CN103196719B - Used in transmission electron microscope micro-nano particle sample carries net storage facility and sample preparation methods - Google Patents
Used in transmission electron microscope micro-nano particle sample carries net storage facility and sample preparation methods Download PDFInfo
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- CN103196719B CN103196719B CN201310083611.2A CN201310083611A CN103196719B CN 103196719 B CN103196719 B CN 103196719B CN 201310083611 A CN201310083611 A CN 201310083611A CN 103196719 B CN103196719 B CN 103196719B
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Abstract
The invention provides a kind of used in transmission electron microscope micro-nano particle sample and carry net storage facility, comprise grip shank, sample carries net and bottom tray; Described bottom tray has a hollow bulb, and described sample carries net and is arranged at described hollow bulb, and has a gap with the edge of described hollow bulb, and described gap is water conservancy diversion and viewport; Described grip shank is connected with bottom tray, for clamping described bottom tray, and is fixed on the supporting base that closes with the matching form of bottom tray and grip shank.The invention has the advantages that, with the use of novel year net storage grid in Sample Preparation Procedure, carry net unsettled placement in storage grid, while fixing year net, avoid a year net to contact with other solid state medium, and available optical microscopical end light directly observes the distribution situation of carrying online particulate samples.Thus overcome 3 deficiencies of above-mentioned traditional preparation methods, improve sample preparation efficiency.
Description
Technical field
The present invention relates to a kind of preparation method of transmission electron microscope micro-nano particle sample, belong to micro-nano particle quality of materials detection technique field.
Background technology
For the particle of micron, nano-scale, transmission electron microscope is one of effective testing tool few in number observed its microscopic appearance, structure, chemical composition, detect.When using transmission electron microscope to carry out observation analysis, particulate samples must be placed on special the carrying on net supporting film of microscope, therefore needs before observation, adopt suitable method sample dispersion being carried on net supporting film.Sample, carrying density, homogeneity that net supporting film distributes, directly can have influence on the quality of microphoto.
The conventional preparation method of current transmission electron microscope micro-nano particle sample is: will carry net supporting film and directly be placed on filter paper, is then dropped in by the suspension containing particulate samples and carries on the net, complete preparation finally by oven dry.But this method uncontrollable factor is more, the most outstanding 3 are: 1. year net is except with except sample contacts, also contacts with filter paper, if filter paper contains impurity, and may contaminated samples; 2. year net is only placed on filter paper, there is no other fixation, therefore in preparation process, when such as suspension drips, external air flow changes, may make to carry and net mobile, upset, cause sample preparation failed; 3., due to the existence of filter paper, make to use the end light of optical microscope effectively to observe the distribution density of carrying online sample, thus effectively cannot determine suitable suspension dripping quantity, sample preparation efficiency is not high.
Summary of the invention
Technical matters to be solved by this invention is, provides a kind of used in transmission electron microscope micro-nano particle sample to carry net storage facility and sample preparation methods.
In order to solve the problem, the invention provides a kind of used in transmission electron microscope micro-nano particle sample and carrying net storage facility, comprising grip shank, sample carries net and bottom tray; Described bottom tray has a hollow bulb, and described sample carries net and is arranged at described hollow bulb, and has a gap with the edge of described hollow bulb, and described gap is water conservancy diversion and viewport; Described grip shank is connected with bottom tray, for clamping described bottom tray, and is fixed on the supporting base that closes with the matching form of bottom tray and grip shank.
Invention further provides a kind of sample preparation methods, adopt above-mentioned device, comprise the steps: the suspension that testing sample is provided; Sample is carried the hollow bulb that net is placed on bottom tray; Gripping grip shank, will carry net storage facility and be placed on filter paper; Drip suspension to carrying online and drying; Obtained sample is placed on supporting base to preserve together with carrying net storage facility.
Optionally, after dropping suspension, comprise the steps: storage grid to be placed in optical microscope further, utilize top light and end light to observe and carry online distribution of particles density; If density is less, repeats to drip, until obtain suitable particle density, complete sample preparation, if density is too high, again prepare suspension, and repeat above-mentioned in steps.
Optionally, the preparation method of described testing sample suspension comprises: the sample powder that takes a morsel puts into test tube; Situation per sample, adds suitable quantity of water or easy volatile solvent; Test tube is put into supersonic cleaning machine, sample powder is fully disperseed in a solvent.
The invention has the advantages that, with the use of novel year net storage grid in Sample Preparation Procedure, carry net unsettled placement in storage grid, while fixing year net, avoid a year net to contact with other solid state medium, and available optical microscopical end light directly observes the distribution situation of carrying online particulate samples.Thus overcome 3 deficiencies of above-mentioned traditional preparation methods, improve sample preparation efficiency.
Accompanying drawing explanation
Accompanying drawing 1 is the front view of device described in the specific embodiment of the invention.
Accompanying drawing 2 is cut-open views of accompanying drawing 1.
Embodiment
Below in conjunction with accompanying drawing, the embodiment that used in transmission electron microscope micro-nano particle sample provided by the invention carries net storage facility and sample preparation methods is elaborated.
