本發明(ming)屬于導(dao)電材料的技術領域(yu)，具體涉及一種鍍銀納米石墨微片導(dao)電填料的制備(bei)方法。

背景技術：

導(dao)電(dian)(dian)膠是(shi)指具有一定導(dao)電(dian)(dian)性(xing)能的特殊(shu)膠黏劑(ji)，主要是(shi)通過在有機聚合物基體中(zhong)加(jia)入(ru)固(gu)(gu)化(hua)劑(ji)、導(dao)電(dian)(dian)填料以及其他(ta)添(tian)加(jia)劑(ji)等(deng)固(gu)(gu)化(hua)而得，且具有與(yu)金屬相近的導(dao)電(dian)(dian)性(xing)能。按(an)導(dao)電(dian)(dian)膠中(zhong)導(dao)電(dian)(dian)粒子的種類不(bu)同，可分(fen)為金、銀、銅(tong)和(he)碳系導(dao)電(dian)(dian)膠。

石(shi)墨(mo)(mo)不僅具有(you)(you)天然(ran)(ran)的導(dao)(dao)電性，而且(qie)兼有(you)(you)性能(neng)穩定、良(liang)(liang)好的耐酸(suan)耐堿(jian)性和(he)分散性等優(you)點，是(shi)(shi)制備導(dao)(dao)電膠(jiao)的優(you)良(liang)(liang)材料(liao)。石(shi)墨(mo)(mo)資源豐富(fu)、成本低廉，相(xiang)對(dui)(dui)于金屬(shu)導(dao)(dao)電填(tian)料(liao)而言，石(shi)墨(mo)(mo)具有(you)(you)絕對(dui)(dui)的價格優(you)勢，所以，石(shi)墨(mo)(mo)導(dao)(dao)電膠(jiao)具有(you)(you)良(liang)(liang)好的應用前景(jing)。但是(shi)(shi)，天然(ran)(ran)石(shi)墨(mo)(mo)通常(chang)以微米級鱗(lin)片(pian)粉(fen)末形式存(cun)在，直接(jie)把它作(zuo)為導(dao)(dao)電填(tian)料(liao)，填(tian)充量較大，制品的密(mi)度高，力學性能(neng)差，因此，在許多導(dao)(dao)電膠(jiao)制品方面的應用受到了限制。

納(na)米(mi)材(cai)料處(chu)于介觀尺(chi)度(du)、比表面積(ji)大。由此而帶來(lai)的量(liang)子限域(yu)效(xiao)(xiao)果(guo)、表面效(xiao)(xiao)應(ying)、小尺(chi)寸(cun)效(xiao)(xiao)應(ying)、宏觀量(liang)子隧(sui)道效(xiao)(xiao)應(ying)使(shi)其具(ju)備了獨特(te)的理化性質(zhi)。利(li)用納(na)米(mi)材(cai)料的特(te)點(dian)來(lai)改善導(dao)電(dian)膠(jiao)(jiao)的各(ge)項性能(neng)，改性傳統鱗片(pian)石墨成納(na)米(mi)尺(chi)度(du)的導(dao)電(dian)填(tian)料被引入到導(dao)電(dian)膠(jiao)(jiao)復(fu)合材(cai)料體系當中，相關的研究逐漸成為(wei)了導(dao)電(dian)膠(jiao)(jiao)領域(yu)的新型熱點(dian)之(zhi)一。

技術實現要素：

本發明所(suo)要解決的技術(shu)問題(ti)是(shi)：針對傳(chuan)統石(shi)(shi)墨(mo)導電填料以天然鱗片石(shi)(shi)墨(mo)直(zhi)接添加(jia)，填充量較大，導致(zhi)制品密度高，力學性(xing)能下(xia)降的問題(ti)，提供了一種鍍銀納(na)米石(shi)(shi)墨(mo)微片導電填料的制備方法。

為解決上述技(ji)術問(wen)題，本發明(ming)采(cai)用(yong)如下所述的技(ji)術方案：

（1）將鱗片石(shi)(shi)墨氧化后膨脹后制得膨脹石(shi)(shi)墨，將膨脹石(shi)(shi)墨與石(shi)(shi)油醚保壓(ya)后瞬間(jian)泄壓(ya)，再經冷卻、過濾和(he)干(gan)燥后制得納(na)米石(shi)(shi)墨微片；

（2）將銀(yin)氨溶液與納米石(shi)(shi)墨微(wei)片混合，以乙醛為還(huan)原(yuan)劑，經反應后(hou)過濾、洗滌和干燥，即(ji)得鍍銀(yin)納米石(shi)(shi)墨微(wei)片導(dao)電填料。

本發明與(yu)其他方法相比，有益技術效(xiao)果是：

（1）本發明使(shi)鱗片石墨(mo)(mo)(mo)膨脹(zhang)后，于高壓(ya)條件(jian)下，使(shi)石油醚蒸氣(qi)(qi)進(jin)入膨脹(zhang)石墨(mo)(mo)(mo)孔隙中(zhong)(zhong)，并在孔隙中(zhong)(zhong)冷凝成(cheng)液態(tai)石油醚，再(zai)經瞬(shun)間(jian)(jian)泄壓(ya)，使(shi)孔隙中(zhong)(zhong)的液態(tai)石油醚瞬(shun)間(jian)(jian)轉化(hua)為石油醚蒸氣(qi)(qi)，并使(shi)膨脹(zhang)石墨(mo)(mo)(mo)碎裂，形成(cheng)納(na)米石墨(mo)(mo)(mo)微片，再(zai)以乙醛為還原劑，在石墨(mo)(mo)(mo)微片表面還原沉積產生(sheng)銀，進(jin)一(yi)步增強(qiang)產品的導電性(xing)能；

