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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有空再補啊，現(xiàn)在沒多余的時間了。 7.12 無意中遺留于標本表面的浸蝕液殘留物揮發(fā)出的氫氟酸會對顯微鏡物鏡造成毀壞。當標本或封片膠含有孔道結構或者墊層材料（如酚醛塑料）由于沒有緊固在標本上而產(chǎn)生邊緣滲漏時，這種情況尤為常見。因此， 任何情況下都應該特別注意在將標本置于鏡臺前均應對其進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（15）提供各種合金蝕刻解決方案和技術的補充建議。 8.精度和偏差 8.1.因為沒有進行定量測定，所以這種做法的精度或偏差無法詳細說明。 9.關鍵詞 9.1 刻蝕；蝕刻劑；干涉法；金相學；金屬；微蝕刻；微觀結構/顯微結構；Pepperhoff method（不知道是什么方法）；色調蝕刻 |
2樓2010-10-13 10:32:54
高興星期五
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3樓2010-10-13 20:15:05
高興星期五
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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 色調浸蝕液（9, 11-13)通常通過浸漬來使用而非涂刷，因為后者會阻礙膜的形成。待用的標本需要經(jīng)過非常高品質的拋光，因為色調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照明中是不可見的。標本拋光后，其表面必須仔細清洗。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）。用鉗子將標本置于溶液中，拋光面朝上。輕輕攪動溶液，同時觀察拋光表面。開始著色后，保持溶液靜止不動。當標本表面顯紫色時將其從浸蝕液中取出，沖洗，干燥。色調浸蝕之后再用一般的化學浸蝕液對標本進行輕微的預浸蝕，這樣會使標本的結構輪廓更清晰。 |
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
| 在進行氣相沉積制備干擾薄膜(“Pepperhoff”)前，樣品應該仔細清洗。少量的腐蝕液以及拋光粉的殘留都會導致沉積相成分上巨大的偏差。沉積應該在真空蒸發(fā)皿中進行，這種蒸發(fā)皿是那種用來制備電鏡復樣的儀器。對一個或多個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）顏色變化順序為: 黃色、綠色、紅色、淺紫色、深紫、藍色、銀藍色。當顏色變?yōu)闇\紫色到紫深時再停止增發(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 在進行氣相沉積制備干擾薄膜(“Pepperhoff”)前，樣品應該仔細清洗。少量的腐蝕液以及拋光粉的殘留都會導致沉積相成分上巨大的偏差。沉積應該在真空蒸發(fā)皿中進行，這種蒸發(fā)皿是那種用來制備電鏡復樣的儀器。對一個或多個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）顏色變化順序為: 黃色、綠色、紅色、淺紫色、深紫、藍色、銀藍色。當顏色變?yōu)闇\紫色到紫深時再停止增發(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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