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高興星期五鐵桿木蟲 (著名寫手)
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7.12 Microscope objectives can be ruined by exposure to hydrofluoric acid fumes from etchant residue inadvertently left on the specimen. This problem is very common when the specimen or mounting media contain porosity and when the mounting material (such as Bakelite) does not bond tightly to the specimen resulting in seepage along the edges of the specimen. In all cases, extreme care should be taken to remove all traces of the etchant by thorough washing and complete drying of the specimen before placing it on the microscope stage. 7.13 Tint etchants (9, 11-13) are always used by immersion,never by swabbing, as this would inhibit film formation. An extremely high quality polish is required as tint etchants will reveal remaining polishing damage even if it is not visible with bright field illumination. After polishing, the surface must be carefully cleaned. Use a polyethylene beaker to contain the etchant if it contains fluorine ions (for example, etchants containing ammonium bifluoride, NH4 FHF). The specimen is placed in the solution using tongs, polished face up. Gently agitate the solution while observing the polished surface. After coloration begins, allow the solution to settle and remain motionless. Remove the specimen from the etchant when the surface is colored violet, rinse and dry. A light pre-etch with a general-purpose chemical etchant may lead to sharper delineation of the structure after tint etching. 7.14 Specimens should be carefully cleaned before use of a vapor-deposition interference film (“Pepperhoff”) method (9,11-14). A light pre-etch, or a slight amount of polishing relief, may lead to sharper delination of the constituents after vapor deposition. The deposition is conducted inside a vacuum evaporator of the type used to prepare replicas for electron microscopy. One or several small lumps of a suitable dielectric compound with the desired index of refraction is heated under a vacuum until it evaporates. A vacuum level of 1.3 to 0.013 Pa (10−3 to 10−5 mm Hg) is adequate and the polished surface should be about 10–15 cm beneath the device that holds the dielectric compound. Slowly evaporate the lumps and observe the surface of the specimen. It may be helpful to place the specimen on a small piece of white paper. As the film thickness increases, the surface (and the paper) will become colored with the color sequence changing in the order yellow, green, red, purple, violet, blue, silvery blue. Stop the evaporation when the color is purple to violet, although in some cases, thinner films with green or red colors have produced good results. 7.15 Metals Handbook (15) provides additional advice on etching solutions and techniques for various alloys. 8. Precision and Bias 8.1 It is not possible to specify the precision or bias of this practice since quantitative measurements are not made. 9. Keywords 9.1 etch; etchant; interference method; metallography; metals; microetch; microscope; microstructure; Pepperhoff method; tint etch |
