 nm in size. Further, the effects of the molar ratio of ethylene glycol to yttrium ion,calcination temperature on crystallite size of the products were also studied. In summary,the synthetic method is easy to control, shortens the time to form xerogel and avoids segregation when doping.
The results in catalysis show that the 2wt.％Y_2O_3 and Nd_2O_3 respectively reduce thetemperature ofAP exothermic peak by 106.7℃and 96.2℃as well as enhance the apparentdecomposition heat by 645 J/g and 625 J/g. When doping 3.4％Fe~(3+), Co~(2+), Ni~(2+), Cu~(2+) andMn~(2+) into Y_2O_3 and Nd_2O_3, respectively, the doped resultants further decrease thetemperature of AP high temperature decomposition peak by 1～10℃and increases theapparent decomposition heat of AP. As the amount of doped Co~(2+) increases, the dopedY_2O_3 and Nd_2O_3 increase the apparent decomposition heat of AP, and have no greatinfluence on or reduce the temperature of AP high temperature decomposition peak.
In an effort to synthesize nano-sized NdCoO_3 a on a large scale, chapter 5investigates the preparation of nano-sized perovskite NdCoO_3 via a mechanochemicalprocess of NdCl_3·6H_2O+CoCl_2·6H_2O+6NaOH. It is observed that the NaCl derived in-situduring milling and added NaCl can improve the dispersibility and morphology of theas-synthesized particles owing to inhibiting agglomeration and accelerating mass transfer.Moreover, an increasing addition of NaCl not only improves particle dispersibility,increases specific surface area of the product but also promotes the formation of perovskiteNdCoO_3. It is interesting that highly dispersed NdCoO_3 nanocubes or nanorods can beprepared under the proper conditions. The preparative method is characterized byavailability in raw materials, convenient operation, simple process, high yield and potentialindustrialization.
In another effort, the well dispersed elliptical NdCoO_3 with particle size in the rangeof 10～23nm was prepared via wet-solid -phase milling and subsequent calcination ofNd_2O_3 and Co_3O_4 mixture, wherein the ZnO diluent was added after some milling period.The results reveal that an increasing addition of ZnO increases the specific surface area ofthe as-prepared NdCoO_3 from 7.39 m~2/g in the absence of ZnO to 36.11m~2/g and thatincreasing the calcination temperature results in crystallite growth and reduction in specificsurface area However, the synthetic process has such disadvantage as long preparativeperiod, high energy comsumption and difficulty in complete separation of ZnO diluent.
In the last part of chapter 5, we investigates catalytic properties of the nano-sizedNdCoO_3 prepared by a mechanochemical route, respectively using oxide and hydratechloride as raw materials, for the thermal decomposition of AP. The catalytic activityinvestigation demonstrates that the former decreases the temperature of AP hightemperature decomposition peak by 144.3℃and increases the apparent decompositionheat of AP by 632 J/g at most while the latter decreases the temperature of AP high temperature decomposition peak by 144.3℃and increases the apparent decompositionheat of AP by 695 J/g at most. As to the nano-sized NdCoO_3 synthesized by the same route,the larger the specific surface area is, the higher the catalytic activity is. The addition of3wt.％amorphous NdCoO_3 nanoparticles into the AP/HTPB composite solid propellantincorporates two exothermic peaks of the composite solid propellant into one exothermicpeak, decreases the temperature of the exothermic peak by 33℃。
The experiments in combustion characteristics show that the addition of 3wt.％nano-sized NdCoO_3 nanoparticles into the AP/HTPB composite solid propellant,respectively, enhances the burning rate at the pressures of about 4MPa, 7 PMa and 10MPby 40.0％, 40.6％and 23.7％, reduces the pressure exponents in the pressure scopes of4～7 MPa, 7～10MPa and 4～10 MPa by 16.05％, 44.4％and 32.1％. In summary, theamorphous nano-sized NdCoO_3 is expected to be an excellent and promising modifier forcombustion of the AP/HTPB composite solid propellant.
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