CN103196719A - Micro/nano-particle sample carrying mesh storage device for transmission electron microscope, and sample preparation method - Google Patents
Micro/nano-particle sample carrying mesh storage device for transmission electron microscope, and sample preparation method Download PDFInfo
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- CN103196719A CN103196719A CN2013100836112A CN201310083611A CN103196719A CN 103196719 A CN103196719 A CN 103196719A CN 2013100836112 A CN2013100836112 A CN 2013100836112A CN 201310083611 A CN201310083611 A CN 201310083611A CN 103196719 A CN103196719 A CN 103196719A
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Abstract
The invention provides a micro/nano-particle sample carrying mesh storage device for a transmission electron microscope. The micro/nano-particle sample carrying mesh storage device comprises a clamping handle, a sample carrying mesh and a bottom tray, wherein the bottom tray is provided with a hollow part; the sample carrying mesh is arranged in the hollow part; a clearance is formed between the sample carrying mesh and the edge of the hollow part; the clearance is a flow guide and observation hole; and the clamping handle is connected with the bottom tray, is used for clamping the bottom tray, and is fixed on a matched base is matched with the bottom tray and the clamping handle in shape. The micro/nano-particle sample carrying mesh storage device for the transmission electron microscope has the advantages that in a sample preparation process, the novel carrying mesh and a storage grid are cooperatively used, and the carrying mesh is suspended in the storage grid; and during the fixation of the carrying mesh, the contact between the carrying mesh and each of other solid media is avoided, and the distribution situation of particle samples on the carrying mesh can be directly observed by using bottom light of an optical microscope. Therefore, three defects of the conventional preparation method are overcome, and the sample preparation efficiency is improved.
Description
Technical field
The present invention relates to a kind of transmission electron microscope with the preparation method of micro-nano particulate samples, belong to micro-nano particulate material technical field of quality detection.
Background technology
For the particle of micron, nano-scale, transmission electron microscope is one of effective testing tool few in number that its microscopic appearance, structure, chemical constitution are observed, detected.When using transmission electron microscope to carry out observation analysis, particulate samples must be placed on carrying on the net supporting film of microscope special use, therefore need adopt suitable method that sample dispersion is being carried on the net supporting film before observation.Sample is carrying density, the homogeneity that the net supporting film distributes, and can directly have influence on the quality of microphoto.
Transmission electron microscope with the preparation method commonly used of micro-nano particulate samples is at present: will carry the net supporting film and directly be placed on the filter paper, the suspension that will contain particulate samples then drops in and carries on the net, finishes preparation finally by oven dry.But this method uncontrollable factor is more, and the most outstanding 3 are: 1. year net also contacts with filter paper except with sample contacts, if filter paper contains impurity, and may contaminated samples; 2. carry net and only be placed on the filter paper, there is no other fixation, therefore in preparation process, during such as suspension dropping, extraneous variations in flow, may make and carry mobile, the upset of net, cause sample preparation to be failed; 3. because the existence of filter paper makes the end light that can't use optical microscope effectively observe the distribution density of carrying online sample, thereby can't effectively determine suitable suspension dripping quantity that sample preparation efficient is not high.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of used in transmission electron microscope micro-nano particulate samples to carry net storage facility and sample preparation methods.
In order to address the above problem, the invention provides a kind of used in transmission electron microscope micro-nano particulate samples and carry the net storage facility, comprise that grip shank, sample carry 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, is used for the described bottom tray of clamping, and is fixed on the supporting base that matches with the shape of bottom tray and grip shank.
The present invention further provides a kind of sample preparation methods, adopted above-mentioned device, comprised the steps: to provide the suspension of testing sample; Sample is carried the hollow bulb that net is placed on bottom tray; The gripping grip shank will be carried the net storage facility and will be placed on the filter paper; Drip suspension to carrying online and oven dry; The sample that makes is placed on the supporting base in order to preserve together with carrying the net storage facility.
