WO2023087474A1 - Preparation device and method for powder sample - Google Patents

Preparation device and method for powder sample Download PDF

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Publication number
WO2023087474A1
WO2023087474A1 PCT/CN2021/139549 CN2021139549W WO2023087474A1 WO 2023087474 A1 WO2023087474 A1 WO 2023087474A1 CN 2021139549 W CN2021139549 W CN 2021139549W WO 2023087474 A1 WO2023087474 A1 WO 2023087474A1
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WIPO (PCT)
Prior art keywords
tank
grid
sample
carrying
powder sample
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PCT/CN2021/139549
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French (fr)
Chinese (zh)
Inventor
王彤彤
刘雪涛
李子依
王永康
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深圳晶泰科技有限公司
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Publication of WO2023087474A1 publication Critical patent/WO2023087474A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G01N23/2005Preparation of powder samples therefor

Definitions

  • the application belongs to the technical field of microcrystal electron diffraction testing, and in particular relates to a powder sample preparation device and method.
  • Microcrystal Electron Diffraction (Microcrystal Electron Diffraction, MicroED) needs to continuously rotate crystal particles with a size of 0.2 to 2 microns at a certain angle under the electron beam in a transmission electron microscope, and collect a series of electron diffraction data at different angles at the same time. Analyze the molecular structure of the crystal. Therefore, the MicroED test needs to uniformly disperse micron or even nanometer-sized crystal particles on a 3.05mm diameter grid, which is composed of a copper (gold) grid at the bottom and a carbon film on the upper layer, and then send the grid into the transmission Microscope for testing. The process of attaching a crystal powder sample to a grid is called sample preparation.
  • Another type of method is to directly stick the powder ground to a particle size of 0.2 to 2 microns on the carrier net through a variety of different operating modes.
  • One operation is to use tweezers to clamp the edge of the grid to directly pick up the ground powder, so that the crystal particles are attached to the carbon film of the grid, and then gently tap the tweezers to remove the excess crystal particles, thus completing a sample preparation.
  • Another operation is to put the carrier net into a small centrifuge tube containing about 2 mg of powder, shake the centrifuge tube gently to make the powder stick to the carrier net, then use tweezers to clamp the carrier net, and blow off the excess powder with the ear washing ball. Complete sample preparation.
  • the solvent evaporation method can disperse moisture-absorbing and easily agglomerated powders in the air, it takes more time, more than one day, and the method is slightly complicated and the efficiency is low. Therefore, it is more suitable for the preparation of special easily agglomerated powders, but not suitable for the sample preparation of conventional powders.
  • the technical problem to be solved in this application is to provide a powder sample preparation device and method in order to solve the technical problem of poor repeatability of the powder sample preparation method in the prior art.
  • the first aspect of the present application provides a powder sample preparation device, comprising:
  • the sample carrying platform is provided with successively connected pipelines, sample tanks, and air jet pinholes;
  • the front end of the pipeline is provided with a net-carrying tank for accommodating the net-carrying tank, and the net-carrying tank communicates with the pipeline.
  • a second aspect of the present application provides a powder sample preparation method, comprising the following steps:
  • the gas is injected into the sample slot through the gas injection needle hole by the gas injection device, and the carrier grid with the powder sample attached is obtained.
  • the powder sample is attached to the carrier net by means of air jet, which can fix various conditions in the powder sample preparation process, improve the repeatability of the powder preparation method, and prepare the powder sample. High efficiency, especially suitable for preparing powder samples for microcrystalline electron diffraction test.
  • Figure 1 is a schematic diagram of the overall structure of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application;
  • FIG. 2 is a schematic diagram of the exploded structure of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application;
  • Fig. 3 is a schematic diagram of the structure of a sample tank of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application;
  • Fig. 4 is a schematic structural diagram of a sample carrying platform of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application.
  • first, second, third and so on may be used in this application to describe various information, such information should not be limited to these terms. These terms are only used to distinguish information of the same type from one another.
  • first information may also be called second information, and similarly, second information may also be called first information.
  • second information may also be called first information.
  • a feature defined as “first” and “second” may explicitly or implicitly include one or more of these features.
  • “plurality” means two or more, unless otherwise specifically defined.
  • a powder sample preparation device including:
  • the sample carrying platform is provided with successively connected pipelines, sample tanks and air injection pinholes;
  • the front end of the pipeline is provided with a net-carrying tank for accommodating the net-carrying tank, and the net-carrying tank communicates with the pipeline.
  • the sample tank is used to accommodate powder samples;
  • the size and shape of the grid tank is adapted to the grid for fixing and accommodating the grid;
  • the powder sample preparation device can be connected to the The jetting equipment is docked; the jetting equipment injects gas into the sample tank of the powder sample preparation device through the jetting pinhole, and then drives the powder sample on the sample tank to spray on the grid on the grid tank along the pipeline, thereby completing the preparation of the powder sample.
  • the powder sample preparation device in this embodiment can take various conditions in the powder sample preparation process (including but not limited to the amount of powder sample, the amount of injected gas, the speed of injected gas, the carrier grid, the powder sample placed on the sample tank, The mutual distance between the three air-jet pinholes, etc.) is fixed, which improves the repeatability of the powder preparation method, and the efficiency of preparing powder samples is high, and is especially suitable for preparing powder samples for microcrystalline electron diffraction tests.
  • various conditions in the powder sample preparation process including but not limited to the amount of powder sample, the amount of injected gas, the speed of injected gas, the carrier grid, the powder sample placed on the sample tank, The mutual distance between the three air-jet pinholes, etc.
  • the powder sample preparation device further includes a grid tank cover for fixing the grid.
  • the present application has various implementation schemes.
  • the net-carrying tank is arranged on the net-carrying tank cover, that is, in the net-carrying tank cover or the end face of the net-carrying tank cover (the net-carrying tank is composed of the end face of the net-carrying tank cover where it is located and the end face of the sample carrying platform. enclosed).
  • the net-carrying tank When the net-carrying tank is arranged in the net-carrying tank cover, the net-carrying tank communicates with the pipeline through the first hole.
  • the first hole is preferably arranged in the cover of the grid tank.
  • the first hole and the pipe are cylindrical pipes; the central axis of the first hole and the pipe is on or close to the same line as the center/center of the grid placed behind the grid tank, so that the air Flow, the powder sample can be more evenly distributed on the grid under the drive of the gas injected into the pipeline, thereby improving the quality of the sample attached to the grid for testing.
  • the grid-carrying trough is set on the connecting portion between the grid-carrying trough cover and the pipeline, that is, in the connecting portion or on the end face of the connecting portion; preferably, the grid-carrying trough is set
  • the end face of the connecting part between the described net-carrying tank cover and the pipeline is enclosed by the end face of the described net-carrying tank cover and the end face of the connecting part (see Figure 2), and the connecting part is provided with A second hole communicated with the grid tank, the second hole communicated with the pipeline.
  • the second tunnel and the pipeline are cylindrical pipelines; the central axis of the second tunnel and the pipeline is positioned at or nearly on the same straight line as the center/center of the grid placed behind the grid tank, so that the air Flow, the powder sample can be more evenly distributed on the grid under the drive of the gas injected into the pipeline, thereby improving the quality of the sample attached to the grid for testing.
  • the grid tank is surrounded by the end face of the grid tank cover and the sample carrier platform, that is, the end face of the grid tank cover and the sample carrier platform
  • the end face is provided with grooves that cooperate with each other to form a grid-carrying groove.
  • the grid-carrying tank is arranged on the sample carrier platform, and the grid-carrying tank, the pipeline, the sample tank, and the air injection pinhole are sequentially connected.
  • the pipeline is a cylindrical pipeline, and the central axis of the pipeline and the center/center of the grid placed behind the grid tank are on or close to the same straight line, so as to facilitate air flow,
  • the powder sample can be more evenly distributed on the carrier grid driven by the gas injected into the pipeline.
  • the grid-carrying tank is a groove, in order to make the grid-carrying grid can be placed on the grid-carrying tank more easily, it is convenient to assemble, and the shaking in the sample preparation process is reduced as much as possible, thereby improving the amount of material attached to the grid-carrying net for testing.
