炸药微观结构对性能的影响研究
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摘要
本论文以硝酸铵(AN)和TATB两种不同性质、不同应用领域的炸药原材料为研究对象,较全面表征了原料及相应炸药配方的微观结构和性能,得到了炸药微观结构对性能的影响关系。重点研究了硝酸铵及铵油炸药(ANFO)的微观结构及对热分解温度、雷管起爆感度等性能的影响,同时研究了TATB粉体和TATB基复合含能体系的微观结构及对热感度等性能的影响。
从N_2吸附等温线形状判断,几种硝酸铵样品均属于大孔材料;硝酸铵及铵油炸药样品的微观结构因样品状态不同而有所不同:工业未膨化样品的密度大,孔隙度低,粒子表面光滑,颗粒表面突起、孔隙和裂纹相对较少;膨化后样品平均孔径未发生明显改变,但密度降低、孔隙度提高、孔隙数量显著增加,晶形严重歧化,粒子表面存在大量棱角、突起、毛孔和裂纹等缺陷,不同膨化样品的孔隙状态和表面特征又与制备条件密切相关;粉碎、过筛过程使样品颗粒尺寸更接近、形貌更规则且部分孔隙遭到破坏,因此孔隙数量减少、孔隙度降低、比表面积有所减小。
论文引入分形理论研究硝酸铵体系分形情况及颗粒粗糙程度,选择并修正了适于对硝酸铵颗粒粗糙度进行相对定量比较的分维公式,由压汞曲线和N_2吸附曲线得到的分维值顺序均与SEM得到的粒子表面粗糙度顺序相吻合;分维值表明未过筛硝酸铵样品间的颗粒粗糙度差异较大,而40目样品间的颗粒粗糙度差异相对较小。
研究发现硝酸铵及铵油炸药的热感度和雷管起爆感度主要取决于样品中的孔隙数量,孔隙越多,则外界热作用或冲击波作用下形成的热点数量越多,炸药越易发生反应和起爆。铵油炸药状态和装药条件对爆轰性能影响明显,在一定范围内,铵油炸药爆轰能力随着水分含量减少、粒度降低、装药高度增加、装药密度提高、装药直径增大而提高。雷管起爆和爆轰实验发现,在其它条件相同情况下,铵油炸药爆轰能力大小与硝酸铵样品颗粒粗糙程度(分维)顺序一致,而与样品孔隙度或比表面积顺序不一致,表明铵油炸药颗粒粗糙程度是决定炸药爆轰能力的主要因素。有机玻璃法测试结果也表明,与普通铵油炸药相比,膨化铵油炸药爆轰更完全、爆速和爆压更高,粒度减小也有利于提高铵油炸药的爆压。在实验基础上阐述了铵油炸药起爆及爆轰反应机理,即其起爆和爆轰发展过程存在着两个不同的反应阶段一热点形成和点火阶段、爆轰发展阶段。
几种无机添加剂改性铵油炸药的微观结构没有发生明显改变,但其雷管起爆感度和爆轰能力得到了提高;几种有机表面活性剂改性铵油炸药的微观结构存在显著差异,其起爆感度和爆轰能力也存在较大不同,爆轰能力大小与颗粒粗糙程度顺序一致。
对不同状态硝酸铵的相转变行为研究发现,粒度减小有助于抑制硝酸铵Ⅳ-Ⅲ、Ⅲ-Ⅱ的相转变;硝酸铵相转变行为似乎与样品颗粒表面特征之间存在着一定联系:CsNO_3等无机物对AN微观结构影响不大,相应AN的相转变行为无显著改变;钾盐使AN颗粒表面变光滑、规则,钾盐可有效抑制Ⅳ-Ⅲ的相转变行为;所研究的氧化物、Cu(NO_3)_2、MgSO_4等无机物使AN颗粒表面变粗糙、颗粒表面裂纹及碎小颗粒等缺陷增多,它们可有效抑制Ⅲ-Ⅱ的相转变行为。但此规律还需得到更多实验证实或修正。
TATB微观结构与样品制备方法密切相关:直接合成样品的绝大部分粒子粒径在10μm以上,比表面积低,粒子呈类球形、大小不均匀,表面粗糙;几种细化方法得到的超细样品平均粒径均处于亚微米级,98%以上粒子粒径小于200nm,气流粉碎样品及重结晶样品的比表面积较接近,而机械研磨样品比表面积较低;气流粉碎样品粒子呈类球形,表面较光滑;重结晶样品粒子形状不规则,低倍数下呈片状或球状,粒子形状差异大,高倍数下呈条形,重结晶样品再经气流粉碎后粒子变得较均匀、规则;SEM法得到的各样品粒子粗糙度顺序与分维顺序一致。采用两种方法研究了TATB的孔隙结构,N_2吸附法测试表明:合成样品孔隙极少,重结晶样品存在较多孔隙,气流粉碎样品和重结晶再气流粉碎样品含有少量孔隙;同步辐射X射线小角散射实验(SAXS)测量结果表明:制备方法对TATB微观结构影响明显,由分维数据可得到各样品颗粒表面粗糙度顺序。
TATB热分解温度、5秒爆发点温度和短脉冲起爆感度均与TATB微观结构密切相关,主要取决于样品中孔隙数量,即孔隙越多,其热分解温度和热爆炸温度越低,炸药越易被短脉冲作用所起爆。TATB短脉冲起爆感度和爆轰完全程度也与装药密度成反比、与孔隙度成正比;在孔隙度相近情况下,爆轰能力主要由分维决定。
溶剂快速驱除法和高能撞击法得到的TATB基复合粒子各组分在微纳尺度上复合良好,粒子大小均匀、形貌接近;机械混合体系中的各组分粒子形态明显,粒子间接触面积有限,且有部分敏感炸药粒子裸露在外面。TATB基复合粒子的热稳定性和机械撞击感度受复合粒子微观结构的显著影响:BT体系出现BTF的熔化峰,HT体系未出现HMX的熔化峰,且HT体系的TATB分解放热峰温度较BT体系降低10℃以上,复合体系的机械撞击感度也显著降低。
