日立台式扫描电镜TM4000的使用注意事项

可在样品仓内加装光学相机来拍摄照片，

以往通过经验寻找目标位置，现在可在显示屏上直接操作。在拍摄SEM图像时，由于TM4000和TM4000Plus配置双轴马达，原来需手动调整的操作，现在只需在显示器上选择要观察的位置即可。

寻找目标位置：指确认正在观察的样品位置和寻找要观察的样品位置的操作。一般情况下，电子显微镜放大倍率较高，不仅仅需要观察局部图像，还要观察整体的图像。

*2双轴马达台：根据操作人员的观察需求，可自动将样品移动到SEM图像拍摄位置的装置。

在确认拍摄的SEM图像时，由于SEM图像放大倍率高，找到所有SEM图像的观察位置需要花费一定时间。而这种机型可使用软件将低倍率和高倍率SEM图像的位置关系进行关联，并将结果显示在显示器上，使各图像的位置更为直观。

烧结试样的 SEM 分析采用日本日立公司生产的 S-520 扫描电子显微镜完成。首先将试样的新鲜断裂面在 IB-3 离子溅射渡膜仪中喷渡厚度约为 10 ～20 nm 的金，对结构致密的部分试样断裂面采用 40%浓度的氢氟酸 ( HF) 侵蚀 20min 后进行镀金，然后放入 SEM样品室内进行观察，电子枪电压采用 20kV，电子束流为 150 mA，并用照相方式记录样品的二次电子图像 ( 或称之为形貌像) 。

帖子看到晚了一点，抱歉，翻译绝对专业，楼主一看就清楚了。

First, fine BaTi2O5 powders were made by a sol–gel method. Ba(OC2H5)2 and Ti[OCH(CH3)2]4 with a molar ratio of 1 : 2 were mixed in a solution of methanol and 2-methoxyethanol in a glove box with N2 gas flow. 首先用溶胶－凝胶制备微细的BaTi2O5粉末。将摩尔比为1：2的Ba(OC2H5)2 和Ti[OCH(CH3)2]4在甲醇和2甲氧基乙醇的溶液中混合，这在通氮气流的手套操作箱中进行。 The yellow clear solution obtained was put into a cool-stirrer (CSB-900 N) and was cooled to 0 ◦C to form a colorless transparent sol. 将得到的黄色清澈的溶液放进一个冷却搅拌器（CSB－900N）中，并冷却到0℃，从而形成一种无色透明的溶胶。Then it was sprayed with water for hydrolysis while being stirred until it became a transparent gel with a high viscosity. 然后将溶胶用水喷淋进行水解，同时进行搅拌，直至溶胶变成高粘度的透明凝胶为止。After it was aged at 50 ◦C for 24 h, we obtained a dark-yellow amorphous precursor which was subsequently pulverized, ground, and calcined twice, at 650 ◦C for 12 h andat 1000 ◦Cfor2 h, respectively. 在经过50℃下24h的老化后，我们就得到了一种暗黄色的无定形前驱体，它随后被粉碎、研磨和煅烧两次，分别在650℃下煅烧12h，和在1000℃下煅烧2h。As a consequence, white powders of BaTi2O5 with a size ranging from 20 nm to 200 nm were obtained. KF-doped BaTi2O5 ceramics were synthesized by solid state

reaction of mixed KF (Merck, 99%) and the above sol–gel-derived BaTi2O5 powders. 结果，得到了尺寸范围从20nm到200nm的BaTi2O5白色粉末。掺杂KF的BaTi2O5陶瓷用混合的KF（Merck公司，99％）和上面的溶胶－凝胶衍生的BaTi2O5粉末进行固态反应而合成。According to Shannon ionic radii values [10] and charge neutrality requirements, the chemical formula should be Ba1−xKxTi2O5−xFx . 根据香农离子半径值[10]和电荷中性要求，化学方程式应该为Ba1−xKxTi2O5−xFx 。Several compositions were made in this study: x = 0, 0.01, 0.02, 0.05, 0.097, and 0.24. 在本研究中制备了好几种组分：x = 0,0.01, 0.02, 0.05, 0.097, 和 0.24。The mixed powders were ground in ethanol and dried, then pressed into pellets with a uniaxial pressure around 300 MPa, and sintered at 1150 ◦C for 2 h in air.这种混合的粉末在乙醇中研磨，并干燥，然后用大约300MPa的单轴压力加压成小颗粒，并在1150℃下于空气中烧结2h。The phase purity was checked by XRD analysis using a Rigaku RINT2000 diffractometer with Cu Kα1 radiation. 用采用Cu Ka1辐射的Rigaku RINT2000衍射仪进行XRD（X射线衍射）分析，检验相纯度。The data were collected in step-scan mode with a step angle of 0.01◦ and a sampling time of 2 s. 用步进扫描方式采集数据，步进角度为0.01°，采样时间为2s。Microstructure observation was performed with a Hitachi S-3000N scanning electron microscope (SEM). Chemical composition was checked by electron probe microanalysis (EPMA). 用Hitachi（日立）S-3000N扫描电子显微镜（SEM）进行微结构观察。用电子探针微分析（EPMA）检验化学组分。The density of ceramic samples was calculated by measuring the thickness, diameter and weight of the pellets. 陶瓷样本的密度通过测量小颗粒的厚度、直径和重量加以计算。Dielectric measurements were carried out with HP 4284A and HP 4285A LCR meters over a frequency range of 100 Hz–10MHz and over a temperature range of room temperature to ∼ 560 ◦C. We used silver electrodes with gold lead wires which were fired at 500 ◦C. 用HP 4284A and HP 4285A万能表（LCR meter）在100Hz～10MHz频率范围和室温到560℃的温度范围联系了电介质测量。我们采用了带金引线的银电极，它们被在500℃下加以燃烧。

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