  • the quality of the sample can be specially set for the grid tank. For example:
  • the depth of the grid-carrying tank is adapted to the thickness of the grid-carrying tank, so as to minimize possible displacement after the grid-carrying tank is placed on the grid-carrying tank. For example the same, or substantially the same/approximately the same.
  • the bottom edge/bottom surface in contact with the grid in the grid tank has an angle of a with the horizontal plane, 0 ⁇ a ⁇ 90°; more preferably, 30° ⁇ a ⁇ 90° or 45° ⁇ a ⁇ 75°.
  • the part for accommodating the net in the net-carrying tank is in the shape of a slanted column or a truncated truss, preferably in the shape of a slanted cylindrical, truncated circular or rhomboidal column.
  • the diameter of said oblique cylinder is slightly larger than that of the loading net;
  • the face of the frustum closer to the pipe has a larger diameter.
  • the center/center of the grid placed behind the grid tank coincides or almost coincides with the central axis of the gas outlet of the pipeline.
  • the above-mentioned several embodiments can make the loading net can be placed on the loading grid slot more easily, ensure the repeatability of the sample used for testing on the loading grid prepared based on the device, and improve the sample size attached to the loading grid for testing. the quality of the sample.
  • the bottom edge/bottom surface in contact with the carrying net in the carrying net tank is arranged to have a certain angle with the horizontal plane, which can reduce the manufacturing cost of this application. The difficulty and cost of the installation.
  • the depth of the grid-carrying tank is adapted to the thickness of the clamping device for clamping the grid-carrying tank, so as to minimize possible displacement of the clamping device after it is placed on the grid-carrying tank .
  • the clamping device for clamping the grid is used to clamp the grid, and can expose the carbon film on the grid.
  • the sample groove is a groove; preferably, the surface carrying the powder sample on the groove is an arc surface, more preferably an arc surface; so that the powder sample in the sample groove can More evenly is blown and evenly distributed on the grid.
  • the scale mark can only mark a certain part of the sample tank, such as the middle part, or can mark the entire sample tank (see Figure 3), which is convenient for the user to adjust the powder sample to be placed in the sample tank in combination with conditions such as the gas injected into the sample tank.
  • the position and amount of the sample are recorded and recorded, thereby improving the quality of the sample attached to the grid for testing.
  • the upper part of the sample tank is provided with an openable sample tank cover, which is used to close the open space on the upper part of the sample tank.
  • an openable sample tank cover which is used to close the open space on the upper part of the sample tank.
  • the powder sample preparation device further includes a base, and the base is arranged at the bottom of the sample carrying platform.
  • the base is connected to the sample carrier by screws.
  • the powder sample preparation device further includes an outer cover, the outer cover is used to cover the sample carrier platform and the base, and the outer cover is provided with an opening, which is convenient for the air outlet end of the air injection device to connect with the air injection needle.
  • the communication between the holes; the outer cover is provided with an opening and closing device, which is convenient for adding samples to the sample tank and/or replacing the grid.
  • the application also provides a powder sample preparation method, comprising the following steps:
  • the gas is injected into the sample slot through the gas injection needle hole by the gas injection device, and the carrier grid with the powder sample attached is obtained.
  • the powder sample preparation method based on the aforementioned powder sample preparation device is simple and efficient, and the prepared test samples on the carrier net have good repeatability.
  • the air spraying equipment includes an air compression pump and a spray gun, the air inlet of the spray gun communicates with the air outlet of the air compression pump, the air outlet of the spray gun communicates with the intake end of the communication device, and the communication
  • the air outlet of the device is connected with the air injection pinhole; during sample preparation, a fixed flow rate of air is injected into the sample tank through the communication device through the spray gun, and the powder sample is sprayed on the carrier net along the pipeline.
  • the communication device in this embodiment is not particularly limited, and preferably includes a cylindrical inner cavity, so that the gas can pass through evenly and enter the sample tank.
  • the communication device is a microsampler with the piston removed.
  • This embodiment provides a powder sample preparation device for microcrystal electron diffraction testing, as shown in Figures 1 and 2, including:
  • the sample carrying platform is provided with a sample tank 6 for accommodating powder samples, and is also provided with an air jet pinhole 7 and a pipeline 5; the air jet pinhole 7 is arranged at the rear end of the sample tank 6 for docking with an air jet device, so Said pipeline 5 is arranged on the front end of said sample tank 6, and is used for docking carrying net 10;
  • Pipeline 5 is a cylindrical pipeline;
  • Air jet pinhole 7 is a circular hole;
  • the front end of the sample tank 6 is provided with a grid tank 4 for accommodating the grid 10 , and the grid tank 4 communicates with the pipeline 5 .
  • the grid tank 4 includes a cylindrical shape (the part where the grid 10 is placed) and a rectangular parallelepiped (to facilitate the loading and unloading of the grid 10 ).
  • the powder sample preparation device for microcrystalline electron diffraction test of this embodiment also includes a grid tank cover 3 installed on the front end of the sample carrier, and the grid A grid-carrying tank 4 is provided at the connection between the tank cover 3 and the sample carrier; the end surface of the connecting part is provided with a groove to form the grid-carrying tank 4 .
  • the depth of the net-carrying tank 4 can be set to be approximately the same as the thickness of the net-carrying tank 10, so that the net-carrying tank 10 is not easy to shake after the net-carrying tank cover 3 is fixed, and the attachment to the carrier net can be improved. The quality of the samples available online for testing.
  • the powder sample preparation device for microcrystalline electron diffraction test of this embodiment as shown in Figures 1 and 2 , the mesh tank cover 3 and the sample carrier are connected and fixed by buckles 1 .
  • the buckle 1 is convenient for the disassembly and assembly of the net tank cover 3 .
  • the powder sample preparation device for microcrystal electron diffraction test of this embodiment as shown in Figures 1 and 2, the front end of the grid tank cover 3 is provided with a handle 2 for holding.
  • the handle 2 is convenient for holding the net tank cover 3 and is convenient for installation.
  • the powder sample preparation device for microcrystal electron diffraction test of this embodiment further includes a base 9, and the base 9 is arranged at the bottom of the sample carrying platform.
  • the base 9 is convenient to raise the sample carrier platform so that the operator can use it.
  • the base 9 is designed as an I-shape.
  • the powder sample preparation device for microcrystal electron diffraction test of this embodiment is provided with screw holes around the sample carrier, and the base 9 is connected to the sample carrier. Attached by screw 8.
  • the sample tank 6 is a groove with an open top; preferably, the groove carries powder
  • the surface of the sample is an arc surface, more preferably an arc surface; so that the powder sample in the sample tank can be blown more evenly and evenly distributed on the grid.
  • the surface of the sample chamber 6 is engraved with a scale mark 61 in the powder sample preparation device for microcrystal electron diffraction test in this embodiment.
  • the optimal strategy is to place the powder in the sample tank each time without knowing the static electricity of the powder and without performing a test experiment. Use as little powder as possible (about 1 mg), observe the particle distribution on the carrier net after spraying once, and decide whether to re-spray according to the particle distribution.
  • scale markings with an interval of 1 mm, 2 mm or other units can be set on the sample slot with a total length of 20 mm, for example.
  • the optimal strategy is to place the powder in the middle of the sample tank as much as possible, as shown in Figure 3.
  • the device of this embodiment is also provided with an outer cover (acrylic cover) to cover the sample carrier platform and the base 9 .
  • the outer cover is provided with an opening for connecting the front end (needle) of the micro-sampler to the air jet pinhole, and the top of the outer cover can also be provided with a flip door to facilitate the loading and unloading of the carrier net.
  • This embodiment provides a powder sample preparation method for microcrystal electron diffraction test, using the above-mentioned powder sample preparation device for microcrystal electron diffraction test in this embodiment, including the following steps:
  • the upper part of the preparation device is the part for placing the grid and powder samples
  • the lower part is the base.
  • the side of the carbon film used for attaching particles on the carrier net faces the direction of the pipeline 5 , and snaps it into the grid tank 4 between the pipeline 5 and the grid tank cover 3 .
  • the aperture on the net-carrying tank cover 3 is the buckle that the net-carrying tank cover is fixed on the device. Then, place about 1 mg of the ground powder sample in the middle of the sample tank 6 with a spatula.
