
活性炭摻雜二氧化鈦的介電研究
本文介紹(shao)了活性炭與(yu)二氧化鈦(tai)混合(he)的介電研(yan)(yan)究TiO 2不同摩爾(er)比壓丸中的介電響應(ying)研(yan)(yan)究將樣品置于氮氣和氦氣氛中,并(bing)在50個Hz至(zhi)5MHz從室溫到723K研(yan)(yan)究復合(he)材(cai)料的電性能(neng)。
二氧(yang)(yang)(yang)化(hua)(hua)鈦(tai)因其物(wu)理(li)化(hua)(hua)學(xue)(xue)性(xing)(xing)(xing)質而被(bei)廣(guang)泛研究,使其成為各種應用(yong)(yong)的(de)(de)(de)合適(shi)材(cai)料(。它(ta)是(shi)一種光敏半導體,吸(xi)收近紫外(wai)線區域的(de)(de)(de)電(dian)(dian)磁輻(fu)射(she),化(hua)(hua)學(xue)(xue)性(xing)(xing)(xing)質非常穩定。由(you)于上述特點,它(ta)是(shi)*常用(yong)(yong)的(de)(de)(de)光催化(hua)(hua)劑,目前(qian)用(yong)(yong)于水凈化(hua)(hua)過程中(zhong)(zhong)(zhong)有機分子(zi)的(de)(de)(de)降解。它(ta)還被(bei)用(yong)(yong)作(zuo)白色(se)顏(yan)料、防(fang)腐涂料、氣體傳感(gan)器,通(tong)常用(yong)(yong)于陶瓷工業。該(gai)化(hua)(hua)合物(wu)有三(san)(san)個晶相:金(jin)紅(hong)石(四方結(jie)構(gou))、銳鈦(tai)礦(八(ba)(ba)面(mian)(mian)結(jie)構(gou))和板鈦(tai)礦(斜(xie)方晶結(jie)構(gou))。根據靜電(dian)(dian)價(jia)格原理(li)的(de)(de)(de)要求(qiu),每個氧(yang)(yang)(yang)原子(zi)由(you)三(san)(san)個八(ba)(ba)面(mian)(mian)體共(gong)享(xiang)。對(dui)于二氧(yang)(yang)(yang)化(hua)(hua)鈦(tai)摻雜活(huo)(huo)(huo)性(xing)(xing)(xing)炭(tan),已證明活(huo)(huo)(huo)性(xing)(xing)(xing)炭(tan)適(shi)合作(zuo)為外(wai)部原子(zi),其中(zhong)(zhong)(zhong)摻入3.2eV(純鈦(tai)礦)帶隙至(zhi)2.32eV(碳(tan)摻雜相)所需的(de)(de)(de)波長已增加到535納米。因此,與活(huo)(huo)(huo)性(xing)(xing)(xing)炭(tan)混合的(de)(de)(de)二氧(yang)(yang)(yang)化(hua)(hua)鈦(tai)比純二氧(yang)(yang)(yang)化(hua)(hua)鈦(tai)更有效。因為這個報告中(zhong)(zhong)(zhong)的(de)(de)(de)活(huo)(huo)(huo)性(xing)(xing)(xing)炭(tan)TiO 2的(de)(de)(de)影(ying)響(xiang)基體也預計會影(ying)響(xiang)材(cai)料的(de)(de)(de)介電(dian)(dian)性(xing)(xing)(xing)能。因此,本文研究了碳(tan)雜質對(dui)氧(yang)(yang)(yang)化(hua)(hua)鈦(tai)電(dian)(dian)性(xing)(xing)(xing)能的(de)(de)(de)影(ying)響(xiang),從商業粉(fen)末和不同摩爾(er)分數(shu)的(de)(de)(de)活(huo)(huo)(huo)性(xing)(xing)(xing)炭(tan)中(zhong)(zhong)(zhong)實現(xian)了該(gai)復合材(cai)料的(de)(de)(de)電(dian)(dian)性(xing)(xing)(xing)能。
實驗程序
為(wei)了制備與活(huo)性炭樣品混合(he)的(de)TiO 2,使用TiO 2純度為(wei)99.5%的(de)銳鈦礦相(xiang)粒徑(jing)為(wei)21nm活(huo)性炭粉。化學計量計算(suan)已(yi)經計算(suan)并獲得(de)X = 0.09,0.04,0.03和(he)0.摩(mo)爾分(fen)(fen)數02所需的(de)量。過程結(jie)束后(hou),將前體手工(gong)浸泡在瑪瑙研(yan)缽中約3小時,直至均勻。在室(shi)溫下將獲得(de)的(de)化合(he)物壓制成液壓機中的(de)丸劑形式。分(fen)(fen)光計中復合(he)材(cai)料的(de)紅外(wai)光譜FTIR標(biao)記Shimadzu Prestige 21上用含有(you)樣噲?平衡(heng)。在pH活(huo)性炭對水(shui)溶液中吡啶的(de)吸附(fu)能力*高。因此,選擇該pH研(yan)究活(huo)性炭上吡啶的(de)吸附(fu)率。