（2）本發明所得產品作為導電填料應用于導電膠中，因導電性能的提高，填充量減少，制品的力學性能得以提高，所制得的導電膠體積電阻率為10^-5～10^-3ω·cm，抗剪切(qie)強度(du)為(wei)180～200mpa，使用(yong)壽(shou)命較常規導電膠延長2～4年。

具體實施方式

本發明所(suo)需的原(yuan)料有：鱗(lin)片石墨(mo)、98%硫酸(suan)、65%硝(xiao)酸(suan)、高錳酸(suan)鉀、氮氣、膨脹石墨(mo)、石油(you)醚、2%硝(xiao)酸(suan)銀(yin)溶液(ye)、2～4%氨水。

稱取(qu)40～60kg鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)，倒(dao)入(ru)(ru)托盤中，再(zai)(zai)(zai)(zai)(zai)將(jiang)托盤轉(zhuan)入(ru)(ru)真(zhen)空(kong)干(gan)燥箱中，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)80～90℃條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)，干(gan)燥16～24h，得(de)(de)干(gan)燥鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)，再(zai)(zai)(zai)(zai)(zai)于(yu)(yu)(yu)聚四氟乙(yi)烯內(nei)襯反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)中，依次加入(ru)(ru)20～30l質(zhi)(zhi)量(liang)(liang)分(fen)數(shu)為(wei)(wei)(wei)(wei)98%硫酸(suan)(suan)(suan)(suan)，10～12l質(zhi)(zhi)量(liang)(liang)分(fen)數(shu)為(wei)(wei)(wei)(wei)65%硝(xiao)酸(suan)(suan)(suan)(suan)，1～3kg高錳酸(suan)(suan)(suan)(suan)鉀(jia)，35～40kg所得(de)(de)干(gan)燥鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)55～65℃，轉(zhuan)速(su)(su)為(wei)(wei)(wei)(wei)500～600r/min條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)，恒(heng)溫(wen)(wen)攪(jiao)拌(ban)反(fan)(fan)(fan)應(ying)(ying)(ying)12～18h，利(li)用(yong)高錳酸(suan)(suan)(suan)(suan)鉀(jia)在酸(suan)(suan)(suan)(suan)性條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)，氧(yang)化(hua)(hua)(hua)(hua)鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)，待(dai)(dai)(dai)(dai)反(fan)(fan)(fan)應(ying)(ying)(ying)結束，將(jiang)聚四氟乙(yi)烯內(nei)襯反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)中物(wu)料(liao)過(guo)濾(lv)，得(de)(de)氧(yang)化(hua)(hua)(hua)(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)濾(lv)餅(bing)，用(yong)去離(li)子水洗滌氧(yang)化(hua)(hua)(hua)(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)濾(lv)餅(bing)直至洗滌液(ye)呈中性，再(zai)(zai)(zai)(zai)(zai)將(jiang)洗滌后(hou)的(de)(de)(de)氧(yang)化(hua)(hua)(hua)(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)濾(lv)餅(bing)轉(zhuan)入(ru)(ru)烘(hong)箱中，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)105～110℃條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)干(gan)燥至恒(heng)重后(hou)轉(zhuan)入(ru)(ru)馬弗爐，以(yi)(yi)10～15ml/min速(su)(su)率(lv)向(xiang)爐內(nei)通入(ru)(ru)氮氣，在氮氣保護狀(zhuang)態(tai)下(xia)，以(yi)(yi)10～15℃/min速(su)(su)率(lv)持續升(sheng)溫(wen)(wen)至1000～1100℃，保溫(wen)(wen)20～30s，經(jing)高溫(wen)(wen)煅燒(shao)(shao)(shao)使(shi)(shi)(shi)氧(yang)化(hua)(hua)(hua)(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)膨(peng)脹(zhang)(zhang)，隨爐冷卻至室溫(wen)(wen)，出(chu)料(liao)，得(de)(de)膨(peng)脹(zhang)(zhang)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)，稱取(qu)25～30kg膨(peng)脹(zhang)(zhang)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)，倒(dao)入(ru)(ru)盛有50～80l石(shi)(shi)(shi)(shi)(shi)油醚(mi)(mi)的(de)(de)(de)高壓反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)中，以(yi)(yi)600～800r/min轉(zhuan)速(su)(su)攪(jiao)拌(ban)混合20～40min后(hou)，開(kai)啟(qi)反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)加熱器，使(shi)(shi)(shi)反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)內(nei)壓力(li)達1.6～1.8mpa，保壓30～45s，再(zai)(zai)(zai)(zai)(zai)打開(kai)反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)底(di)部(bu)出(chu)料(liao)閥(fa)門，使(shi)(shi)(shi)反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)中物(wu)料(liao)噴射進入(ru)(ru)接收釜(fu)(fu)中，待(dai)(dai)(dai)(dai)接收釜(fu)(fu)中物(wu)料(liao)自然冷卻至室溫(wen)(wen)，將(jiang)接收釜(fu)(fu)中物(wu)料(liao)過(guo)濾(lv)，得(de)(de)含納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)的(de)(de)(de)濾(lv)渣(zha)，并(bing)將(jiang)含納