CN102091569B - 人造金刚石及其制备方法 - Google Patents
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Abstract
本发明公开了一种人造金刚石及其制备方法，将粘结剂溶解于石油醚或丙酮溶剂中形成溶液；将炸药粉、金属粉、石墨干混，并将混好的混合物入到上步的溶液中；将该溶液搅拌，并加热挥发溶剂，当物料出现拉丝现象时停止搅拌；将物料造粒、烘干，抛光处理得到颗粒；将颗粒压制成药柱，并在密闭容器中爆炸合成金刚石。本发明药剂压药密度大于1.7g/cm3；金刚石得率高，每百克药剂可得9克金刚石；产品颗粒粒径分布在200-12000nm，颗粒的中位径1.95μm；产品颗粒外形为不规则的锯齿外形；产品的纯度达99％。
Description
技术领域
本发明属于爆炸法合成硬质材料的药剂和装配技术，特别是一种人造金刚石及其制备方法。
背景技术
爆炸法，包括冲击波法、爆轰波法，是利用炸药爆炸瞬态高温高压环境使一定方式组装的石墨发生相变转化成金刚石，或使用负氧平衡炸药，在爆炸条件下产生的游离碳经过聚结、相变和晶化形成金刚石。经爆炸获得的产品是金刚石和大量杂质形成的混合物，再经过化学提纯过程最后得到比较纯净的金刚石产品。
中国专利CN01114454.8和CN02114842.2是利用炸药驱动飞片打击石墨，靠冲击所产生的高温高压，使石墨转化为金刚石，该技术的原材料比较复杂，不仅要成型药柱，还需要成型石墨和金属飞板；该技术合成的金刚石回收复杂；其所得的金刚石粒径在一微米以下，得率小于3％。
中国专利CN101112678A、是利用负氧平衡炸药中的碳在炸药爆轰的热力学条件下发生聚结和相变生成纳米或微米尺寸的金刚石，粒度分布在1-6000内米区间，颗粒外形呈不规则锯齿形，容易团聚，所用药剂为梯恩梯(TNT)、黑索金(RDX)与奥克托金(HMX)与外加碳源的混合物。其金刚石的得率只有5％。
发明内容
本发明的目的在于提供一种人造金刚石及其制备方法，所制备的金刚石的得率大于9％，其颗粒外形为锋利的锯齿形，用于抛光材料时能显著地提高抛光效果。
实现本发明目的的技术解决方案为：一种人造金刚石，由以下组分混合组成，并通过爆炸制备而得：组分按重量百分比计算：
炸药粉 50％～76％
金属粉 10％～30％
石墨 10％～20％
粘结剂 1％～4％
一种人造金刚石的制备方法，步骤如下：
(a)将粘结剂溶解于石油醚或丙酮溶剂中形成溶液；
(b)将炸药粉、金属粉、石墨干混，并将混好的混合物入到步骤(a)的溶液中；
(c)将该溶液搅拌，并加热挥发溶剂，当物料出现拉丝现象时停止搅拌；
(d)将物料造粒、烘干，抛光处理得到颗粒；
(e)将颗粒压制成药柱，并在密闭容器中爆炸合成金刚石。
本发明与现有技术相比，其显著优点：药剂压药密度大于1.7g/cm3；金刚石得率高，每百克药剂可得9克金刚石；产品颗粒粒径分布在200-12000nm，颗粒的中位径1.95μm；产品颗粒外形为不规则的锯齿外形；产品的纯度达99％。
下面结合附图对本发明作进一步详细描述。
附图说明
图1是药剂的扫描照片。
图2是装配图。
图3是金刚石的电镜照片。
图4是合成的金刚石的衍射图谱。
具体实施方式
本发明人造金刚石，由以下组分混合组成，并通过下述爆炸方法制备而得：组分按重量百分比计算：
炸药粉 50％～76％
金属粉 10％～30％
石墨 10％～20％
粘结剂 1％～4％
本发明人造金刚石的制备方法，步骤如下：
(a)将粘结剂溶解于石油醚或丙酮溶剂中形成溶液。其中粘结剂为地蜡、石蜡、虫胶、硝化棉或热塑型高分子材料，或者它们的混合物。热塑型高分子材料为顺丁橡胶、乙丙橡胶或天然橡胶。
(b)将炸药粉、金属粉、石墨干混，并将混好的混合物入到步骤(a)的溶液中。其中炸药粉为RDX、HMX、PETN中的一种，或者它们的混合物，其粒径小于10微米。金属粉为1～30μm粒径的球状Al、Mg或Al-Mg粉，或者过300目以上的片状Al粉，或者它们的混合物。石墨的平均粒径1～30微米。
(c)将该溶液搅拌，并加热挥发溶剂，当物料出现拉丝现象时停止搅拌；
(d)将物料造粒、烘干，抛光处理得到颗粒；
(e)将颗粒压制成药柱，并在密闭容器中爆炸合成金刚石。
上述步骤(a)、(c)在80℃以下操作。
本发明的药剂可以采用常规压药成型所要求的药柱尺寸，其压药后的药柱密度在1.7～1.85g/cm3，压制的药柱装填厚度不小于4mm的塑料管或厚度不小于0.5mm的钢管中，装填好的药剂在爆炸容器中起爆。
实施例
1、药剂制备
按照质量百分比计算炸药粉、金属粉、石墨、粘结剂。
(1)干料准备
将配方中各种合格的粉状原料按配比和公差进行称量，然后在20～40目筛上进行筛选，在干混设备中混合30min，备用。
(2)粘结剂准备
原料经碾压成薄片，大块蜡破碎成小块，分别放入瓶中备用。
(3)粘结剂配制
先将18～25％炸药重量的溶剂放入搅拌罐中，然后将粘结料加入搅拌罐中搅拌，在溶化的前1～2小时将小蜡块放入熔蜡槽中通入热水加热，待粘结料溶化后将熔化的蜡放入搅拌罐中，搅拌均匀后备用。搅拌中加热介质为热水，一般比所用溶剂沸点低10～20℃。本实施例中采用的溶剂为石油醚，夹套温度在55～60℃，溶解出料时计算溶液浓度。
