本實用新型(xing)涉及(ji)一(yi)種透射(she)電(dian)鏡(jing)(jing)(jing)樣(yang)品(pin)(pin)桿(gan)真空(kong)存儲(chu)與測試裝(zhuang)置,用于對透射(she)電(dian)鏡(jing)(jing)(jing)樣(yang)品(pin)(pin)桿(gan)進(jin)(jin)行(xing)預(yu)抽(chou)真空(kong)存儲(chu),對透射(she)電(dian)鏡(jing)(jing)(jing)樣(yang)品(pin)(pin)在(zai)(zai)進(jin)(jin)入電(dian)鏡(jing)(jing)(jing)之(zhi)前進(jin)(jin)行(xing)預(yu)處理,保證(zheng)樣(yang)品(pin)(pin)桿(gan)及(ji)樣(yang)品(pin)(pin)的干燥(zao)清(qing)潔,縮(suo)短透射(she)電(dian)鏡(jing)(jing)(jing)預(yu)抽(chou)時間(jian),減少(shao)樣(yang)品(pin)(pin)桿(gan)對透射(she)電(dian)鏡(jing)(jing)(jing)的污染,提高(gao)樣(yang)品(pin)(pin)桿(gan)使用壽命,也(ye)可在(zai)(zai)該裝(zhuang)置中對透射(she)電(dian)鏡(jing)(jing)(jing)樣(yang)品(pin)(pin)桿(gan)在(zai)(zai)工作真空(kong)環境進(jin)(jin)行(xing)通電(dian)、加熱等調試測試。本實用新型(xing)屬于透射(she)電(dian)子顯微(wei)鏡(jing)(jing)(jing)真空(kong)配件領域。
背景技術:
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自上世紀三十年代(dai)(dai)透射電(dian)子(zi)(zi)顯(xian)微鏡發(fa)明以來,特別是近二十年,透射電(dian)子(zi)(zi)顯(xian)微學(xue)(xue)技術(shu)在以球差矯正技術(shu)為(wei)(wei)代(dai)(dai)表的(de)空間分辨(bian)率(lv)(lv)、單色光源(yuan)為(wei)(wei)代(dai)(dai)表的(de)能量分辨(bian)率(lv)(lv),飛(fei)秒激光及高(gao)速CCD相機為(wei)(wei)代(dai)(dai)表的(de)時間分辨(bian)率(lv)(lv)等(deng)領域都取得了巨(ju)大進步,為(wei)(wei)物理學(xue)(xue)、材料學(xue)(xue)、化(hua)學(xue)(xue)等(deng)領域的(de)進步和發(fa)展做出了巨(ju)大貢(gong)獻。
透(tou)射(she)電(dian)(dian)子(zi)(zi)顯微鏡(TEM)是(shi)研(yan)究物質微觀結構的(de)(de)現代化大型儀器設備,在(zai)物理、化學(xue)(xue)(xue)、材(cai)料科學(xue)(xue)(xue)及(ji)生(sheng)命科學(xue)(xue)(xue)等領域都有著廣泛的(de)(de)應用。透(tou)射(she)電(dian)(dian)子(zi)(zi)顯微鏡的(de)(de)主體(ti)可以分(fen)(fen)(fen)為三個部(bu)(bu)分(fen)(fen)(fen):電(dian)(dian)子(zi)(zi)光(guang)(guang)學(xue)(xue)(xue)部(bu)(bu)分(fen)(fen)(fen),真(zhen)空部(bu)(bu)分(fen)(fen)(fen)和電(dian)(dian)子(zi)(zi)光(guang)(guang)學(xue)(xue)(xue)部(bu)(bu)分(fen)(fen)(fen)。電(dian)(dian)子(zi)(zi)光(guang)(guang)學(xue)(xue)(xue)部(bu)(bu)分(fen)(fen)(fen)主要包括(kuo)(kuo)(kuo)照明系(xi)統,成像系(xi)統,觀察和記錄系(xi)統,真(zhen)空部(bu)(bu)分(fen)(fen)(fen)包括(kuo)(kuo)(kuo)各種真(zhen)空泵(beng)及(ji)顯示儀表,電(dian)(dian)子(zi)(zi)學(xue)(xue)(xue)部(bu)(bu)分(fen)(fen)(fen)包括(kuo)(kuo)(kuo)各種光(guang)(guang)源、安全系(xi)統和控(kong)制系(xi)統。電(dian)(dian)子(zi)(zi)光(guang)(guang)學(xue)(xue)(xue)部(bu)(bu)分(fen)(fen)(fen)是(shi)電(dian)(dian)子(zi)(zi)顯微鏡的(de)(de)核心部(bu)(bu)分(fen)(fen)(fen),真(zhen)空和電(dian)(dian)子(zi)(zi)學(xue)(xue)(xue)部(bu)(bu)分(fen)(fen)(fen)是(shi)輔助系(xi)統。