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)的(de)(de)(de)濾(lv)渣(zha)置于(yu)(yu)(yu)真(zhen)空(kong)干(gan)燥箱中，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)105～110℃條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)干(gan)燥至恒(heng)重，利(li)用(yong)在反(fan)(fan)(fan)應(ying)(ying)(ying)釜(fu)(fu)高壓條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)，使(shi)(shi)(shi)石(shi)(shi)(shi)(shi)(shi)油醚(mi)(mi)蒸氣進入(ru)(ru)膨(peng)脹(zhang)(zhang)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)孔(kong)隙中，并(bing)在孔(kong)隙中冷凝成液(ye)態(tai)石(shi)(shi)(shi)(shi)(shi)油醚(mi)(mi)，再(zai)(zai)(zai)(zai)(zai)經(jing)瞬間泄壓，使(shi)(shi)(shi)孔(kong)隙中的(de)(de)(de)液(ye)態(tai)石(shi)(shi)(shi)(shi)(shi)油醚(mi)(mi)瞬間轉(zhuan)化(hua)(hua)(hua)(hua)為(wei)(wei)(wei)(wei)石(shi)(shi)(shi)(shi)(shi)油醚(mi)(mi)蒸氣，并(bing)使(shi)(shi)(shi)膨(peng)脹(zhang)(zhang)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)碎(sui)裂，得(de)(de)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)，量(liang)(liang)取(qu)300～500ml質(zhi)(zhi)量(liang)(liang)分(fen)數(shu)為(wei)(wei)(wei)(wei)2%硝(xiao)酸(suan)(suan)(suan)(suan)銀(yin)(yin)(yin)溶液(ye)，倒(dao)入(ru)(ru)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)中，再(zai)(zai)(zai)(zai)(zai)將(jiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)移(yi)(yi)入(ru)(ru)數(shu)顯測(ce)速(su)(su)恒(heng)溫(wen)(wen)磁力(li)攪(jiao)拌(ban)器中，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)55～60℃，轉(zhuan)速(su)(su)為(wei)(wei)(wei)(wei)500～600r/min條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)，通過(guo)滴液(ye)漏斗(dou)向(xiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)中滴加質(zhi)(zhi)量(liang)(liang)分(fen)數(shu)為(wei)(wei)(wei)(wei)2～4%氨(an)水，待(dai)(dai)(dai)(dai)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)中產(chan)生沉淀(dian)后(hou)繼(ji)(ji)續滴加氨(an)水，直至產(chan)生的(de)(de)(de)沉淀(dian)完全溶解為(wei)(wei)(wei)(wei)止，形成銀(yin)(yin)(yin)氨(an)溶液(ye)，再(zai)(zai)(zai)(zai)(zai)向(xiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)中加入(ru)(ru)100～150g上述(shu)所得(de)(de)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)，繼(ji)(ji)續恒(heng)溫(wen)(wen)攪(jiao)拌(ban)混合45～60min，待(dai)(dai)(dai)(dai)恒(heng)溫(wen)(wen)攪(jiao)拌(ban)混合結束，通過(guo)滴液(ye)漏斗(dou)向(xiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)中加入(ru)(ru)10～20ml乙(yi)醛，利(li)用(yong)乙(yi)醛還原(yuan)銀(yin)(yin)(yin)氨(an)溶液(ye)，產(chan)生的(de)(de)(de)銀(yin)(yin)(yin)單質(zhi)(zhi)包裹于(yu)(yu)(yu)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)表面，再(zai)(zai)(zai)(zai)(zai)將(jiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)于(yu)(yu)(yu)超(chao)聲振蕩儀中，以(yi)(yi)40～45khz頻率(lv)超(chao)聲處理10～15s后(hou)，將(jiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)移(yi)(yi)入(ru)(ru)水浴鍋中，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)65～70℃條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)靜置15～20min，再(zai)(zai)(zai)(zai)(zai)將(jiang)三(san)(san)(san)口(kou)(kou)(kou)燒(shao)(shao)(shao)瓶(ping)中物(wu)料(liao)過(guo)濾(lv)，得(de)(de)鍍(du)銀(yin)(yin)(yin)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)濾(lv)餅(bing)，并(bing)用(yong)去離(li)子水洗滌鍍(du)銀(yin)(yin)(yin)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)濾(lv)餅(bing)3～5次，再(zai)(zai)(zai)(zai)(zai)將(jiang)鍍(du)銀(yin)(yin)(yin)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)濾(lv)餅(bing)轉(zhuan)入(ru)(ru)真(zhen)空(kong)干(gan)燥箱中，避免(mian)銀(yin)(yin)(yin)被氧(yang)化(hua)(hua)(hua)(hua)，于(yu)(yu)(yu)溫(wen)(wen)度(du)為(wei)(wei)(wei)(wei)105～110℃條(tiao)(tiao)(tiao)件(jian)(jian)(jian)下(xia)干(gan)燥至恒(heng)重，得(de)(de)鍍(du)銀(yin)(yin)(yin)納(na)米(mi)(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)導電填料(liao)。

