橢偏儀在位表征電化學(xué)沉積的系統(tǒng)搭建（十三）- 形貌及成分

正文

橢偏儀在位表征電化學(xué)沉積的系統(tǒng)搭建（十三）- 形貌及成分

2.5形貌及成分

2.5.1形貌分析

表征樣品的形貌常用的儀器是掃描電子顯微鏡(SEM)跑芳，其原理是通過高能的電子束掃描樣品表面激發(fā)出背散射電子轴总、二次電子和X射線等信號(hào)，然后對(duì)接受到的信號(hào)進(jìn)行放大并顯示成像博个，實(shí)現(xiàn)對(duì)樣品形貌等的監(jiān)測(cè)怀樟。掃描電子微鏡顯具有操作簡(jiǎn)單方便，得到的圖像清晰坡倔，zui大程度還原真實(shí)樣品形貌等優(yōu)點(diǎn)漂佩。通過掃描電子顯微鏡觀察Cu₂O薄膜，得到其表面形貌與顆粒尺寸等信息罪塔，從而對(duì)Cu₂O薄膜有更加直觀了解投蝉。

2.5.2成分分析

得到的樣品薄膜通過X射線衍射譜儀掃描確定其成分。X射線是一種波長(zhǎng)約為20到0.06?的電磁波征堪，利用原子內(nèi)層的電子被高速運(yùn)動(dòng)的電子轟擊產(chǎn)生躍遷光輻射瘩缆，從而產(chǎn)生氣體的電離、熒光物質(zhì)的發(fā)光以及照相乳膠感光等佃蚜。用電子束來轟擊金屬―靶‖材時(shí)將產(chǎn)生X射線庸娱，通過衍射圖譜的分析，可以獲得其成分谐算、內(nèi)部原子或者分子的結(jié)構(gòu)和形態(tài)等信息熟尉。當(dāng)X射線掃描晶體物質(zhì)時(shí)，X射線因晶格間距等效光柵的存在而發(fā)生光的散射和干涉洲脂。干涉效應(yīng)使得X射線的散射強(qiáng)度增強(qiáng)或減弱斤儿，其中強(qiáng)度zui大的光被認(rèn)為是X射線衍射線。圖2-5是晶面間距是d的n級(jí)反射圖示恐锦。在布拉格公式中：

d為晶面間距往果，θ為布拉格角，λ為入射波長(zhǎng)一铅。當(dāng)入射光照射到晶面上時(shí)會(huì)發(fā)生輻射陕贮，且輻射部分將成為球面波同步傳播，其光程差是波長(zhǎng)的整數(shù)倍潘飘。一部分入射光的偏轉(zhuǎn)角度是2θ肮之，會(huì)在衍射圖案中產(chǎn)生反射點(diǎn)。通過已知波長(zhǎng)X射線測(cè)量出的θ角卜录，得到晶面間距d局骤，從而可分解析出材料的內(nèi)部原子、或分子結(jié)構(gòu)暴凑。由衍射峰的強(qiáng)度可得出晶體結(jié)晶度，再利用謝樂公式(Scherrer)即能計(jì)算出晶粒平均尺寸赘来。謝樂公式(Scherrer)：

式中K是Scherrer常數(shù)现喳，如果β是衍射峰的半高寬凯傲，那么K=0.89，如果β是衍射峰的積分高寬嗦篱，則K=1冰单；D為晶粒垂直于晶面方向的平均厚度(nm)；θ為布拉格衍射角灸促；λ為X射線波長(zhǎng)诫欠，λ=0.154056nm。

圖2-5X射線的晶體衍射圖

2.6實(shí)驗(yàn)主要化學(xué)試劑及設(shè)備

本小節(jié)主要對(duì)涉及到的化學(xué)試劑進(jìn)行陳述浴栽。

2.6.1主要化學(xué)試劑

本實(shí)驗(yàn)所用的化學(xué)試劑如表2-1所示：

表2-1實(shí)驗(yàn)主要化學(xué)試劑

2.6.2主要制備及表征設(shè)備

本實(shí)驗(yàn)所用的主要制備及表征設(shè)備如表2-2所示：

表2-2主要制備及表征設(shè)備

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