CN101216386A - Thin film material transmission electron microscope sample preparation method - Google Patents
Thin film material transmission electron microscope sample preparation method Download PDFInfo
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- CN101216386A CN101216386A CNA2007101441177A CN200710144117A CN101216386A CN 101216386 A CN101216386 A CN 101216386A CN A2007101441177 A CNA2007101441177 A CN A2007101441177A CN 200710144117 A CN200710144117 A CN 200710144117A CN 101216386 A CN101216386 A CN 101216386A
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Abstract
The preparation method of a transmission electronic microscope sample containing thin-film material relates to an electronic microscope sample, in particular to a method for preparing the transmission electronic microscope sample containing thin-film materials of various components and thicknesses by magnetron sputtering at a temperature below 400 DEG C. The preparation method has simple preparation process and higher success rate. The method comprises the following steps of: plating a film on a thin film substrate made of thermosetting polyimide by magnetron sputtering coating method, placing the plated thin film in a double-connection net; soaking the double-connection net and the thin film in 80% hydrazine hydrate, taking out, and cleaning in ethanol when the thermosetting polyimide dissolves completely; and thinning the cleaned double-connection net by an ion milling at an angle of 6 to 9 DEG until the double-connection net is leaked.
Description
Technical field
The present invention relates to a kind of electron microscopic sample, especially relate to the preparation method of sample for use in transmitted electron microscope of the membraneous material of a kind of various compositions that are suitable for magnetron sputtering below 400 ℃ preparation, all thickness.
Background technology
Transmission electron microscope is one of important instrument of research material micromechanism, but the prerequisite that can observe on transmission electron microscope is the electron beam of transmission electron microscope can penetrate sample, and transmission electron microscope observing to the quality of image depend on sample thickness strongly, so the observed position of sample must be extremely thin.The ability that electron beam penetrates solid sample depends primarily on the atomic number that accelerating potential and sample are formed.In general, accelerating potential is high more, and the sample atoms ordinal number is more little, and electron beam can penetrate that sample thickness is just big more, and general sample thickness will be controlled at 5～200mm, and this brings very big difficulty just for transmission electron microscope sample preparation work.For non-dusty material, successfully observe transmission electron microscope, 90% energy consumption is in sample preparation.At present, transmission electron microscope observing is a thinning technique with the basic preparation method of sample, earlier to the bulk sample punching, adopts the pre-attenuate of mechanical buffing or chemically polishing method then, when being thinned to below the 50 μ m pit in advance again, handles until about 30 μ m material, at last attenuate again.The method of attenuate have ultra-thin section, electropolishing, chemical polishing and ion milling etc. (Yang Nanru. Inorganic Non-metallic Materials method of testing [M], Wuhan: publishing house of Wuhan University of Technology, 2004:125-126).Material success ratio after a series of pre-reduction processing of process is very low, and causes pollution easily and introduce illusion, has a strong impact on the analysis of sample.At present,, yet there are no effective solution in the existing literature record, depend on the experience for preparing the people to a great extent for these problems.
Summary of the invention
The objective of the invention is to contaminated easily at film sample in the preparation process of existing sample for use in transmitted electron microscope, break and introduce problems such as illusion, the preparation method of the sample for use in transmitted electron microscope of the membraneous material that a kind of preparation process is simple, success ratio is higher is provided.
Technical scheme of the present invention is:
1) adopt magnetron sputtering coating method to prepare film, the substrate of film is Thermocurable polyimide (polyimide);
2) film behind the plated film is put into the duplex net;
3) in the hydrazine hydrate with duplex net and film immersion 80%, treat that Thermocurable polyimide dissolves fully, taking-up is put into alcohol and is cleaned;
4) the duplex net after will cleaning is put into the ion milling instrument, and use angle carries out attenuate for 6～9 °, till subtracting leakage.
Adopting magnetron sputtering coating method to prepare the base vacuum degree of film minimum is 10
-4Pa magnitude, sputtering atmosphere are Ar gas, and air pressure is 0.5～1.3Pa, and sputtering power is 200～300W, and sputter temperature is-260～400 ℃.The thickness of Thermocurable polyimide can be 30～80 μ m.
Film behind the plated film is preferably made the film that is of a size of (2～3) mm * (2～3) mm, puts into the duplex net again.