實例1

稱取40kg鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，倒(dao)入(ru)(ru)(ru)托盤中(zhong)(zhong)(zhong)(zhong)(zhong)，再(zai)將(jiang)(jiang)托盤轉(zhuan)(zhuan)入(ru)(ru)(ru)真(zhen)(zhen)空干(gan)(gan)(gan)燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)80℃條件(jian)下，干(gan)(gan)(gan)燥(zao)(zao)16h，得干(gan)(gan)(gan)燥(zao)(zao)鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，再(zai)于(yu)(yu)聚四氟乙(yi)(yi)烯內襯反(fan)(fan)應(ying)釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)，依(yi)次(ci)加(jia)入(ru)(ru)(ru)20l質(zhi)(zhi)量(liang)分數為(wei)(wei)(wei)(wei)(wei)(wei)98%硫酸，10l質(zhi)(zhi)量(liang)分數為(wei)(wei)(wei)(wei)(wei)(wei)65%硝酸，1kg高錳(meng)酸鉀，35kg所得干(gan)(gan)(gan)燥(zao)(zao)鱗(lin)片(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)55℃，轉(zhuan)(zhuan)速為(wei)(wei)(wei)(wei)(wei)(wei)500r/min條件(jian)下，恒(heng)溫(wen)(wen)(wen)攪(jiao)拌反(fan)(fan)應(ying)12h，待反(fan)(fan)應(ying)結束，將(jiang)(jiang)聚四氟乙(yi)(yi)烯內襯反(fan)(fan)應(ying)釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物(wu)料(liao)(liao)(liao)過(guo)濾(lv)，得氧(yang)(yang)(yang)化(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)濾(lv)餅(bing)，用去離(li)子水(shui)洗滌氧(yang)(yang)(yang)化(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)濾(lv)餅(bing)直至洗滌液(ye)(ye)呈中(zhong)(zhong)(zhong)(zhong)(zhong)性，再(zai)將(jiang)(jiang)洗滌后(hou)(hou)的氧(yang)(yang)(yang)化(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)濾(lv)餅(bing)轉(zhuan)(zhuan)入(ru)(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)105℃條件(jian)下干(gan)(gan)(gan)燥(zao)(zao)至恒(heng)重(zhong)后(hou)(hou)轉(zhuan)(zhuan)入(ru)(ru)(ru)馬(ma)弗爐(lu)，以10ml/min速率向(xiang)爐(lu)內通(tong)入(ru)(ru)(ru)氮(dan)(dan)氣，在氮(dan)(dan)氣保護狀態下，以10℃/min速率持續(xu)升溫(wen)(wen)(wen)至1000℃，保溫(wen)(wen)(wen)20s，隨爐(lu)冷(leng)卻至室(shi)溫(wen)(wen)(wen)，出料(liao)(liao)(liao)，得膨脹石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，稱取25kg膨脹石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，倒(dao)入(ru)(ru)(ru)盛有50l石(shi)(shi)(shi)(shi)(shi)油醚(mi)的高壓反(fan)(fan)應(ying)釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)，以600r/min轉(zhuan)(zhuan)速攪(jiao)拌混(hun)合20min后(hou)(hou)，開啟反(fan)(fan)應(ying)釜(fu)(fu)加(jia)熱器，使反(fan)(fan)應(ying)釜(fu)(fu)內壓力達1.6mpa，保壓30s，再(zai)打開反(fan)(fan)應(ying)釜(fu)(fu)底部出料(liao)(liao)(liao)閥門，使反(fan)(fan)應(ying)釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物(wu)料(liao)(liao)(liao)噴射進入(ru)(ru)(ru)接(jie)收釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)，待接(jie)收釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物(wu)料(liao)(liao)(liao)自然(ran)冷(leng)卻至室(shi)溫(wen)(wen)(wen)，將(jiang)(jiang)接(jie)收釜(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物(wu)料(liao)(liao)(liao)過(guo)濾(lv)，得含納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)的濾(lv)渣，并(bing)將(jiang)(jiang)含納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)的濾(lv)渣置于(yu)(yu)真(zhen)(zhen)空干(gan)(gan)(gan)燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)105℃條件(jian)下干(gan)(gan)(gan)燥(zao)(zao)至恒(heng)重(zhong)，再(zai)經瞬間(jian)泄壓，使膨脹石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)碎裂，得納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)，量(liang)取300ml質(zhi)(zhi)量(liang)分數為(wei)(wei)(wei)(wei)(wei)(wei)2%硝酸銀(yin)溶(rong)液(ye)(ye)，倒(dao)入(ru)(ru)(ru)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)，再(zai)將(jiang)(jiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)移(yi)入(ru)(ru)(ru)數顯測速恒(heng)溫(wen)(wen)(wen)磁力攪(jiao)拌器中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)55℃，轉(zhuan)(zhuan)速為(wei)(wei)(wei)(wei)(wei)(wei)500r/min條件(jian)下，通(tong)過(guo)滴(di)液(ye)(ye)漏(lou)斗向(xiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)滴(di)加(jia)質(zhi)(zhi)量(liang)分數為(wei)(wei)(wei)(wei)(wei)(wei)2%氨(an)水(shui)，待三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)產生沉淀(dian)(dian)后(hou)(hou)繼續(xu)滴(di)加(jia)氨(an)水(shui)，直至產生的沉淀(dian)(dian)完全溶(rong)解為(wei)(wei)(wei)(wei)(wei)(wei)止(zhi)，形成(cheng)銀(yin)氨(an)溶(rong)液(ye)(ye)，再(zai)向(xiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)加(jia)入(ru)(ru)(ru)100g上述所得納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)，繼續(xu)恒(heng)溫(wen)(wen)(wen)攪(jiao)拌混(hun)合45min，待恒(heng)溫(wen)(wen)(wen)攪(jiao)拌混(hun)合結束，通(tong)過(guo)滴(di)液(ye)(ye)漏(lou)斗向(xiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)加(jia)入(ru)(ru)(ru)10ml乙(yi)(yi)醛，利用乙(yi)(yi)醛還原銀(yin)氨(an)溶(rong)液(ye)(ye)，產生的銀(yin)單(dan)質(zhi)(zhi)包裹(guo)于(yu)(yu)納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)表面，再(zai)將(jiang)(jiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)于(yu)(yu)超(chao)(chao)聲振蕩儀中(zhong)(zhong)(zhong)(zhong)(zhong)，以40khz頻(pin)率超(chao)(chao)聲處理10s后(hou)(hou)，將(jiang)(jiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)移(yi)入(ru)(ru)(ru)水(shui)浴鍋中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)65℃條件(jian)下靜置15min，再(zai)將(jiang)(jiang)三(san)(san)口(kou)(kou)燒(shao)(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)物(wu)料(liao)(liao)(liao)過(guo)濾(lv)，得鍍銀(yin)納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)濾(lv)餅(bing)，并(bing)用去離(li)子水(shui)洗滌鍍銀(yin)納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)濾(lv)餅(bing)3次(ci)，再(zai)將(jiang)(jiang)鍍銀(yin)納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)濾(lv)餅(bing)轉(zhuan)(zhuan)入(ru)(ru)(ru)真(zhen)(zhen)空干(gan)(gan)(gan)燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)度(du)(du)為(wei)(wei)(wei)(wei)(wei)(wei)105℃條件(jian)下干(gan)(gan)(gan)燥(zao)(zao)至恒(heng)重(zhong)，得鍍銀(yin)納(na)(na)米(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)(wei)(wei)片(pian)導電填料(liao)(liao)(liao)。