In order to better understand the effects of explosive microstructures on properties, two kinds of explosive materials, inorganic compound ammonium nitrate(AN) and organic compound 1,3,5-triamino-2,4,6-trinitrobenzene(TATB) which have different natures and application fields, and their explosive formulations have been discussed. The microstructures(porosity,pore structure,surface character,etc.) and properties(suck as thermal decompose temperature, detonator ignition sensitivity,etc.) of different state AN and ANFO have been mainly researched. Synchronously, the microstructures and properties of TATB powder and TATB based composite also have been studied.
Judged by N_2 adsorbtion isotherm, AN samples should belong to coarse pore materials. The microstructures of different states AN and ANFO are much different, for example, the density of industry unexpanded sample is high and porosity is low relatively, particles' surface is smooth, the number of protuberance,hole and crack is also less than expanded samples. After expanded, the average pore diameter has no remarkable change, but pore volume increase and density falls markedly, the aberrance of crystal shape is severe, there are many defects of protuberances, pointedness, pores and cracks appear on the particles surface, so the particles surface shows a accidented structure characteristics. The pore structure and particles surface charaters of expanded samples are ralated with their prepared conditions. The process of smashing and sieving make particles size and shape much close, some pores are destroyed, so the pore number decreases, porosity reduces and specific surface area falls.
Fractal dimension is used to compare the coarse degree of AN particles relatively quantificationally in our research and the fractal dimension calculate formula suited for treating AN's mercury intrusion adsorption curve is selected and modified. The order of fractal dimension value obtained respectively from mercury intrusion adsorption curve and N_2 adsorbtion isotherm is accordant and consistent with the order of particles coarse degree which obtained by SEM. Fractal dimension values indicate that the coarse degree of unsieving AN samples is much different while 40 mesh AN samples have a little difference.
