CN109668816B - 一种测定微纳米炸药晶体粉末比表面积的方法 - Google Patents
一种测定微纳米炸药晶体粉末比表面积的方法 Download PDFInfo
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Abstract
本发明公开了一种测定微纳米炸药晶体粉末比表面积的方法。该方法包括如下步骤:首先将待测微纳米炸药晶体粉末装入石英样品盒,然后做小角散射测试,并对小角散射实验数据进行处理获得绝对强度散射曲线,然后通过Porod拟合和计算获得微纳米炸药晶体粉末的比表面积。本发明的测定微纳米炸药晶体粉末比表面积的方法是一种快速无损测定微纳米炸药晶体粉末比表面积的方法,具有快速、安全、绿色环保的优点。本发明测定的微纳米炸药晶体粉末比表面积是表征微纳米炸药晶体粉末微观形态特征的重要参数,可用于进一步深入探索炸药晶体粉末形态特征对其宏观感度、力学性能、爆燃特性等的影响。
Description
技术领域
本发明属于核技术应用领域,具体涉及一种测定微纳米炸药晶体粉末比表面积的方法。
背景技术
炸药晶体粉末是含能材料(推进剂、焰火剂、混合炸药和聚合物粘结炸药等)爆炸做功过程的主要能量来源,广泛应用于军事和国民经济的各领域。特别是微纳米炸药晶体粉末作为一种新型功能材料,在应用中具有显著优势:(1)感度可选择;(2)能量释放速率更快;(3)临界直径更小;(4)燃烧更快更充分。微纳米炸药晶体粉末一般通过溶液重结晶生长出来或者机械球磨制备,微纳米炸药晶体粉末是粒径几十纳米到几百微米粒径的颗粒物,这就导致成型的微纳米炸药晶体粉末不可避免带有许多表面开孔和裂纹缺陷,开孔和裂纹还可能会在后续加工、使用等过程的温度和力学载荷作用下发生演化。微纳米炸药晶体粉末中的开孔缺陷一方面会显著影响炸药晶体本身的感度和力学性能,另一方面则会通过影响炸药的爆燃特性进而影响做功过程。对微纳米炸药晶体粉末表面特征的准确表征是深入研究其对感度、力学性能、爆燃特性等宏观性能影响关系的重要基础,是表征微纳米炸药晶体粉末微观形态特征的一个重要方面。
目前,对微纳米炸药晶体粉末比表面积的常见测定方法有BET法、压汞法等。BET法需要对样品进行高温脱气等预处理,需要的样品量较大,并且测量时间较久,微纳米炸药晶体粉末易团聚给测试带来误差(预处理干燥过程中形成晶桥,使得部分微纳米炸药晶体粉末结块成粒径较大的团聚体,表面积减少),并且高温预处理微纳米炸药晶体粉末还具有一定的危险性。压汞法需要的样品量也较大,该方法更适用于大孔材料的测定,由于在高压条件下许多孔洞发生变形或塌陷,因此对于纳米级孔洞的测量准确度不高,测试完成后样品无法继续使用,而且使用后的汞为不易处理的有毒重金属,容易带来环境污染。
综上,现有的微纳米炸药晶体粉末常规比表面积测定方法仍不能完全满足实践中对无损、快速、安全、绿色环保等需求,需要发展新的测试方法。
发明内容
本发明所要解决的技术问题是提供一种测定微纳米炸药晶体粉末比表面积的方法。
本发明的测定微纳米炸药晶体粉末比表面积的方法包括如下步骤:
a.称取待测微纳米炸药晶体粉末并记录重量;
b.将称取的待测微纳米炸药晶体粉末置于光程为0.5mm~5mm的小角散射专用样品容器中,并轻轻震荡直至装填均匀,记录装填高度,得到待测微纳米炸药晶体样品;
c.对待测微纳米炸药晶体样品进行小角散射测试,获得待测微纳米炸药晶体样品的小角散射实验数据;