實例2

稱取60kg鱗(lin)片(pian)(pian)(pian)(pian)(pian)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)，倒(dao)(dao)入(ru)(ru)(ru)托(tuo)(tuo)盤(pan)中(zhong)(zhong)(zhong)，再(zai)(zai)將(jiang)(jiang)(jiang)托(tuo)(tuo)盤(pan)轉(zhuan)(zhuan)(zhuan)入(ru)(ru)(ru)真空干燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)90℃條(tiao)件(jian)下，干燥(zao)(zao)24h，得(de)(de)(de)(de)干燥(zao)(zao)鱗(lin)片(pian)(pian)(pian)(pian)(pian)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)，再(zai)(zai)于(yu)(yu)聚四(si)氟乙烯內(nei)襯反(fan)(fan)(fan)應(ying)(ying)釜中(zhong)(zhong)(zhong)，依次加(jia)(jia)入(ru)(ru)(ru)30l質量分(fen)數(shu)(shu)(shu)為(wei)(wei)(wei)98%硫酸，12l質量分(fen)數(shu)(shu)(shu)為(wei)(wei)(wei)65%硝酸，3kg高錳酸鉀，40kg所得(de)(de)(de)(de)干燥(zao)(zao)鱗(lin)片(pian)(pian)(pian)(pian)(pian)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)65℃，轉(zhuan)(zhuan)(zhuan)速為(wei)(wei)(wei)600r/min條(tiao)件(jian)下，恒溫(wen)(wen)(wen)(wen)攪拌(ban)(ban)(ban)反(fan)(fan)(fan)應(ying)(ying)18h，待反(fan)(fan)(fan)應(ying)(ying)結束，將(jiang)(jiang)(jiang)聚四(si)氟乙烯內(nei)襯反(fan)(fan)(fan)應(ying)(ying)釜中(zhong)(zhong)(zhong)物(wu)料(liao)(liao)過(guo)(guo)濾(lv)(lv)(lv)，得(de)(de)(de)(de)氧化(hua)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)濾(lv)(lv)(lv)餅(bing)，用去離子水(shui)(shui)洗滌氧化(hua)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)濾(lv)(lv)(lv)餅(bing)直(zhi)至(zhi)(zhi)(zhi)洗滌液(ye)(ye)(ye)(ye)呈(cheng)中(zhong)(zhong)(zhong)性，再(zai)(zai)將(jiang)(jiang)(jiang)洗滌后(hou)(hou)的(de)(de)(de)氧化(hua)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)濾(lv)(lv)(lv)餅(bing)轉(zhuan)(zhuan)(zhuan)入(ru)(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)110℃條(tiao)件(jian)下干燥(zao)(zao)至(zhi)(zhi)(zhi)恒重(zhong)后(hou)(hou)轉(zhuan)(zhuan)(zhuan)入(ru)(ru)(ru)馬(ma)弗爐(lu)，以15ml/min速率向(xiang)爐(lu)內(nei)通入(ru)(ru)(ru)氮(dan)氣(qi)，在氮(dan)氣(qi)保護狀態下，以15℃/min速率持(chi)續升(sheng)溫(wen)(wen)(wen)(wen)至(zhi)(zhi)(zhi)1100℃，保溫(wen)(wen)(wen)(wen)30s，隨爐(lu)冷卻(que)至(zhi)(zhi)(zhi)室溫(wen)(wen)(wen)(wen)，出料(liao)(liao)，得(de)(de)(de)(de)膨(peng)脹(zhang)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)，稱取30kg膨(peng)脹(zhang)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)，倒(dao)(dao)入(ru)(ru)(ru)盛有80l石(shi)(shi)(shi)(shi)(shi)(shi)油醚的(de)(de)(de)高壓(ya)反(fan)(fan)(fan)應(ying)(ying)釜中(zhong)(zhong)(zhong)，以800r/min轉(zhuan)(zhuan)(zhuan)速攪拌(ban)(ban)(ban)混合(he)40min后(hou)(hou)，開啟反(fan)(fan)(fan)應(ying)(ying)釜加(jia)(jia)熱(re)器，使(shi)(shi)反(fan)(fan)(fan)應(ying)(ying)釜內(nei)壓(ya)力(li)(li)達(da)1.8mpa，保壓(ya)45s，再(zai)(zai)打開反(fan)(fan)(fan)應(ying)(ying)釜底部(bu)出料(liao)(liao)閥(fa)門，使(shi)(shi)反(fan)(fan)(fan)應(ying)(ying)釜中(zhong)(zhong)(zhong)物(wu)料(liao)(liao)噴射(she)進入(ru)(ru)(ru)接收釜中(zhong)(zhong)(zhong)，待接收釜中(zhong)(zhong)(zhong)物(wu)料(liao)(liao)自然冷卻(que)至(zhi)(zhi)(zhi)室溫(wen)(wen)(wen)(wen)，將(jiang)(jiang)(jiang)接收釜中(zhong)(zhong)(zhong)物(wu)料(liao)(liao)過(guo)(guo)濾(lv)(lv)(lv)，得(de)(de)(de)(de)含納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)的(de)(de)(de)濾(lv)(lv)(lv)渣(zha)，并(bing)將(jiang)(jiang)(jiang)含納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