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高兴星期五铁杆木虫 (著名写手)
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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(金币+1):谢谢参与 2010-10-13 17:51:57
高兴星期五(金币+80):非常感谢 2010-10-15 18:22:28
wypward(金币+1):谢谢参与 2010-10-13 17:51:57
高兴星期五(金币+80):非常感谢 2010-10-15 18:22:28
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参考。7.13和14有空再补啊，现在没多余的时间了。 7.12 无意中遗留于标本表面的浸蚀液残留物挥发出的氢氟酸会对显微镜物镜造成毁坏。当标本或封片胶含有孔道结构或者垫层材料（如酚醛塑料）由于没有紧固在标本上而产生边缘渗漏时，这种情况尤为常见。因此， 任何情况下都应该特别注意在将标本置于镜台前均应对其进行彻底清洗和干燥以清除其上浸蚀液的所有痕迹。 7.15金属手册（15）提供各种合金蚀刻解决方案和技术的补充建议。 8.精度和偏差 8.1.因为没有进行定量测定，所以这种做法的精度或偏差无法详细说明。 9.关键词 9.1 刻蚀；蚀刻剂；干涉法；金相学；金属；微蚀刻；微观结构/显微结构；Pepperhoff method（不知道是什么方法）；色调蚀刻 |
2楼2010-10-13 10:32:54
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3楼2010-10-13 20:15:05
高兴星期五
铁杆木虫 (著名写手)
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4楼2010-10-13 20:15:57
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wypward(金币+1):谢谢参与 2010-10-15 13:28:57
wypward(金币+1):谢谢参与 2010-10-15 13:28:57
| 7.13 色调浸蚀液（9, 11-13)通常通过浸渍来使用而非涂刷，因为后者会阻碍膜的形成。待用的标本需要经过非常高品质的抛光，因为色调浸蚀液能够显示出遗留下的抛光损伤，即使这种损伤在明视场照明中是不可见的。标本抛光后，其表面必须仔细清洗。用聚乙烯烧杯来盛含氟离子浸蚀液（如，含有氟化氢铵的浸蚀液，NH4 FHF）。用钳子将标本置于溶液中，抛光面朝上。轻轻搅动溶液，同时观察抛光表面。开始着色后，保持溶液静止不动。当标本表面显紫色时将其从浸蚀液中取出，冲洗，干燥。色调浸蚀之后再用一般的化学浸蚀液对标本进行轻微的预浸蚀，这样会使标本的结构轮廓更清晰。 |
5楼2010-10-14 09:25:38
高兴星期五(金币+120, 翻译EPI+1):非常感谢 2010-10-15 18:22:02
| 在进行气相沉积制备干扰薄膜(“Pepperhoff”)前，样品应该仔细清洗。少量的腐蚀液以及抛光粉的残留都会导致沉积相成分上巨大的偏差。沉积应该在真空蒸发皿中进行，这种蒸发皿是那种用来制备电镜复样的仪器。对一个或多个具备所需的折射率的合适的介电化合物小块体在真空条件下加热, 直到它蒸发。1.3 到0.013 Pa (10−3 到 10−5 mm Hg)的真空度是足够的，抛光面应该放置于低于装夹介电化合物的装置下10-15厘米的位置。慢慢蒸发块体并观察试样的表面。如果把样品放置于小片白纸上更好。随着薄膜厚度增加，样品表面（纸面）颜色变化顺序为: 黄色、绿色、红色、浅紫色、深紫、蓝色、银蓝色。当颜色变为浅紫色到紫深时再停止增发。虽然在某些情况下, 绿色或红颜色更薄的薄膜产生良好的效果 |
6楼2010-10-14 17:46:24
| 7.14 在进行气相沉积制备干扰薄膜(“Pepperhoff”)前，样品应该仔细清洗。少量的腐蚀液以及抛光粉的残留都会导致沉积相成分上巨大的偏差。沉积应该在真空蒸发皿中进行，这种蒸发皿是那种用来制备电镜复样的仪器。对一个或多个具备所需的折射率的合适的介电化合物小块体在真空条件下加热, 直到它蒸发。1.3 到0.013 Pa (10−3 到 10−5 mm Hg)的真空度是足够的，抛光面应该放置于低于装夹介电化合物的装置下10-15厘米的位置。慢慢蒸发块体并观察试样的表面。如果把样品放置于小片白纸上更好。随着薄膜厚度增加，样品表面（纸面）颜色变化顺序为: 黄色、绿色、红色、浅紫色、深紫、蓝色、银蓝色。当颜色变为浅紫色到紫深时再停止增发。虽然在某些情况下, 绿色或红颜色更薄的薄膜产生良好的效果 |
7楼2010-10-14 17:46:50