在(zai)透(tou)射(she)電(dian)(dian)(dian)子(zi)顯微鏡(jing)中,凡是電(dian)(dian)(dian)子(zi)運(yun)行(xing)的(de)區(qu)域都要求有盡可能(neng)高的(de)真(zhen)空(kong)度;反之,則會(hui)(hui)影響透(tou)射(she)電(dian)(dian)(dian)子(zi)顯微鏡(jing)的(de)正常工作。若沒(mei)有高的(de)真(zhen)空(kong)度,高速電(dian)(dian)(dian)子(zi)與氣體分(fen)子(zi)相(xiang)(xiang)遇并相(xiang)(xiang)互作用(yong)(yong)會(hui)(hui)導致隨(sui)機電(dian)(dian)(dian)子(zi)散射(she),引起“炫(xuan)光”和削(xue)弱像(xiang)的(de)襯度;電(dian)(dian)(dian)子(zi)槍還會(hui)(hui)發生電(dian)(dian)(dian)離和防(fang)電(dian)(dian)(dian),導致電(dian)(dian)(dian)子(zi)束不穩定和閃爍;殘余(yu)氣體會(hui)(hui)腐(fu)蝕熾熱的(de)燈(deng)絲(si),縮短燈(deng)絲(si)的(de)使用(yong)(yong)壽(shou)命;殘余(yu)氣體會(hui)(hui)嚴重污染樣(yang)品,影響圖像(xiang)的(de)拍攝。因此透(tou)射(she)電(dian)(dian)(dian)鏡(jing)始終要保持(chi)在(zai)高真(zhen)空(kong)狀態(tai)。
透(tou)射(she)電(dian)鏡(jing)(jing)(jing)(jing)電(dian)子(zi)光學系統在長期的工作中十分(fen)(fen)容易(yi)受到污(wu)染(ran),物鏡(jing)(jing)(jing)(jing)是透(tou)射(she)電(dian)鏡(jing)(jing)(jing)(jing)中最(zui)為(wei)精密的部(bu)件;電(dian)鏡(jing)(jing)(jing)(jing)觀察時,極(ji)易(yi)從外界(jie)帶入污(wu)染(ran)物或(huo)易(yi)分(fen)(fen)解的樣品本身也(ye)會成為(wei)污(wu)染(ran)源,從而污(wu)染(ran)物鏡(jing)(jing)(jing)(jing)。物鏡(jing)(jing)(jing)(jing)污(wu)染(ran)將直接影響電(dian)鏡(jing)(jing)(jing)(jing)的分(fen)(fen)辨(bian)率。若物鏡(jing)(jing)(jing)(jing)光闌(lan)或(huo)極(ji)靴上有污(wu)染(ran)物,透(tou)射(she)電(dian)鏡(jing)(jing)(jing)(jing)可能會出現分(fen)(fen)辨(bian)率下降(jiang)、圖像漂移(yi)等(deng)故障。
測(ce)角(jiao)臺作(zuo)(zuo)為透射電(dian)鏡(jing)(jing)與外(wai)界連(lian)接的(de)(de)(de)(de)(de)(de)部件,除機器老(lao)化或測(ce)角(jiao)臺本身質(zhi)量問(wen)題外(wai),導致(zhi)(zhi)測(ce)角(jiao)臺故障的(de)(de)(de)(de)(de)(de)主要原因是樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)前期處理不(bu)夠,以及進(jin)(jin)樣(yang)(yang)(yang)(yang)(yang)、取(qu)樣(yang)(yang)(yang)(yang)(yang)操作(zuo)(zuo)不(bu)當;進(jin)(jin)樣(yang)(yang)(yang)(yang)(yang)或取(qu)樣(yang)(yang)(yang)(yang)(yang)時旋轉(zhuan)樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)困(kun)難主要與測(ce)角(jiao)臺銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)變形(xing)有(you)關(guan),因進(jin)(jin)樣(yang)(yang)(yang)(yang)(yang)和取(qu)樣(yang)(yang)(yang)(yang)(yang)操作(zuo)(zuo)樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)帶著銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)一(yi)(yi)起轉(zhuan)動,如果(guo)用力不(bu)均會(hui)使樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)在(zai)垂直方向上(shang)碰到(dao)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan),長時間會(hui)導致(zhi)(zhi)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)在(zai)開(kai)口處變形(xing),增大鋼質(zhi)套(tao)管(guan)(guan)(guan)與銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)間的(de)(de)(de)(de)(de)(de)摩擦(ca)而導致(zhi)(zhi)樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)旋轉(zhuan)困(kun)難;其(qi)次插拔(ba)樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)時銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)很澀,進(jin)(jin)樣(yang)(yang)(yang)(yang)(yang)取(qu)樣(yang)(yang)(yang)(yang)(yang)都較困(kun)難也(ye)都與銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)上(shang)附著有(you)臟(zang)(zang)物有(you)關(guan)。若樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)/樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)進(jin)(jin)入透射電(dian)鏡(jing)(jing)前未經(jing)清(qing)潔干燥(zao)處理,使進(jin)(jin)入鏡(jing)(jing)筒的(de)(de)(de)(de)(de)(de)樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)/樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)上(shang)有(you)污(wu)(wu)(wu)染(ran)物,其(qi)中(zhong)一(yi)(yi)些污(wu)(wu)(wu)染(ran)物在(zai)取(qu)出(chu)樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)的(de)(de)(de)(de)(de)(de)過程(cheng)中(zhong)會(hui)被鏡(jing)(jing)筒中(zhong)的(de)(de)(de)(de)(de)(de)氣體吹出(chu)鏡(jing)(jing)筒并吸附在(zai)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)內(nei)壁(bi),或是通過銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)的(de)(de)(de)(de)(de)(de)“─”形(xing)缺(que)口進(jin)(jin)入到(dao)鋼質(zhi)套(tao)管(guan)(guan)(guan)內(nei)壁(bi)與銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)外(wai)壁(bi)之間。