  • This embodiment provides a powder sample preparation device for microcrystalline electron diffraction test, as shown in Figure 4, the difference from the sample carrier structure of the preparation device in Example 1 is as follows: there is no grid tank cover 3, and The front end of the sample carrying platform is directly provided with a semi-open net-carrying tank 4 , the net-carrying tank 4 is semi-cylindrical, and the net-carrying tank 10 is vertically placed in the net-carrying tank 4 .
  • the advantage of this fixing method is that the placement and replacement of the carrier grid does not need to open the cover, which is more convenient.

Abstract

A preparation device and method for a powder sample. The preparation device comprises: a sample bearing stage, which is provided with a pipe (5), a sample groove (6) and a jetting needle hole (7), which are sequentially in communication with each other, wherein a front end of the pipe (5) is provided with a bearing mesh slot (4), the bearing mesh slot (4) is used to accommodate a bearing mesh (10), and the bearing mesh slot (4) is in communication with the pipe (5). By means of adhering a powder sample to the bearing mesh (10) in an air jetting manner, various conditions in the process of powder preparation can be fixed, which improves the reproducibility of the powder preparation method and increases the efficiency of preparing the powder sample, and is suitable for preparing a powder sample for microcrystal electron diffraction testing.

Description

一种粉末样品制备装置及方法A kind of powder sample preparation device and method
本申请要求于2021年11月19日提交国家知识产权局、申请号为202111401760.X、申请名称为“一种粉末样品制备装置及方法”的中国专利申请的优先权,其全部内容通过引用结合在本申请中。This application claims the priority of a Chinese patent application filed with the State Intellectual Property Office on November 19, 2021, with application number 202111401760.X and application title "A device and method for preparing powder samples", the entire contents of which are incorporated by reference in this application.
技术领域technical field
本申请属于微晶电子衍射测试技术领域,尤其是涉及一种粉末样品制备装置及方法。The application belongs to the technical field of microcrystal electron diffraction testing, and in particular relates to a powder sample preparation device and method.
背景技术Background technique
微晶电子衍射(Microcrystal Electron Diffraction,MicroED)需要在透射电子显微镜中,将0.2~2微米大小的晶体颗粒在电子束下连续旋转一定角度,同时收集一系列不同角度下的电子衍射数据,目的是解析得到晶体的分子结构。因此,MicroED测试需要将微米甚至纳米尺寸的晶体颗粒均匀分散地附着在3.05mm直径的载网上,该载网由底层的铜(金)网和上层的碳膜组成,然后将载网送进透射电镜进行测试。将晶体粉末样品附着在载网上的过程称为样品制备(Sample Preparation)。Microcrystal Electron Diffraction (Microcrystal Electron Diffraction, MicroED) needs to continuously rotate crystal particles with a size of 0.2 to 2 microns at a certain angle under the electron beam in a transmission electron microscope, and collect a series of electron diffraction data at different angles at the same time. Analyze the molecular structure of the crystal. Therefore, the MicroED test needs to uniformly disperse micron or even nanometer-sized crystal particles on a 3.05mm diameter grid, which is composed of a copper (gold) grid at the bottom and a carbon film on the upper layer, and then send the grid into the transmission Microscope for testing. The process of attaching a crystal powder sample to a grid is called sample preparation.
粉末样品的制备通常有两类方法,一类是溶剂蒸发法,将2~5毫克研磨至0.2~2微米粒径的粉末投入1~5毫升不良溶剂中超声分散20~40分钟,得到分散良好的悬浊液,然后通过移液枪将1~3微升悬浊液滴在载网(圆片,约20微米厚,直径为3毫米左右)上,之后通过室温晾干或真空干燥将溶剂蒸发,只留下晶体颗粒在载网上,这样就完成了一个样品的制备。There are usually two methods for the preparation of powder samples. One is the solvent evaporation method. 2-5 mg of powder ground to a particle size of 0.2-2 microns is put into 1-5 ml of poor solvent for ultrasonic dispersion for 20-40 minutes to obtain a well-dispersed Then drop 1 to 3 microliters of the suspension on the grid (disc, about 20 microns thick, about 3 mm in diameter) through a pipette gun, and then dry the solvent at room temperature or vacuum Evaporate, leaving only crystal particles on the grid, thus completing the preparation of a sample.
另一类方法是通过多种不同操作方式直接将研磨至0.2~2微米粒径的粉末沾在载网上。一种操作是用镊子夹住载网边缘直接沾取研磨后的粉末,使晶体颗粒附着在载网的碳膜上,然后轻轻敲击镊子以去掉多余的晶体颗粒,这样就完成了一个样品的制备。另一种操作是将载网投入盛有2毫克左右粉末的小离心管,轻轻摇晃离心管,使粉末沾在载网上,再用镊子夹出载网,用洗耳球吹去多余粉末,完成样品制备。Another type of method is to directly stick the powder ground to a particle size of 0.2 to 2 microns on the carrier net through a variety of different operating modes. One operation is to use tweezers to clamp the edge of the grid to directly pick up the ground powder, so that the crystal particles are attached to the carbon film of the grid, and then gently tap the tweezers to remove the excess crystal particles, thus completing a sample preparation. Another operation is to put the carrier net into a small centrifuge tube containing about 2 mg of powder, shake the centrifuge tube gently to make the powder stick to the carrier net, then use tweezers to clamp the carrier net, and blow off the excess powder with the ear washing ball. Complete sample preparation.
溶剂蒸发法虽然可以分散在空气中吸潮易团聚的粉末,但耗时较多, 用时大于一天,且方法略复杂,效率较低。因此更适用于对特殊易团聚粉末进行制备,并不适用于常规粉末的样品制备。Although the solvent evaporation method can disperse moisture-absorbing and easily agglomerated powders in the air, it takes more time, more than one day, and the method is slightly complicated and the efficiency is low. Therefore, it is more suitable for the preparation of special easily agglomerated powders, but not suitable for the sample preparation of conventional powders.
第二类方法中无论是用镊子夹住载网直接沾取粉末,还是将载网投入粉末进行摇晃,可重复性都较差,制备出的载网样品质量不稳定,容易出现较大颗粒团聚体附着在碳膜上且通过敲击镊子或洗耳球吹气的方式很难去掉,或者附着颗粒过于密集。另外手的力度不好控制,容易在粉末中划破脆弱的碳膜,以上这些情况都导致样品制备的失败。In the second type of method, no matter whether you use tweezers to clamp the grid to directly pick up the powder, or put the grid into the powder for shaking, the repeatability is poor, the quality of the prepared grid sample is unstable, and larger particles are prone to agglomeration The body is attached to the carbon film and it is difficult to remove it by tapping the tweezers or blowing the ear ball, or the attached particles are too dense. In addition, the strength of the hand is not well controlled, and it is easy to scratch the fragile carbon film in the powder. All of the above situations lead to the failure of sample preparation.
技术问题technical problem
本申请要解决的技术问题是:为解决现有技术中粉末样品制备方法可重复性差的技术问题,从而提供一种粉末样品制备装置及方法。The technical problem to be solved in this application is to provide a powder sample preparation device and method in order to solve the technical problem of poor repeatability of the powder sample preparation method in the prior art.
技术解决方案technical solution
本申请的第一方面提供了一种粉末样品制备装置,包括:The first aspect of the present application provides a powder sample preparation device, comprising:
样本承载台,设有依次连通的管道、样品槽、喷气针孔;The sample carrying platform is provided with successively connected pipelines, sample tanks, and air jet pinholes;
所述管道的前端设置有载网槽,所述载网槽用于容纳载网,所述载网槽与所述管道连通。The front end of the pipeline is provided with a net-carrying tank for accommodating the net-carrying tank, and the net-carrying tank communicates with the pipeline.
本申请的第二方面提供了一种粉末样品制备方法,包括以下步骤:A second aspect of the present application provides a powder sample preparation method, comprising the following steps:
将载网安装到如上所述的粉末样品制备装置的载网槽内,并将载网上用于附着颗粒的碳膜一面朝向管道方向;Install the grid into the grid tank of the powder sample preparation device as described above, and place the carbon film side of the grid for attaching particles to the direction of the pipeline;
将粉末样品放在样品槽中;Place the powder sample in the sample holder;
通过喷气设备将气体通过喷气针孔注入样品槽中,获得附着粉末样品的载网。The gas is injected into the sample slot through the gas injection needle hole by the gas injection device, and the carrier grid with the powder sample attached is obtained.
