富勒烯在新型高能燃料中的燃烧机理
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摘要
NEPE推进剂是新型的硝酸酯增塑聚醚固体火箭推进剂。它集中了双基推进剂和复合推进剂的优点,属于新型高能燃料,不仅能量高、低温延伸率大,而且工艺性能、安全性能也较好,超过了现有的各种推进剂,是国际上现装备中能量最高的品种之一。但其在燃烧性能方面存在一些亟待解决的问题,特别是压强指数较高,能量性能与燃烧性能之间的矛盾,燃速与压强指数之间的矛盾,尚无有效的解决方法。燃烧机理的独特性,使得已有的双基或复合推进剂燃烧机理对它失效。以C_(60)为代表的富勒烯系列催化剂是近年来应用较广的催化剂材料之一,独特的封闭球状结构使得它们在许多方面都具有十分优良的催化性能,它们作为燃速催化剂在固体火箭推进剂中也有着十分显著的效果。
本论文研究了以C_(60)为代表的富勒烯对NEPE推进剂中主要氧化剂、粘合剂的热分解机理以及对推进剂燃速和压强指数的影响,发现少量的富勒烯灰(FS)催化剂就可以有效催化高氯酸铵(AP)热分解,抑制聚乙二醇(PEG)老化等。同时,获得了能有效降低RDX/AP-CMDB推进剂压强指数的0.5%FS/2.5%邻苯二甲酸铅(φ-Pb)/0.5%己二酸铜(J-Cu)复合催化剂配比,以及具有较高能量、较高燃速和较低压强指数的AP+PEG/硝化甘油(NG)/1,2,4-丁三醇三硝酸酯(BTTN)+2%FS推进剂配方范围。
(1)通过富勒烯和炭黑(CB)催化剂对推进剂中氧化剂AP热分解影响的实验研究发现,5%FS使得AP的起始分解温度(T_0),低温分解峰温(T_L)和高温分解峰温(T_H)分别提前了32℃,34℃和45℃,而5%EFS和5%C_(60)对AP的T_0,T_L和T_H影响都较小。5%CB使得AP的T_0,T_L和T_H分别降低了11℃,27℃和44℃。
通过FS和CB含量对AP热分解影响的研究结果可以看出,FS和CB对AP热分解都表现出了很好的催化作用,相对而言,FS的催化效果更好一些。3%FS就可以明显促进AP的起始分解,低温分解和高温分解过程,随着FS含量的提高,催化作用更加明显,当FS含量增加到8%时,AP的高低温分解过程发生重合。3%CB不影响AP的起始分解阶段,抑制了AP的低温分解阶段,但5%,8%和10%CB均促进了AP的起始分解,低温分解和高温分解过程。同样,当CB含量增加到8%时,AP的高低温分解过程发生重合。
(2)通过对AP+5%FS和AP+5%CB的热分解动力学研究可以看出,5%FS和5%CB均使得AP的高温热分解活化能明显降低。5%FS和5%CB使得AP的高温热分解活化能分别降低了约37%和34%。两种催化剂均使AP高温热分解反应的指前因子显著增加,说明催化剂能明显增加活化分子在总反应分子数中的百分比。所有催化剂均可以降低AP的着火温度,特别是5%FS可以使AP的着火温度下降47.4℃,而5%EFS,5%C_(60)和5%CB可以使AP的着火温度分别降低5.6℃,9.7℃和12.3℃。
(3)通过对富勒烯(或CB)/φ-Pb复合催化剂对AP热分解特性影响的实验研究发现,所有复合催化剂均使AP的起始分解温度显著提前,其中FS/φ-Pb复合催化剂对AP的起始分解过程催化最为明显,5%FS/φ-Pb使得AP的起始分解温度提前约40℃,随着FS含量从5%提高到10%,AP的起始分解温度也相应提前约8℃,但随着FS含量的进一步升高,AP的起始分解温度几乎保持不变。通过复合催化剂对AP恒容燃烧热影响的结果可以看出,相对于纯AP来说,70%AP/15%φ-Pb/15%FS和70%AP/15%φ-Pb/15%CB的恒容燃烧热分别增加了约146%和115%。
(4)富勒烯(或CB)催化剂对奥克托金(HMX)和六硝基六氮杂异戊兹烷(CL-20)的热分解特性研究结果显示,5%FS可以使得HMX的起始分解温度提前46℃,15%FS可使得HMX的分解峰温提前约15℃,而其它催化剂对HMX的热分解影响均不明显。FS使得CL-20的起始分解、分解峰温和分解结束温度都明显提前。纯CL-20的热分解和载气气氛没有关系,而氮气环境比空气环境更有利于FS对CL-20热分解的催化作用。
(5)根据富勒烯对推进剂中粘合剂端羟基聚丁二烯(HTPB)热分解和裂解特性影响的实验研究可以看出,HTPB的热分解动力学特性仅取决于HTPB的主链结构。应用裂解-气相色谱/质谱联用技术分析了HTPB的主要裂解产物,发现在280,320,350和380℃四个不同的裂解温度下,HTPB的裂解产物中都含有4-乙烯基-1-环己烯、苯乙烯等16种产物。对缩水甘油叠氮聚醚(GAP)的热分析实验结果显示,10%FS不影响GAP的低温分解过程,当FS含量增加到30%和50%后,GAP的低温分解峰温分别提前6℃和9℃。
(6)根据富勒烯对PEG热分解、原位升温红外光谱和裂解-气相色谱/质谱研究可以看出,FS使得PEG的起始分解温度和最大失重速率处的温度都有明显升高,同时也提高了PEG气相分解的温度,FS抑制了PEG的分解,它和PEG之间没有发生化学反应,没有生成新的具有红外吸收的官能团,它们之间仅仅是范德华力的作用。FS并没有从根本上改变PEG的分解机理,仅使得PEG的热分解峰温显著增加。FS对PEG的凝聚相分解过程影响并不明显,但使得PEG的气相分解温度明显升高,这主要是由于FS吸附的PEG气相分解产物覆盖了PEG的分解活化中心,从而抑制了PEG的气相分解。