Optionally, after dripping suspension, further comprise the steps: the storage grid is placed in the optical microscope, utilize top light and end light to observe and carry online distribution of particles density; If less then repetition of density drips, until obtaining suitable particle density, finish specimen preparation, if density is too high then to prepare suspension again, and repeat above-mentioned institute in steps.
Optionally, the preparation method of described testing sample suspension comprises: the sample powder that takes a morsel is put into test tube; Situation adds suitable quantity of water or easy volatile solvent per sample; Test tube is put into the ultrasonic cleaning machine, sample powder is fully disperseed in solvent.
The invention has the advantages that, in the specimen preparation process, be used novel year net and stored grid, carry net unsettled placement in storing grid, when fixing year nets, avoided year net to contact with other solid state medium, and light of the microscopical end of available optics is directly observed the distribution situation of carrying online particulate samples.Thereby overcome 3 deficiencies of above-mentioned traditional preparation process method, improved specimen preparation efficient.
Description of drawings
Accompanying drawing 1 is the front view of the described device of 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 particulate samples provided by the invention carries net storage facility and sample preparation methods is elaborated.
Provide the structural representation that used in transmission electron microscope micro-nano particulate samples of the present invention carries the net storage facility at first by reference to the accompanying drawings, accompanying drawing 1 is the front view of the described device of this embodiment, and accompanying drawing 2 is cut-open views of accompanying drawing 1.With reference to the accompanying drawings 1 and accompanying drawing 2 shown in, described year net storage facility comprises that grip shank 3, sample carry 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, is used for the described bottom tray 1 of clamping, and is fixed on the supporting base that matches with the shape of bottom tray 1 and grip shank 3.
From accompanying drawing 2 as can be seen, sample carries net 2 in hollow bulb, and two relative marginal portion and bottom tray 1 overlap, and play fixation, and remainder and bottom tray 1 have the space, and this space can be used as water conservancy diversion and viewport 4.
Owing to be provided with bottom tray 1, sample carries net 2 can unsettledly be placed, and has avoided the problems of using filter paper to bring.
Adopt said apparatus that sample is prepared, generally include following method:
1, the micro-nano particulate samples powder that takes a morsel is put into test tube, and situation per sample adds in right amount such as easy volatile solvent such as water, alcohol then; Test tube is put into the ultrasonic cleaning machine, the micro-nano particle is fully disperseed in solvent, it is stand-by to obtain suspension;
2, will carry net with tweezers is placed in the storage grid;
3, clamp the grip shank of storing grid with tweezers, will store grid and be placed on the filter paper, a year net is faced up;
4, use dropper, drip 1-2 and drip suspension to carrying on the net;
5, use infrared lamp will carry the net oven dry;
6, will store grid and be placed in the optical microscope, and utilize top light and end light to observe and carry online distribution of particles density;
7, if the less then repeating step 4 to 6 of density until obtaining suitable particle density, is finished specimen preparation; If the too high suspension concentration that then reduces of density, repeating step 1 to 6 until obtaining suitable particle density, is finished specimen preparation;
8, the sample that makes is placed on the supporting base in order to preserve together with storing grid.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle 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. a used in transmission electron microscope micro-nano particulate samples carries the net storage facility, it is characterized in that, comprises that grip shank, sample carry 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, is used for the described bottom tray of clamping, and is fixed on the supporting base that matches with the shape of bottom tray and grip shank.
2. a sample preparation methods adopts the described device of claim 1, it is characterized in that, comprises the steps:
The suspension of testing sample is provided;
Sample is carried the hollow bulb that net is placed on bottom tray;
The gripping grip shank will be carried the net storage facility and will be placed on the filter paper;
Drip suspension to carrying online and oven dry;
The sample that makes is placed on the supporting base in order to preserve together with carrying the net storage facility.
