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1、27rp1 硝酸蒸汽测试方法硝酸蒸汽测试方法 1. TEST METHOD 试验方法试验方法 The nitric acid used in this test is a strong acid and special caution should be taken. Read Material Safety Data Sheet before starting the test. The test is done in a fume hood. Suitable protective cloths, gloves and eye protection must be used. During

2、 the whole test process, particular caution is required for contact areas in sample handling, avoiding any touching/scratching by hands and tools. 用在该项试验中的硝酸是一种强酸性,应特别警示。试验前阅读 MSDS。 这项试验在一个通风橱中进行。必须穿防护衣服/手套/保护眼睛器具。 在整个试验过程中,尤其要注意样品处理时与地面接触区域的警示,避免接触及划伤。 1.1 Test Equipment and Chemicals 试验设备试验设备/药品药品

3、 Below is a list of equipment needed to perform the test: 清单 2 x vacuum desiccators with ground joint and tap (e.g. Model Novus, Schott NS24/ id. 250 mm) 2 个带磨口连接和活栓的干燥器 Dessiccant, Blue Silica Gel 干的/蓝硅胶 Sample holder made of inert material (e.g. PTFE / Teflon) Nitric acid, reagent grade, concentra

4、ted (692%) HNO3, relative density (20C) 1.39 to 1.42 硝酸,试剂等级,浓缩(692%) HNO3,相对密度(20C) 1.39 to 1.42 g/cm3. Read Material Safety Data Sheet before starting the test! 试验前阅读试验前阅读 MSDS Density hydrometer (e.g. Widder, scale 1.00- 1.50) 密度液体比重计(如,方,刻度 1.00- 1.50) Graduated glass (cylinder) 500 ml 有刻度的玻璃杯(圆

5、柱形)500 ml Glass funnel 玻璃漏斗 Timer (alarm clock) 计时器(闹钟) Oven for drying the tested samples 27rp2 烘箱 Microscope for analyzing samples 显微镜 oOptical microscopes (Stereo/metallurgical microscope) 光学显微镜 oSEM, Scanning electron microscope 标准电子块,扫描电子显微镜 Protective Gloves (e.g. nitrile-base) 保护手套 Safety gog

6、gles 防护眼镜 NaHCO3 to neutralization splashes form table or floor (in case of accident). For skin use tap water to dilute acid splashes. (若发生事故)用 NaHCO3 中和台面和地面的喷着 点,若滴落皮肤上,用自来水稀释酸的喷着点 NaHCO3, Fume hood 通风橱 1.2 Test setup Figure 1. Graduated glass cylinder, nitric acid bottle and test chamber in the f

7、ume hood. 图一,带刻度的玻璃杯,硝酸瓶,通风橱控制下的试验区 The following procedure is performed in a fume hood. The test is done in the fume hood. Measure 500 ml Nitic acid with the glass cylinder and pour it carefully into the empty and clean dessicator. Close the lid and let the test vessel stabilitze for atleast 30 min

8、utes. 下面的试验要在通风橱内进行.将装有 500 ml 的硝酸小心倒入空的/干净的干燥器中,盖上盖子, 将测试器具旋转至少 30 分钟以上. 27rp3 Figure 2. Samples prepared for the test and fixed hanging on the sample holder. 图 2.准备好测试用样品并将其固定在样品固定器上. Depending on the samples different methods for attaching the samples may be required, e.g. sample jigs. In the fig

9、ure two connector samples are attached to each other with a soldered wire. This makes it possible to hang the samples in the desiccators on a sample holder. 根据样品的不同采用用不同的试验方法.,例如用夹具.在图二中,两个连接器用一根焊接线连接在 一起,这样做可以将在一个样品固定器同一干燥器里的样品挂起. 27rp4 Figure 3. Samples are hanging on the sample holder in the desi

10、ccators. 图 3.挂在在干燥器里样品固定器上的样品。 In the figure the tested samples are hanging on the sample holder. 图中被试验的样品挂在样品固定器上。 Figure 4. The fume hood door is kept closed during the test. 图 4 试验中通风橱的门要保持关闭状态。 27rp5 Figure 5. The tested samples are removed from the chamber and put on a glass plate 图 5 将被试验的样品从试