Duplex net and film immersed in 80% the hydrazine hydrate 3h at least.
Compare with the preparation method of existing sample for use in transmitted electron microscope, outstanding advantage of the present invention is: provide a kind of technology simple, the sample for use in transmitted electron microscope preparation method that success ratio is high, solved in the sample for use in transmitted electron microscope traditional preparation process process film sample contaminated easily, break and introduce problems such as illusion.The present invention is fit to the various compositions of magnetron sputtering preparation, the sample for use in transmitted electron microscope of all thickness film, its topmost characteristics are not need complicated pre-thinning process to prepare sample, do not damage the original structure and the composition of sample, and cost is low, process is simple, uses very extensive.
Description of drawings
Fig. 1 prepares Co-V thin film transmission electron microscope microstructure photograph for embodiment of the invention magnetron sputtering.In Fig. 1, scale is 20nm.
Embodiment
Embodiment 1
Adopt magnetron sputtering plating, the Co-V alloys target is a negative electrode, and polyimide is fixed in pallet as substrate.Be evacuated to 10 earlier during sputter
-4The pa magnitude feeds a certain amount of Ar gas then, and air pressure is controlled at 0.7Pa.Sputtering power is 300W, and sputter temperature is 300 ℃, and sputtering time is 30min, and recording thickness is 600nm.The substrate that plates film is fixed in the duplex net, put into 80% hydrazine hydrate and soak 3h, treat that polyimide dissolves fully, put into alcohol then and clean, put into two spray ion milling instrument attenuates at last until light leak, just obtain transmission electron microscope observing sample (referring to Fig. 1).
Embodiment 2
Adopt magnetron sputtering coating method to prepare film, adopt the Co-V alloys target.The substrate of film is Thermocurable polyimide (polyimide), and thickness is 50 μ m; The base vacuum degree is 8 * 10
-4Pa, sputtering atmosphere are Ar gas, and air pressure is 0.7Pa, and sputtering power is 300W, and sputtering time is 30min, and sputter temperature is 400 ℃; Film behind the plated film made be of a size of 2mm * 3mm, put into the duplex net then; 3h in the hydrazine hydrate of duplex net and film immersion 80%, treat that Thermocurable polyimide dissolves fully, taking-up is put into alcohol and is cleaned; Duplex net after cleaning is put into the ion milling instrument, and use angle carries out attenuate for 6 °, till subtracting leakage.
Embodiment 3
Adopt magnetron sputtering coating method to prepare film, adopt the Co-V alloys target.The substrate of film is Thermocurable polyimide (polyimide), and thickness is 30 μ m; The base vacuum degree is 8 * 10
-4Pa, sputtering atmosphere are Ar gas, and air pressure is 0.5Pa, and sputtering power is 200W, and sputtering time is 30min, and sputter temperature is a room temperature; Film behind the plated film made be of a size of 3mm * 3mm, put into the duplex net then; 4h in the hydrazine hydrate of duplex net and film immersion 80%, treat that Thermocurable polyimide dissolves fully, taking-up is put into alcohol and is cleaned; Duplex net after cleaning is put into the ion milling instrument, and use angle carries out attenuate for 8 °, till subtracting leakage.
Embodiment 4
Adopt magnetron sputtering coating method to prepare film, adopt the Co-V alloys target.The substrate of film is Thermocurable polyimide (polyimide), and thickness is 801 μ m; The base vacuum degree is 8 * 10
-4Pa, sputtering atmosphere are Ar gas, and air pressure is 1.3Pa, and sputtering power is 300W, and sputtering time is 30min, and it is-196 ℃ that substrate adopts the cooled with liquid nitrogen temperature; Film behind the plated film made be of a size of 2mm * 2mm, put into the duplex net then; 8h in the hydrazine hydrate of duplex net and film immersion 80%, treat that Thermocurable polyimide dissolves fully, taking-up is put into alcohol and is cleaned; Duplex net after cleaning is put into the ion milling instrument, and use angle carries out attenuate for 9 °, till subtracting leakage.