長時間會(hui)導致(zhi)(zhi)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)內(nei)外(wai)壁(bi)上(shang)污(wu)(wu)(wu)染(ran)物越(yue)積越(yue)多(duo),會(hui)造成樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)與銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)之間的(de)(de)(de)(de)(de)(de)摩擦(ca)增大,使樣(yang)(yang)(yang)(yang)(yang)品(pin)(pin)(pin)(pin)桿(gan)(gan)(gan)插拔(ba)不(bu)易、旋轉(zhuan)困(kun)難。如果(guo)用蘸有(you)無水乙醇的(de)(de)(de)(de)(de)(de)無毛(mao)紙(zhi)擦(ca)拭(shi)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)內(nei)壁(bi),就(jiu)會(hui)發現(xian)無毛(mao)紙(zhi)上(shang)沾了許多(duo)黑(hei)色的(de)(de)(de)(de)(de)(de)臟(zang)(zang)東(dong)(dong)西。拆下(xia)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan),會(hui)發現(xian)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)“─”形(xing)缺(que)口外(wai)壁(bi)也(ye)有(you)一(yi)(yi)層黑(hei)色的(de)(de)(de)(de)(de)(de)臟(zang)(zang)東(dong)(dong)西。這些臟(zang)(zang)東(dong)(dong)西都是取(qu)樣(yang)(yang)(yang)(yang)(yang)時被鏡(jing)(jing)筒內(nei)氮氣吹出(chu)并附著在(zai)銅(tong)(tong)(tong)(tong)(tong)(tong)管(guan)(guan)(guan)內(nei)外(wai)壁(bi)上(shang)的(de)(de)(de)(de)(de)(de)污(wu)(wu)(wu)染(ran)物。
透射電鏡維護與故(gu)障處理專業性(xing)很(hen)強,一旦透射電鏡出現(xian)故(gu)障,要(yao)請專職人員(yuan)來維修(xiu),不僅需要(yao)預約和等待(dai)時(shi)間,而(er)且儀器(qi)(qi)使用(yong)單位需要(yao)支(zhi)付維修(xiu)費用(yong),降低儀器(qi)(qi)的利用(yong)率。
樣(yang)品(pin)桿是透射(she)(she)電(dian)鏡最(zui)重(zhong)要的(de)(de)(de)組件之一,起到承載樣(yang)品(pin)的(de)(de)(de)作用;對(dui)于一些特(te)制樣(yang)品(pin)桿上,它還兼具對(dui)樣(yang)品(pin)進行加熱、通電(dian)、施加應力等功(gong)能。樣(yang)品(pin)桿是否(fou)清(qing)(qing)潔以(yi)及(ji)本身的(de)(de)(de)儲氣狀態(tai)將(jiang)直接影(ying)響(xiang)透射(she)(she)電(dian)鏡真(zhen)(zhen)(zhen)空(kong)(kong)系(xi)統(tong)的(de)(de)(de)清(qing)(qing)潔程度(du)以(yi)及(ji)預抽真(zhen)(zhen)(zhen)空(kong)(kong)的(de)(de)(de)時間,一旦透射(she)(she)電(dian)鏡真(zhen)(zhen)(zhen)空(kong)(kong)系(xi)統(tong)被污(wu)染,透射(she)(she)電(dian)鏡真(zhen)(zhen)(zhen)空(kong)(kong)系(xi)統(tong)中零部件如(ru)物鏡、物鏡光闌、極靴(xue)、測(ce)角(jiao)臺等將(jiang)會受到不同程度(du)的(de)(de)(de)污(wu)染,影(ying)響(xiang)透射(she)(she)電(dian)鏡的(de)(de)(de)正常使用。