(7)通过富勒烯(或CB)/φ-Pb/J-Cu复合催化剂对RDX/AP-CMDB推进剂催化作用的实验研究可以看出,富勒烯/φ-Pb/J-Cu复合催化剂对RDX/AP-CMDB推进剂的热分解过程影响不大,只略微促进了RDX/AP-CMDB推进剂中硝化棉(NC)的固相分解以及RDX的液相分解。富勒烯/φ-Pb/J-Cu复合催化剂均使得RDX/AP-CMDB推进剂的恒容燃烧热略有降低,相对于不同的催化剂来说,推进剂的恒容燃烧热可表示如下:HX-013(EFS)＞HX-014(C_(60))=HX-009(CB)＞HX-011(FS)。0.5%FS/2.5%φ-Pb/0.5%J-Cu使得推进剂HX-010的压强指数从基础配方的0.77降到0.64,降低了20%,在所有的催化剂组合中最为有效。
(8)通过FS对AP+GAP/NG/BTTN,HMX/AP+GAP/NG/BTTN和AP+PEG/NG/BTTN,HMX/AP+PEG/NG/BTTN推进剂的热分解、恒容燃烧热和燃速的影响结果可以得出,HMX有利于推进剂热分解过程,而AP则有利于推进剂燃速的提高。对于HMX/AP+GAP/NG/BTTN和HMX/AP+PEG/NG/BTTN推进剂来说,2%FS均比1%FS+1%PbO催化剂对推进剂的热分解和恒容燃烧热有利。其中对于AP+GAP/NG/BTTN和HMX/AP+GAP/NG/BTTN推进剂来说,2%FS可使它们的恒容燃烧热分别增加321 J·g~(-1)和851 J·g~(-1);而对于AP+PEG/NG/BTTN和HMX/AP+PEG/NG/BTTN推进剂来说,2%FS可使它们的恒容燃烧热分别增加201 J·g~(-1)和153 J·g~(-1)。特别是对于AP+PEG/NG/BTTN推进剂来说,用2%FS取代1%FS+1%PbO催化剂,在2.94MPa、4.90MPa、6.86MPa和8.83MPa压强下分别使推进剂的燃速增加78.4%、72.2%、55.5%和50.2%。
NEPE propellant is a new type of nitrate ester plasticized polyether solid rocket propellant.It concentrates both the advantages of double base(DB)and composite solid propellants.It not only has high energy,large low temperature elongation,but also has good technical process and safe property,which are better than other current equipped propellants.The N-15 propellant is a kind of the highest energetic propellants equipped in the modern world.But there are some problems to be solved about its combustion characteristics,such as higher pressure exponent,the contradiction between energy performance and combustion characteristics and the contradiction between burning rate and pressure exponents,etc.Thus its unique combustion mechanism leads to the invalidation of the traditional combustion mechanisms used in investigating DB and composite solid propellants.The fullerene catalysts are one of the most popular materials used in recent years,and the unique enclosed spherical structure promotes the catalytic ability in many fields.The fullerenes used as burning rate catalysts in solid propellant have very dramatic effects. This dissertation includes the effects of fullerenes on the thermal decomposition of the main oxides and binders,and the effects of fullerenes on the burning rates and pressure exponents of NEPE propellants.According to the results of these investigations,a small amount of fullerene soot(FS)could obviously promote the thermal decomposition of ammonium perchlorate(AP)and inhibit the aging process of polyethylene glycol(PEG).One 0.5%FS/2.5%lead phthalic acid(Φ-Pb)/0.5% copper adipic acid(J-Cu)composite catalysts which could effectively decrease the pressure exponents of cyclotrimethylene trinitramine(RDX)/AP-composite modified double-base(CMDB)propellant have been obtained,and another AP+PEG/ nitroglycerin(NG)/1,2,4- butantriol trinitrate(BTTN)+2%FS propellant which has large combustion heat,high buming rate and low pressure exponent is also gained.