The thermal sensitivity and detonator ignition sensitivity of AN and ANFO mainly depend on the number of pores, the more the number of pores is, the more the hot spots formed under outside thermal action and shock wave have, so explosives happen reaction and ignition more easily. The experimental results also show that ANFO states and charge conditions have an evident effect on formulations' detonation properties, in a certain range, the explosive detonation capability increases along with the water content reduces, particles size decreases, charge height enhances, charge density increases and charge diameter augments. When other conditions are restricted, the order of ANFO detonation capability is accorded with the order of AN particles coarse degree (i.e. fractal dimension) while isn't accorded with the order of specific surface area or porosity, so ANFO particles coarse degree is the remarkable factor of determining explosive detonation capability. The experimental results of polymethyl methacrylate method also indicate expanded ANFO has much higher detonation velocity and detonation pressure than common ANFO sample, the detonation pressure increase with the reduce of explosives particles size,too. Based on these results of ignition and detonation capability, the ignition and detonation reaction mechanism of ANFO are expounded, i.e., there are two different reaction phases during ANFO's ignition and detonation developing process, one is the phase of hot spots forming and ignition, the other is the phase of detonation growing.
When some selective inorganic additives are added into ANFO formulations, although the explosive's micro structures have no evident change, the ignition and detonation capability increase. However, the selective organic surfactant can change ANFO sample microstructures, so the ignition sensitivity and detonation capability change, the order of detonation capability is agree with the order of particles coarse degree.
The phase transition behavior of different state AN are also studied, the results show that the reduce of particles size is helpful to restrain the phase transition of III-II, and there seems have some relations between the AN phase transition behavior and particles surface characters, that is: when modified AN particle surface microstructure has little change, the phase transition behavior doesn't has remarkable change; potassic salts can smooth the AN particles surface, so the modified AN samples have little phase transition of IV-III; Oxide,Cu(NO_3)_2, (NH_4)_2SO_4,MgSO_4 and other mineral coarsen the AN particles surface, so the phase transition behavior of III-II can be restrained. But this rule should be further approved or modified by more systemic experiments.
TATB samples microstructures are correlated nearly with the preparation methods. Most directly synthesizing sample's particles size is beyond 10μm, specific surface area is low, particles shape is similar to sphericity and particles size is asymmetry, particles surface is coarse. While the samples' average size which prepared by several fined methods is within submicron grade, above 98% particles size is smaller than 200nm, the specific surface area of air-flow smashing sample is close to that of recrystalling samples, while the specific surface area of mechanical milling samples is quite low. The particles shape of air-flow smashing samples is also similar to sphericity and particles surface is smooth.For recrystalling samples, the particles shape is erose, profile is similar to slice or spherical and shape's difference is great under low multiple SEM, while under high multiple SEM,the particles shape is similar to strip. When the recrystalling samples are smashed by air-flow, the particles shape becomes symmetrical and regular. The order of particles coarse degree obtained by SEM is accorded with the order of fractal dimision gained by small anglex ray scattering method(SAXS).TATB pore structures are investigated by two methods, one is N_2 absorption method, the other is synchrotron radiation SAXS technique.The measuring results of N_2 method show that synthesizing samples have little pores but recrystalling samples have many pores, air-flow smashing samples and recrystalling-airflow smashing samples have a few pores. The SAXS testing results also show that preparation methods have an obvious effect on TATB microstructures and the samples particles surface coarse degree can be compared by fractal dimension value.
The thermal decompose temperature,5seconds explosion point temperature and short pulse ignition sensitivity are correlated with TATB microstructures, especially rest on the pore number.The short pulse ignition sensitivity and detonation complete degree are inverse with charge density and direct with porosity, when the porosity is adjacent, the detonation capability mainly determined by fractal dimension.