有益效果Beneficial effect
依据本申请的粉末样品制备装置和方法,采用喷气方式将粉末样品附着在载网上,能将粉末样品制备过程中的各种条件固定,提高了粉末制备方法的可重复性,且制备粉末样品的效率高,尤其适用于制备微晶电子衍射测试的粉末样品。According to the powder sample preparation device and method of the present application, the powder sample is attached to the carrier net by means of air jet, which can fix various conditions in the powder sample preparation process, improve the repeatability of the powder preparation method, and prepare the powder sample. High efficiency, especially suitable for preparing powder samples for microcrystalline electron diffraction test.
应当理解的是,以上的一般描述和后文的细节描述仅是示例性和解释 性的,并不能限制本申请。It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application.
附图说明Description of drawings
通过结合附图对本申请示例性实施方式进行更详细的描述,本申请的上述以及其它目的、特征和优势将变得更加明显,其中,在本申请示例性实施方式中,相同的参考标号通常代表相同部件。The above and other objects, features and advantages of the present application will become more apparent by describing the exemplary embodiments of the present application in more detail with reference to the accompanying drawings, wherein, in the exemplary embodiments of the present application, the same reference numerals generally represent same parts.
图1是本申请在一些实施例中的用于微晶电子衍射测试的粉末样品制备装置整体结构示意图;Figure 1 is a schematic diagram of the overall structure of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application;
图2是本申请在一些实施例中的用于微晶电子衍射测试的粉末样品制备装置爆炸结构示意图;2 is a schematic diagram of the exploded structure of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application;
图3是本申请在一些实施例中的用于微晶电子衍射测试的粉末样品制备装置样品槽结构示意图;Fig. 3 is a schematic diagram of the structure of a sample tank of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application;
图4是本申请在一些实施例中的用于微晶电子衍射测试的粉末样品制备装置的样本承载台结构示意图。Fig. 4 is a schematic structural diagram of a sample carrying platform of a powder sample preparation device for microcrystal electron diffraction testing in some embodiments of the present application.
图中的附图标记为:The reference signs in the figure are:
1  卡扣1 buckle
2  手柄2 handles
3  载网槽盖3 Loading grid slot cover
4  载网槽4 Network slots
5  管道5 pipes
6  样品槽6 sample slots
61 刻度标识61 Scale mark
7  喷气针孔7 jet pinhole
8  螺钉8 screws
9  底座9 base
10 载网。10 load net.
本发明的实施方式Embodiments of the present invention
下面将参照附图更详细地描述本申请的实施方式。虽然附图中显示了本申请的实施方式,然而应该理解,可以以各种形式实现本申请而不应被 这里阐述的实施方式所限制。相反,提供这些实施方式是为了使本申请更加透彻和完整,并且能够将本申请的范围完整地传达给本领域的技术人员。Embodiments of the present application will be described in more detail below with reference to the accompanying drawings. Although embodiments of the present application are shown in the drawings, it should be understood that the present application may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this application will be thorough and complete, and will fully convey the scope of this application to those skilled in the art.
在本申请使用的术语是仅仅出于描述特定实施例的目的,而非旨在限制本申请。在本申请和所附权利要求书中所使用的单数形式的“一种”、“所述”和“该”也旨在包括多数形式,除非上下文清楚地表示其他含义。还应当理解,本文中使用的术语“和/或”是指并包含一个或多个相关联的列出项目的任何或所有可能组合。The terminology used in this application is for the purpose of describing particular embodiments only, and is not intended to limit the application. As used in this application and the appended claims, the singular forms "a", "the", and "the" are intended to include the plural forms as well, unless the context clearly dictates otherwise. It should also be understood that the term "and/or" as used herein refers to and includes any and all possible combinations of one or more of the associated listed items.
应当理解,尽管在本申请可能采用术语“第一”、“第二”、“第三”等来描述各种信息,但这些信息不应限于这些术语。这些术语仅用来将同一类型的信息彼此区分开。例如,在不脱离本申请范围的情况下,第一信息也可以被称为第二信息,类似地,第二信息也可以被称为第一信息。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本申请的描述中,“多个”的含义是两个或两个以上,除非另有明确具体的限定。It should be understood that although the terms "first", "second", "third" and so on may be used in this application to describe various information, such information should not be limited to these terms. These terms are only used to distinguish information of the same type from one another. For example, without departing from the scope of the present application, first information may also be called second information, and similarly, second information may also be called first information. Thus, a feature defined as "first" and "second" may explicitly or implicitly include one or more of these features. In the description of the present application, "plurality" means two or more, unless otherwise specifically defined.
下面将参考附图并结合实施例来详细说明本申请的技术方案。The technical solution of the present application will be described in detail below with reference to the accompanying drawings and embodiments.
为了解决现有技术中存在的问题,在本申请提供了一种粉末样品制备装置,包括:In order to solve the problems in the prior art, the application provides a powder sample preparation device, including:
样本承载台,设有依次连通的管道、样品槽和喷气针孔;The sample carrying platform is provided with successively connected pipelines, sample tanks and air injection pinholes;
所述管道的前端设置有载网槽,所述载网槽用于容纳载网,所述载网槽与所述管道连通。The front end of the pipeline is provided with a net-carrying tank for accommodating the net-carrying tank, and the net-carrying tank communicates with the pipeline.
需要说明的是,所述样品槽用于容纳粉末样品;所述载网槽的大小和形状与载网适配,用于固定和容纳载网;所述粉末样品制备装置可通过喷气针孔与喷气设备对接;喷气设备通过喷气针孔将气体注入粉末样品制备装置的样品槽中,进而带动样品槽上的粉末样品顺着管道喷在载网槽上的载网上,从而完成粉末样品的制备。即,本实施例中的粉末样品制备装置能将粉末样品制备过程中的各种条件(包括但不限于粉末样品量,注入气体量,注入气体速度,载网、样品槽上放置的粉末样品、喷气针孔三者之间的相互距离等)固定,提高了粉末制备方法的可重复性,且制备粉末样品的效率高,尤其适用于制备微晶电子衍射测试的粉末样品。It should be noted that the sample tank is used to accommodate powder samples; the size and shape of the grid tank is adapted to the grid for fixing and accommodating the grid; the powder sample preparation device can be connected to the The jetting equipment is docked; the jetting equipment injects gas into the sample tank of the powder sample preparation device through the jetting pinhole, and then drives the powder sample on the sample tank to spray on the grid on the grid tank along the pipeline, thereby completing the preparation of the powder sample. That is, the powder sample preparation device in this embodiment can take various conditions in the powder sample preparation process (including but not limited to the amount of powder sample, the amount of injected gas, the speed of injected gas, the carrier grid, the powder sample placed on the sample tank, The mutual distance between the three air-jet pinholes, etc.) is fixed, which improves the repeatability of the powder preparation method, and the efficiency of preparing powder samples is high, and is especially suitable for preparing powder samples for microcrystalline electron diffraction tests.
为了便于载网的取放,在本申请的一实施例中,所述粉末样品制备装 置还包括用于固定载网的载网槽盖。In order to facilitate the loading and placing of the grid, in an embodiment of the present application, the powder sample preparation device further includes a grid tank cover for fixing the grid.
针对载网槽的位置,本申请有多种实现方案。For the position of the grid-carrying tank, the present application has various implementation schemes.
在一实施例中,所述载网槽设置在载网槽盖上,即载网槽盖中或载网槽盖的端面(载网槽由其所在的载网槽盖端面与样本承载台端面围合而成)。当载网槽设置在载网槽盖中时,所述载网槽通过第一孔道与所述管道连通。所述第一孔道优选设于所述载网槽盖中。更优选的,所述第一孔道和管道均为圆柱形管道;所述第一孔道和管道的中心轴与载网放置在载网槽后的圆心/中心位于或接近位于同一直线,以便于空气流动,粉末样品在注入管道的气体的带动下能更均匀的分布在载网上,从而提高附着在载网上的用于测试的样品的质量。In one embodiment, the net-carrying tank is arranged on the net-carrying tank cover, that is, in the net-carrying tank cover or the end face of the net-carrying tank cover (the net-carrying tank is composed of the end face of the net-carrying tank cover where it is located and the end face of the sample carrying platform. enclosed). When the net-carrying tank is arranged in the net-carrying tank cover, the net-carrying tank communicates with the pipeline through the first hole. The first hole is preferably arranged in the cover of the grid tank. More preferably, the first hole and the pipe are cylindrical pipes; the central axis of the first hole and the pipe is on or close to the same line as the center/center of the grid placed behind the grid tank, so that the air Flow, the powder sample can be more evenly distributed on the grid under the drive of the gas injected into the pipeline, thereby improving the quality of the sample attached to the grid for testing.