11、验区移出放置在玻璃器皿中。 Figure 6. The tested samples are put into the oven for drying at 80 C for 60 minutes. 27rp6 图 6 被试验的样品放入烘箱 80 度烘烤 60 分钟。 2. ANALYSIS OF TESTED SAMPLES 样品分析样品分析 The dryed and cooled samples are analyzed using optical (stereo microscope/metallurgical microscope) microscopes or scanning e

12、lectron microscope (SEM). Images of the tested connector springs are imaged and the images are saved. These images are compared with respective gauge and are given a score according to the gauge scale. 风干/冷却后的样品使用光学显微镜或扫描电子显微镜进行分析。这些图像选用不同测量仪进行 对比及记录。 2.1 Optical gauge 光学测量仪光学测量仪 This optical gauge

13、is imaged with a Hirox KH-3000 stereo microscope. 这个光学测量仪与 Hirox KH-3000 立体显微镜很相似。 Figure 7. Optical gauge with scores 0, 1 and 2. 图 7 光学测量仪 0-2 Figure 8. Old optical gauge with scores 0-5. 图 8 老的光学测量仪 0-5 2.2 Scanning Electron Microscope (SEM) gauge 扫描电子显微镜扫描电子显微镜 测量测量 3.2 扫描电子显微镜 This SEM gauge is

14、 imaged with a FEI-FEG ESEM Electron Scanning Microscope in LowVac Mode. 扫描电子显微镜与 FEI-FEG ESEM 的电子扫描显微镜极为相似. 0 1 2 3 4 5 012 27rp7 Figure 9. SEM gauge with scores 0, 1 and 2. 图九 SEM 下的图 0-2 Figure 10. Old SEM gauge with scores 0-5. 图 10 老式 SEM 下的图 0-5 2.3 Requirements and acceptance criteria 要求和接收标准

15、要求和接收标准 2.3.1 Requirements 要求 Minimum sample amount is 6 connectors. The plating strips of contacts can also be used and the minimum amount of contacts is 6 times the number of pins per connector. All samples should be tested at same time. 最少的样品量为 6 个连接器。电镀条片的接触,也可用于及最低数额的接触是 6 倍的数量每引 脚连接器。所有样品应在同一时

16、间进行检验。 The examination and records are applied to the critical area of individual contact. The definition of critical area of contacts is decribed in Appendix I. 检查和记录,是适用于临界区域的个别接触。定义中的关键领域进行接触,是描述在附录一。 Recommandation for the magnifications used for optical microscope observation is described in Ap

17、pendix II. 建议使用倍率光学显微镜进行检验,见附录二描述。 2.3.2 Acceptance criteria 验收标准 The score for the tested sample is got by comparing the microscope image of the tested sample with the gauge, Figure 7-Figure 10. 通过不同的显微镜进行样品对比,得出不同的测试结果。图 7 -图 10 。 0 1 2 3 4 5 012 27rp8 More information for the criteria is describe

18、d in Appendix III. 关于标准的更多信息见描述。 Table 1. Score, Result and Actions ScoreResultActions 0Accepted 接受- 1Accepted with actions 整改后接受 Action plan needs to be created by supplier and sent to Nokia which includes:整改计划包括下面几方面,由 供应商制作完成后送交 NOKIA。 Actions for root cause analysis 原因分析 Time schedule 时间表 Correc

19、tion needs to be implemented according root cause analysis 根据原因分析执行整改措施 Improved samples need to be delivered to Nokia for testing and analysing.改进后的样品送交 NOKIA 作测试 及分析。 2Rejected 不合格Nokia may issue a hold on further delivery or request a statistic analysis Action plan needs to be created by supplier

20、 and sent to Nokia which includes: 整改计划包括下面几方面,由 供应商制作完成后送交 NOKIA。 Actions for root cause analysis 原因分析 Time schedule 时间表 Correction needs to be implemented according root cause analysis 根据原因分析执行整改措施 Improved samples need to be delivered to Nokia for testing and analysing. 改进后的样品送交 NOKIA 作测 试及分析。 2.