The ingredients of TATB based composite prepared by solvent quick removing method and high energy impacting method can be composited at micro-nano scale, composite particles size is symmetrical and shape is similar.While the ingredients particles shape of machanical mixtures is distinct, the particles contact area is limited and some sensitive explosive particles are bared and expose to external action, so its impact sensitivity is higher than that of composite.
从N_2吸附等温线形状判断,几种硝酸铵样品均属于大孔材料;硝酸铵及铵油炸药样品的微观结构因样品状态不同而有所不同:工业未膨化样品的密度大,孔隙度低,粒子表面光滑,颗粒表面突起、孔隙和裂纹相对较少;膨化后样品平均孔径未发生明显改变,但密度降低、孔隙度提高、孔隙数量显著增加,晶形严重歧化,粒子表面存在大量棱角、突起、毛孔和裂纹等缺陷,不同膨化样品的孔隙状态和表面特征又与制备条件密切相关;粉碎、过筛过程使样品颗粒尺寸更接近、形貌更规则且部分孔隙遭到破坏,因此孔隙数量减少、孔隙度降低、比表面积有所减小。
论文引入分形理论研究硝酸铵体系分形情况及颗粒粗糙程度,选择并修正了适于对硝酸铵颗粒粗糙度进行相对定量比较的分维公式,由压汞曲线和N_2吸附曲线得到的分维值顺序均与SEM得到的粒子表面粗糙度顺序相吻合;分维值表明未过筛硝酸铵样品间的颗粒粗糙度差异较大,而40目样品间的颗粒粗糙度差异相对较小。
研究发现硝酸铵及铵油炸药的热感度和雷管起爆感度主要取决于样品中的孔隙数量,孔隙越多,则外界热作用或冲击波作用下形成的热点数量越多,炸药越易发生反应和起爆。铵油炸药状态和装药条件对爆轰性能影响明显,在一定范围内,铵油炸药爆轰能力随着水分含量减少、粒度降低、装药高度增加、装药密度提高、装药直径增大而提高。雷管起爆和爆轰实验发现,在其它条件相同情况下,铵油炸药爆轰能力大小与硝酸铵样品颗粒粗糙程度(分维)顺序一致,而与样品孔隙度或比表面积顺序不一致,表明铵油炸药颗粒粗糙程度是决定炸药爆轰能力的主要因素。有机玻璃法测试结果也表明,与普通铵油炸药相比,膨化铵油炸药爆轰更完全、爆速和爆压更高,粒度减小也有利于提高铵油炸药的爆压。在实验基础上阐述了铵油炸药起爆及爆轰反应机理,即其起爆和爆轰发展过程存在着两个不同的反应阶段一热点形成和点火阶段、爆轰发展阶段。
几种无机添加剂改性铵油炸药的微观结构没有发生明显改变,但其雷管起爆感度和爆轰能力得到了提高;几种有机表面活性剂改性铵油炸药的微观结构存在显著差异,其起爆感度和爆轰能力也存在较大不同,爆轰能力大小与颗粒粗糙程度顺序一致。
对不同状态硝酸铵的相转变行为研究发现,粒度减小有助于抑制硝酸铵Ⅳ-Ⅲ、Ⅲ-Ⅱ的相转变;硝酸铵相转变行为似乎与样品颗粒表面特征之间存在着一定联系:CsNO_3等无机物对AN微观结构影响不大,相应AN的相转变行为无显著改变;钾盐使AN颗粒表面变光滑、规则,钾盐可有效抑制Ⅳ-Ⅲ的相转变行为;所研究的氧化物、Cu(NO_3)_2、MgSO_4等无机物使AN颗粒表面变粗糙、颗粒表面裂纹及碎小颗粒等缺陷增多,它们可有效抑制Ⅲ-Ⅱ的相转变行为。但此规律还需得到更多实验证实或修正。
TATB微观结构与样品制备方法密切相关:直接合成样品的绝大部分粒子粒径在10μm以上,比表面积低,粒子呈类球形、大小不均匀,表面粗糙;几种细化方法得到的超细样品平均粒径均处于亚微米级,98%以上粒子粒径小于200nm,气流粉碎样品及重结晶样品的比表面积较接近,而机械研磨样品比表面积较低;气流粉碎样品粒子呈类球形,表面较光滑;重结晶样品粒子形状不规则,低倍数下呈片状或球状,粒子形状差异大,高倍数下呈条形,重结晶样品再经气流粉碎后粒子变得较均匀、规则;SEM法得到的各样品粒子粗糙度顺序与分维顺序一致。采用两种方法研究了TATB的孔隙结构,N_2吸附法测试表明:合成样品孔隙极少,重结晶样品存在较多孔隙,气流粉碎样品和重结晶再气流粉碎样品含有少量孔隙;同步辐射X射线小角散射实验(SAXS)测量结果表明:制备方法对TATB微观结构影响明显,由分维数据可得到各样品颗粒表面粗糙度顺序。
TATB热分解温度、5秒爆发点温度和短脉冲起爆感度均与TATB微观结构密切相关,主要取决于样品中孔隙数量,即孔隙越多,其热分解温度和热爆炸温度越低,炸药越易被短脉冲作用所起爆。TATB短脉冲起爆感度和爆轰完全程度也与装药密度成反比、与孔隙度成正比;在孔隙度相近情况下,爆轰能力主要由分维决定。
溶剂快速驱除法和高能撞击法得到的TATB基复合粒子各组分在微纳尺度上复合良好,粒子大小均匀、形貌接近;机械混合体系中的各组分粒子形态明显,粒子间接触面积有限,且有部分敏感炸药粒子裸露在外面。TATB基复合粒子的热稳定性和机械撞击感度受复合粒子微观结构的显著影响:BT体系出现BTF的熔化峰,HT体系未出现HMX的熔化峰,且HT体系的TATB分解放热峰温度较BT体系降低10℃以上,复合体系的机械撞击感度也显著降低。