(1)From the results of the effects of fullerenes and carbon black(CB)catalysts on the thermal decomposition of AP,one could see that the initial decomposition temperature(T_0),low and high temperature decomposition peak temperature(T_L and T_H)of AP were advanced 32℃,34℃and 45℃by 5%FS catalyst.Also,the T_0,T_L, and T_H of AP were advanced 11℃,27℃and 44℃by 5%CB catalyst.Therefore,the T_0,T_L,and T_H of AP were affected a little by 5%EFS and 5%C_(60).
The effects of FS and CB contents on the thermal decomposition of AP indicated that both FS and CB showed splendid catalytic effects on the thermal decomposition of AP,and the effect of FS was better.The initial decomposition,low and high temperature decomposition processes of AP were promoted by 3%FS,and the higher of FS contents,the better of the catalytic effects were.The low and high temperature decomposition processes of AP were overlapped by adding 8%or 10%FS.The To of AP was not affected,but the low temperature decomposition processes was inhibited by 3%CB.Therefore,these three decomposition processes of AP were promoted by 5%,8%and 10%CB.Also,the low and high temperature decomposition processes of AP were overlapped by adding 8%or 10%CB.
(2)A comparison of the thermal decomposition dynamics parameters of AP+5%FS and AP+5%CB indicated that the thermal decomposition activation energy of AP were lowered by 5%FS and 5%CB.The thermal decomposition activation energy of AP was lowered about 37%and 34%by 5%FS and 5%CB respectively.The thermal decomposition activation energy of AP+5%FS was a little smaller than that of AP+5%CB showed the better catalytic effect of FS.The pre-exponential factor of AP thermal decomposition was increased by these two catalysts,and this phenomenon showed the percentage of active molecules was increased by 5%FS and 5%CB.The ignition temperatures of AP were lowered about 5.6℃,9.7℃and 12.3℃by 5%EFS, 5%C_(60)and 5%CB respectively.Among all catalysts,FS showed the best effect and the ignition temperature of AP was lowered about 47.4℃by 5%FS.