初始吡(bi)(bi)(bi)啶(ding)濃度(du)從20到(dao)10000mg / L不等。吡(bi)(bi)(bi)啶(ding)溶液(ye)與活性(xing)炭(tan)顆粒保持接觸,直至(zhi)達(da)(da)到(dao)平(ping)衡(heng)。定(ding)期測量溶液(ye)pH值(zhi),并(bing)通(tong)過(guo)(guo)適當添加(jia)0.01和0.1M的HCl和NaOH保持溶液(ye)恒(heng)定(ding)。達(da)(da)到(dao)平(ping)衡(heng)后,溶液(ye)中吡(bi)(bi)(bi)啶(ding)的濃度(du)通(tong)過(guo)(guo)分光(guang)光(guang)度(du)法測定(ding),平(ping)衡(heng)吸(xi)附(fu)的吡(bi)(bi)(bi)啶(ding)質量通(tong)過(guo)(guo)使(shi)吡(bi)(bi)(bi)啶(ding)的質量平(ping)衡(heng)計算(suan)。在之前沒有活性(xing)炭(tan)的運行(xing)中,證明吡(bi)(bi)(bi)啶(ding)不吸(xi)附(fu)在尼(ni)龍袋上。
測定水(shui)溶(rong)液中吡(bi)啶濃度
通(tong)過(guo)UV-水(shui)溶(rong)液中(zhong)測定水(shui)溶(rong)液中(zhong)吡啶(ding)的(de)(de)濃(nong)度(du)。UV-24960分光(guang)光(guang)度(du)計.5nm吡啶(ding)溶(rong)液的(de)(de)吸光(guang)啶(ding)溶(rong)液的(de)(de)吸光(guang)度(du)。因此,濃(nong)度(du)范圍為10-50mg / L樣品的(de)(de)吡啶(ding)濃(nong)度(du)由五種標(biao)準吡啶(ding)溶(rong)液制備的(de)(de)校準曲線(吸光(guang)對濃(nong)度(du))估(gu)算。
獲取吸附數據的方法
利用旋轉籃(lan)式批次吸(xi)(xi)附器獲得吡(bi)啶在活性(xing)炭上(shang)的吸(xi)(xi)附濃度分布。吸(xi)(xi)附器1L三頸反應(ying)燒瓶(ping)和葉片由不銹鋼(gang)籃(lan)的葉輪組成。將(jiang)吡(bi)啶溶液倒(dao)入(ru)(ru)吸(xi)(xi)附器中,將(jiang)活性(xing)炭顆(ke)粒(li)放(fang)入(ru)(ru)連接(jie)到變速電(dian)機(ji)的軸(zhou)上(shang)的不銹鋼(gang)網(wang)籃(lan)中。將(jiang)吸(xi)(xi)附器部分浸入(ru)(ru)恒溫浴中。
適當混合0.01N HCl和(he)(he)(he)NaOH溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)來制備pH = 10的(de)(de)溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(800-980mL)并加(jia)(jia)入吸(xi)附(fu)器(qi)。活性炭(1-5g)籃子放在幾(ji)個轉速(su)條件(100,150,200rpm)下。適當添加(jia)(jia)0.01和(he)(he)(he)0.1N NaOH控(kong)制溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)的(de)(de)溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)pH。直到(dao)(dao)溫度(du)和(he)(he)(he)活性炭保(bao)(bao)持接觸(chu)pH保(bao)(bao)持恒定。然后關閉攪拌器(qi),迅(xun)速(su)將已知濃(nong)度(du)提高到(dao)(dao)pH = 將吡(bi)(bi)啶溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)等分(fen)樣(yang)品(pin)倒入吸(xi)附(fu)劑溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)中,以(yi)獲得所需(xu)的(de)(de)初始濃(nong)度(du)。溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)后,溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)總(zong)體(ti)(ti)積為(wei)1L。