• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    This invention belongs to the technical field of sample preparation with the transmission electron microscope (TEM). In particular, it relates to a method of preparing a sample of powder particles with the transmission electron microscope. The invention provides a method of preparing a sample of powder particles with the transmission electron microscope to overcome the problems to be solved in the prior art, such as the complicated process, the small thin area of the TEM sample preparation, and the high cost of the sample preparation. In order to achieve the above-mentioned purpose, the solution provided by the present invention is: Obtaining the TEM sample with thinner areas by placing powder particles in a non-magnetic support foam structure for further ion dilution. The method is simple and easy to perform, the cost is low, and the TEM powder samples with thinner areas can be obtained. The invention is applicable to various conventional particles and the particle size is on the order of submicron, micron or submillimeter; At the same time, the invention is generally applicable and is not only suitable for metal particles, but also for non-metal particles.
    公开号:BE1027467B1
    申请号:E20205010
    申请日:2020-01-08
    公开日:2021-06-01
    发明作者:Chongfeng Sun；Shengqi Xi；Jianping Li；Yongchun Guo；Zhong Yang；Ruihua Zhu；Yaping Bai；Yuan Gao
    申请人:Univ Xian Technological；Univ Xi An Jiaotong；
    IPC主号:
    专利说明:

    [0001] Technical field: This invention belongs to the technical field of sample preparation with the transmission electron microscope (TEM). In particular, it relates to a method of preparing a sample of powder particles with the transmission electron microscope.
    [0002] Background Technology: Transmission electron microscopy is more widely used in scientific research fields such as materials science and engineering, etc. TEM sample preparation plays a very important role as technical support in research work of metal electron microscopy. Since electrons can easily be scattered or absorbed by the object and due to the properties of low penetration force when passing through the TEM sample, the thickness of the sample could significantly influence the imaging quality of the TEM sample. A good film sample must first be prepared in order to achieve a satisfactory TEM observation effect. The prerequisite for effective TEM observation (especially observation with high-resolution transmission electron microscope-HRTEM) is therefore the achievement of an ultra-thin area with a large area on a TEM sample. (The thickness of the thin area below 100 nm).
    [0003] According to the shape and size of the material sample, the sample can be in block materials, nanomaterials (nanofilms, nanowires and nanoparticles) and conventional powder materials (powder particle size on a scale of
    [0004] In addition to the powder preparation technique for TEM-F samples of powder materials at present, the powder particles can additionally be embedded with organic matter such as resin and the embedded powders are further processed by ion dilution process step; Alternatively, the powder particles can be chemically or electroplated and those with sample powder particles! embedded films are further processed by ion dilution. Finally, with the above two methods, thin area with a certain thickness can be obtained. However, both of these methods have their own shortcomings. First, the resin material and the powder particles, particularly, the wettability of the inorganic non-metal and metal particles is poor, resulting in poor interfacial strength between powder particles and resin and even a large crack therebetween. Poor interfacial strength and cracks between the particles and the resin matrix could lead to easy falling off around the ion-reduced holes {i.e. around
    [0005] Summary of the Invention: The invention provides the method of preparing a sample of powder particles with the transmission electron microscope in order to overcome the problems of complicated procedures, many factors and high cost in the prior art.
    [0006] In order to achieve the above purposes, the solution provided by the present invention is: A preparation method of a sample of powder particles with the transmission electron microscope includes the following
    [0007] In step 5), the thickness of the sheets is 20 µm to 50 µm.
    [0008] In step 1} the support foam structure is foam copper or foam nickel lattice
    [0009] Compared to the prior art, the advantages of the present invention are:
    [0010] 2. Compared to conventional powder preparation, the method adds the process of ion dilution. For particles other than the nanometer scale, better thin areas can only be obtained by ion dilution. It is difficult for the TEM observation to collect the powder directly.
    [0011] 3. The preparatory process of the method is simple and the equipments used are also general, therefore the production costs are low.
    [0012] 4. The invention is applicable to various conventional particles and the particle size is on the submicron, micron or submillimeter scale. The invention is of general validity and is suitable not only for metal particles but also for non-metal particles.
    [0013] Description of the images: Image 1 is a TEM photo in the conventional powder preparation; Figure 2 is a TEM photo in the process of this invention; Image 3 is HRTEM photo in the process of this invention;
    [0014] Specific implementation: The invention will now be described in detail in connection with the drawings and embodiments.