若樣(yang)(yang)品(pin)桿(gan)(gan)/暴(bao)露(lu)在大(da)氣中(zhong)(zhong)其表面普遍會(hui)受到污染(ran),不僅(jin)影(ying)(ying)響樣(yang)(yang)品(pin)桿(gan)(gan)本(ben)身的(de)壽命,還對(dui)透(tou)(tou)(tou)射電(dian)鏡(jing)(jing)真(zhen)空系統(tong)造成破(po)壞,污染(ran)透(tou)(tou)(tou)射電(dian)鏡(jing)(jing)零部件;同時,若長(chang)期暴(bao)露(lu)在大(da)氣中(zhong)(zhong)也會(hui)使(shi)(shi)樣(yang)(yang)品(pin)桿(gan)(gan)儲(chu)存一定的(de)氣體,從而影(ying)(ying)響透(tou)(tou)(tou)射電(dian)鏡(jing)(jing)預(yu)抽真(zhen)空。因(yin)此發展一種使(shi)(shi)用(yong)方便,真(zhen)空度高,抽真(zhen)空速度快、能夠配合透(tou)(tou)(tou)射電(dian)鏡(jing)(jing)樣(yang)(yang)品(pin)桿(gan)(gan)使(shi)(shi)用(yong)的(de)樣(yang)(yang)品(pin)桿(gan)(gan)存儲(chu)裝置(zhi),使(shi)(shi)樣(yang)(yang)品(pin)桿(gan)(gan)/樣(yang)(yang)品(pin)保持在清(qing)潔的(de)真(zhen)空環(huan)境(jing),將縮短透(tou)(tou)(tou)射電(dian)鏡(jing)(jing)預(yu)抽時間,減少樣(yang)(yang)品(pin)桿(gan)(gan)對(dui)透(tou)(tou)(tou)射電(dian)鏡(jing)(jing)的(de)污染(ran),提高樣(yang)(yang)品(pin)桿(gan)(gan)使(shi)(shi)用(yong)壽命提供了有利(li)工具。
技術實現要素:
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為解決上述問題,本實用新型提供一種用于透射電子顯微鏡樣品桿真空存儲與測試裝置,對透射電鏡樣品桿/樣品進行預抽真空,使樣品桿/樣品保持在清潔的工作真空環境,可同時存儲多于6根樣品桿,5分鐘內可從空氣氣壓抽到4×10-4Pa,極限真空可達5×10-5Pa,從而保證(zheng)樣(yang)(yang)品(pin)(pin)(pin)桿(gan)(gan)/樣(yang)(yang)品(pin)(pin)(pin)干燥清潔以及樣(yang)(yang)品(pin)(pin)(pin)桿(gan)(gan)的(de)真空環(huan)境(jing)調(diao)試測試,縮短透(tou)射電鏡預抽時間,減少樣(yang)(yang)品(pin)(pin)(pin)桿(gan)(gan)對透(tou)射電鏡的(de)污染,提高樣(yang)(yang)品(pin)(pin)(pin)桿(gan)(gan)使(shi)用壽命。本裝置操作使(shi)用方(fang)便(bian),真空度好,易于添加樣(yang)(yang)品(pin)(pin)(pin)桿(gan)(gan)存儲工位(wei),適用性廣(guang)。
為(wei)實現(xian)上述目(mu)的,本實用新型是通過如下技(ji)術方案實現(xian):
一種用于透(tou)射(she)電鏡樣品桿(gan)的真(zhen)空(kong)存(cun)儲(chu)與(yu)測試(shi)裝置(zhi)(zhi),該(gai)裝置(zhi)(zhi)包括可(ke)移動機架,真(zhen)空(kong)泵系統(tong)(tong),真(zhen)空(kong)測量組件與(yu)顯示系統(tong)(tong),閥門系統(tong)(tong),真(zhen)空(kong)罩(zhao),樣品桿(gan)存(cun)儲(chu)組件及堵(du)塞;