Claims (9)
1. the preparation method of the sample for use in transmitted electron microscope of a membraneous material is characterized in that the steps include:
1) adopt magnetron sputtering coating method to prepare film, the substrate of film is a Thermocurable polyimide;
2) film behind the plated film is put into the duplex net;
3) in the hydrazine hydrate with duplex net and film immersion 80%, treat that Thermocurable polyimide dissolves fully, taking-up is put into alcohol and is cleaned;
4) the duplex net after will cleaning is put into the ion milling instrument, and use angle carries out attenuate for 6～9 °, till subtracting leakage.
2. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1, it is characterized in that the base vacuum degree that adopts magnetron sputtering coating method to prepare film minimum be 10
-4The pa magnitude.
3. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1 is characterized in that sputtering atmosphere is an Ar gas.
4. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1 is characterized in that air pressure is 0.5～1.3Pa.
5. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1 is characterized in that sputtering power is 200～300W.
6. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1 is characterized in that sputter temperature is-260～400 ℃.
7. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1, the thickness that it is characterized in that Thermocurable polyimide is 30～80 μ m.
8. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1 is characterized in that the film behind the plated film is made the film that is of a size of (2～3) mm * (2～3) mm.
9. the preparation method of the sample for use in transmitted electron microscope of a kind of membraneous material as claimed in claim 1 is characterized in that duplex net and film are immersed in 80% the hydrazine hydrate 3h at least.
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| CNA2007101441177A CN101216386A (en) | 2007-12-26 | 2007-12-26 | Thin film material transmission electron microscope sample preparation method |
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| CNA2007101441177A CN101216386A (en) | 2007-12-26 | 2007-12-26 | Thin film material transmission electron microscope sample preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101581637B (en) * | 2009-06-19 | 2011-08-17 | 武汉钢铁(集团)公司 | Method for preparing electron microscope film sample with silicon steel sheet coating |
| CN102235945A (en) * | 2010-04-23 | 2011-11-09 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| CN105628468A (en) * | 2015-12-28 | 2016-06-01 | 西安电子科技大学 | Method for preparing GaN-based heterojunction transparent film transmission electron microscope sectional sample |
| CN106769162A (en) * | 2017-02-20 | 2017-05-31 | 广西大学 | A kind of transmission electron microscope magnetic sample preprocessor |
| CN106872344A (en) * | 2017-02-27 | 2017-06-20 | 北京科技大学 | The method for quick of combined material chip Sensitivity of Stress Corrosion |
| CN107167485A (en) * | 2017-04-14 | 2017-09-15 | 广西大学 | A kind of preparation method of the power-up transmission electron microscope cross-sectional sample in situ of hetero-junction thin-film |
| CN109839392A (en) * | 2017-11-28 | 2019-06-04 | 中国科学院金属研究所 | A kind of self-supporting film class transmission electron microscope sample and preparation method thereof |
-
2007
- 2007-12-26 CN CNA2007101441177A patent/CN101216386A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101581637B (en) * | 2009-06-19 | 2011-08-17 | 武汉钢铁(集团)公司 | Method for preparing electron microscope film sample with silicon steel sheet coating |
| CN102235945A (en) * | 2010-04-23 | 2011-11-09 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| CN102235945B (en) * | 2010-04-23 | 2013-02-20 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| CN105628468A (en) * | 2015-12-28 | 2016-06-01 | 西安电子科技大学 | Method for preparing GaN-based heterojunction transparent film transmission electron microscope sectional sample |
| CN105628468B (en) * | 2015-12-28 | 2018-05-15 | 西安电子科技大学 | GaN base hetero-junctions transparent membrane transmission electron microscope cross-sectional sample preparation method |
| CN106769162A (en) * | 2017-02-20 | 2017-05-31 | 广西大学 | A kind of transmission electron microscope magnetic sample preprocessor |
| CN106769162B (en) * | 2017-02-20 | 2023-06-06 | 广西大学 | Transmission electron microscope magnetic sample preprocessor |
| CN106872344A (en) * | 2017-02-27 | 2017-06-20 | 北京科技大学 | The method for quick of combined material chip Sensitivity of Stress Corrosion |
| CN107167485A (en) * | 2017-04-14 | 2017-09-15 | 广西大学 | A kind of preparation method of the power-up transmission electron microscope cross-sectional sample in situ of hetero-junction thin-film |
| CN109839392A (en) * | 2017-11-28 | 2019-06-04 | 中国科学院金属研究所 | A kind of self-supporting film class transmission electron microscope sample and preparation method thereof |
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