本文選題：載荷因子 + 面積函數(shù)��； 參考：《安徽工業(yè)大學(xué)》2017年碩士論文

【摘要】：納米壓痕儀由于其較高的力和位移分辨率,較高的定位精度等優(yōu)點,在薄膜新材料和MEMS微器件等領(lǐng)域得到了越來越廣泛的應(yīng)用,由于在使用過程中,壓痕儀的針尖會發(fā)生磨損,沒有經(jīng)過校準(zhǔn)的納米壓痕儀會對于測試的結(jié)果產(chǎn)生顯著的影響,在較小的壓入深度下這種影響更加明。本文對于納米壓痕儀的校準(zhǔn)模型進行研究,建立新的校準(zhǔn)模型應(yīng)用到納米壓痕儀的校準(zhǔn)中對儀器的載荷因子、機架柔度以及針尖面積函數(shù)進行校準(zhǔn),在校準(zhǔn)完成的基礎(chǔ)上對于藍寶石標(biāo)樣進行定值。定值完成后的藍寶石標(biāo)樣塊可作為納米壓痕儀的標(biāo)準(zhǔn)樣品,實現(xiàn)不納米壓痕儀測量結(jié)果的準(zhǔn)確可靠和等效可比。首先對于納米壓痕儀的載荷因子建立了校準(zhǔn)模型,通過在0.5 mN-10 m N之間等比率選取20個力值進行納米壓痕測試,利用電磁力天平的稱重模塊與納米壓痕儀針尖實現(xiàn)加載卸載過程,在天平上測出實際的加載力值。每一次的加載過程納米壓痕儀都會給出一個加載的力值,對于兩個力值進行線性擬合,擬合出來的直線的斜率即為校準(zhǔn)完成的載荷因子。通過載荷因子校準(zhǔn)模型校準(zhǔn)完成后進行壓痕測試發(fā)現(xiàn),載荷因子校準(zhǔn)后的納米壓痕儀測量得到的標(biāo)準(zhǔn)熔融石英樣的硬度與彈性模量值比校準(zhǔn)前更加的準(zhǔn)確。在載荷因子校準(zhǔn)完成的基礎(chǔ)上,使用AFM直接法與迭代法兩種不同的校準(zhǔn)模型共四種校準(zhǔn)方法對于納米壓痕儀機架柔度與針尖面積函數(shù)進行校準(zhǔn)。校準(zhǔn)完成后對于四種校準(zhǔn)方法得到的機架柔度與面積函數(shù)結(jié)果應(yīng)用到壓痕儀器中進行壓痕實驗可以得到:在納米壓痕儀針尖淺壓入深度下單晶鎢與熔融石英迭代法校準(zhǔn)獲得的機架柔度與面積函數(shù)較其他三種準(zhǔn)校準(zhǔn)方法準(zhǔn)確;當(dāng)壓入深度逐漸變大,四種校準(zhǔn)方法所得到的面積函數(shù)與機架柔度都趨近于準(zhǔn)確值。在橫向的比較中單晶鎢對于機架柔度的校準(zhǔn)比熔融石英要好;對于面積函數(shù)的校準(zhǔn)中AFM直接法在淺壓入深度下對于儀器的校準(zhǔn)要比間接法校準(zhǔn)準(zhǔn)確的多;當(dāng)壓入深度在60 nm以下時,針尖曲率半徑對于測試結(jié)果的準(zhǔn)確性影響較大,在極淺的壓入深度下,采用針尖曲率半徑小的針尖會得到比較準(zhǔn)確的測試數(shù)據(jù)。最后將校準(zhǔn)得到的載荷因子以及擇優(yōu)選擇最佳校準(zhǔn)模型校準(zhǔn)后得到機架柔度與面積函數(shù)應(yīng)用到納米壓痕儀器中,利用TriboIndenter-900型納米壓痕儀對于定值實驗過程中的均勻性帶來的不確定度、穩(wěn)定性帶來的不確定度、壓痕實驗重復(fù)性帶來的不確定度以及儀器自身帶來的不確定度進行分析評定,算出定值實驗帶來的總的合成不確定度;確定擴展因子,計算定值需要的擴展不確定度;然后對于藍寶石標(biāo)樣候選物的折合模量與硬度值進行定值。
[Abstract]:Because of its advantages of high force and displacement resolution, high positioning accuracy and so on, nano-indentation instrument has been more and more widely used in the field of new thin film materials and MEMS microdevices, because the tip of indentation instrument will wear out in the process of application. The uncalibrated nanoindentation will have a significant effect on the results of the test, especially at a lower depth of indentation. In this paper, the calibration model of nano indentation instrument is studied, and the new calibration model is established to calibrate the load factor, frame flexibility and tip area function in the calibration of nano indentation instrument. On the basis of calibration completion, the sapphire standard sample is determined. The standard sapphire sample can be used as the standard sample of nano indentation instrument, which can realize the accuracy, reliability and equivalent comparison of the measurement results of non nano indentation instrument. First of all, the calibration model of the load factor of the nano-indentation instrument is established, and the nano-indentation is tested by selecting 20 force values in the range of 0.5 mN-10 mn. The loading and unloading process is realized by using the weighing module of the electromagnetic force balance and the tip of the nano-indentation instrument, and the actual loading force is measured on the balance. For each loading process, a loading force is given by the nano-indentation instrument, and the two force values are fitted linearly. The slope of the fitted line is the load factor completed by calibration. After the calibration of the load factor calibration model, the indentation test shows that the hardness and elastic modulus of the standard fused quartz samples measured by the nano-indentation instrument after the load factor calibration are more accurate than those before calibration. On the basis of the load factor calibration, four calibration methods, AFM direct method and iterative method, are used to calibrate the flexibility and tip area function of nano-indentation machine frame. After calibration, the results of flexibility and area function of four calibration methods are applied to indentation test. The results are as follows: single crystal tungsten and fused quartz are iterated at shallow indentation depth of nano-indentation instrument. Compared with the other three quasi-calibration methods, the frame flexibility and area function obtained by the method are more accurate. When the indentation depth increases gradually, the area function and the frame flexibility obtained by the four calibration methods are close to the exact values. In transverse comparison, the calibration of frame flexibility by single crystal tungsten is better than that by fused quartz, and the calibration of the instrument by AFM direct method is much more accurate than that by indirect method at shallow indentation depth in the area function calibration. When the depth of penetration is below 60 nm, the accuracy of the test results is greatly affected by the radius of curvature of the tip. At the very shallow depth of penetration, more accurate test data can be obtained by using the tip with small radius of curvature of the needle. Finally, after calibrating the load factor and the optimal calibration model, the frame flexibility and area function are applied to the nano-indentation instrument. Using TriboIndenter-900 nano-indentation instrument, the uncertainty caused by uniformity, stability, repeatability of indentation experiment and the uncertainty brought by the instrument itself are analyzed and evaluated. The total synthetic uncertainty caused by the fixed value experiment is calculated; the expansion factor is determined and the extended uncertainty required for the fixed value is calculated; then the equivalent modulus and hardness of the sapphire standard sample candidate are determined.
【學(xué)位授予單位】：安徽工業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TH87;TQ164

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