本文關(guān)鍵詞：摻硼金剛石薄膜的制備及電化學(xué)性能研究　出處：《天津理工大學(xué)》2013年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 熱絲CVD 直流電弧等離子噴射CVD 硼摻雜金剛石薄膜 電化學(xué) L-半胱氨酸 多巴胺 抗壞血酸

【摘要】：目前，化學(xué)氣相沉積（CVD）硼摻雜金剛石具有良好的物理、化學(xué)特性，這使其非常適合作為新型電極材料。硼摻雜金剛石(BDD)既具有金剛石極高的硬度和化學(xué)穩(wěn)定性的特性，還具有良好的導(dǎo)電性、低背景電流、寬電勢(shì)窗口等優(yōu)點(diǎn)。因此BDD電極的性能優(yōu)于傳統(tǒng)的玻碳、石墨及其他形式的電極，在電化學(xué)檢測(cè)、合成、分解等領(lǐng)域具有廣闊的應(yīng)用前景。 針對(duì)目前硼摻雜金剛石薄膜的不同CVD制備特點(diǎn)和優(yōu)缺點(diǎn)，本文在熱絲、直流電弧等離子體噴射摻硼金剛石薄膜（BDD）的工藝研究、BDD電極的基本電化學(xué)性能研究及應(yīng)用檢測(cè)多巴胺等方面開展了如下工作： （1）熱絲化學(xué)氣相沉積法（hot filament chemical vapor deposition，HFCVD）制備金剛石薄膜。通過研究燈絲碳化條件解決了燈絲熔斷問題，進(jìn)一步研究形核和生長(zhǎng)參數(shù)（溫度、氣壓、時(shí)間），得到納米級(jí)別金剛石晶粒，其單一性好，C-C以sp~3結(jié)合為主。缺點(diǎn)是燈絲的揮發(fā)易引入污染，不利于研究摻雜金剛石薄膜的導(dǎo)電性能研究。 （2）利用直流電弧等離子噴射（DC arc plasma jet CVD）制備硼摻雜金剛石薄膜，采用特制石墨基臺(tái)控制基臺(tái)的溫度平衡，從而控制硅襯底的溫度；通過控制條件（壓強(qiáng)、氣體比例等）得到單一性較好的(100)和（111）晶向硅基金剛石薄膜，且生長(zhǎng)速率高。此外又進(jìn)行硼的摻雜（原位摻雜），，制得的摻硼金剛石薄膜在保持金剛石性能同時(shí)，可達(dá)到0.009·cm的電導(dǎo)率。本文首次利用該方法制備出了重硼摻雜金剛石薄膜。 （3）制得BDD電極，不經(jīng)任何修飾，將其作為電化學(xué)工作站陽極，在硫酸鈉空白溶液及鐵氰化鉀/亞鐵氰化鉀混合液中循環(huán)伏安掃描，電極的電化學(xué)窗戶達(dá)到4V（-2V~2V），表現(xiàn)出很高的反應(yīng)速率和電化學(xué)穩(wěn)定性能，電極表面不易被污染。 （4）將L-半胱氨酸電聚合修飾到該BDD電極表面，研究了多巴胺在該修飾電極上的電化學(xué)性能。改變掃描速率使多巴胺在電極上的氧化還原反應(yīng)得到最佳響應(yīng)，探測(cè)不同濃度（以10為數(shù)量級(jí)）的多巴胺中在該電極上的響應(yīng)，得到檢測(cè)限度為1×10~(-11)mol/L，經(jīng)過分析在1×10~(-9)~1×10~(-6)mol/L范圍內(nèi)，多巴胺溶液的濃度對(duì)數(shù)與氧化峰電流成線性關(guān)系，該結(jié)論在實(shí)際任意濃度的測(cè)量中得到了驗(yàn)證。在高濃度抗壞血酸共存下，BDD對(duì)于多巴胺的檢測(cè)不受影響，實(shí)驗(yàn)驗(yàn)證了隨機(jī)濃度的多巴胺濃度，理論與實(shí)際的偏差小于6%，具有一定的使用價(jià)值。
[Abstract]:At present, chemical vapor deposition (CVD) boron doped diamond has good physical and chemical properties. Boron doped diamond BDDs not only have high hardness and chemical stability of diamond, but also have good electrical conductivity and low background current. Therefore, the performance of BDD electrode is superior to that of traditional glassy carbon, graphite and other kinds of electrodes. It has a broad application prospect in electrochemical detection, synthesis, decomposition and other fields. According to the characteristics, advantages and disadvantages of different boron doped diamond films prepared by CVD, this paper studies the technology of hot filament, DC arc plasma jet boron doped diamond film BDDs. The basic electrochemical performance of BDD electrode and its application in the detection of dopamine have been studied as follows: 1) hot filament chemical vapor deposition. Diamond films were prepared by HFCVD. The melting problem of filament was solved by studying the carbonization conditions of filament. The nucleation and growth parameters (temperature, pressure, time) were further studied, and nanocrystalline diamond grains were obtained. The singularity of C-C is mainly composed of sp~3. The disadvantage is that the volatilization of filament is easy to lead into pollution, which is not conducive to the study of conductive properties of doped diamond films. B doped diamond films were prepared by DC arc plasma jet DC arc plasma jet CVD. The temperature balance of the substrate was controlled by a special graphite base platform. Thus, the temperature of silicon substrate is controlled; By controlling the conditions (pressure, gas ratio, etc.), the diamond films with good singularity and crystal orientation were obtained, and the growth rate was high. In addition, boron doping (in situ doping) was carried out. The obtained boron doped diamond films can achieve a conductivity of 0.009 路cm while maintaining the diamond properties. In this paper, the heavily boron doped diamond films have been prepared by this method for the first time. BDD electrode was prepared and used as anode for electrochemical workstation without any modification. The electrode was scanned by cyclic voltammetry in sodium sulfate blank solution and potassium ferricyanide / potassium ferricyanide mixture solution. The electrochemical window of the electrode reaches 4V ~ 2V ~ (2) V ~ (-1), showing high reaction rate and electrochemical stability, and the electrode surface is not easy to be contaminated. L- cysteine was electropolymerized onto the surface of the BDD electrode. The electrochemical performance of dopamine on the modified electrode was studied. The redox reaction of dopamine on the electrode was optimized by changing the scanning rate. The response of dopamine at different concentrations (10 orders of magnitude) to the electrode was detected, and the detection limit was 1 脳 10 ~ (-1) -11 mol / L. The linear relationship between the concentration logarithm of dopamine solution and the oxidation peak current was analyzed in the range of 1 脳 10 ~ (-1) ~ (-9) ~ (-1) mol / L ~ (-1 脳 10 ~ (-1)) ~ (-1) ~ (-1) mol / L. This conclusion has been verified in the actual measurement of any concentration of ascorbic acid. BDD has no effect on the detection of dopamine in the presence of high concentration of ascorbic acid, and the random concentration of dopamine has been verified by the experiment. The deviation between theory and practice is less than 6.
【學(xué)位授予單位】：天津理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2013
【分類號(hào)】：O484.1

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