本文選題：SmCo永磁 + 顯微分析��； 參考：《電子科技大學(xué)》2015年碩士論文

【摘要】：2:17型釤鈷永磁材料憑借其在居里溫度、溫度穩(wěn)定性和抗腐蝕等方面的突出性能,在航空、航天、航海等強調(diào)工作環(huán)境在較高溫度和惡劣場合的領(lǐng)域發(fā)揮著不可替代的作用。近年來隨著國防軍工行業(yè)的快速發(fā)展,對永磁材料的使用溫度和溫度穩(wěn)定性提出了更為嚴(yán)苛的要求。磁體工藝條件的控制直接影響著材料微觀形貌和成分的均勻性,進(jìn)而對產(chǎn)品最終的磁性能產(chǎn)生至關(guān)重要的影響。本文正是針對材料生產(chǎn)工藝中的一致性問題,借助包括掃描電子顯微鏡、X射線能譜儀和X射線熒光光譜儀等多種現(xiàn)代電子顯微分析技術(shù)對釤鈷合金的相關(guān)問題進(jìn)行了深入研究和討論,主要工作內(nèi)容和成果如下。(1)研究電子顯微分析技術(shù)在釤鈷永磁材料研究中的應(yīng)用。利用掃描電鏡的背散射成像和電子探針微區(qū)分析,明確了摻Gd釤鈷和鉺鈷鑄錠微觀金相的分布情況和對應(yīng)的微區(qū)成分變化;對比不同磨粉工藝得到粉末顆粒的微觀形貌像,選擇合適的工藝和粉體;觀察不同時效時間試樣金相圖中析出相的分布情況,結(jié)合相關(guān)理論確定時效工藝的最佳時間。上述應(yīng)用對該類材料粉末冶金工藝各個生產(chǎn)環(huán)節(jié)中的微觀分析工作具有指導(dǎo)意義,奠定了后續(xù)工作的基礎(chǔ)。(2)研究磁體高溫時磁性能下降的原因。根據(jù)材料不同的相變溫度,設(shè)置多個溫度試驗,對比不同溫度處理后磁體的物相結(jié)構(gòu)和標(biāo)準(zhǔn)材料之間的差異,并借助熱金相顯微鏡對材料進(jìn)行實時的高溫金相觀察,明確了其金相隨溫度的變化規(guī)律,最后根據(jù)樣品的微觀形貌和析出相成分分析結(jié)果,結(jié)合相關(guān)理論解釋了磁性能下降的原因。(3)研究摻雜Er的低溫度系數(shù)型釤鈷永磁合金的成分測定問題。通過實際測量確定了合適的測試譜線和對應(yīng)精確的衍射角從而削弱了譜線間相互干擾,采用粉末壓片法配備不同Er含量的標(biāo)準(zhǔn)樣品系列從而建立各元素的校正曲線,并通過標(biāo)準(zhǔn)曲線法消除了不同元素之間的吸收增強效應(yīng),建立了針對該類材料的X射線熒光光譜分析方法,同時結(jié)合理論計算和實際測量結(jié)果明確了實際工藝生產(chǎn)過程中引入的微量氧對分析結(jié)果造成的影響,最終實際測試結(jié)果表明本法的精密度和準(zhǔn)確度滿足一致性分析的需要,并且適用于工藝生產(chǎn)各個步驟得到的試樣。(4)設(shè)計開發(fā)稀土鈷永磁體微觀分析案例及圖譜庫。利用Access存儲底層數(shù)據(jù),在Visual Studio平臺上開發(fā)了數(shù)據(jù)庫軟件,并將歷年來相關(guān)分析得到的原始數(shù)據(jù)和典型案例報告添加至此數(shù)據(jù)庫,實現(xiàn)了檢索、查閱、修改和添加等功能,保證了這些珍貴實驗資料的有限存儲和安全訪問,使得后續(xù)研究人員可以高效率的借鑒這些研究成果。上述工作豐富了釤鈷永磁微觀研究理論和成分分析方法,為材料進(jìn)一步理論研究和工藝控制提供了依據(jù)和參考。
[Abstract]:With its outstanding properties in Curie temperature, temperature stability and corrosion resistance, 2:17 samarium cobalt permanent magnet plays an irreplaceable role in the fields of aviation, aerospace and navigation. In recent years, with the rapid development of national defense industry, the temperature and temperature stability of permanent magnet materials are more stringent. The control of the process conditions of the magnets has a direct impact on the microstructure and the homogeneity of the composition of the materials, which in turn has a crucial effect on the final magnetic properties of the products. In this paper, we aim at the consistency problem in material production process. The related problems of samarium cobalt alloy have been deeply studied and discussed by means of many modern electron microanalysis techniques, including scanning electron microscope (SEM) and X-ray fluorescence spectrometer (XRF). The main contents and results are as follows: 1) the application of electron microanalysis in the study of samarium cobalt permanent magnet materials. By means of SEM backscattering imaging and electron probe microanalysis, the distribution of microstructures and the corresponding composition changes of Gd-doped cobalt and erbium-doped cobalt ingot were determined, and the morphology of powder particles was obtained by comparing different grinding processes. The proper process and powder were selected, the distribution of precipitated phase in the metallographic diagram of different aging time was observed, and the optimum time of aging process was determined by combining with relevant theory. The above application is of guiding significance to the microscopic analysis of the powder metallurgy process of this kind of material, and lays a foundation for further research on the reasons for the decrease of magnetic properties of magnets at high temperature. According to the different phase transition temperatures of the materials, several temperature tests were set to compare the phase structure of the magnets and the differences between the standard materials after different temperature treatments, and the real time high temperature metallographic observation of the materials was carried out by means of the thermal metallographic microscope. The variation of metallography with temperature is clarified. Finally, according to the microstructure of the sample and the analysis results of the precipitated phase composition, In this paper, the reason for the decrease of magnetic properties is explained by the relevant theory.) the composition determination of low temperature coefficient samarium cobalt permanent magnet alloy doped with er is studied. Through the actual measurement, the appropriate test lines and the corresponding exact diffraction angles are determined, which reduces the interference between the spectral lines. The calibration curves of the elements are established by using the powder pressing method with standard sample series with different er contents. The absorption enhancement effect between different elements was eliminated by the standard curve method, and the X-ray fluorescence spectrum analysis method for this kind of material was established. At the same time, combined with the theoretical calculation and the actual measurement results, the influence of the trace oxygen introduced in the actual production process on the analysis results is clarified. The final test results show that the precision and accuracy of the method meet the needs of the consistency analysis. It is suitable for the design and development of rare earth cobalt permanent magnet microanalysis case and atlas library. This paper uses Access to store the underlying data, develops the database software on the Visual Studio platform, and adds the original data and typical case reports from related analysis over the years to the database, which realizes the functions of searching, consulting, modifying and adding, etc. It ensures the limited storage and secure access of these precious experimental data, so that the follow-up researchers can learn from these research results efficiently. The above work enriches the microcosmic research theory and component analysis method of samarium cobalt permanent magnet and provides the basis and reference for further theoretical research and technological control of materials.
【學(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：TM273

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