(3)The investigation of the effects of fullerenes(or CB)/Φ-Pb composite catalysts on the thermal decomposition characteristics of AP showed that the initial decomposition process of AP was apparently promoted by these composite catalysts, among which FS/Φ-Pb showed the best catalytic effect,and the T_0 of AP was decreased about 40℃by 5%FS/15%Φ-Pb composite catalysts.The T_0 of AP was decreased about 8℃when the content of FS was increased from 5%to 15%.The combustion heat of 70%AP/15%Φ-Pb/15%FS and 70%AP/15%Φ-Pb/15%CB were increased about 146%and 115%when compared to that of pure AP.
(4)The effects of fullerenes and CB on the thermal decomposition characteristics of cyclotetramethylenete tranitramine(HMX)and hexanitrohexaaza-isowurtzitane (CL-20)were investigated by TG-DTG,DTA,and PDSC.The results showed that the initial decomposition temperature of HMX was advanced 46℃by 5%FS,and the decomposition peak temperature of HMX was lowered about 15℃by 15%FS.The initial decomposition temperature,decomposition peak temperature and the decomposition terminated temperature of CL-20 were obviously promoted by FS.The thermal decomposition of pure CL-20 didn't depend on the carrier gases and it was nitrogen not air atmosphere that was in favor of the catalytic ability of FS.
(5)The results of the effects of fullerenes on the thermal decomposition and pyrolysis characteristics of HTPB showed the thermal decomposition dynamic characteristic of HTPB is only depending on the main-chain structure of HTPB.The pyrolysis-GC/MS results of HTPB at 280,320,350 and 380℃showed that there exists 16 main products at all four different temperatures,including 4-ethenyl-cyclohexene,styrene,etc.The thermal decomposition results of glycidyl azide polymer(GAP)showed that the low temperature decomposition of GAP was not affected by 10%FS.Therefore,that of GAP were advanced 6℃and 9℃by 30%FS and 50%FS.
(6)The effects of fullerenes on the thermal decomposition of PEG have been investigated by TG,in-situ FTIR and pyrolysis-gas chromatography/mass spectrometry(Py-GC/MS).The results showed that the addition of fullerenes obviously restrained the thermal decomposition of PEG.The initial decomposition temperatures and maximum decomposition peak temperatures were evidently postponed by FS.There is no chemical reaction between FS and PEG,no new functional group with IR absorptive activity,but only vander's force between FS and PEG.FS didn't alter the thermal decomposition mechanism of PEG,but restrained the thermal decomposition of PEG.The effect of FS on the condense phase decomposition of PEG was not obvious,but FS made the increase of the gaseous decomposition temperature of PEG.This is mainly because the absorbance of gaseous decomposition products of PEG covered the surface of PEG.
(7)According to the results of the effects of fullerenes or CB/Φ-Pb/J-Cu composite catalysts on the combustion characteristics of RDX/AP-CMDB propellant, we found that the thermal decomposition of RDX/AP-CMDB propellant wasn't affected by these composite catalysts,but only the solid phase decomposition of nitrocellulose(NC)and liquid phase decomposition of RDX were slightly promoted by fullerenes/Φ-Pb/J-Cu composite catalysts.The combustion heat of RDX/AP-CMDB propellant was slightly decreased by fullerenes and the combustion heat values of RDX/AP-CMDB propellant with different catalysts are HX-013(EFS)＞HX-014(C_(60))=HX-009(CB)＞HX-011(FS).Compared to the basis formulation,the pressure exponent of HX-010 was lowered about 20%by 0.5%FS/2.5%Φ-Pb/0.5%J-Cu,and among all composite catalysts this is the best one.
(8)The results of the effects of FS on the thermal decomposition,combustion heats and burning rates of AP+GAP/NG/BTTN,HMX/AP+GAP/NG/BTTN, AP+PEG/NG/BTTN and HMX/AP+ PEG/NG/BTTN propellants showed that the thermal decomposition processes of these four propellants were benefitted with the addition of HMX and the burning rates of these four propellants were benefitted with the addition of AP.The combustion heats and buming rates of HMX/AP+GAP/NG/BTTN and HMX/AP+PEG/NG/BTTN propellants were benefitted by 2%FS with respect to 1%FS+1%PbO.When using 2%FS instead of 1%FS+1%PbO,the combustion heats of AP+GAP/NG/BTTN,HMX/AP+ GAP/NG/BTTN,AP+PEG/NG/BTTN and HMX/AP+PEG/NG/BTTN propellants were increased 321 J·g~(-1),851 J·g~(-1),201 J·g~(-1)and 153 J·g~(-1)respectively.Also the burning rates of AP+PEG/NG/BTTN propellant were increased about 78.4%,72.2%, 55.5%and 50.2%at 2.94MPa,4.90MPa,6.86MPa and 8.83MPa when using 2%FS instead of 1%FS+1%PbO.