)的(de)(de)(de)濾(lv)(lv)(lv)渣(zha)置于(yu)(yu)真空干燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)110℃條(tiao)件(jian)下干燥(zao)(zao)至(zhi)(zhi)(zhi)恒重(zhong)，再(zai)(zai)經瞬(shun)間泄(xie)壓(ya)，使(shi)(shi)膨(peng)脹(zhang)石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)碎裂，得(de)(de)(de)(de)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)，量取500ml質量分(fen)數(shu)(shu)(shu)為(wei)(wei)(wei)2%硝酸銀(yin)(yin)溶液(ye)(ye)(ye)(ye)，倒(dao)(dao)入(ru)(ru)(ru)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)，再(zai)(zai)將(jiang)(jiang)(jiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)移(yi)入(ru)(ru)(ru)數(shu)(shu)(shu)顯測速恒溫(wen)(wen)(wen)(wen)磁力(li)(li)攪拌(ban)(ban)(ban)器中(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)60℃，轉(zhuan)(zhuan)(zhuan)速為(wei)(wei)(wei)600r/min條(tiao)件(jian)下，通過(guo)(guo)滴(di)液(ye)(ye)(ye)(ye)漏斗(dou)向(xiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)滴(di)加(jia)(jia)質量分(fen)數(shu)(shu)(shu)為(wei)(wei)(wei)4%氨(an)(an)(an)水(shui)(shui)，待三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)產(chan)生沉(chen)淀(dian)后(hou)(hou)繼續滴(di)加(jia)(jia)氨(an)(an)(an)水(shui)(shui)，直(zhi)至(zhi)(zhi)(zhi)產(chan)生的(de)(de)(de)沉(chen)淀(dian)完全溶解(jie)為(wei)(wei)(wei)止，形成銀(yin)(yin)氨(an)(an)(an)溶液(ye)(ye)(ye)(ye)，再(zai)(zai)向(xiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)加(jia)(jia)入(ru)(ru)(ru)150g上述(shu)所得(de)(de)(de)(de)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)，繼續恒溫(wen)(wen)(wen)(wen)攪拌(ban)(ban)(ban)混合(he)60min，待恒溫(wen)(wen)(wen)(wen)攪拌(ban)(ban)(ban)混合(he)結束，通過(guo)(guo)滴(di)液(ye)(ye)(ye)(ye)漏斗(dou)向(xiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)加(jia)(jia)入(ru)(ru)(ru)20ml乙醛，利用乙醛還原銀(yin)(yin)氨(an)(an)(an)溶液(ye)(ye)(ye)(ye)，產(chan)生的(de)(de)(de)銀(yin)(yin)單質包裹于(yu)(yu)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)表面(mian)，再(zai)(zai)將(jiang)(jiang)(jiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)于(yu)(yu)超(chao)聲振蕩(dang)儀中(zhong)(zhong)(zhong)，以45khz頻率超(chao)聲處理(li)15s后(hou)(hou)，將(jiang)(jiang)(jiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)移(yi)入(ru)(ru)(ru)水(shui)(shui)浴鍋中(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)70℃條(tiao)件(jian)下靜置20min，再(zai)(zai)將(jiang)(jiang)(jiang)三(san)口燒(shao)(shao)瓶(ping)(ping)(ping)中(zhong)(zhong)(zhong)物(wu)料(liao)(liao)過(guo)(guo)濾(lv)(lv)(lv)，得(de)(de)(de)(de)鍍(du)銀(yin)(yin)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)濾(lv)(lv)(lv)餅(bing)，并(bing)用去離子水(shui)(shui)洗滌鍍(du)銀(yin)(yin)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)濾(lv)(lv)(lv)餅(bing)5次，再(zai)(zai)將(jiang)(jiang)(jiang)鍍(du)銀(yin)(yin)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)濾(lv)(lv)(lv)餅(bing)轉(zhuan)(zhuan)(zhuan)入(ru)(ru)(ru)真空干燥(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)，于(yu)(yu)溫(wen)(wen)(wen)(wen)度(du)為(wei)(wei)(wei)110℃條(tiao)件(jian)下干燥(zao)(zao)至(zhi)(zhi)(zhi)恒重(zhong)，得(de)(de)(de)(de)鍍(du)銀(yin)(yin)納(na)(na)米石(shi)(shi)(shi)(shi)(shi)(shi)墨(mo)微(wei)(wei)(wei)片(pian)(pian)(pian)(pian)(pian)導(dao)電填料(liao)(liao)。

