CN1206697C - Micro grating for transmissive electron microscope and its making process - Google Patents

Micro grating for transmissive electron microscope and its making process Download PDF

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Publication number
CN1206697C
CN1206697C CN 03105357 CN03105357A CN1206697C CN 1206697 C CN1206697 C CN 1206697C CN 03105357 CN03105357 CN 03105357 CN 03105357 A CN03105357 A CN 03105357A CN 1206697 C CN1206697 C CN 1206697C
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China
Prior art keywords
film
electron microscope
acetone
collodion
amyl acetate
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CN 03105357
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CN1433044A (en
Inventor
李巧玲
叶云
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North University of China
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李巧玲
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Abstract

The present invention relates to a micro grating for a transmission electron microscope and a manufacturing method thereof. The present invention mainly solves the technical problems of complicated manufacture, low productive efficiency, low thermal stability and easy deformation which exist in the existing micro grating. The present invention has the technical scheme that the micro grating for the transmission electron microscope is made from the ingredients of the following weight percentages: 1% to 5% of acetone, 39% to 60% of Amyl acetate and 38% to 60% of collodion. The manufacturing method of the micro grating comprises: (1) first, the amyl acetate and the collodion are mixed and prepared; then, the acetone is added to the mixed liquid, and the acetone and the mixed liquid which are made uniform are made into mixed liquid; (2) the mixed liquid is dripped in a culture dish drip by drip, and a copper screen is placed on the liquid surface immediately; (3) after a layer of film is formed on the liquid surface, filter paper is flatly attached onto the film; subsequently, the film is lifted out of the water surface together with the copper screen; (4) the film is cut off, and the film which comprises the copper screen is put into a sample chamber in the transmission electron microscope; (5) high pressure is added to the microscope, and the micro grating for a transmission electron microscope is made.

Description

Micro grating for transmissive electron microscope and preparation method thereof
One, technical field:
The present invention relates to a kind of Micro grating for transmissive electron microscope and preparation method thereof, it belongs to little grid that a kind of transmission electron microscope uses and preparation method thereof.
Two, background technology:
Astigmatism be the electron microscope endoporus circle, up and down pole shoe axial offset, make around the irregular and pole shoe bore of the material material of pole shoe reason such as local pollution and cause.This nonrotary symmetry in lens magnetic field can make its focusing power in different directions difference occur, can not be focused into a bit on as the plane after making imaging object point scioptics, directly influences the resolution of electron microscope.In order to solve this difficult point, people work out little grid to solve the astigmatism problem of electron microscope.As little grid of " Electron Microscopy " (the luxuriant male work P55 page or leaf of [Japan] sakata) record is exactly wherein a kind of.This little grid are made with collodion.Its manufacture method is: put into water earlier in the container of producing the collodion supporting film, floating all around have ice cube, the metallic plate submerged, is placed with sheet glass on the plate, is placed with wire netting on sheet glass; Then 10% collodion is splashed into one, drop launches at the water surface at once, breathes out without a break on the drop surface after several minutes, and about mistake just can be pulled wire netting and film out after two minutes together, drying, and little grid are promptly made in the processing of burning at last.Though this little grid can solve the astigmatism problem of electron microscope, there is make complicated, production efficiency is low and poor heat stability and shortcoming such as yielding.
Three, summary of the invention:
The objective of the invention is to solve low and poor heat stability of making complexity, production efficiency that existing little grid exist and yielding technological difficulties and provide a kind of makings simply, production efficiency is high and Heat stability is good and on-deformable Micro grating for transmissive electron microscope and preparation method thereof.
For realizing above-mentioned task, the technical solution used in the present invention is: this Micro grating for transmissive electron microscope, and it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 1~5% n-amyl acetate 39~60% collodions 38~60%.
The production method of above-mentioned Micro grating for transmissive electron microscope is: it comprises the following steps:
1) at first is 39~60% n-amyl acetate and 38~60% collodion mixed preparing with percentage by weight, be that 1~5% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and make it even, make the mixed liquor of n-amyl acetate, collodion and acetone;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor with diameter;
3) after several minutes after forming thin film on the liquid level of culture dish, be pressed in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) along the copper mesh edge film is severed, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, acetone is evaporated from film form the micropore hole.
Because the present invention adopted technique scheme, therefore compare with background technology, have make simple, production efficiency is high and Heat stability is good and advantage such as not yielding.Product percent of pass of the present invention can reach more than 98%, and is higher more than 20% than the qualification rate of background technology.
Four, embodiment:
Embodiment 1:
Micro grating for transmissive electron microscope in the present embodiment, it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 1% n-amyl acetate 39% collodion 60%.
The production method of above-mentioned Micro grating for transmissive electron microscope is: it comprises the following steps:
1) at first is 39% n-amyl acetate and 60% collodion mixed preparing, is that 1% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and makes it even, make the mixed liquor of n-amyl acetate, collodion and acetone percentage by weight;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor at once with diameter;
3) after 3 minutes after forming thin film on the liquid level of culture dish, be pressed into gently in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) carefully film is severed along the copper mesh edge, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, make acetone promptly from film evaporation form the micropore hole and promptly make Micro grating for transmissive electron microscope.
Embodiment 2:
Micro grating for transmissive electron microscope in the present embodiment, it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 5% n-amyl acetate 55% collodion 40%.
The production method of above-mentioned Micro grating for transmissive electron microscope is: it comprises the following steps:
1) at first is 55% n-amyl acetate and 40% collodion mixed preparing, is that 5% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and makes it even, make the mixed liquor of n-amyl acetate, collodion and acetone percentage by weight;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor at once with diameter;
3) after 2 minutes after forming thin film on the liquid level of culture dish, be pressed into gently in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) carefully film is severed along the copper mesh edge, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, make acetone promptly from film evaporation form the micropore hole and promptly make Micro grating for transmissive electron microscope.
Embodiment 3:
Micro grating for transmissive electron microscope in the present embodiment, it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 2% n-amyl acetate 60% collodion 38%.
The production method of above-mentioned Micro grating for transmissive electron microscope is: it comprises the following steps:
1) at first is 60% n-amyl acetate and 38% collodion mixed preparing, is that 2% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and makes it even, make the mixed liquor of n-amyl acetate, collodion and acetone percentage by weight;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor at once with diameter;
3) after 4 minutes after forming thin film on the liquid level of culture dish, be pressed into gently in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) carefully film is severed along the copper mesh edge, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, make acetone promptly from film evaporation form the micropore hole and promptly make Micro grating for transmissive electron microscope.
Embodiment 4:
Micro grating for transmissive electron microscope in the present embodiment, it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 3% n-amyl acetate 50% collodion 47%.
The production method of above-mentioned Micro grating for transmissive electron microscope is: it comprises the following steps:
1) at first is 50% n-amyl acetate and 47% collodion mixed preparing, is that 3% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and makes it even, make the mixed liquor of n-amyl acetate, collodion and acetone percentage by weight;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor at once with diameter;
3) after 2 minutes after forming thin film on the liquid level of culture dish, be pressed into gently in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) carefully film is severed along the copper mesh edge, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, make acetone promptly from film evaporation form the micropore hole and promptly make Micro grating for transmissive electron microscope.
Embodiment 5:
Micro grating for transmissive electron microscope in the present embodiment, it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 4% n-amyl acetate 45% collodion 51%.
The production method of above-mentioned Micro grating for transmissive electron microscope is: it comprises the following steps:
1) at first is 45% n-amyl acetate and 51% collodion mixed preparing, is that 4% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and makes it even, make the mixed liquor of n-amyl acetate, collodion and acetone percentage by weight;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor at once with diameter;
3) after 3 minutes after forming thin film on the liquid level of culture dish, be pressed into gently in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) carefully film is severed along the copper mesh edge, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, make acetone promptly from film evaporation form the micropore hole and promptly make Micro grating for transmissive electron microscope.