本论文研究了以C_(60)为代表的富勒烯对NEPE推进剂中主要氧化剂、粘合剂的热分解机理以及对推进剂燃速和压强指数的影响,发现少量的富勒烯灰(FS)催化剂就可以有效催化高氯酸铵(AP)热分解,抑制聚乙二醇(PEG)老化等。同时,获得了能有效降低RDX/AP-CMDB推进剂压强指数的0.5%FS/2.5%邻苯二甲酸铅(φ-Pb)/0.5%己二酸铜(J-Cu)复合催化剂配比,以及具有较高能量、较高燃速和较低压强指数的AP+PEG/硝化甘油(NG)/1,2,4-丁三醇三硝酸酯(BTTN)+2%FS推进剂配方范围。
(1)通过富勒烯和炭黑(CB)催化剂对推进剂中氧化剂AP热分解影响的实验研究发现,5%FS使得AP的起始分解温度(T_0),低温分解峰温(T_L)和高温分解峰温(T_H)分别提前了32℃,34℃和45℃,而5%EFS和5%C_(60)对AP的T_0,T_L和T_H影响都较小。5%CB使得AP的T_0,T_L和T_H分别降低了11℃,27℃和44℃。
通过FS和CB含量对AP热分解影响的研究结果可以看出,FS和CB对AP热分解都表现出了很好的催化作用,相对而言,FS的催化效果更好一些。3%FS就可以明显促进AP的起始分解,低温分解和高温分解过程,随着FS含量的提高,催化作用更加明显,当FS含量增加到8%时,AP的高低温分解过程发生重合。3%CB不影响AP的起始分解阶段,抑制了AP的低温分解阶段,但5%,8%和10%CB均促进了AP的起始分解,低温分解和高温分解过程。同样,当CB含量增加到8%时,AP的高低温分解过程发生重合。
(2)通过对AP+5%FS和AP+5%CB的热分解动力学研究可以看出,5%FS和5%CB均使得AP的高温热分解活化能明显降低。5%FS和5%CB使得AP的高温热分解活化能分别降低了约37%和34%。两种催化剂均使AP高温热分解反应的指前因子显著增加,说明催化剂能明显增加活化分子在总反应分子数中的百分比。所有催化剂均可以降低AP的着火温度,特别是5%FS可以使AP的着火温度下降47.4℃,而5%EFS,5%C_(60)和5%CB可以使AP的着火温度分别降低5.6℃,9.7℃和12.3℃。
(3)通过对富勒烯(或CB)/φ-Pb复合催化剂对AP热分解特性影响的实验研究发现,所有复合催化剂均使AP的起始分解温度显著提前,其中FS/φ-Pb复合催化剂对AP的起始分解过程催化最为明显,5%FS/φ-Pb使得AP的起始分解温度提前约40℃,随着FS含量从5%提高到10%,AP的起始分解温度也相应提前约8℃,但随着FS含量的进一步升高,AP的起始分解温度几乎保持不变。通过复合催化剂对AP恒容燃烧热影响的结果可以看出,相对于纯AP来说,70%AP/15%φ-Pb/15%FS和70%AP/15%φ-Pb/15%CB的恒容燃烧热分别增加了约146%和115%。
(4)富勒烯(或CB)催化剂对奥克托金(HMX)和六硝基六氮杂异戊兹烷(CL-20)的热分解特性研究结果显示,5%FS可以使得HMX的起始分解温度提前46℃,15%FS可使得HMX的分解峰温提前约15℃,而其它催化剂对HMX的热分解影响均不明显。FS使得CL-20的起始分解、分解峰温和分解结束温度都明显提前。纯CL-20的热分解和载气气氛没有关系,而氮气环境比空气环境更有利于FS对CL-20热分解的催化作用。
(5)根据富勒烯对推进剂中粘合剂端羟基聚丁二烯(HTPB)热分解和裂解特性影响的实验研究可以看出,HTPB的热分解动力学特性仅取决于HTPB的主链结构。应用裂解-气相色谱/质谱联用技术分析了HTPB的主要裂解产物,发现在280,320,350和380℃四个不同的裂解温度下,HTPB的裂解产物中都含有4-乙烯基-1-环己烯、苯乙烯等16种产物。对缩水甘油叠氮聚醚(GAP)的热分析实验结果显示,10%FS不影响GAP的低温分解过程,当FS含量增加到30%和50%后,GAP的低温分解峰温分别提前6℃和9℃。
(6)根据富勒烯对PEG热分解、原位升温红外光谱和裂解-气相色谱/质谱研究可以看出,FS使得PEG的起始分解温度和最大失重速率处的温度都有明显升高,同时也提高了PEG气相分解的温度,FS抑制了PEG的分解,它和PEG之间没有发生化学反应,没有生成新的具有红外吸收的官能团,它们之间仅仅是范德华力的作用。FS并没有从根本上改变PEG的分解机理,仅使得PEG的热分解峰温显著增加。FS对PEG的凝聚相分解过程影响并不明显,但使得PEG的气相分解温度明显升高,这主要是由于FS吸附的PEG气相分解产物覆盖了PEG的分解活化中心,从而抑制了PEG的气相分解。
(7)通过富勒烯(或CB)/φ-Pb/J-Cu复合催化剂对RDX/AP-CMDB推进剂催化作用的实验研究可以看出,富勒烯/φ-Pb/J-Cu复合催化剂对RDX/AP-CMDB推进剂的热分解过程影响不大,只略微促进了RDX/AP-CMDB推进剂中硝化棉(NC)的固相分解以及RDX的液相分解。富勒烯/φ-Pb/J-Cu复合催化剂均使得RDX/AP-CMDB推进剂的恒容燃烧热略有降低,相对于不同的催化剂来说,推进剂的恒容燃烧热可表示如下:HX-013(EFS)＞HX-014(C_(60))=HX-009(CB)＞HX-011(FS)。0.5%FS/2.5%φ-Pb/0.5%J-Cu使得推进剂HX-010的压强指数从基础配方的0.77降到0.64,降低了20%,在所有的催化剂组合中最为有效。