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wypward(金幣+1):謝謝參與 2010-10-13 17:51:57
高興星期五(金幣+80):非常感謝 2010-10-15 18:22:28
wypward(金幣+1):謝謝參與 2010-10-13 17:51:57
高興星期五(金幣+80):非常感謝 2010-10-15 18:22:28
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參考。7.13和14有空再補(bǔ)啊，現(xiàn)在沒多余的時(shí)間了。 7.12 無意中遺留于標(biāo)本表面的浸蝕液殘留物揮發(fā)出的氫氟酸會(huì)對(duì)顯微鏡物鏡造成毀壞。當(dāng)標(biāo)本或封片膠含有孔道結(jié)構(gòu)或者墊層材料（如酚醛塑料）由于沒有緊固在標(biāo)本上而產(chǎn)生邊緣滲漏時(shí)，這種情況尤為常見。因此， 任何情況下都應(yīng)該特別注意在將標(biāo)本置于鏡臺(tái)前均應(yīng)對(duì)其進(jìn)行徹底清洗和干燥以清除其上浸蝕液的所有痕跡。 7.15金屬手冊(cè)（15）提供各種合金蝕刻解決方案和技術(shù)的補(bǔ)充建議。 8.精度和偏差 8.1.因?yàn)闆]有進(jìn)行定量測(cè)定，所以這種做法的精度或偏差無法詳細(xì)說明。 9.關(guān)鍵詞 9.1 刻蝕；蝕刻劑；干涉法；金相學(xué)；金屬；微蝕刻；微觀結(jié)構(gòu)/顯微結(jié)構(gòu)；Pepperhoff method（不知道是什么方法）；色調(diào)蝕刻 |
2樓2010-10-13 10:32:54
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3樓2010-10-13 20:15:05
高興星期五
鐵桿木蟲 (著名寫手)
- 應(yīng)助: 0 (幼兒園)
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4樓2010-10-13 20:15:57
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wypward(金幣+1):謝謝參與 2010-10-15 13:28:57
wypward(金幣+1):謝謝參與 2010-10-15 13:28:57
| 7.13 色調(diào)浸蝕液（9, 11-13)通常通過浸漬來使用而非涂刷，因?yàn)楹笳邥?huì)阻礙膜的形成。待用的標(biāo)本需要經(jīng)過非常高品質(zhì)的拋光，因?yàn)樯{(diào)浸蝕液能夠顯示出遺留下的拋光損傷，即使這種損傷在明視場(chǎng)照明中是不可見的。標(biāo)本拋光后，其表面必須仔細(xì)清洗。用聚乙烯燒杯來盛含氟離子浸蝕液（如，含有氟化氫銨的浸蝕液，NH4 FHF）。用鉗子將標(biāo)本置于溶液中，拋光面朝上。輕輕攪動(dòng)溶液，同時(shí)觀察拋光表面。開始著色后，保持溶液靜止不動(dòng)。當(dāng)標(biāo)本表面顯紫色時(shí)將其從浸蝕液中取出，沖洗，干燥。色調(diào)浸蝕之后再用一般的化學(xué)浸蝕液對(duì)標(biāo)本進(jìn)行輕微的預(yù)浸蝕，這樣會(huì)使標(biāo)本的結(jié)構(gòu)輪廓更清晰。 |
5樓2010-10-14 09:25:38
高興星期五(金幣+120, 翻譯EPI+1):非常感謝 2010-10-15 18:22:02
| 在進(jìn)行氣相沉積制備干擾薄膜(“Pepperhoff”)前，樣品應(yīng)該仔細(xì)清洗。少量的腐蝕液以及拋光粉的殘留都會(huì)導(dǎo)致沉積相成分上巨大的偏差。沉積應(yīng)該在真空蒸發(fā)皿中進(jìn)行，這種蒸發(fā)皿是那種用來制備電鏡復(fù)樣的儀器。對(duì)一個(gè)或多個(gè)具備所需的折射率的合適的介電化合物小塊體在真空條件下加熱, 直到它蒸發(fā)。1.3 到0.013 Pa (10−3 到 10−5 mm Hg)的真空度是足夠的，拋光面應(yīng)該放置于低于裝夾介電化合物的裝置下10-15厘米的位置。慢慢蒸發(fā)塊體并觀察試樣的表面。如果把樣品放置于小片白紙上更好。隨著薄膜厚度增加，樣品表面（紙面）顏色變化順序?yàn)? 黃色、綠色、紅色、淺紫色、深紫、藍(lán)色、銀藍(lán)色。當(dāng)顏色變?yōu)闇\紫色到紫深時(shí)再停止增發(fā)。雖然在某些情況下, 綠色或紅顏色更薄的薄膜產(chǎn)生良好的效果 |
6樓2010-10-14 17:46:24
| 7.14 在進(jìn)行氣相沉積制備干擾薄膜(“Pepperhoff”)前，樣品應(yīng)該仔細(xì)清洗。少量的腐蝕液以及拋光粉的殘留都會(huì)導(dǎo)致沉積相成分上巨大的偏差。沉積應(yīng)該在真空蒸發(fā)皿中進(jìn)行，這種蒸發(fā)皿是那種用來制備電鏡復(fù)樣的儀器。對(duì)一個(gè)或多個(gè)具備所需的折射率的合適的介電化合物小塊體在真空條件下加熱, 直到它蒸發(fā)。1.3 到0.013 Pa (10−3 到 10−5 mm Hg)的真空度是足夠的，拋光面應(yīng)該放置于低于裝夾介電化合物的裝置下10-15厘米的位置。慢慢蒸發(fā)塊體并觀察試樣的表面。如果把樣品放置于小片白紙上更好。隨著薄膜厚度增加，樣品表面（紙面）顏色變化順序?yàn)? 黃色、綠色、紅色、淺紫色、深紫、藍(lán)色、銀藍(lán)色。當(dāng)顏色變?yōu)闇\紫色到紫深時(shí)再停止增發(fā)。雖然在某些情況下, 綠色或紅顏色更薄的薄膜產(chǎn)生良好的效果 |
7樓2010-10-14 17:46:50
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