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快速壓致凝固法制備兩種非晶硫及其結(jié)構(gòu)研究

發(fā)布時(shí)間:2018-02-27 23:12

  本文關(guān)鍵詞: 非晶硫 液態(tài)硫λ轉(zhuǎn)變 放熱熔化 長(zhǎng)條形壓砧 出處:《西南交通大學(xué)》2016年碩士論文 論文類型:學(xué)位論文


【摘要】:本論文包含兩部分研究?jī)?nèi)容,第一部分是采用快速增壓法將λ轉(zhuǎn)變前后的液態(tài)硫快壓凝固為兩種非晶硫。兩種非晶硫表現(xiàn)出不同的顏色和透明度,與λ轉(zhuǎn)變前后液態(tài)硫的顏色變化對(duì)應(yīng),因此我們推測(cè)這兩種非晶硫包含λ轉(zhuǎn)變的信息。對(duì)非晶硫樣品進(jìn)行了拉曼散射光譜分析、差示掃描量熱分析及X射線衍射分析等,結(jié)果表明:即使是從TTλ的條件下凝固下來(lái)得到的非晶硫中也存在著較大體積分?jǐn)?shù)的聚合鏈。通過比較不同的壓力溫度條件下制備的非晶硫中聚合鏈的含量,發(fā)現(xiàn)提高增壓幅度及增壓速率比提高液態(tài)硫的溫度可以獲得更高的聚合鏈含量。熱分析的結(jié)果表明兩種非晶硫都具有高熱穩(wěn)定性,在10K/min的升溫速率下可以避免晶化直接轉(zhuǎn)變?yōu)橐簯B(tài)硫,并且都是反常放熱熔化。綜上,我們推測(cè)聚合鏈?zhǔn)强焖僭鰤哼^程中形成的,并且是否含有聚合鏈并不是引起兩種非晶硫顏色及透明性差別的原因。本論文的第二部分內(nèi)容是對(duì)長(zhǎng)條形壓砧進(jìn)行壓力標(biāo)定及壓力分布均勻性進(jìn)行研究。針對(duì)圓形端面平面對(duì)頂壓砧裝置中壓力梯度大的問題,本課題組洪時(shí)明教授設(shè)計(jì)了一種長(zhǎng)條形端面的平面對(duì)頂壓砧,并且推測(cè)這種壓砧可在沿壓砧中心線的狹長(zhǎng)區(qū)域內(nèi)產(chǎn)生均勻分布的高壓力。實(shí)驗(yàn)結(jié)果表明:長(zhǎng)條形端面(長(zhǎng)20mm、寬5mm)的硬質(zhì)合金對(duì)頂壓砧裝置可產(chǎn)生10GPa以上的高壓,沿長(zhǎng)條形中心線上至少12mm長(zhǎng)度范圍內(nèi)壓力分布是均勻的,在2.55GPa壓力時(shí)測(cè)量偏差小于2.0%,在7.7GPa時(shí)測(cè)量偏差小于3.6%。長(zhǎng)條形平面對(duì)頂壓砧的壓力分布特點(diǎn)非常有利于對(duì)長(zhǎng)條形樣品進(jìn)行高壓物性測(cè)量。
[Abstract]:In the first part, the liquid sulfur before and after 位 transition is solidified into two kinds of amorphous sulfur by rapid pressurization method. The two kinds of amorphous sulfur show different color and transparency. In accordance with the color change of liquid sulfur before and after 位 transition, we speculate that these two kinds of amorphous sulfur contain the information of 位 transition. Raman scattering spectroscopy, differential scanning calorimetry and X-ray diffraction analysis of amorphous sulfur samples are carried out. The results show that even the amorphous sulfur obtained from the solidification of TT 位 has a large volume fraction of the polymeric chain. The content of the polymeric chain in the amorphous sulfur prepared at different pressure and temperature is compared. It is found that the higher polymerization chain content can be obtained by increasing the pressure amplitude and the pressurization rate than by increasing the temperature of liquid sulfur. The results of thermal analysis show that both kinds of amorphous sulfur have high thermal stability. At a heating rate of 10 K / min, crystallization can be avoided directly into liquid sulfur, and both are anomalous exothermic melting. In summary, we speculate that the polymerization chain is formed during the rapid pressurization process. And the existence of polymeric chains is not the cause of the difference in color and transparency between the two kinds of amorphous sulfur. The second part of this thesis is to study the pressure calibration and pressure distribution uniformity of the long strip anvil. The problem of large pressure gradient in the device of face plane to top anvil, Professor Hong Shiming, our research group, has designed a plane-to-top anvil with long stripe end face. It is inferred that this anvil can produce high pressure distributed uniformly in the narrow and narrow region along the center of the anvil. The experimental results show that the high pressure over 10GPa can be generated by the cemented carbide anvil with long strip end face (20mm in length and 5mm in width). The pressure distribution is uniform in the length range of at least 12mm along the long strip centerline, The measurement deviation is less than 2.0 at 2.55 GPA and less than 3.6 at 7.7 GPA. The pressure distribution characteristics of the long plane-to-top anvil are very favorable for the measurement of the high pressure physical properties of the long strip sample.
【學(xué)位授予單位】:西南交通大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2016
【分類號(hào)】:O613.51

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