21、3.3 Result evaluation Observation/examination need to be carried out for all contacts under the test. The scores for all contacts under test should be recorded in the report. 试验中所以接触点都要做检查及测试,并记录测试结果。 Depending on the test results, a statistic analysis may be requested. 应根据检查结果做出统计分析。 The requiremen

22、ts and procedures for statistic analysis are documented separately. 与统计分析相关的证明报告需单独列出来。 27rp9 3. MAINTENANCE 维护维护 Remove the sample holder from the test vessel after the test and wash it using water. The Nitric acid can be stored in the vessel. If the vapor in the test vessel is turned into brown or

23、 red-brown the lid needs to be opened to let the dark colored vapor out from the vessel. Close the lid again when the chamber looks clear. Note that the lid needs to be closed 30 minutes before a new test can start. A too warm test solution makes the vapour change color. After every two weeks the te

24、st solution is poured back to 500 ml graduated glass. Amount of nitric acid is checked and added up to 500 ml if need. Density of acid must check using density hydrometer. After every three months the whole test solution must be change. Disposals of HNO3 waste need to be done according to local lega

25、l instructions. The test solution must be changed immediately if any of the samples falls into the acid. The test solution must be changed immediately if any visual color change of the acid solution occurs. 试验的将样品固定器从试验器皿中移出来,水洗干净。 硝酸可将之储存在试验器皿上。 如果蒸气在试验容器变成褐色或红褐色,需要将盖子打开,让深色汽从试验器皿散出。当试验区 变得清晰些的时候再将

26、盖子盖上。需要注意的是,要将盖子关闭三十分钟后,才可开始一项新的 实验。太热的试验溶液,将使汽体变色。 每两个星期做的试验,是将溶液倒入有刻度的 500 毫升的玻璃瓶中。检查硝酸的容量,若需要要 加至 500 毫升,酸的密度必须使用密度比重计进行检查。 每 3 个月,试验用的溶液必须更换。硝酸废物的处理,必须按照当地的法律指示执行。 当样品落入酸里时,试验用的溶液必须更换。 如果酸溶液里能够看到气体变色,试验用的溶液必须更换。 4. PROCESS 4.1 Sample preparation 准备样品准备样品 The type of sample needs to be taken into

27、 account when the samples are prepared for the test. The surfaces objected to the tests need to be undamaged and untouched. The samples need to be fixed in the test vessel. One option is to hang the samples using acid proof material like PTFE. One easy solution is to connect two connectors by solder

28、in a short wire (5-10 cm) between two legs. Wet cleaning is not recommended since it will affect the test results. External solid depositions on contact surface can be removed by compressed air. 准备试验时,必须考虑到样品类型满足试验需要。样品表面需保持完好并原封不动。样品必须 固定在试验容器里。一种选择是像如聚四氟乙烯一样使用耐酸材料将样品挂上。一个简单的办 法是通过焊焊接的方式将两个连接器样品之间的

29、两条腿用一条小金属线( 5-10 厘米)连接上。 27rp10 不建议湿洗,因为它会影响测试结果。接触面的表面固体沉积,可由压缩空气去除。 Figure 11. Connector samples connected together by soldering a short wire between two legs of the connectors to make it easy to hang the samples in the test vessel. 图 11 通过焊接的方式将两个连接器样品之间的两条腿用一条小金属线( 5-10 厘米)连接上。 4.2 Test chamber

30、preparation 试验区准备试验区准备 Use a clean and completely dry vacuum dessicator. Keep the dessicator in the fume hood. Measure 500 ml fresh HNO3 in a graduated glass cylinder and poor it carefully into the vacuum dessicator. Close the lid and let the test chamber stabilize for at least 30 min. 使用清洁和完全干燥的真空干

31、燥器 。将干燥器放在抽风橱中。将 500 ml 的新的 HNO3 小心倒 入真空干燥器中,盖上盖子,保持稳定状态放置至少 30 分钟。 4.3 Testing 试验试验 Insert the samples using suitable fixture 将样品放入合适的装置中 Close the cover and start the timer. There are two testing durations according to the thickness of the plating. 1h exposure: used for the Au plating (including P

32、d-Ni) thickness = 0.2 micrometer Remove the samples from the test vessel and place them on a glass plate. Dry the samples on the glass plate in an oven for 60 minutes at 80C Put the dried samples in a dessicator with active dessicant to cool down to room temperature for 15 minutes. 密切封面,并开始计时。根据厚度的镀层做两个试验。 27rp11 暴露 1 小时:用于镀金(包括钯镍)厚度= 0.2 微米 将样品从试验容器里拿出来,放在一个玻璃盘上。 将样品放在烘

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