實例3

稱取(qu)50kg鱗片(pian)(pian)(pian)(pian)(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，倒入(ru)(ru)(ru)(ru)(ru)托盤(pan)(pan)中(zhong)(zhong)(zhong)(zhong)(zhong)，再(zai)(zai)將(jiang)托盤(pan)(pan)轉入(ru)(ru)(ru)(ru)(ru)真(zhen)空(kong)干(gan)燥(zao)(zao)(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為85℃條(tiao)(tiao)(tiao)件(jian)(jian)下，干(gan)燥(zao)(zao)(zao)(zao)20h，得(de)干(gan)燥(zao)(zao)(zao)(zao)鱗片(pian)(pian)(pian)(pian)(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，再(zai)(zai)于(yu)(yu)(yu)聚(ju)四氟乙烯內襯(chen)反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)，依次(ci)加(jia)入(ru)(ru)(ru)(ru)(ru)25l質(zhi)(zhi)量(liang)(liang)分(fen)(fen)數(shu)(shu)為98%硫(liu)酸，11l質(zhi)(zhi)量(liang)(liang)分(fen)(fen)數(shu)(shu)為65%硝酸，2kg高錳酸鉀，38kg所得(de)干(gan)燥(zao)(zao)(zao)(zao)鱗片(pian)(pian)(pian)(pian)(pian)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為60℃，轉速為550r/min條(tiao)(tiao)(tiao)件(jian)(jian)下，恒溫(wen)(wen)(wen)攪拌(ban)反(fan)應(ying)(ying)(ying)15h，待反(fan)應(ying)(ying)(ying)結束(shu)，將(jiang)聚(ju)四氟乙烯內襯(chen)反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物料過(guo)濾(lv)(lv)(lv)(lv)，得(de)氧(yang)(yang)化(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)濾(lv)(lv)(lv)(lv)餅，用去離子水洗(xi)滌氧(yang)(yang)化(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)濾(lv)(lv)(lv)(lv)餅直(zhi)至(zhi)洗(xi)滌液呈中(zhong)(zhong)(zhong)(zhong)(zhong)性，再(zai)(zai)將(jiang)洗(xi)滌后(hou)(hou)的(de)(de)氧(yang)(yang)化(hua)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)濾(lv)(lv)(lv)(lv)餅轉入(ru)(ru)(ru)(ru)(ru)烘箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為108℃條(tiao)(tiao)(tiao)件(jian)(jian)下干(gan)燥(zao)(zao)(zao)(zao)至(zhi)恒重(zhong)后(hou)(hou)轉入(ru)(ru)(ru)(ru)(ru)馬弗爐(lu)(lu)，以(yi)13ml/min速率向(xiang)爐(lu)(lu)內通(tong)入(ru)(ru)(ru)(ru)(ru)氮氣，在氮氣保護狀態下，以(yi)13℃/min速率持續(xu)(xu)升溫(wen)(wen)(wen)至(zhi)1050℃，保溫(wen)(wen)(wen)25s，隨爐(lu)(lu)冷(leng)卻(que)至(zhi)室溫(wen)(wen)(wen)，出料，得(de)膨(peng)脹石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，稱取(qu)28kg膨(peng)脹石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)，倒入(ru)(ru)(ru)(ru)(ru)盛有65l石(shi)(shi)(shi)(shi)(shi)油醚(mi)的(de)(de)高壓反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)，以(yi)700r/min轉速攪拌(ban)混(hun)合30min后(hou)(hou)，開啟反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)加(jia)熱器，使(shi)反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)內壓力(li)達1.7mpa，保壓37s，再(zai)(zai)打開反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)底部出料閥門，使(shi)反(fan)應(ying)(ying)(ying)釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物料噴射進入(ru)(ru)(ru)(ru)(ru)接收釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)，待接收釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物料自然冷(leng)卻(que)至(zhi)室溫(wen)(wen)(wen)，將(jiang)接收釜(fu)(fu)(fu)中(zhong)(zhong)(zhong)(zhong)(zhong)物料過(guo)濾(lv)(lv)(lv)(lv)，得(de)含(han)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)的(de)(de)濾(lv)(lv)(lv)(lv)渣(zha)，并將(jiang