(8)通过FS对AP+GAP/NG/BTTN,HMX/AP+GAP/NG/BTTN和AP+PEG/NG/BTTN,HMX/AP+PEG/NG/BTTN推进剂的热分解、恒容燃烧热和燃速的影响结果可以得出,HMX有利于推进剂热分解过程,而AP则有利于推进剂燃速的提高。对于HMX/AP+GAP/NG/BTTN和HMX/AP+PEG/NG/BTTN推进剂来说,2%FS均比1%FS+1%PbO催化剂对推进剂的热分解和恒容燃烧热有利。其中对于AP+GAP/NG/BTTN和HMX/AP+GAP/NG/BTTN推进剂来说,2%FS可使它们的恒容燃烧热分别增加321 J·g~(-1)和851 J·g~(-1);而对于AP+PEG/NG/BTTN和HMX/AP+PEG/NG/BTTN推进剂来说,2%FS可使它们的恒容燃烧热分别增加201 J·g~(-1)和153 J·g~(-1)。特别是对于AP+PEG/NG/BTTN推进剂来说,用2%FS取代1%FS+1%PbO催化剂,在2.94MPa、4.90MPa、6.86MPa和8.83MPa压强下分别使推进剂的燃速增加78.4%、72.2%、55.5%和50.2%。
NEPE propellant is a new type of nitrate ester plasticized polyether solid rocket propellant.It concentrates both the advantages of double base(DB)and composite solid propellants.It not only has high energy,large low temperature elongation,but also has good technical process and safe property,which are better than other current equipped propellants.The N-15 propellant is a kind of the highest energetic propellants equipped in the modern world.But there are some problems to be solved about its combustion characteristics,such as higher pressure exponent,the contradiction between energy performance and combustion characteristics and the contradiction between burning rate and pressure exponents,etc.Thus its unique combustion mechanism leads to the invalidation of the traditional combustion mechanisms used in investigating DB and composite solid propellants.The fullerene catalysts are one of the most popular materials used in recent years,and the unique enclosed spherical structure promotes the catalytic ability in many fields.The fullerenes used as burning rate catalysts in solid propellant have very dramatic effects. This dissertation includes the effects of fullerenes on the thermal decomposition of the main oxides and binders,and the effects of fullerenes on the burning rates and pressure exponents of NEPE propellants.According to the results of these investigations,a small amount of fullerene soot(FS)could obviously promote the thermal decomposition of ammonium perchlorate(AP)and inhibit the aging process of polyethylene glycol(PEG).One 0.5%FS/2.5%lead phthalic acid(Φ-Pb)/0.5% copper adipic acid(J-Cu)composite catalysts which could effectively decrease the pressure exponents of cyclotrimethylene trinitramine(RDX)/AP-composite modified double-base(CMDB)propellant have been obtained,and another AP+PEG/ nitroglycerin(NG)/1,2,4- butantriol trinitrate(BTTN)+2%FS propellant which has large combustion heat,high buming rate and low pressure exponent is also gained.