所述(shu)的真空泵系統包括渦(wo)旋干泵與(yu)分子(zi)泵,可移動機架上設置分子(zi)泵2,分子(zi)泵2通(tong)過前級閥(fa)3與(yu)渦(wo)旋干泵4連接(jie),渦(wo)旋干泵4通(tong)過預抽(chou)閥(fa)5和主管(guan)道8連接(jie);
所述(shu)的真(zhen)(zhen)空(kong)罩(zhao)用于連接主閥,并連接分(fen)子泵(beng)與電離規(gui);電離規(gui)12安裝(zhuang)(zhuang)在真(zhen)(zhen)空(kong)罩(zhao)13上(shang)探測高真(zhen)(zhen)空(kong)通(tong)過(guo)真(zhen)(zhen)空(kong)計11顯(xian)示,電阻規(gui)9安裝(zhuang)(zhuang)在主管(guan)道8上(shang)探測低真(zhen)(zhen)空(kong)通(tong)過(guo)真(zhen)(zhen)空(kong)計11顯(xian)示;
所述的(de)閥(fa)(fa)門系統包(bao)括前(qian)(qian)級(ji)閥(fa)(fa)、預抽(chou)閥(fa)(fa)、主閥(fa)(fa)、放(fang)氣(qi)閥(fa)(fa),前(qian)(qian)級(ji)閥(fa)(fa)用(yong)于控(kong)制渦(wo)旋(xuan)干泵與(yu)分(fen)子泵之間連(lian)通(tong)/斷開(kai),預抽(chou)閥(fa)(fa)用(yong)于控(kong)制渦(wo)旋(xuan)干泵與(yu)樣(yang)(yang)品桿(gan)(gan)(gan)存(cun)儲(chu)(chu)組(zu)件(jian)連(lian)通(tong)/斷開(kai),主閥(fa)(fa)用(yong)于控(kong)制分(fen)子泵與(yu)樣(yang)(yang)品桿(gan)(gan)(gan)存(cun)儲(chu)(chu)組(zu)件(jian)連(lian)通(tong)/斷開(kai),放(fang)氣(qi)閥(fa)(fa)用(yong)于插(cha)拔樣(yang)(yang)品桿(gan)(gan)(gan)時排氣(qi),便于拔出樣(yang)(yang)品桿(gan)(gan)(gan);
所述的(de)樣品(pin)桿(gan)存儲組件主(zhu)管(guan)道(dao)上設有(you)多個(ge)個(ge)工位(wei),能同時(shi)插入6根樣品(pin)桿(gan),支撐法(fa)蘭(lan)管(guan)套與(yu)主(zhu)管(guan)道(dao)通(tong)過螺釘連接(jie),兩者(zhe)之間裝有(you)密封(feng)(feng)圈保證真空(kong),玻(bo)璃管(guan)嵌入主(zhu)管(guan)道(dao),外接(jie)法(fa)蘭(lan)套管(guan)通(tong)過螺釘與(yu)管(guan)道(dao)主(zhu)體連接(jie);主(zhu)管(guan)道(dao)、玻(bo)璃管(guan)與(yu)外接(jie)法(fa)蘭(lan)套管(guan)三者(zhe)之間的(de)真空(kong)密封(feng)(feng)。
所述的(de)堵(du)塞罩上(shang)裝有密封圈,密封圈規格與(yu)樣(yang)品桿(gan)(gan)上(shang)密封圈規格相同,用于(yu)將(jiang)樣(yang)品桿(gan)(gan)取(qu)出(chu)后,替代樣(yang)品桿(gan)(gan)插入并(bing)密封支撐法蘭(lan)套管。
應(ying)(ying)用(yong)(yong)所述裝置的方法,其特征在(zai)于,初次(ci)使用(yong)(yong)時(shi),將多個樣品(pin)桿依(yi)次(ci)插入對應(ying)(ying)工位,當樣品(pin)桿數目不夠(gou)的話用(yong)(yong)堵塞7代(dai)替樣品(pin)桿,保(bao)證樣品(pin)桿存儲組件密(mi)封;
打開渦旋干泵和前級閥,將分子泵抽至10Pa以下,打開分子泵,待分子泵工作后,關閉前級閥和打開預抽閥,當樣品桿存儲組件真空低于7Pa時,關閉預抽閥,打開前級閥和主閥,在5分鐘之內將樣品桿存儲組件抽至4×10-4Pa以下;
需要使用樣品桿時,關閉主閥,打開放氣閥,將樣品桿拔出,插入堵塞,關閉放氣閥,打開預抽閥,將樣品桿存儲組件預抽至7Pa以下,當真空度低于7Pa時,關閉預抽閥,打開前級閥后,打開主閥,5分鐘內將系統抽至4×10-4Pa以下。