在另一实施例中,所述载网槽设于所述载网槽盖与所述管道之间的连接部上,即连接部中或连接部的端面;优选的,所述载网槽设于所述载网槽盖与所述管道之间的连接部的端面,由所述载网槽盖端面与所述连接部端面围合而成(参见图2),所述连接部设有与载网槽连通的第二孔道,所述第二孔道与所述管道连通。更优选的,所述第二孔道和管道均为圆柱形管道;所述第二孔道和管道的中心轴与载网放置在载网槽后的圆心/中心位于或接近位于同一直线,以便于空气流动,粉末样品在注入管道的气体的带动下能更均匀的分布在载网上,从而提高附着在载网上的用于测试的样品的质量。In another embodiment, the grid-carrying trough is set on the connecting portion between the grid-carrying trough cover and the pipeline, that is, in the connecting portion or on the end face of the connecting portion; preferably, the grid-carrying trough is set The end face of the connecting part between the described net-carrying tank cover and the pipeline is enclosed by the end face of the described net-carrying tank cover and the end face of the connecting part (see Figure 2), and the connecting part is provided with A second hole communicated with the grid tank, the second hole communicated with the pipeline. More preferably, the second tunnel and the pipeline are cylindrical pipelines; the central axis of the second tunnel and the pipeline is positioned at or nearly on the same straight line as the center/center of the grid placed behind the grid tank, so that the air Flow, the powder sample can be more evenly distributed on the grid under the drive of the gas injected into the pipeline, thereby improving the quality of the sample attached to the grid for testing.
在另一实施例中,所述载网槽由所述载网槽盖的端面和所述样本承载台的端面围合而成,即所述载网槽盖的端面和所述样本承载台的端面设有相互配合的凹槽,形成载网槽。In another embodiment, the grid tank is surrounded by the end face of the grid tank cover and the sample carrier platform, that is, the end face of the grid tank cover and the sample carrier platform The end face is provided with grooves that cooperate with each other to form a grid-carrying groove.
在另一实施例中,所述载网槽设于样本承载台上,所述载网槽、管道、样品槽、喷气针孔依次连通。In another embodiment, the grid-carrying tank is arranged on the sample carrier platform, and the grid-carrying tank, the pipeline, the sample tank, and the air injection pinhole are sequentially connected.
在上述两个实施例中,优选的,所述管道为圆柱形管道,所述管道的中心轴与载网放置在载网槽后的圆心/中心位于或接近位于同一直线,以便于空气流动,粉末样品在注入管道的气体的带动下能更均匀的分布在载网上。In the above two embodiments, preferably, the pipeline is a cylindrical pipeline, and the central axis of the pipeline and the center/center of the grid placed behind the grid tank are on or close to the same straight line, so as to facilitate air flow, The powder sample can be more evenly distributed on the carrier grid driven by the gas injected into the pipeline.
所述载网槽为凹槽,为了使得载网能够较轻松的放置在载网槽上,便于装配,并尽可能降低在样品制备过程中的晃动,从而提高附着在载网上 的用于测试的样品的质量,可对载网槽进行特殊设置。例如:The grid-carrying tank is a groove, in order to make the grid-carrying grid can be placed on the grid-carrying tank more easily, it is convenient to assemble, and the shaking in the sample preparation process is reduced as much as possible, thereby improving the amount of material attached to the grid-carrying net for testing. The quality of the sample can be specially set for the grid tank. For example:
在本申请的一实施例中,所述载网槽的深度与载网的厚度适配,以尽可能减少载网放置在载网槽上后可能发生的位移为宜。例如相同,或基本一致/大致相同。In an embodiment of the present application, the depth of the grid-carrying tank is adapted to the thickness of the grid-carrying tank, so as to minimize possible displacement after the grid-carrying tank is placed on the grid-carrying tank. For example the same, or substantially the same/approximately the same.
在本申请的另一个实施例中,所述载网槽中与载网接触的底边/底面,与水平面的夹角为a,0<a<90°;更优选的,30°<a<90°或45°<a<75°。In another embodiment of the present application, the bottom edge/bottom surface in contact with the grid in the grid tank has an angle of a with the horizontal plane, 0<a<90°; more preferably, 30°<a< 90° or 45°<a<75°.
在本申请的另一实施例中,所述载网槽中用于容纳载网的部分为斜柱形或斜台形,优选斜圆柱形、斜圆台形或斜方柱形。当为斜圆柱形时,所述斜圆柱的直径较载网稍大;当为斜方柱形时,所述斜方柱的截面较载网稍大;当为斜圆台形时,所述斜圆台中更靠近管道的面的直径较大。In another embodiment of the present application, the part for accommodating the net in the net-carrying tank is in the shape of a slanted column or a truncated truss, preferably in the shape of a slanted cylindrical, truncated circular or rhomboidal column. When it is oblique cylindrical, the diameter of said oblique cylinder is slightly larger than that of the loading net; The face of the frustum closer to the pipe has a larger diameter.
在本申请的另一实施例中,所述载网放置在载网槽后的圆心/中心与管道出气口的中心轴重合或几乎重合。In another embodiment of the present application, the center/center of the grid placed behind the grid tank coincides or almost coincides with the central axis of the gas outlet of the pipeline.
上述几个实施例均能使得载网能够较轻松的放置在载网槽上,保证基于本装置制备出的载网上的用于测试的样品的可重复性,提高附着在载网上的用于测试的样品的质量。The above-mentioned several embodiments can make the loading net can be placed on the loading grid slot more easily, ensure the repeatability of the sample used for testing on the loading grid prepared based on the device, and improve the sample size attached to the loading grid for testing. the quality of the sample.
需要说明的是,考虑到载网的厚度非常薄(大约为20微米),将载网槽中与载网接触的底边/底面,与水平面设置成有一定的夹角,可降低制造本申请的装置的难度和成本。It should be noted that, considering that the thickness of the carrying net is very thin (about 20 microns), the bottom edge/bottom surface in contact with the carrying net in the carrying net tank is arranged to have a certain angle with the horizontal plane, which can reduce the manufacturing cost of this application. The difficulty and cost of the installation.
在本申请的一实施例中,所述载网槽的深度与夹持载网的夹持装置的厚度适配,以尽可能减少夹持装置放置在载网槽上后可能发生的位移为宜。例如相同,或基本一致/大致相同,所述夹持载网的夹持装置用于夹持载网,并能将载网上的碳膜暴露。In an embodiment of the present application, the depth of the grid-carrying tank is adapted to the thickness of the clamping device for clamping the grid-carrying tank, so as to minimize possible displacement of the clamping device after it is placed on the grid-carrying tank . For example, the same, or basically the same/approximately the same, the clamping device for clamping the grid is used to clamp the grid, and can expose the carbon film on the grid.
在本申请的一实施例中,所述样品槽为凹槽;优选的,所述凹槽上承载粉末样品的面为弧面,更优选为圆弧面;以使样品槽中的粉末样品能够更均匀的被吹散并均匀分布在载网上。In one embodiment of the present application, the sample groove is a groove; preferably, the surface carrying the powder sample on the groove is an arc surface, more preferably an arc surface; so that the powder sample in the sample groove can More evenly is blown and evenly distributed on the grid.
在本申请的一实施例中,所述样品槽的表面或侧边有刻度标识。In an embodiment of the present application, there are scale marks on the surface or side of the sample tank.
需要说明的是,在制备用于微晶电子衍射测试的粉末样品时,因为所需的粉末样品量极少(以mg记,例如2mg),而粉末样品添加的量对于最终制备获得的用于测试的载网上的样品影响极大。基于所述刻度标识, 使用者可较方便的控制加入的粉末样品量,从而提高附着在载网上的用于测试的样品的质量。It should be noted that when preparing the powder sample for microcrystal electron diffraction test, because the required powder sample amount is very small (in mg, such as 2mg), and the amount of powder sample added is for the final preparation obtained for The sample on the grid under test is highly influential. Based on the scale marks, the user can more conveniently control the amount of powder sample to be added, thereby improving the quality of the test sample attached to the grid.