(1)From the results of the effects of fullerenes and carbon black(CB)catalysts on the thermal decomposition of AP,one could see that the initial decomposition temperature(T_0),low and high temperature decomposition peak temperature(T_L and T_H)of AP were advanced 32℃,34℃and 45℃by 5%FS catalyst.Also,the T_0,T_L, and T_H of AP were advanced 11℃,27℃and 44℃by 5%CB catalyst.Therefore,the T_0,T_L,and T_H of AP were affected a little by 5%EFS and 5%C_(60).
The effects of FS and CB contents on the thermal decomposition of AP indicated that both FS and CB showed splendid catalytic effects on the thermal decomposition of AP,and the effect of FS was better.The initial decomposition,low and high temperature decomposition processes of AP were promoted by 3%FS,and the higher of FS contents,the better of the catalytic effects were.The low and high temperature decomposition processes of AP were overlapped by adding 8%or 10%FS.The To of AP was not affected,but the low temperature decomposition processes was inhibited by 3%CB.Therefore,these three decomposition processes of AP were promoted by 5%,8%and 10%CB.Also,the low and high temperature decomposition processes of AP were overlapped by adding 8%or 10%CB.
(2)A comparison of the thermal decomposition dynamics parameters of AP+5%FS and AP+5%CB indicated that the thermal decomposition activation energy of AP were lowered by 5%FS and 5%CB.The thermal decomposition activation energy of AP was lowered about 37%and 34%by 5%FS and 5%CB respectively.The thermal decomposition activation energy of AP+5%FS was a little smaller than that of AP+5%CB showed the better catalytic effect of FS.The pre-exponential factor of AP thermal decomposition was increased by these two catalysts,and this phenomenon showed the percentage of active molecules was increased by 5%FS and 5%CB.The ignition temperatures of AP were lowered about 5.6℃,9.7℃and 12.3℃by 5%EFS, 5%C_(60)and 5%CB respectively.Among all catalysts,FS showed the best effect and the ignition temperature of AP was lowered about 47.4℃by 5%FS.
(3)The investigation of the effects of fullerenes(or CB)/Φ-Pb composite catalysts on the thermal decomposition characteristics of AP showed that the initial decomposition process of AP was apparently promoted by these composite catalysts, among which FS/Φ-Pb showed the best catalytic effect,and the T_0 of AP was decreased about 40℃by 5%FS/15%Φ-Pb composite catalysts.The T_0 of AP was decreased about 8℃when the content of FS was increased from 5%to 15%.The combustion heat of 70%AP/15%Φ-Pb/15%FS and 70%AP/15%Φ-Pb/15%CB were increased about 146%and 115%when compared to that of pure AP.