In order to better understand the effects of explosive microstructures on properties, two kinds of explosive materials, inorganic compound ammonium nitrate(AN) and organic compound 1,3,5-triamino-2,4,6-trinitrobenzene(TATB) which have different natures and application fields, and their explosive formulations have been discussed. The microstructures(porosity,pore structure,surface character,etc.) and properties(suck as thermal decompose temperature, detonator ignition sensitivity,etc.) of different state AN and ANFO have been mainly researched. Synchronously, the microstructures and properties of TATB powder and TATB based composite also have been studied.
Judged by N_2 adsorbtion isotherm, AN samples should belong to coarse pore materials. The microstructures of different states AN and ANFO are much different, for example, the density of industry unexpanded sample is high and porosity is low relatively, particles' surface is smooth, the number of protuberance,hole and crack is also less than expanded samples. After expanded, the average pore diameter has no remarkable change, but pore volume increase and density falls markedly, the aberrance of crystal shape is severe, there are many defects of protuberances, pointedness, pores and cracks appear on the particles surface, so the particles surface shows a accidented structure characteristics. The pore structure and particles surface charaters of expanded samples are ralated with their prepared conditions. The process of smashing and sieving make particles size and shape much close, some pores are destroyed, so the pore number decreases, porosity reduces and specific surface area falls.
Fractal dimension is used to compare the coarse degree of AN particles relatively quantificationally in our research and the fractal dimension calculate formula suited for treating AN's mercury intrusion adsorption curve is selected and modified. The order of fractal dimension value obtained respectively from mercury intrusion adsorption curve and N_2 adsorbtion isotherm is accordant and consistent with the order of particles coarse degree which obtained by SEM. Fractal dimension values indicate that the coarse degree of unsieving AN samples is much different while 40 mesh AN samples have a little difference.