d.对小角散射实验数据依次进行扣背底修正和绝对强度修正,获得绝对强度散射曲线;
e.对绝对强度散射曲线做Porod拟合,计算获得微纳米炸药晶体粉末比表面积的绝对数值。
所述的装填均匀是指待测炸药晶体粉末分散均匀,无分层断层。
所述的小角散射为中子小角散射、X射线小角散射、超小角中子散射、超小角X射线散射中的一种或两种及以上。
本发明的测定微纳米炸药晶体粉末比表面积的方法涉及到操作微纳米炸药晶体粉末,是一种含能材料,故所有实验过程一定要遵守含能材料相关的安全操作规程和注意事项,相关操作都由具备资质的人员在特定的场所完成。
本发明的测定微纳米炸药晶体粉末比表面积的方法,具有如下优点:
1.待测微纳米炸药晶体粉末样品制备过程简单,整个测试过程对待测炸药晶体样品无损伤,不带来任何宏观和微观的结构破坏或改变,测试完后待测微纳米炸药晶体粉末可直接回收再使用。
2.能够快速给出待测微纳米炸药晶体粉末的比表面积信息,还可以通过进一步分析绝对强度散射曲线获得待测微纳米炸药晶体粉末的表面分型特征。
3.待测微纳米炸药晶体粉末样品的测试区域为厘米级范围,能够给出待测微纳米炸药晶体粉末的体相统计平均信息。
4.获得的微纳米炸药晶体粉末的比表面积绝对数值是表征炸药晶体微观形态特征的重要参数,可用于进一步深入探索微纳米炸药晶体粉末表面形态特征对其宏观感度、力学性能、爆燃特性的影响关系。
本发明的测定微纳米炸药晶体粉末比表面积的方法是一种快速无损测定微纳米炸药晶体粉末比表面积的方法,具有快速、安全、绿色环保的优点。
附图说明
图1为实施例1中的微纳米炸药晶体粉末样品的绝对强度散射曲线;
图2 为实施例3中的微纳米炸药晶体粉末样品的绝对强度散射曲线;
图3 为实施例6中的微纳米炸药晶体粉末样品的绝对强度散射曲线;
图4 为实施例7中的微纳米炸药晶体粉末样品的绝对强度散射曲线。
具体实施方式
下面结合具体实例对本发明作进一步说明,但本发明并不限于以下实例。下述实例中如无特别说明,所述方法均为常规方法。下述实例中所用的待测微纳米炸药晶体粉末均可通过商业途径购买或由特定生产单位定制合成获得。
实施例1
本实施例的待测微纳米炸药晶体粉末为第一种TATB炸药晶体粉末,命名为μTATB-1,小角散射专用样品容器为光程为1mm的石英比色皿,小角散射测试仪器为中国绵阳研究堆的狻猊中子小角散射谱仪,具体步骤如下:
a.称取待测微纳米炸药晶体粉末并记录重量;
b.将称取的待测微纳米炸药晶体粉末置于光程为1mm的小角散射专用样品容器中,并轻轻震荡直至装填均匀,记录装填高度,得到待测微纳米炸药晶体样品;
c.对待测微纳米炸药晶体样品进行小角散射测试,获得待测微纳米炸药晶体样品的小角散射实验数据;
d.对小角散射实验数据依次进行扣背底修正和绝对强度修正,获得绝对强度散射曲线;
e.对绝对强度散射曲线做Porod拟合,计算获得微纳米炸药晶体粉末比表面积的绝对数值。
Porod拟合为,在Porod区(大Q区)待测炸药晶体粉末的绝对散射强度与散射矢量的负四次方成正比,其中比例系数正比于待测炸药晶体粉末的比表面积,具体如公式所示
本实施例的装填均匀是指待测炸药晶体粉末分散均匀,无分层断层。
本实施例的小角散射为X射线小角散射、超小角中子散射、超小角X射线散射中的一种,或中子小角散射、X射线小角散射、超小角中子散射、超小角X射线散射中两种及以上。