(4)The effects of fullerenes and CB on the thermal decomposition characteristics of cyclotetramethylenete tranitramine(HMX)and hexanitrohexaaza-isowurtzitane (CL-20)were investigated by TG-DTG,DTA,and PDSC.The results showed that the initial decomposition temperature of HMX was advanced 46℃by 5%FS,and the decomposition peak temperature of HMX was lowered about 15℃by 15%FS.The initial decomposition temperature,decomposition peak temperature and the decomposition terminated temperature of CL-20 were obviously promoted by FS.The thermal decomposition of pure CL-20 didn't depend on the carrier gases and it was nitrogen not air atmosphere that was in favor of the catalytic ability of FS.
(5)The results of the effects of fullerenes on the thermal decomposition and pyrolysis characteristics of HTPB showed the thermal decomposition dynamic characteristic of HTPB is only depending on the main-chain structure of HTPB.The pyrolysis-GC/MS results of HTPB at 280,320,350 and 380℃showed that there exists 16 main products at all four different temperatures,including 4-ethenyl-cyclohexene,styrene,etc.The thermal decomposition results of glycidyl azide polymer(GAP)showed that the low temperature decomposition of GAP was not affected by 10%FS.Therefore,that of GAP were advanced 6℃and 9℃by 30%FS and 50%FS.
(6)The effects of fullerenes on the thermal decomposition of PEG have been investigated by TG,in-situ FTIR and pyrolysis-gas chromatography/mass spectrometry(Py-GC/MS).The results showed that the addition of fullerenes obviously restrained the thermal decomposition of PEG.The initial decomposition temperatures and maximum decomposition peak temperatures were evidently postponed by FS.There is no chemical reaction between FS and PEG,no new functional group with IR absorptive activity,but only vander's force between FS and PEG.FS didn't alter the thermal decomposition mechanism of PEG,but restrained the thermal decomposition of PEG.The effect of FS on the condense phase decomposition of PEG was not obvious,but FS made the increase of the gaseous decomposition temperature of PEG.This is mainly because the absorbance of gaseous decomposition products of PEG covered the surface of PEG.
(7)According to the results of the effects of fullerenes or CB/Φ-Pb/J-Cu composite catalysts on the combustion characteristics of RDX/AP-CMDB propellant, we found that the thermal decomposition of RDX/AP-CMDB propellant wasn't affected by these composite catalysts,but only the solid phase decomposition of nitrocellulose(NC)and liquid phase decomposition of RDX were slightly promoted by fullerenes/Φ-Pb/J-Cu composite catalysts.The combustion heat of RDX/AP-CMDB propellant was slightly decreased by fullerenes and the combustion heat values of RDX/AP-CMDB propellant with different catalysts are HX-013(EFS)＞HX-014(C_(60))=HX-009(CB)＞HX-011(FS).Compared to the basis formulation,the pressure exponent of HX-010 was lowered about 20%by 0.5%FS/2.5%Φ-Pb/0.5%J-Cu,and among all composite catalysts this is the best one.
(8)The results of the effects of FS on the thermal decomposition,combustion heats and burning rates of AP+GAP/NG/BTTN,HMX/AP+GAP/NG/BTTN, AP+PEG/NG/BTTN and HMX/AP+ PEG/NG/BTTN propellants showed that the thermal decomposition processes of these four propellants were benefitted with the addition of HMX and the burning rates of these four propellants were benefitted with the addition of AP.The combustion heats and buming rates of HMX/AP+GAP/NG/BTTN and HMX/AP+PEG/NG/BTTN propellants were benefitted by 2%FS with respect to 1%FS+1%PbO.When using 2%FS instead of 1%FS+1%PbO,the combustion heats of AP+GAP/NG/BTTN,HMX/AP+ GAP/NG/BTTN,AP+PEG/NG/BTTN and HMX/AP+PEG/NG/BTTN propellants were increased 321 J·g~(-1),851 J·g~(-1),201 J·g~(-1)and 153 J·g~(-1)respectively.Also the burning rates of AP+PEG/NG/BTTN propellant were increased about 78.4%,72.2%, 55.5%and 50.2%at 2.94MPa,4.90MPa,6.86MPa and 8.83MPa when using 2%FS instead of 1%FS+1%PbO.
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