The thermal sensitivity and detonator ignition sensitivity of AN and ANFO mainly depend on the number of pores, the more the number of pores is, the more the hot spots formed under outside thermal action and shock wave have, so explosives happen reaction and ignition more easily. The experimental results also show that ANFO states and charge conditions have an evident effect on formulations' detonation properties, in a certain range, the explosive detonation capability increases along with the water content reduces, particles size decreases, charge height enhances, charge density increases and charge diameter augments. When other conditions are restricted, the order of ANFO detonation capability is accorded with the order of AN particles coarse degree (i.e. fractal dimension) while isn't accorded with the order of specific surface area or porosity, so ANFO particles coarse degree is the remarkable factor of determining explosive detonation capability. The experimental results of polymethyl methacrylate method also indicate expanded ANFO has much higher detonation velocity and detonation pressure than common ANFO sample, the detonation pressure increase with the reduce of explosives particles size,too. Based on these results of ignition and detonation capability, the ignition and detonation reaction mechanism of ANFO are expounded, i.e., there are two different reaction phases during ANFO's ignition and detonation developing process, one is the phase of hot spots forming and ignition, the other is the phase of detonation growing.
When some selective inorganic additives are added into ANFO formulations, although the explosive's micro structures have no evident change, the ignition and detonation capability increase. However, the selective organic surfactant can change ANFO sample microstructures, so the ignition sensitivity and detonation capability change, the order of detonation capability is agree with the order of particles coarse degree.
The phase transition behavior of different state AN are also studied, the results show that the reduce of particles size is helpful to restrain the phase transition of III-II, and there seems have some relations between the AN phase transition behavior and particles surface characters, that is: when modified AN particle surface microstructure has little change, the phase transition behavior doesn't has remarkable change; potassic salts can smooth the AN particles surface, so the modified AN samples have little phase transition of IV-III; Oxide,Cu(NO_3)_2, (NH_4)_2SO_4,MgSO_4 and other mineral coarsen the AN particles surface, so the phase transition behavior of III-II can be restrained. But this rule should be further approved or modified by more systemic experiments.
TATB samples microstructures are correlated nearly with the preparation methods. Most directly synthesizing sample's particles size is beyond 10μm, specific surface area is low, particles shape is similar to sphericity and particles size is asymmetry, particles surface is coarse. While the samples' average size which prepared by several fined methods is within submicron grade, above 98% particles size is smaller than 200nm, the specific surface area of air-flow smashing sample is close to that of recrystalling samples, while the specific surface area of mechanical milling samples is quite low. The particles shape of air-flow smashing samples is also similar to sphericity and particles surface is smooth.For recrystalling samples, the particles shape is erose, profile is similar to slice or spherical and shape's difference is great under low multiple SEM, while under high multiple SEM,the particles shape is similar to strip. When the recrystalling samples are smashed by air-flow, the particles shape becomes symmetrical and regular. The order of particles coarse degree obtained by SEM is accorded with the order of fractal dimision gained by small anglex ray scattering method(SAXS).TATB pore structures are investigated by two methods, one is N_2 absorption method, the other is synchrotron radiation SAXS technique.The measuring results of N_2 method show that synthesizing samples have little pores but recrystalling samples have many pores, air-flow smashing samples and recrystalling-airflow smashing samples have a few pores. The SAXS testing results also show that preparation methods have an obvious effect on TATB microstructures and the samples particles surface coarse degree can be compared by fractal dimension value.
The thermal decompose temperature,5seconds explosion point temperature and short pulse ignition sensitivity are correlated with TATB microstructures, especially rest on the pore number.The short pulse ignition sensitivity and detonation complete degree are inverse with charge density and direct with porosity, when the porosity is adjacent, the detonation capability mainly determined by fractal dimension.
The ingredients of TATB based composite prepared by solvent quick removing method and high energy impacting method can be composited at micro-nano scale, composite particles size is symmetrical and shape is similar.While the ingredients particles shape of machanical mixtures is distinct, the particles contact area is limited and some sensitive explosive particles are bared and expose to external action, so its impact sensitivity is higher than that of composite.
引文
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