所述刻度标识可仅标识所述样品槽的某一部分,例如中部,也可标识整个样品槽(参见图3),这样便于使用者结合注入样品槽的气体等条件,调整粉末样品放置在样品槽的位置以及量,并进行记录,从而提高附着在载网上的用于测试的样品的质量。The scale mark can only mark a certain part of the sample tank, such as the middle part, or can mark the entire sample tank (see Figure 3), which is convenient for the user to adjust the powder sample to be placed in the sample tank in combination with conditions such as the gas injected into the sample tank. The position and amount of the sample are recorded and recorded, thereby improving the quality of the sample attached to the grid for testing.
在本申请的一实施例中,所述样品槽的上部设有可开合的样品槽盖,用于封闭样品槽上部的开放空间,当使用者使用本申请的装置进行粉末样品制备时,将样品槽盖关上,使得样品槽与外界空气隔绝,避免粉末样品被扬起后漂浮在实验环境中造成的不同实验之间的相互污染/影响问题。In an embodiment of the present application, the upper part of the sample tank is provided with an openable sample tank cover, which is used to close the open space on the upper part of the sample tank. When the user uses the device of the present application for powder sample preparation, the The cover of the sample tank is closed to isolate the sample tank from the outside air, avoiding the problem of mutual pollution/influence between different experiments caused by the powder sample being lifted up and floating in the experimental environment.
在本申请的另一实施例中,所述粉末样品制备装置还包括底座,所述底座设置在所述样本承载台的底部。优选的,所述样本承载台的四周设有螺孔,所述底座与所述样本承载台通过螺钉连接。In another embodiment of the present application, the powder sample preparation device further includes a base, and the base is arranged at the bottom of the sample carrying platform. Preferably, screw holes are provided around the sample carrier, and the base is connected to the sample carrier by screws.
在本申请的另一实施例中,所述粉末样品制备装置还包括外罩,所述外罩用于将样本承载台和底座罩住,所述外罩设有开口,便于喷气设备的出气端与喷气针孔之间的连通;所述外罩上设有可开合装置,便于样品槽加样和/或载网的更换。In another embodiment of the present application, the powder sample preparation device further includes an outer cover, the outer cover is used to cover the sample carrier platform and the base, and the outer cover is provided with an opening, which is convenient for the air outlet end of the air injection device to connect with the air injection needle. The communication between the holes; the outer cover is provided with an opening and closing device, which is convenient for adding samples to the sample tank and/or replacing the grid.
本申请还提供了一种粉末样品制备方法,包括以下步骤:The application also provides a powder sample preparation method, comprising the following steps:
将载网安装到如上所述的粉末样品制备装置的载网槽内,并将载网上用于附着颗粒的碳膜一面朝向管道方向;Install the grid into the grid tank of the powder sample preparation device as described above, and place the carbon film side of the grid for attaching particles to the direction of the pipeline;
将粉末样品放在样品槽中;Place the powder sample in the sample holder;
通过喷气设备将气体通过喷气针孔注入样品槽中,获得附着粉末样品的载网。The gas is injected into the sample slot through the gas injection needle hole by the gas injection device, and the carrier grid with the powder sample attached is obtained.
基于前述的粉末样品制备装置的粉末样品制备方法简单、效率高,制备所得的载网上的用于测试的样品的可重复性好。The powder sample preparation method based on the aforementioned powder sample preparation device is simple and efficient, and the prepared test samples on the carrier net have good repeatability.
在本申请的一实施例中,所述喷气设备包括空气压缩泵和喷枪,喷枪的进气端与空气压缩泵的出气端连通,喷枪的出气口与连通装置的进气端连通,所述连通装置的出气端与喷气针孔连通;在制样时,通过喷枪将固定流量的空气通过连通装置注入样品槽并带动粉末样品顺着管道喷在载网上。In an embodiment of the present application, the air spraying equipment includes an air compression pump and a spray gun, the air inlet of the spray gun communicates with the air outlet of the air compression pump, the air outlet of the spray gun communicates with the intake end of the communication device, and the communication The air outlet of the device is connected with the air injection pinhole; during sample preparation, a fixed flow rate of air is injected into the sample tank through the communication device through the spray gun, and the powder sample is sprayed on the carrier net along the pipeline.
需要说明的是,本实施例中的连通装置无特殊限定,优选含有圆柱形内腔,便于气体均匀通过并进入到样品槽中。在一些实施例中,所述连通装置为已拔除活塞的微量进样器。It should be noted that the communication device in this embodiment is not particularly limited, and preferably includes a cylindrical inner cavity, so that the gas can pass through evenly and enter the sample tank. In some embodiments, the communication device is a microsampler with the piston removed.
实施例1Example 1
本实施例提供一种用于微晶电子衍射测试的粉末样品制备装置,如图1、2所示,包括:This embodiment provides a powder sample preparation device for microcrystal electron diffraction testing, as shown in Figures 1 and 2, including:
样本承载台,设有用于容纳粉末样品的样品槽6,还设有喷气针孔7、管道5;所述喷气针孔7设置在所述样品槽6的后端,用于对接喷气设备,所述管道5设置在所述样品槽6的前端,用于对接载网10;管道5为圆柱形管道;喷气针孔7为圆形孔;The sample carrying platform is provided with a sample tank 6 for accommodating powder samples, and is also provided with an air jet pinhole 7 and a pipeline 5; the air jet pinhole 7 is arranged at the rear end of the sample tank 6 for docking with an air jet device, so Said pipeline 5 is arranged on the front end of said sample tank 6, and is used for docking carrying net 10; Pipeline 5 is a cylindrical pipeline; Air jet pinhole 7 is a circular hole;
所述样品槽6的前端设置有载网槽4,所述载网槽4用于容纳载网10,所述载网槽4与所述管道5连通。所述载网槽4包括圆柱形(放置载网10的部分)和长方体形(便于载网10的取放)。The front end of the sample tank 6 is provided with a grid tank 4 for accommodating the grid 10 , and the grid tank 4 communicates with the pipeline 5 . The grid tank 4 includes a cylindrical shape (the part where the grid 10 is placed) and a rectangular parallelepiped (to facilitate the loading and unloading of the grid 10 ).
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如图1、2所示,还包括载网槽盖3,安装在所述样本承载台的前端,所述载网槽盖3与所述样本承载台之间的连接部设有载网槽4;所述连接部的端面设有凹槽以形成所述载网槽4。通过设置可拆卸的载网槽盖3,能够将载网槽4的深度设置到和载网10厚度大致相同,这样在固定载网槽盖3之后载网10不容易晃动,能提高附着在载网上的用于测试的样品的质量。Preferably, the powder sample preparation device for microcrystalline electron diffraction test of this embodiment, as shown in Figures 1 and 2, also includes a grid tank cover 3 installed on the front end of the sample carrier, and the grid A grid-carrying tank 4 is provided at the connection between the tank cover 3 and the sample carrier; the end surface of the connecting part is provided with a groove to form the grid-carrying tank 4 . By arranging the detachable net-carrying tank cover 3, the depth of the net-carrying tank 4 can be set to be approximately the same as the thickness of the net-carrying tank 10, so that the net-carrying tank 10 is not easy to shake after the net-carrying tank cover 3 is fixed, and the attachment to the carrier net can be improved. The quality of the samples available online for testing.
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如图1、2所示,所述载网槽盖3与所述样本承载台之间通过卡扣1连接固定。卡扣1便于载网槽盖3的拆装。Preferably, the powder sample preparation device for microcrystalline electron diffraction test of this embodiment, as shown in Figures 1 and 2 , the mesh tank cover 3 and the sample carrier are connected and fixed by buckles 1 . The buckle 1 is convenient for the disassembly and assembly of the net tank cover 3 .
