本文選題：單晶金剛石　切入點：CVD法　出處：《哈爾濱工業(yè)大學(xué)》2016年碩士論文　論文類型：學(xué)位論文

【摘要】：金剛石具有極高硬度、熱導(dǎo)率、優(yōu)異的光學(xué)及電學(xué)性質(zhì),在多個應(yīng)用領(lǐng)域都可能成為不可替代的最佳材料。針對單晶金剛石的CVD的生長和尺寸增大嚴(yán)重受到籽晶襯底尺寸的限制的問題,本文對Mosaic拼接法高質(zhì)量大尺寸單晶金剛石生長進(jìn)行了較為詳實的理論分析和實驗研究,通過對幾塊HPHT籽晶拼接放置,在其上同時進(jìn)行生長,使得CVD生長層連接成為一個整體,突破單塊籽晶生長因邊界的多晶生成而限制了外延生長層尺寸的難題,以獲得大尺寸CVD單晶金剛石層。首先對單晶金剛石生長的化學(xué)本質(zhì)和沉積過程中初期的生長模式進(jìn)行了總結(jié)分析與實驗論證。研究了CVD生長的化學(xué)本質(zhì)及生長過程中幾種重要組分如原子[H],CH*等及其相關(guān)反應(yīng)方程式的程度對反應(yīng)速率的而影響。通過實驗和理論分析討論了同質(zhì)外延初期生長模式為島狀生長向?qū)訝钆_階流動模式的轉(zhuǎn)變現(xiàn)象。附著物會隨著生長過程鑲嵌于CVD生長層中,造成晶格畸變和內(nèi)應(yīng)力;而大刻蝕坑所揭露的深層位錯或包裹體也會由于晶格錯配和位錯擴(kuò)展,使得其上的CVD生長層具有較高的缺陷密度,這都會嚴(yán)重影響CVD外延生長層的質(zhì)量。對單晶金剛石生長進(jìn)行了較為系統(tǒng)的分析,并對影響其生長質(zhì)量和速率的各種因素分別進(jìn)行了實驗研究。通過PL譜、X射線搖擺曲線和等離子體刻蝕處理,表征籽晶的質(zhì)量和缺陷密度,總結(jié)出高質(zhì)量HPHT籽晶所必須具備的指標(biāo)。此外,籽晶側(cè)面是否拋光、溫度、微波功率、碳源濃度和雜質(zhì)元素對籽晶生長的速率和質(zhì)量都有著極大的影響。側(cè)面拋光的籽晶可以使得側(cè)邊生長的多晶相推遲出現(xiàn),進(jìn)而提升使CVD外延生長層面積增大的可能性,且溫度越高、碳源濃度越高,CVD層生長速率越快,但質(zhì)量也相對越低。所以采用了較為折中的生長工藝320mbar,4600W,850℃進(jìn)行生長,實現(xiàn)了高品質(zhì)和高速率協(xié)同的CVD單晶金剛石生長。對Mosaic拼接法進(jìn)行了實驗研究和探索,以實現(xiàn)CVD單晶金剛石面積的突破性增大。對雙籽晶拼接中的界面處進(jìn)行了研究,探究了影響界面處生長質(zhì)量的籽晶因素。進(jìn)而對生長后樣品的界面處進(jìn)行了晶體質(zhì)量,缺陷和摻雜濃度等表征。同時,對雙籽晶拼接生長進(jìn)行了激光切割和拋光,并對橫截面的拼接界面處進(jìn)行了Raman mapping測試,發(fā)現(xiàn)隨著CVD生長層的增厚,界面處由于存在應(yīng)力和晶格錯配以及一定的缺陷,導(dǎo)致界面應(yīng)力區(qū)的寬度逐漸增加,Raman半高寬也隨之逐漸增大,表明應(yīng)力區(qū)的晶體質(zhì)量有所降低,缺陷密度增加。且最大應(yīng)力點始終與Raman峰半高寬最大值位置相對應(yīng),表明了拼接界面的所在位置。此外,對三籽晶和四籽晶的拼接生長進(jìn)行了研究,探究拼接方式對界面處形貌的影響和N原子摻雜濃度信息,獲得了大尺寸的單晶金剛石。
[Abstract]:Diamond has extremely high hardness, thermal conductivity, excellent optical and electrical properties, The growth and size increase of CVD for single crystal diamond is seriously limited by the size of seed substrate. In this paper, the growth of high quality and large size monocrystalline diamond by Mosaic splicing method is analyzed and experimentally studied in detail. By placing several HPHT seeds together and growing on them at the same time, the CVD growth layer is connected as a whole. Breaking through the problem of monolithic seed growth limiting the size of epitaxial growth layer due to the formation of polycrystals at the boundary, In order to obtain large size CVD monocrystalline diamond layer, the chemical nature of monocrystalline diamond growth and the initial growth pattern during the deposition process were summarized, analyzed and experimentally demonstrated. The chemical nature and growth history of CVD growth were studied. Several important components in the process, such as atom [H] Ch * and the degree of reaction equation, affect the reaction rate. The initial growth mode of homogeneous epitaxy is discussed by experiment and theoretical analysis. The initial growth mode of homoepitaxy is island growth to stratified step flow mode. The attachment is embedded in the CVD growth layer as it grows. The deep dislocations or inclusions exposed by the large etching pits also have high defect density due to lattice mismatch and dislocation propagation. This will seriously affect the quality of CVD epitaxial growth layer. The growth of single crystal diamond is analyzed systematically. The effects of various factors on the growth quality and growth rate were studied experimentally. The mass and defect density of seed crystal were characterized by PL spectrum X-ray rocking curve and plasma etching treatment. In addition, whether the side side of the seed is polished, temperature, microwave power, The concentration of carbon source and impurity elements have great influence on the growth rate and quality of seed crystal. The side-polished seed crystal can delay the appearance of polycrystalline phase on the side side, and then increase the possibility of increasing the area of epitaxial growth layer of CVD. The higher the temperature, the faster the growth rate and the lower the mass of CVD layer, the higher the concentration of carbon source. The growth of CVD single crystal diamond with high quality and high speed has been realized. The Mosaic splicing method has been studied experimentally and explored in order to realize the breakthrough increase of the area of CVD single crystal diamond. The interface of double seed crystal splicing has been studied. The factors affecting the growth quality at the interface were investigated. The crystal quality, defects and doping concentration were characterized at the interface of the grown samples. At the same time, the laser cutting and polishing of the double seed splicing growth were carried out. The results of Raman mapping test show that with the thickening of the CVD growth layer, there are some defects in the interface due to the stress and lattice mismatch. As a result, the width of the interfacial stress region increases gradually and the width of the Raman half maximum increases, which indicates that the crystal quality of the stress region decreases and the defect density increases, and the maximum stress point always corresponds to the maximum position of the half width of the Raman peak. In addition, the splicing growth of tri-seed and tetra-seed was studied. The influence of splicing mode on the morphology of interface and the information of N atom doping concentration were investigated, and large size single crystal diamond was obtained.
【學(xué)位授予單位】：哈爾濱工業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：TQ163

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