本实施例获得的绝对强度散射曲线,如图1所示,可知μTATB-1样品的散射强度曲线在散射矢量为0.06nm-1~0.9nm-1区间内均满足Porod定理,说明炸药晶体表面为光滑界面,不存在表面分形特征。本实施例获得的待测炸药晶体粉末的比表面积的绝对数值见表1。
实施例2
本实施例与实施例1的实施方式基本相同,主要区别见表1。本实施例获得的待测微纳米炸药晶体粉末的比表面积的绝对数值见表1。
实施例3
本实施例与实施例1的实施方式基本相同,主要区别见表1。本实施例获得的绝对强度散射曲线,如图2所示,可知nTATB-1样品的散射强度曲线在散射矢量为0.06nm-1~1nm-1区间内均满足Porod定理,说明炸药晶体表面为光滑界面,不存在表面分形特征。本实施例获得的待测微纳米炸药晶体粉末的比表面积的绝对数值见表1。
实施例4
本实施例与实施例1的实施方式基本相同,主要区别见表1。本实施例获得的待测微纳米炸药晶体粉末的比表面积的绝对数值见表1。
实施例5
本实施例与实施例1的实施方式基本相同,主要区别见表1。本实施例获得的待测微纳米炸药晶体粉末的比表面积的绝对数值见表1。
实施例6
本实施例与实施例1的实施方式基本相同,主要区别见表1。本实施例获得的绝对强度散射曲线,如图3所示,可知RDX样品的散射强度曲线在散射矢量为0.06nm-1~0.38nm-1区间内均满足Porod定理,说明炸药晶体表面为光滑界面,不存在表面分形特征。本实施例获得的待测微纳米炸药晶体粉末的比表面积的绝对数值见表1。
实施例7
本实施例与实施例1的实施方式基本相同,主要区别见表1。本实施例获得的绝对强度散射曲线,如图4所示,可知LLM-105样品的散射强度曲线在散射矢量为0.06nm-1~0.35nm-1区间内均满足Porod定理,说明炸药晶体表面为光滑界面,不存在表面分形特征。本实施例获得的待测微纳米炸药晶体粉末的比表面积的绝对数值见表1。
表1为各实施例的测试条件和porod拟合后获得的待测微纳米炸药晶体粉末的比表面积的绝对数值表,可知两种μTATB具有相同数量级的比表面积,三种nTATB具有相同数量级的比表面积,其中LLM-105样品具有最小的比表面积0.0773 m2/g,nTATB-2样品具有最大的比表面积10.2 m2/g。
Claims (3)
1.一种测定微纳米炸药晶体粉末比表面积的方法,其特征在于,所述的方法包括如下步骤:
a.称取待测微纳米炸药晶体粉末并记录重量;
b.将称取的待测微纳米炸药晶体粉末置于光程为0.5mm~5mm的小角散射专用样品容器中,并轻轻震荡直至装填均匀,记录装填高度,得到待测微纳米炸药晶体样品;
c.对待测微纳米炸药晶体样品进行小角散射测试,获得待测微纳米炸药晶体样品的小角散射实验数据;
d.对小角散射实验数据依次进行扣背底修正和绝对强度修正,获得绝对强度散射曲线;
e.对绝对强度散射曲线做Porod拟合,计算获得微纳米炸药晶体粉末比表面积的绝对数值。
2.根据权利要求1所述的测定微纳米炸药晶体粉末比表面积的方法,其特征在于:所述的装填均匀是指待测炸药晶体粉末分散均匀,无分层断层。
3.根据权利要求1所述的测定微纳米炸药晶体粉末比表面积的方法,其特征在于:所述的小角散射为中子小角散射、X射线小角散射、超小角中子散射、超小角X射线散射中的一种或两种及以上。
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