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如图1、2所示,所述载网槽盖3的前端设有供握持的手柄2。手柄2便于载网槽盖3的握持而便于安装。Preferably, the powder sample preparation device for microcrystal electron diffraction test of this embodiment, as shown in Figures 1 and 2, the front end of the grid tank cover 3 is provided with a handle 2 for holding. The handle 2 is convenient for holding the net tank cover 3 and is convenient for installation.
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如图1、2所示,还包括底座9,所述底座9设置在所述样本承载台的底部。底座9便于垫高样本承载台,以便于操作人员使用。本实施例中,将底座9设计为工字型。Preferably, the powder sample preparation device for microcrystal electron diffraction test of this embodiment, as shown in Figures 1 and 2, further includes a base 9, and the base 9 is arranged at the bottom of the sample carrying platform. The base 9 is convenient to raise the sample carrier platform so that the operator can use it. In this embodiment, the base 9 is designed as an I-shape.
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如 图1、2所示,所述样本承载台的四周设有螺孔,所述底座9与所述样本承载台通过螺钉8连接。Preferably, the powder sample preparation device for microcrystal electron diffraction test of this embodiment, as shown in Figures 1 and 2, is provided with screw holes around the sample carrier, and the base 9 is connected to the sample carrier. Attached by screw 8.
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如图1-3所示,所述样品槽6为上部敞开的凹槽;优选的,所述凹槽上承载粉末样品的面为弧面,更优选为圆弧面;以使样品槽中的粉末样品能够更均匀的被吹散并均匀分布在载网上。Preferably, the powder sample preparation device for microcrystalline electron diffraction test of this embodiment, as shown in Figures 1-3, the sample tank 6 is a groove with an open top; preferably, the groove carries powder The surface of the sample is an arc surface, more preferably an arc surface; so that the powder sample in the sample tank can be blown more evenly and evenly distributed on the grid.
优选地,本实施例的用于微晶电子衍射测试的粉末样品制备装置,如图3所示,所述样品槽6的表面刻有刻度标识61。由于载网上样品颗粒的附着量,受粉末带静电情况的影响很大,因此,在不知道粉末带静电情况,且未进行测试实验的情况下,最优的策略是每次在样品槽中放置尽量少的粉末(约1mg),喷气一次后观察载网上的颗粒分布,根据颗粒分布情况决定是否补喷。为了控制每次放置的粉末量,可以在例如总长为20mm的样品槽上设置间隔为1mm、2mm或其他单位的刻度标识。在一些实施例中,放置粉末样品时,使一小堆粉末不超过一格刻度为佳。需要说明的是,粉末样品的位置距喷气针头越近,则越多的粉末样品被扬起到周围空气中,到达载网的粉末量相对变少;粉末样品距载网槽越近,则载网上附着的粉末颗粒越多。在不清楚粉末带静电情况时,最优的策略就是使粉末放置的位置尽量在样品槽的中间部分,如图3所示。Preferably, as shown in FIG. 3 , the surface of the sample chamber 6 is engraved with a scale mark 61 in the powder sample preparation device for microcrystal electron diffraction test in this embodiment. Since the amount of sample particles attached to the grid is greatly affected by the static electricity of the powder, the optimal strategy is to place the powder in the sample tank each time without knowing the static electricity of the powder and without performing a test experiment. Use as little powder as possible (about 1 mg), observe the particle distribution on the carrier net after spraying once, and decide whether to re-spray according to the particle distribution. In order to control the amount of powder placed each time, scale markings with an interval of 1 mm, 2 mm or other units can be set on the sample slot with a total length of 20 mm, for example. In some embodiments, when placing the powder sample, it is better to make a small pile of powder no more than one division scale. It should be noted that, the closer the powder sample is to the jet needle, the more powder sample will be lifted into the surrounding air, and the amount of powder reaching the loading net will be relatively less; the closer the powder sample is to the loading grid tank, the The more powder particles attached to the net. When the static electricity of the powder is not known, the optimal strategy is to place the powder in the middle of the sample tank as much as possible, as shown in Figure 3.
为了避免喷枪吹气时样品粉末在空气中大范围扬起,本实施例的装置还设置一个外罩(亚克力罩)将样本承载台、底座9罩住。外罩设有开口供微量进样器的前端(针头)和喷气针孔连接,所述外罩顶部还可设置翻盖门,方便载网的取放。In order to prevent the sample powder from blowing up in the air in a large area when the spray gun blows air, the device of this embodiment is also provided with an outer cover (acrylic cover) to cover the sample carrier platform and the base 9 . The outer cover is provided with an opening for connecting the front end (needle) of the micro-sampler to the air jet pinhole, and the top of the outer cover can also be provided with a flip door to facilitate the loading and unloading of the carrier net.
本实施例提供一种用于微晶电子衍射测试的粉末样品制备方法,使用本实施例上述的用于微晶电子衍射测试的粉末样品制备装置,包括以下步骤:This embodiment provides a powder sample preparation method for microcrystal electron diffraction test, using the above-mentioned powder sample preparation device for microcrystal electron diffraction test in this embodiment, including the following steps:
如图1、2所示,制备装置上半部分是放置载网和粉末样品的部件,下部分是底座。首先,将载网上用于附着颗粒的碳膜一面朝向管道5方向,卡入管道5和载网槽盖3之间的载网槽4里中。载网槽盖3上的小孔是将载网槽盖固定在装置上的卡扣。然后,用刮勺将约1mg研磨后的粉末样品放在样品槽6的中部。As shown in Figures 1 and 2, the upper part of the preparation device is the part for placing the grid and powder samples, and the lower part is the base. Firstly, the side of the carbon film used for attaching particles on the carrier net faces the direction of the pipeline 5 , and snaps it into the grid tank 4 between the pipeline 5 and the grid tank cover 3 . The aperture on the net-carrying tank cover 3 is the buckle that the net-carrying tank cover is fixed on the device. Then, place about 1 mg of the ground powder sample in the middle of the sample tank 6 with a spatula.
准备一个空气压缩泵,在出气口通过6mm外径的橡胶气管连接一个喷枪的进气口,喷枪的出气口通过橡胶管连接一个已经拔除活塞的微量进样器,将微量进样器的针头穿过喷气针孔7并固定。Prepare an air compression pump, connect the air inlet of a spray gun through a rubber air tube with an outer diameter of 6mm at the air outlet, connect the air outlet of the spray gun to a micro sampler with the piston removed through the rubber tube, and insert the needle of the micro sampler into the Pass the air jet pinhole 7 and fix it.
制样时,先打开空气压缩泵的开关,空气压缩泵开始工作;然后按动一次喷枪的开关,微量进样器的针头喷出一次固定流量的压缩空气,气流穿过样品槽6带动粉末样品顺着管道5喷在载网槽4中的载网上,这样就完成一次样品制备。When preparing samples, first turn on the switch of the air compression pump, and the air compression pump starts to work; then press the switch of the spray gun once, and the needle of the micro-sampler sprays compressed air with a fixed flow rate once, and the air flow passes through the sample tank 6 to drive the powder sample Spray on the grid in the grid tank 4 along the pipeline 5, thus completing a sample preparation.
实施例2Example 2
本实施例提供一种用于微晶电子衍射测试的粉末样品制备装置,如图4所示,与实施例1中的制备装置的样本承载台结构区别如下:不具有载网槽盖3,而是在样本承载台的前端直接设置半敞开的载网槽4,载网槽4为半圆柱形,载网10竖直放在载网槽4中。这种固定方式的优点是载网的放置和更换不需要打开盖子,更加便捷。This embodiment provides a powder sample preparation device for microcrystalline electron diffraction test, as shown in Figure 4, the difference from the sample carrier structure of the preparation device in Example 1 is as follows: there is no grid tank cover 3, and The front end of the sample carrying platform is directly provided with a semi-open net-carrying tank 4 , the net-carrying tank 4 is semi-cylindrical, and the net-carrying tank 10 is vertically placed in the net-carrying tank 4 . The advantage of this fixing method is that the placement and replacement of the carrier grid does not need to open the cover, which is more convenient.
以上已经描述了本申请的各实施例,上述说明是示例性的,并非穷尽性的,并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下,对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。本文中所用术语的选择,旨在最好地解释各实施例的原理、实际应用或对市场中的技术的改进,或者使本技术领域的其它普通技术人员能理解本文披露的各实施例。Having described various embodiments of the present application above, the foregoing description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and alterations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen to best explain the principle of each embodiment, practical application or improvement of technology in the market, or to enable other ordinary skilled in the art to understand each embodiment disclosed herein.