)含(han)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)的(de)(de)濾(lv)(lv)(lv)(lv)渣(zha)置(zhi)于(yu)(yu)(yu)真(zhen)空(kong)干(gan)燥(zao)(zao)(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為108℃條(tiao)(tiao)(tiao)件(jian)(jian)下干(gan)燥(zao)(zao)(zao)(zao)至(zhi)恒重(zhong)，再(zai)(zai)經瞬間泄壓，使(shi)膨(peng)脹石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)碎裂，得(de)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)，量(liang)(liang)取(qu)400ml質(zhi)(zhi)量(liang)(liang)分(fen)(fen)數(shu)(shu)為2%硝酸銀(yin)(yin)溶(rong)液，倒入(ru)(ru)(ru)(ru)(ru)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)，再(zai)(zai)將(jiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)移(yi)入(ru)(ru)(ru)(ru)(ru)數(shu)(shu)顯(xian)測速恒溫(wen)(wen)(wen)磁力(li)攪拌(ban)器中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為58℃，轉速為550r/min條(tiao)(tiao)(tiao)件(jian)(jian)下，通(tong)過(guo)滴(di)(di)液漏斗向(xiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)滴(di)(di)加(jia)質(zhi)(zhi)量(liang)(liang)分(fen)(fen)數(shu)(shu)為3%氨(an)水，待三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)產生(sheng)(sheng)沉(chen)淀后(hou)(hou)繼(ji)續(xu)(xu)滴(di)(di)加(jia)氨(an)水，直(zhi)至(zhi)產生(sheng)(sheng)的(de)(de)沉(chen)淀完(wan)全溶(rong)解(jie)為止，形成銀(yin)(yin)氨(an)溶(rong)液，再(zai)(zai)向(xiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)加(jia)入(ru)(ru)(ru)(ru)(ru)125g上述所得(de)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)，繼(ji)續(xu)(xu)恒溫(wen)(wen)(wen)攪拌(ban)混(hun)合52min，待恒溫(wen)(wen)(wen)攪拌(ban)混(hun)合結束(shu)，通(tong)過(guo)滴(di)(di)液漏斗向(xiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)加(jia)入(ru)(ru)(ru)(ru)(ru)15ml乙醛，利(li)用乙醛還原銀(yin)(yin)氨(an)溶(rong)液，產生(sheng)(sheng)的(de)(de)銀(yin)(yin)單質(zhi)(zhi)包(bao)裹于(yu)(yu)(yu)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)表(biao)面，再(zai)(zai)將(jiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)于(yu)(yu)(yu)超聲振蕩儀中(zhong)(zhong)(zhong)(zhong)(zhong)，以(yi)42khz頻率超聲處理13s后(hou)(hou)，將(jiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)移(yi)入(ru)(ru)(ru)(ru)(ru)水浴鍋中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為68℃條(tiao)(tiao)(tiao)件(jian)(jian)下靜置(zhi)18min，再(zai)(zai)將(jiang)三(san)(san)(san)口(kou)燒(shao)(shao)瓶(ping)(ping)中(zhong)(zhong)(zhong)(zhong)(zhong)物料過(guo)濾(lv)(lv)(lv)(lv)，得(de)鍍(du)銀(yin)(yin)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)濾(lv)(lv)(lv)(lv)餅，并用去離子水洗(xi)滌鍍(du)銀(yin)(yin)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)濾(lv)(lv)(lv)(lv)餅4次(ci)，再(zai)(zai)將(jiang)鍍(du)銀(yin)(yin)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)濾(lv)(lv)(lv)(lv)餅轉入(ru)(ru)(ru)(ru)(ru)真(zhen)空(kong)干(gan)燥(zao)(zao)(zao)(zao)箱(xiang)中(zhong)(zhong)(zhong)(zhong)(zhong)，于(yu)(yu)(yu)溫(wen)(wen)(wen)度(du)為108℃條(tiao)(tiao)(tiao)件(jian)(jian)下干(gan)燥(zao)(zao)(zao)(zao)至(zhi)恒重(zhong)，得(de)鍍(du)銀(yin)(yin)納(na)米(mi)(mi)石(shi)(shi)(shi)(shi)(shi)墨(mo)(mo)(mo)微(wei)片(pian)(pian)(pian)(pian)(pian)導電填料。