(4)工艺设置参数
按照捏合锅的使用容积的70％进行制备药剂；桨叶与锅壁间隙是4mm，桨叶与桨叶间隙是4mm，粘结剂的浓度15ml溶剂∶1g粘结料，设备桨叶转速控制在30转/min，实验锅体内温度分别控制在55℃。
(5)捏合
先将配制好的粘结剂按一定比例加入到捏合锅中，再将过筛后的炸药粉、金属粉、石墨或预混好的炸药粉、金属粉和石墨混合物依次加入到捏合锅中，捏合40分钟后，当物料出现拉丝状并自动散开时，捏合结束。捏合后的药剂形态如图1所示。
(6)取出药剂，进行造粒、烘干，抛光处理。
(7)药剂性能分析方法
采用高效液相色谱法分析炸药组分含量，红外光谱法分析粘结剂，按GB/T 3521-2008《石墨化学分析方法》规定方法分析石墨组分含量，按GB/T 3169.6-1982《铝粉化学分析方法》规定的气体容量法分析金属粉含量。扫描电镜观测捏合后组分分散状态。所用液相色谱仪，型号：HP1100，(惠普公司产品)；红外光谱仪，型号：MB154FTIR，(波曼公司产品)，扫描电镜，型号：EDAX200
(8)压药
采用压装形式将药剂压成密度为1.75g/cm3的药柱，压制的药柱装填厚度不小于4mm的塑料管。
2、爆炸合成
按照图2进行装配。先将8号电工业雷管1，压装传爆药柱2，原料药柱3，塑料管壳4组装起来，放入水介质中。然后置于爆炸罐中引爆。
3、预处理爆轰灰
将混有含有杂质的爆轰灰爆炸罐中取出，经洗涤、过滤除去机械杂质，在120℃温度下烘干，即可得到爆轰灰。
4、提纯、洗涤烘干
配料
物料及规格：爆轰灰，含水量≤0.5％；浓硝酸、浓硫酸——浓度98％；
配比：爆轰灰(g)∶浓硝酸(ml)＝1∶4
将爆轰灰按配比称量，先在浓硫酸中浸泡3小时后，投入反应斧中，搅拌加热，在180℃--200℃温度下反应6小时。将产物用去离子水洗涤至中性，放入烘箱中在100℃温度下烘干。
5、检测
检测仪器：德国D8ADVANCE X射线衍射仪，美国场发射扫描电镜，BT-9300H激光粒度分布仪。
取干粉产品约0.1克用场发射扫描电镜观察外貌，图3是合成的微米聚晶金刚石的电镜照片，从图3可见其外形呈锯齿外形。
取干粉产品约0.4克用D8 ADVANCE型X射线衍射仪进行检测，衍射角(2θ)范围10-120°。所述微米聚晶金刚石的衍射图谱特征为：特征峰在41°、43°、75°、91°四处，41°、43°处二峰大部重叠，41°峰以43°的肩峰的形式出现。(如图4)。
取干粉0.1克分散于200毫升去离子水中，用BT-9300H激光粒度分布仪测试其颗粒度，其粒度分布区间在20nm-12000nm范围内，中值粒径为d50＝3.5μm-6.5μm。
用X射线衍射(XRD)测试样品看有无杂峰，用等离子发射光谱(ICP)测试杂质含量。
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | |
| 聚晶金刚石粉(g) | 10.5 | 9.8 | 10.1 | 9.4 |
| 粒度分布(nm) | 200～12000 | 100～13000 | 100～12000 | 150～11000 |
| 颗粒的中位径(μm) | 1.95 | 2.01 | 1.83 | 1.91 |
通过以上测试，可证明产品为较纯净的聚晶金刚石，产品的纯度在99％以上。
Claims (2)
1.一种人造金刚石的制备方法，其特征在于步骤如下：
(a)将粘结剂溶解于石油醚或丙酮溶剂中形成溶液；
(b)将炸药粉、金属粉、石墨干混，并将混好的混合物入到步骤(a)的溶液中；
(c)将该溶液搅拌，并加热挥发溶剂，当物料出现拉丝现象时停止搅拌；
(d)将物料造粒、烘干，抛光处理得到颗粒；
(e)将颗粒压制成药柱，并在密闭容器中爆炸合成金刚石；
组分按重量百分比计算：
炸药粉 50％～76％
金属粉 10％～30％
石墨 10％～20％
粘结剂 1％～4％
其中，金属粉为1～30μm粒径的球状Al、Mg或Al-Mg粉，或者过300目以上的片状Al粉，或者它们的混合物。
2.根据权利要求1所述的人造金刚石的制备方法，其特征在于步骤(a)、(c)在80℃以下操作。
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| CN1385365A (zh) * | 2001-05-10 | 2002-12-18 | 浣石 | 用炸药爆轰合成纳米金刚石的方法 |
| CN101112678A (zh) * | 2006-07-24 | 2008-01-30 | 北京理工大学 | 宽颗粒度分布的多晶金刚石微粒的制备方法 |
| CN101906004A (zh) * | 2010-07-09 | 2010-12-08 | 北京理工大学 | 控制爆源体积能量密度的炸药、震源及其制造工艺 |
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