透射電鏡樣品桿真空存儲與測試裝置包括可移動機架,真空泵系統,真空測量與顯示系統,閥門系統,真空罩,樣品桿存儲組件及堵塞,可對透射電鏡樣品桿/樣品進行預抽真空,使樣品桿/樣品保持在工作真空環境,可同時存儲多于6根樣品桿,5分鐘內可從空氣氣壓達到4×10-4Pa,極限真空可達5×10-5Pa,在樣品桿存儲的同時可(ke)對(dui)樣品桿進行通電,加熱(re)測(ce)試。
進(jin)一步,所述的可移動機架用于支(zhi)撐整(zheng)個裝(zhuang)置,其(qi)框架由(you)工業(ye)鋁合金組裝(zhuang)而成。
進一步,所述的真空泵系統包括渦旋干泵與分子泵,渦旋干泵用于將樣品桿存儲組件壓力從大氣壓至低真空(7Pa),分子泵控制樣品桿存儲組件壓力從低真空至高真空(5×10-5Pa),兩者為樣品桿存儲組件組件提供干燥清潔的高真空,經測試該真空泵系統可使該機組5分鐘內可從空氣氣壓達到4×10-4Pa。
進一步,所述的真空測量組件電阻規用于測量大氣壓力至7Pa的低真空環境,電離規測量7Pa至5×10-5Pa高真(zhen)空(kong)(kong)環境,真(zhen)空(kong)(kong)計(ji)用來實(shi)時顯示樣品桿存儲(chu)組件真(zhen)空(kong)(kong)度。
進(jin)一步(bu),所述的真空罩用于(yu)連接(jie)(jie)主閥(fa),并(bing)連接(jie)(jie)分子泵與(yu)電離規(gui),真空罩與(yu)主閥(fa),分子泵,電離規(gui)均為密封(feng)連接(jie)(jie)。
進一步(bu),所述的(de)閥(fa)門(men)系統包括(kuo)前級(ji)閥(fa)、預抽閥(fa)、主閥(fa)、放(fang)氣(qi)閥(fa),前級(ji)閥(fa)用(yong)于控制渦旋干(gan)泵(beng)與分(fen)子泵(beng)之間連(lian)通(tong)/斷(duan)開,預抽閥(fa)用(yong)于控制渦旋干(gan)泵(beng)與樣(yang)(yang)(yang)品(pin)桿(gan)存儲組(zu)件連(lian)通(tong)/斷(duan)開,主閥(fa)用(yong)于控制分(fen)子泵(beng)與樣(yang)(yang)(yang)品(pin)桿(gan)存儲組(zu)件連(lian)通(tong)/斷(duan)開,放(fang)氣(qi)閥(fa)用(yong)于插拔(ba)樣(yang)(yang)(yang)品(pin)桿(gan)時(shi)排氣(qi),便(bian)于拔(ba)出(chu)樣(yang)(yang)(yang)品(pin)桿(gan),預抽閥(fa)、前級(ji)閥(fa)、主閥(fa)、放(fang)氣(qi)閥(fa)、真空泵(beng)之間通(tong)過(guo)控制電(dian)路(lu)有一定(ding)互(hu)鎖關系,以防止誤操(cao)作給系統造成損壞。
進一步,所(suo)述的(de)樣(yang)品(pin)(pin)桿(gan)存(cun)儲(chu)組件主管(guan)道上共設有6個工(gong)位,可同時插入6根樣(yang)品(pin)(pin)桿(gan);主管(guan)道兩側通(tong)過(guo)法蘭(lan)連(lian)接,便于(yu)(yu)增(zeng)加存(cun)儲(chu)工(gong)位;支撐(cheng)法蘭(lan)管(guan)套用于(yu)(yu)支撐(cheng)樣(yang)品(pin)(pin)桿(gan),其材料為(wei)高強度不銹鋼,通(tong)過(guo)螺釘與主管(guan)道連(lian)接,兩者(zhe)之(zhi)(zhi)間裝有密(mi)(mi)封(feng)(feng)圈(quan)保證(zheng)真空;玻璃管(guan)嵌(qian)入主管(guan)道,便于(yu)(yu)觀察(cha)存(cun)儲(chu)樣(yang)品(pin)(pin)桿(gan)前端(duan);外接法蘭(lan)套管(guan)通(tong)過(guo)螺釘與主管(guan)道連(lian)接,通(tong)過(guo)加工(gong)接觸斜面(mian)壓緊(jin)與主管(guan)道和玻璃管(guan)三(san)者(zhe)之(zhi)(zhi)間密(mi)(mi)封(feng)(feng)圈(quan)來保證(zheng)三(san)者(zhe)之(zhi)(zhi)間的(de)真空密(mi)(mi)封(feng)(feng)。
進(jin)一(yi)步,所(suo)述的堵(du)塞上裝有(you)密封(feng)(feng)圈(quan),密封(feng)(feng)圈(quan)規格與樣(yang)品(pin)桿(gan)(gan)上密封(feng)(feng)圈(quan)規格相同(tong),用于將樣(yang)品(pin)桿(gan)(gan)取出后,替代樣(yang)品(pin)桿(gan)(gan)插入(ru)并密封(feng)(feng)支撐法蘭套管。