First provide by reference to the accompanying drawings the structural representation that used in transmission electron microscope micro-nano particle sample of the present invention carries net storage facility, accompanying drawing 1 is the front view of device described in this embodiment, and accompanying drawing 2 is cut-open views of accompanying drawing 1.With reference to shown in accompanying drawing 1 and accompanying drawing 2, described year net storage facility comprises grip shank 3, sample carries net 2 and bottom tray 1.Described bottom tray 1 has a hollow bulb, and described sample carries net 2 and is arranged at described hollow bulb, and has a gap with the edge of described hollow bulb, and described gap is water conservancy diversion and viewport 4; Described grip shank 3 is connected with bottom tray 1, for clamping described bottom tray 1, and is fixed on the supporting base that closes with the matching form of bottom tray 1 and grip shank 3.
As can be seen from accompanying drawing 2, sample carries net 2 in hollow bulb, and two relative marginal portions and bottom tray 1 overlap, and play fixation, and remainder and bottom tray 1 have space, this space can as water conservancy diversion and viewport 4.
Owing to being provided with bottom tray 1, sample carries net 2 can unsettledly be placed, and avoids the problems using filter paper to bring.
Adopt said apparatus to be prepared sample, generally include following method:
1, the micro-nano particle sample powder that takes a morsel puts into test tube, then situation per sample, adds the appropriate such as easy volatile solvent such as water, alcohol; Test tube is put into supersonic cleaning machine, micro-nano particle is fully disperseed in a solvent, obtains suspension stand-by;
2, will carry net with tweezers is placed in storage grid;
3, clamp the grip shank of storage grid with tweezers, storage grid is placed on filter paper, make to carry net and face up;
4, use dropper, drip 1-2 and drip suspension to carrying on the net;
5, use infrared lamp will carry net to dry;
6, storage grid is placed in optical microscope, utilizes top light and end light to observe and carry online distribution of particles density;
If 7 density are less, repeat step 4 to 6, until obtain suitable particle density, complete sample preparation; If density is too high, reduce turbid liquid concentration, repeat step 1 to 6, until obtain suitable particle density, complete sample preparation;
8, obtained sample is placed on supporting base to preserve together with storage grid.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. used in transmission electron microscope micro-nano particle sample carries a net storage facility, it is characterized in that, comprises grip shank, sample carries net and bottom tray; Described bottom tray has a hollow bulb, described sample carries net and is arranged at described hollow bulb, and described sample carries two relative marginal portions and the bottom tray overlap joint of net, plays fixation, remainder and bottom tray have gap, and described gap is water conservancy diversion and viewport; Described grip shank is connected with bottom tray, for clamping described bottom tray, and is fixed on the supporting base that closes with the matching form of bottom tray and grip shank.
2. a sample preparation methods, adopts the device described in claim 1, it is characterized in that, comprise the steps:
The suspension of testing sample is provided;
Sample is carried the hollow bulb that net is placed on bottom tray;
Gripping grip shank, will carry net storage facility and be placed on filter paper;
Drip suspension to carrying online and drying;
Obtained sample is placed on supporting base to preserve together with carrying net storage facility.
3. according to the sample preparation methods described in claim 2, it is characterized in that, after dropping suspension, comprise the steps: storage grid to be placed in optical microscope further, utilize top light and end light to observe and carry online distribution of particles density;
If density is less, repeats to drip, until obtain suitable particle density, complete sample preparation, if density is too high, again prepare suspension, and repeat above-mentioned in steps.
4. according to the sample preparation methods described in claim 2, it is characterized in that, the preparation method of described testing sample suspension comprises: the sample powder that takes a morsel puts into test tube; Situation per sample, adds suitable quantity of water or easy volatile solvent;
Test tube is put into supersonic cleaning machine, sample powder is fully disperseed in a solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310083611.2A CN103196719B (en) | 2013-03-17 | 2013-03-17 | Used in transmission electron microscope micro-nano particle sample carries net storage facility and sample preparation methods |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310083611.2A CN103196719B (en) | 2013-03-17 | 2013-03-17 | Used in transmission electron microscope micro-nano particle sample carries net storage facility and sample preparation methods |
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| CN103196719A CN103196719A (en) | 2013-07-10 |
| CN103196719B true CN103196719B (en) | 2015-08-05 |
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| CN104198242A (en) * | 2014-08-28 | 2014-12-10 | 中国科学院生物物理研究所 | Sample clamping tool and transferring box for preparing frozen moisture contained chips by focused ion beam method |
| CN104792594B (en) * | 2015-04-22 | 2017-12-12 | 浙江大学 | The combined utensil of piece is dragged for suitable for slit contained network |
| CN105316636B (en) * | 2015-11-20 | 2018-04-06 | 苏州赛森电子科技有限公司 | Depassing unit in magnetic control d.c. sputtering system |
| CN105675636B (en) * | 2016-01-21 | 2018-06-26 | 济南大学 | A kind of XRD quantitative analysis methods based on gypsoide in cement-based material |
| CN105910875B (en) * | 2016-05-27 | 2019-05-14 | 河南中镜科仪科技有限公司 | A kind of fixed device of load sample copper mesh |
| CN110595848B (en) * | 2018-06-12 | 2022-04-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of micron-sized particle transmission electron microscope sample |
| CN109735449A (en) * | 2019-03-08 | 2019-05-10 | 金婧菲 | A kind of online culture apparatus of biological tissue and observation method |
| CN114002246A (en) * | 2021-11-19 | 2022-02-01 | 深圳晶泰科技有限公司 | Powder sample preparation device and method |
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| CN103196719A (en) | 2013-07-10 |
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