Claims (15)

  1. 一种粉末样品制备装置,其特征在于,包括:A powder sample preparation device, characterized in that it comprises:
    样本承载台,设有依次连通的管道(5)、样品槽(6)和喷气针孔(7);The sample carrying platform is provided with a pipeline (5), a sample tank (6) and an air injection pinhole (7) connected in sequence;
    所述管道(5)的前端设置有载网槽(4),所述载网槽(4)用于容纳载网(10),所述载网槽(4)与所述管道(5)连通。The front end of the pipeline (5) is provided with a grid-carrying tank (4), the grid-carrying tank (4) is used to accommodate the grid-carrying tank (10), and the grid-carrying tank (4) communicates with the pipeline (5) .
  2. 根据权利要求1所述的粉末样品制备装置,其特征在于,还包括用于固定载网的载网槽盖(3),所述载网槽(4)设于所述载网槽盖(3)上、所述载网槽盖(3)与所述管道(5)之间的连接部上、或由所述载网槽盖(3)的端面和所述样本承载台的端面围合而成。The powder sample preparation device according to claim 1, characterized in that, it also includes a grid tank cover (3) for fixing the grid, and the grid tank (4) is arranged on the grid tank cover (3) ), on the connecting portion between the grid tank cover (3) and the pipeline (5), or surrounded by the end face of the grid tank cover (3) and the end face of the sample carrier become.
  3. 根据权利要求2所述的粉末样品制备装置,其特征在于,所述载网槽(4)设于所述载网槽盖(3)与所述管道(5)之间的连接部的端面,由所述载网槽盖(3)端面与所述连接部端面围合而成,所述连接部设有与载网槽(4)连通的第二孔道,所述第二孔道与所述管道(5)连通。The powder sample preparation device according to claim 2, characterized in that, the grid-carrying tank (4) is arranged on the end face of the connecting portion between the grid-carrying tank cover (3) and the pipeline (5), It is formed by enclosing the end face of the net carrying tank cover (3) and the end face of the connecting part, the connecting part is provided with a second channel communicating with the carrying net tank (4), and the second channel is connected with the pipeline (5) connected.
  4. 根据权利要求3所述的粉末样品制备装置,其特征在于,所述载网槽(4)包括圆柱形和长方体形。The powder sample preparation device according to claim 3, characterized in that, the grid tank (4) includes a cylindrical shape and a rectangular parallelepiped shape.
  5. 根据权利要求2所述的粉末样品制备装置,其特征在于,所述载网槽盖(3)与所述样本承载台之间通过卡扣(1)连接固定;所述载网槽盖(3)的前端设有供握持的手柄(2);所述样品槽(6)为凹槽,所述凹槽上承载粉末样品的面为弧面。The powder sample preparation device according to claim 2, characterized in that, the mesh-carrying tank cover (3) is connected and fixed by a buckle (1) to the sample carrier table; the net-carrying tank cover (3) ) is provided with a handle (2) for holding; the sample tank (6) is a groove, and the surface of the groove carrying the powder sample is an arc surface.
  6. 根据权利要求5所述的粉末样品制备装置,其特征在于,所述凹槽上承载粉末样品的面为圆弧面。The powder sample preparation device according to claim 5, characterized in that, the surface of the groove carrying the powder sample is an arc surface.
  7. 根据权利要求1所述的粉末样品制备装置,其特征在于,所述载网槽(4)设于所述样本承载台上,所述载网槽(4)、管道(5)、样品槽(6)、喷气针孔(7)依次连通。The powder sample preparation device according to claim 1, characterized in that, the grid-carrying tank (4) is arranged on the sample carrier platform, and the grid-carrying tank (4), pipeline (5), sample tank ( 6), the jet pinholes (7) are connected successively.
  8. 根据权利要求1所述的粉末样品制备装置,其特征在于,所述载网槽(4)的深度与载网(10)的厚度适配;所述载网槽(4)中与载网(10)接触的底边或底面,与水平面的夹角为a,0<a<90°;所述载网槽(4)中用于容纳载网(10)的部分为斜柱形或斜台形;所述载网(10)放置在载网槽(4)后的圆心/中心与管道(5)出气口的中心轴重合或几乎重合。The powder sample preparation device according to claim 1, characterized in that, the depth of the grid-carrying tank (4) is adapted to the thickness of the grid-carrying tank (10); 10) The bottom edge or bottom surface in contact, the angle with the horizontal plane is a, 0<a<90°; the part used to accommodate the carrying net (10) in the carrying net groove (4) is inclined columnar or inclined platform ; The center/center of the grid (10) placed behind the grid tank (4) coincides or almost coincides with the central axis of the gas outlet of the pipeline (5).
  9. 根据权利要求1或5所述的粉末样品制备装置,其特征在于,所述样品槽(6)的表面或侧边有刻度标识(61)。The powder sample preparation device according to claim 1 or 5, characterized in that there are scale marks (61) on the surface or side of the sample tank (6).
  10. 根据权利要求1所述的粉末样品制备装置,其特征在于,所述样品槽(6)的上部设有可开合的样品槽盖;还包括底座(9),所述底座(9)设置在所述样本承载台的底部;所述样本承载台的四周设有螺孔,所述底座(9)与所述样本承载台通过螺钉(8)连接。The powder sample preparation device according to claim 1, characterized in that, the top of the sample tank (6) is provided with a sample tank cover that can be opened and closed; it also includes a base (9), and the base (9) is arranged on The bottom of the sample carrier; screw holes are provided around the sample carrier, and the base (9) is connected to the sample carrier by screws (8).
  11. 根据权利要求10所述的粉末样品制备装置,其特征在于,所述底座(9)为工字型。The powder sample preparation device according to claim 10, characterized in that the base (9) is I-shaped.
  12. 根据权利要求10所述的粉末样品制备装置,其特征在于,还包括:外罩,所述外罩将所述样本承载台、底座(9)罩住,所 述外罩设有供微量进样器的针头和喷气针孔连接的开口。The powder sample preparation device according to claim 10, further comprising: an outer cover, the outer cover covers the sample carrier platform and the base (9), and the outer cover is provided with a needle for a micro-sampler The opening that connects to the jet pinhole.
  13. 根据权利要求12所述的粉末样品制备装置,其特征在于,所述外罩还设置有翻盖门。The powder sample preparation device according to claim 12, wherein the outer cover is also provided with a flip door.
  14. 一种粉末样品制备方法,其特征在于,包括以下步骤:A powder sample preparation method is characterized in that, comprising the following steps:
    将载网(10)安装到如权利要求1所述的粉末样品制备装置的载网槽(4)内,并将载网上用于附着颗粒的碳膜一面朝向管道(5)方向;The carrier net (10) is installed in the carrier net tank (4) of the powder sample preparation device as claimed in claim 1, and the carbon film side for attaching particles on the carrier net is facing the pipeline (5) direction;
    将粉末样品放在样品槽(6)中;The powder sample is placed in the sample tank (6);
    通过喷气设备将气体通过喷气针孔(7)注入样品槽(6)中,获得附着粉末样品的载网。The gas is injected into the sample groove (6) through the gas injection needle hole (7) by the gas injection device, so as to obtain the carrier net with the powder sample attached.
  15. 根据权利要求14所述的粉末样品制备方法,其特征在于,所述喷气设备包括空气压缩泵和喷枪,喷枪的进气端与空气压缩泵的出气端连通,喷枪的出气口与连通装置的进气端连通,所述连通装置的出气端与喷气针孔(7)连通;在制样时,通过喷枪将固定流量的空气通过连通装置注入样品槽(6)并带动粉末样品顺着管道(5)喷在载网上。The powder sample preparation method according to claim 14, characterized in that, the air injection device comprises an air compression pump and a spray gun, the air inlet of the spray gun communicates with the air outlet of the air compression pump, and the air outlet of the spray gun communicates with the inlet of the communication device. The gas end is communicated, and the gas outlet end of the communication device is communicated with the air injection pinhole (7); during sample preparation, the air with a fixed flow rate is injected into the sample tank (6) through the communication device through the spray gun and drives the powder sample along the pipeline (5 ) sprayed on the grid.
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