    [0015] Example 1: A method of preparing a sample of powder particles with the transmission electron microscope comprises the following steps: 1) Selects a foamed copper structure with the pore size according to the particle size of the powder particles slightly larger than the average particle size. (Note: In TEM observation, magnetic samples cause electron beam scattering, which makes the TEM image sharpness worse.) The thickness of the foam grid is 1 mm, and a foam grid with an area of 5x% 5 mm is used (after completion, can at least one TEM sample with a diameter of 3 mm can be obtained); 2) Take small sample powder with cotton swab and distribute it evenly on the foam grid, the thickness of the powder layer being 1/4 the thickness of the foam grid; 3) If the foam grid with a small amount of sample powder is placed on the platform, knock the platform with suitable force so that the powder particles not only gradually seep into the holes in the foam grid, but at the same time do not allow them to scatter onto any platform other than the foam grid; 4) Lightly take the foam mesh with powder particles inlaid in it with tweezers, place it on the hydraulic clamp, apply pressure of 50 MPa to it and
    [0016] Example 2: A method of preparing a sample of powder particles with the transmission electron microscope includes {following steps: 1} Selects a foamed copper structure having the pore size according to the particle size of the powder particles which is slightly larger than the average particle size. (Note: In TEM observation, magnetic samples lead to electron beam scattering, which makes the TEM image sharpness worse.) The thickness of the foam grating is 0.5 mm, and a foam grating with an area of 5x5 mm is used; 2) Take small sample powder with cotton swab and distribute it evenly on the foam grid, the thickness of the powder layer being 1/4 the thickness of the foam grid; 3) If the foam grid with a small amount of sample powder is placed on the platform, the platform knocks with suitable force so that the powder particles not only gradually seep into the holes in the foam grid, and at the same time not onto any platform other than the foam grid
    [0017] The cbige example 1 is a preferred embodiment. It can be determined through experiments, with reference to Fig. 1, for the powder particles with a larger particle size, the conventional powder method acquires very few thin areas of TEM sample, and the bright field image obtained is not clear to perform operation with a high-resolution transmission electron microscope (HRTEM) ; Using the method of the present invention, the TEM photograph as shown in Figure 2 is obtained. It shows that the sample of the method after insertion - mechanical thinning - ion thinning - larger thin areas of the powder particles and clear TEM brightfield image are obtained, at the same time a further clear HRTEM observation can be carried out as in the picture. 3 shows.
    权利要求:
    Claims (2)
    [1]
    1. The preparation method of a sample of powder particles with the transmission electron microscope, which is characterized by the following steps: Step 1) Selects a non-magnetic support foam structure with an average pore size according to the particle size of the powder particles, which is slightly larger than the average particle size, the thickness of the foam metal grid is 0.1 mm to 1 mm. Shears a square foam grid that is at least a 3mm diameter area available; Step 2) Take small sample powders and distribute them evenly on the foam grid, the thickness of the powder layer preferably being 1 / 5-1 / 4 the thickness of the foam grid; Step 3) Place the foam grid on the platform, tap or shake the platform so that the powder particles gradually seep into the holes of the foam grid; Step 4) Take the foam grid with the powder particles inserted in it lightly with a pair of tweezers and smooth the foam grid under pressure; Step 5) sand the compressed foam grid on a sandpaper to get thin sheets; Step 6) Put the sheets in the TEM sample perforator to get round sheets; Step 7) Process the round sheets with ion dilution process step to get a TEM sample with larger thin areas.
    [2]
    2. The method of preparing a sample of powder particles with the transmission electron microscope according to claim 1 is characterized by that in step 5) that the thickness of the sheets is 20 µm to 50 µm.
    10 a. The preparation process of a sample of powder particles with the transmission electron microscope according to claim 1 or 2 is characterized in step 1) that the support foam structure is foam copper or foam nickel lattice.
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    同族专利:
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    CN110487823B|2021-11-09|
    BE1027467A1|2021-02-22|
    ZA201908294B|2020-05-27|
    CN110487823A|2019-11-22|
    引用文献:
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    法律状态:
    2021-07-15| FG| Patent granted|Effective date: 20210601 |
    优先权:
    申请号 | 申请日 | 专利标题
    CN201910743711.0A|CN110487823B|2019-08-13|2019-08-13|Preparation method of powder particle transmission electron microscope sample|
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