進一步,所(suo)述的(de)樣品(pin)桿為不同廠家(jia)、不同尺寸、不同功(gong)能類(lei)型的(de)透射電鏡樣品(pin)桿,可在該裝置中(zhong)進行(xing)調試測試。
附圖說明:
圖(tu)1為發明裝置整(zheng)體示意圖(tu);
圖2為樣品桿存(cun)儲組件(jian)剖(pou)切示意圖;
圖3為樣品桿及堵塞插入樣品桿存儲組件示意圖;
圖中畫面說明如下:
1 可移動機(ji)架 2 分子泵(beng) 3 前級閥 4 渦旋干泵(beng) 5 預抽閥
6 放(fang)氣(qi)閥(fa) 7 堵塞 8 主(zhu)(zhu)管道 9 電阻規 10 主(zhu)(zhu)閥(fa) 11 真空計
12 電離規 13 真空罩(zhao) 14 支撐法蘭(lan)套管 15 螺釘 16 法蘭(lan)盤
17 外接法蘭套管 18 玻璃管 19 樣品桿
具體實施方式:
下面(mian),參(can)考附(fu)(fu)圖,對本實(shi)用(yong)新(xin)型進(jin)行(xing)進(jin)一步說明(ming),附(fu)(fu)圖中示(shi)意出本實(shi)用(yong)新(xin)型的示(shi)例(li)(li)(li)性實(shi)施例(li)(li)(li)。然而,本實(shi)用(yong)新(xin)型可以體(ti)現為多種不同的形(xing)(xing)式(shi)(shi),改變裝置結構形(xing)(xing)式(shi)(shi)或(huo)樣品(pin)桿存儲組件的形(xing)(xing)狀亦可實(shi)現本裝置功能(neng),而非局限于本文敘述的實(shi)例(li)(li)(li)。
初次使用時,將樣品桿19依次插入對應工位,當樣品桿1數目不夠的話可以用堵塞7代替樣品桿19,這樣保證本實用新型裝置是一個封閉容器。打開渦旋干泵4和前級閥3,將分子泵2抽至低真空,打開分子泵2,待分子泵2工作后,關閉前級閥3和打開預抽閥5,當樣品桿存儲組件真空低于7Pa時,關閉預抽閥5,打開前級閥3和主閥10,可在5分鐘之內將樣品桿存儲組件抽至4×10-4Pa,長時間可抽至極限真空5×10-5Pa(接近樣品桿在透射電鏡中使用真空),對樣品桿19(樣品)進行存儲,使樣品桿19(樣品)處在干燥清潔的真空環境不受污染,存儲過程中可對樣品桿19進行加熱,通電等調試測試,可通過玻璃管18觀察樣品桿19前端,也可對樣品桿19上樣品進行加熱等預處理來保證樣品的清潔,需要使用樣品桿19時,關閉主閥10,打開放氣閥6,將樣品桿19拔出,插入堵塞7,關閉放氣閥6,打開預抽閥5,20秒可將樣品桿存儲組件預抽至7Pa以下,當真空度低于7Pa時,關閉預抽閥5,打開前級閥3后,打開主閥10,5分鐘可將系統抽至4×10-4Pa的(de)高(gao)(gao)真空,大大降低了樣(yang)品桿(gan)(gan)(gan)(gan)與大氣環(huan)境的(de)接觸時(shi)間,減(jian)(jian)少(shao)樣(yang)品桿(gan)(gan)(gan)(gan)受(shou)污(wu)染或侵蝕(shi),使樣(yang)品桿(gan)(gan)(gan)(gan)/樣(yang)品保持在清(qing)潔(jie)的(de)工作真空環(huan)境,進而縮短透射電鏡(jing)預(yu)抽(chou)時(shi)間,減(jian)(jian)少(shao)樣(yang)品桿(gan)(gan)(gan)(gan)對(dui)透射電鏡(jing)的(de)污(wu)染,提高(gao)(gao)樣(yang)品桿(gan)(gan)(gan)(gan)使用壽(shou)命(ming),同時(shi)減(jian)(jian)少(shao)電鏡(jing)透射電鏡(jing)出(chu)故障幾率,節約昂(ang)貴的(de)維修費用,提高(gao)(gao)儀器的(de)使用率。該裝置預(yu)抽(chou)閥(fa)(fa)5、前級閥(fa)(fa)3、主閥(fa)(fa)10、放氣閥(fa)(fa)6、真空度之(zhi)間通(tong)過控(kong)制電路有(you)一(yi)定互鎖關(guan)系(xi),前級閥(fa)(fa)3和預(yu)抽(chou)閥(fa)(fa)5總是一(yi)個打開(kai)一(yi)個關(guan)閉進行控(kong)制;以防止誤操作給系(xi)統(tong)造成損壞。