3. sample preparation methods according to claim 2 is characterized in that, after dripping suspension, further comprises the steps:
To store grid and be placed in the optical microscope, and utilize top light and end light to observe and carry online distribution of particles density;
If less then repetition of density drips, until obtaining suitable particle density, finish specimen preparation, if density is too high then to prepare suspension again, and repeat above-mentioned institute in steps.
4. sample preparation methods according to claim 2 is characterized in that, the preparation method of described testing sample suspension comprises:
The sample powder that takes a morsel is put into test tube;
Situation adds suitable quantity of water or easy volatile solvent per sample;
Test tube is put into the ultrasonic cleaning machine, sample powder is fully disperseed in solvent.
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| Application Number | Priority Date | Filing Date | Title |
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| 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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| 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 true CN103196719A (en) | 2013-07-10 |
| CN103196719B CN103196719B (en) | 2015-08-05 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104568565A (en) * | 2014-08-28 | 2015-04-29 | 中国科学院生物物理研究所 | Sample clamping tool and transfer box for frozen water-containing slices prepared by focused ion beam method |
| CN104792594A (en) * | 2015-04-22 | 2015-07-22 | 浙江大学 | Combined appliance suitable for slice fishing of slit grids |
| CN105316636A (en) * | 2015-11-20 | 2016-02-10 | 苏州赛森电子科技有限公司 | Degassing device in magnetic control direct current sputtering system |
| CN105675636A (en) * | 2016-01-21 | 2016-06-15 | 济南大学 | XRD (X-ray diffraction) quantitative analysis method based on gypsum minerals in cement-based materials |
| CN105910875A (en) * | 2016-05-27 | 2016-08-31 | 中国科学院微生物研究所 | Fixing device for sample-loading copper grid |
| CN109735449A (en) * | 2019-03-08 | 2019-05-10 | 金婧菲 | A kind of online culture apparatus of biological tissue and observation method |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 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 |
| WO2023087474A1 (en) * | 2021-11-19 | 2023-05-25 | 深圳晶泰科技有限公司 | Preparation device and method for powder sample |
| CN117804872A (en) * | 2024-02-28 | 2024-04-02 | 广州智达实验室科技有限公司 | Electronic microscope sample preparation system and control method |
| CN118010408A (en) * | 2024-04-09 | 2024-05-10 | 河南工学院 | Concrete strength detection device |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104568565B (en) * | 2014-08-28 | 2017-06-06 | 中国科学院生物物理研究所 | Focused ion beam method prepares the sample clamping tool and transfer box of the aqueous section of freezing |
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| CN104792594A (en) * | 2015-04-22 | 2015-07-22 | 浙江大学 | Combined appliance suitable for slice fishing of slit grids |
| 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 |
| CN105316636A (en) * | 2015-11-20 | 2016-02-10 | 苏州赛森电子科技有限公司 | Degassing device in magnetic control direct current sputtering system |
| CN105675636A (en) * | 2016-01-21 | 2016-06-15 | 济南大学 | XRD (X-ray diffraction) quantitative analysis method based on gypsum minerals in cement-based materials |
| CN105910875A (en) * | 2016-05-27 | 2016-08-31 | 中国科学院微生物研究所 | Fixing device for sample-loading copper grid |
| CN110595848A (en) * | 2018-06-12 | 2019-12-20 | 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 |
| WO2023087474A1 (en) * | 2021-11-19 | 2023-05-25 | 深圳晶泰科技有限公司 | Preparation device and method for powder sample |
| CN117804872A (en) * | 2024-02-28 | 2024-04-02 | 广州智达实验室科技有限公司 | Electronic microscope sample preparation system and control method |
| CN117804872B (en) * | 2024-02-28 | 2024-05-28 | 广州智达实验室科技有限公司 | Electronic microscope sample preparation system and control method |
| CN118010408A (en) * | 2024-04-09 | 2024-05-10 | 河南工学院 | Concrete strength detection device |
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