Claims (2)

1, a kind of Micro grating for transmissive electron microscope is characterized in that: it is made by acetone, n-amyl acetate and collodion, and its percentage by weight is:
Acetone 1~5% n-amyl acetate 39~60% collodions 38~60%.
2, a kind of production method for preparing the described Micro grating for transmissive electron microscope of claim 1, it is characterized in that: it comprises the following steps:
1) at first is 39~60% n-amyl acetate and 38~60% collodion mixed preparing with percentage by weight, be that 1~5% acetone adds in the above-mentioned mixed liquor then with percentage by weight, and make it even, make the mixed liquor of n-amyl acetate, collodion and acetone;
2) in the culture dish of distilled water is housed, the mixed liquor of the n-amyl acetate, collodion and the acetone that prepare is splashed into one, be that the copper mesh of 3mm is put down gently on the liquid level of mixed liquor with diameter;
3) after several minutes after forming thin film on the liquid level of culture dish, be pressed in the water on it with filter paper is smooth, leave the water together with copper mesh and film subsequently;
4) along the copper mesh edge film is severed, the film that makes the film that contains copper mesh separate and will contain copper mesh with filter paper is then put into the sample room of transmission electron microscope;
5) add the high pressure of 150KV to transmission electron microscope, acetone is evaporated from film form the micropore hole.
CN 03105357 2003-02-26 2003-02-26 Micro grating for transmissive electron microscope and its making process Expired - Fee Related CN1206697C (en)

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Application Number Priority Date Filing Date Title
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CN1206697C true CN1206697C (en) 2005-06-15

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101276724B (en) * 2007-03-30 2011-06-22 北京富纳特创新科技有限公司 Transmission electron microscope micro grid and preparing method thereof
US8294098B2 (en) 2007-03-30 2012-10-23 Tsinghua University Transmission electron microscope micro-grid
TWI400738B (en) * 2009-08-31 2013-07-01 Hon Hai Prec Ind Co Ltd Transmission electron microscope grid

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101609771B (en) * 2008-06-20 2010-12-08 清华大学 Method for preparing transmission electron microscope micro-grids
CN102194623B (en) * 2010-03-17 2013-11-20 清华大学 Preparation method of transmission electron microscope microgrid
CN102315058B (en) 2010-07-07 2013-12-11 清华大学 Transmission electron microscope microgrid and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101276724B (en) * 2007-03-30 2011-06-22 北京富纳特创新科技有限公司 Transmission electron microscope micro grid and preparing method thereof
US8294098B2 (en) 2007-03-30 2012-10-23 Tsinghua University Transmission electron microscope micro-grid
TWI400738B (en) * 2009-08-31 2013-07-01 Hon Hai Prec Ind Co Ltd Transmission electron microscope grid

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