立即(ji)啟動葉輪電機和(he)(he)(he)計(ji)時器(qi)。用pH對(dui)溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)進行監測pH以(yi)上調整值。加(jia)(jia)入的(de)(de)NaOH溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)總(zong)體(ti)(ti)積小(xiao)于2mL,占總(zong)體(ti)(ti)積的(de)(de)0.1%。定期(qi)取(qu)樣(yang)溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(5)mL)并分(fen)析確(que)定吡(bi)(bi)啶濃(nong)度(du)。取(qu)樣(yang)時間分(fen)別為(wei)0、1、3、5、10、15、20、25、30、40、60、90、150和(he)(he)(he)180分(fen)鐘。取(qu)樣(yang)后立即(ji)加(jia)(jia)5mL補充(chong)溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)使吸(xi)附(fu)劑溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)(1)L)總(zong)體(ti)(ti)積保(bao)(bao)持恒定。補充(chong)溶(rong)(rong)(rong)(rong)(rong)(rong)液(ye)(ye)的(de)(de)濃(nong)度(du)是(shi)平(ping)衡初始濃(nong)度(du)和(he)(he)(he)*終濃(nong)度(du)的(de)(de)平(ping)均值。添加(jia)(jia)劑的(de)(de)目的(de)(de)是(shi)取(qu)代樣(yang)品(pin)中取(qu)出的(de)(de)吡(bi)(bi)啶的(de)(de)質量(liang)。
圖(tu)像處理和數值解決方(fang)案
用(yong)2400倍放大倍數掃描(miao)電子顯微鏡檢查活(huo)性(xing)炭(tan)的(de)(de)形狀。圖(tu)像用(yong)圖(tu)像處理工具箱處理。程序如下。首(shou)先,通(tong)過(guo)將灰(hui)度轉化為(wei)灰(hui)度(從0(黑(hei)色)到(dao)255(白色),可以改善黑(hei)暗照區(qu)域的(de)(de)對比度。假設這些代表孔(kong)(kong)隙(xi)占(zhan)據的(de)(de)部分(fen)(fen),淺色區(qu)域與(yu)固體(ti)(ti)基質(活(huo)性(xing)炭(tan))有(you)關。這個想法是,每(mei)個象素的(de)(de)灰(hui)度值被(bei)(bei)跟蹤(來自(zi)黑(hei)色)并積累以獲得體(ti)(ti)積分(fen)(fen)數 ε γ 暗像素。其次,所有(you)具有(you)等于或小于閾值的(de)(de)像素都被(bei)(bei)轉換(huan)為(wei)白色(被(bei)(bei)孔(kong)(kong)占(zhan)據的(de)(de)空間(jian)(jian)),而具有(you)較高值的(de)(de)像素則被(bei)(bei)轉換(huan)為(wei)黑(hei)色(實心矩陣)。*后,應(ying)用(yong)濾(lv)波器來增(zeng)強(qiang)輪廓的(de)(de)定義。該程序允許我們獲得*終(zhong)的(de)(de)二值圖(tu)像,其中白色和總像素之間(jian)(jian)的(de)(de)比例等于活(huo)性(xing)炭(tan)的(de)(de)孔(kong)(kong)隙(xi)率(lv)。事實上,來自(zi)SEM顯微照片的(de)(de)處理圖(tu)像提供了(le)解(jie)決(jue)閉合問題的(de)(de)領(ling)域。
從整個(ge)研究(jiu)來看,活性炭吸附吡啶的(de)(de)濃度(du)衰減曲線。發現總有效(xiao)擴(kuo)散系(xi)數(shu)是(shi)吡啶濃度(du)平(ping)衡時的(de)(de)增加(jia)函(han)數(shu),主要(yao)是(shi)由于有效(xiao)的(de)(de)表面擴(kuo)散比孔體(ti)積擴(kuo)散做出了更大的(de)(de)貢(gong)獻。此外,點表面擴(kuo)散系(xi)數(shu)可(ke)以(yi)通過(guo)使用簡單(dan)的(de)(de)微結(jie)構(gou)幾何模型粗略(lve)估計。
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