CN102095897A - Method for preparing macromolecular samples of scanning electron microscope - Google Patents
Method for preparing macromolecular samples of scanning electron microscope Download PDFInfo
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- CN102095897A CN102095897A CN200910216708XA CN200910216708A CN102095897A CN 102095897 A CN102095897 A CN 102095897A CN 200910216708X A CN200910216708X A CN 200910216708XA CN 200910216708 A CN200910216708 A CN 200910216708A CN 102095897 A CN102095897 A CN 102095897A
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- electron microscope
- scanning electron
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- slaine
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Abstract
The invention relates to a method for preparing macromolecular samples required by a scanning electron microscope. Metal salt is used as a colorant, the metal salt is dissolved in water or an organic solvent to form a solution, and after samples come into contact with the solution, metal cations can be selectively retained in a certain or some components in a micro-nanostructure macromolecular material to realize dye; and the samples which are dyed with the metal salt and are dried can be directly used for the observation and imaging by the scanning electron microscope.
Description
Technical field
The invention belongs to nano material and field of nanometer technology.Specifically be to belong to macromolecular material microstructure analysis technical elements, relate generally to the preparation method who is suitable for scanning electron microscope analysis usefulness macromolecular material sample.Slaine optionally is doped to privileged site in the nano-structured macromolecular material, serves as coloring agent, make it to become the sample that is suitable for sem observation.
Background technology
A family macromolecule that with the segmented copolymer is representative in the reunion film forming, by means of the micron-scale phase separation effect between the different molecule of chemical constitution, can constitute different, arrange diversified nanostructured pattern.Under certain condition, this self assembly effect even can in than the large tracts of land scope, realize (square metre magnitude) obtaining regular nanometer arrangement architecture.The small angle X-ray diffraction analytical technology can characterize the arrangement mode and the degree of order of nanostructured.Atomic force microscope can directly reflect the arranging situation of nanostructured in the small size scope, but its sweep velocity and spatial resolution are all comparatively limited.Although transmission electron microscope resolution height, the sample preparation trouble generally need be by professional tool.On the other hand, the scanning electron microscope technology is because sample preparation is simple, image taking speed is fast, resolution is high, is a kind of important analysis means of current micro nano structure organic material, macromolecular material, biomolecule material.
Because most of macromolecular material, such as segmented copolymer is not the good conductor of electronics, and the component of material mainly is made up of elements such as C, N, O, H, cause the cloud density between the different high molecular nanometers phases to be more or less the same, therefore generally can not directly utilize scanning electron microscope to resolve its structure.Therefore, generally need to adopt specific method of operating will special material (coloring agent) selectivity be filled into certain high molecular nanometer mutually in, the general image of this process be called dyeing (its process with act on be similar to common dyeing).At this, coloring agent plays two kinds of effects: because the cloud density of coloring agent is bigger, can improves the secondary rate that is colored the zone, thereby obtain comparatively ideal one-tenth image contrast ratio on the one hand; On the other hand, concerning the scanning electron microscope sample, coloring agent also can weaken even eliminate insulated sample surface charge build-up effect, guarantees to obtain stable image.
Because these specific (special) requirements have only some relatively more special materials can satisfy these needs.RuO commonly
4, OsO
4Deng near the conductive oxide that room temperature, distils easily.But, RuO
4, OsO
4Not only cost an arm and a leg Deng conductive oxide, and toxicity is big especially, and environment is had certain pollution.Therefore, press for the searching low price, toxicity is little, simple new dyeing agent of operating process and colouring method.
Summary of the invention
The objective of the invention is to propose a kind of new dyeing method, this method not only expense is low, environment protecting and power-saving, and also dyeing course is simple to operation, the safety coefficient height.Thereby help improving the sample preparation efficient of the scanning electron microscope sample of macromolecular material, enlarge the range of application of scanning electron microscope.
The present invention as the new dyeing agent, and is prepared as solution with slaine, and sample that then will be to be dyeed contacts a period of time with solution, takes out sample subsequently and carries out drying.Utilize so simple dyeing course, just can realize the preparation of sample.
The slaine of indication of the present invention is to contain metal cation and various types of salt of forming: as KCl, the NaBr etc. of binary; The AgNO of ternary
3, CuSO
4Deng; More the metal inorganic salt of complex form or organic salt or metal cation form the salt of acid group group, as HAuCl
4Deng.Comprise that not only heavy metal ion salt also comprises the salt that the light metal element forms.
The solvent that is adopted is not limited to H
2O can also comprise CH
3OH, C
2H
5Organic solvents such as OH.The concentration of solution can be from 0.1mol/l until saturated solution.Soak time the shortest minute magnitude, the longlyest can reach 24 hours.
Description of drawings
Fig. 1: segmented copolymer chemical constitution synoptic diagram
Fig. 2: (a) segmented copolymer PEO
272-b-PMA (Az)
116The atomic force microscope height mode scanning image of film surface, the regularly arranged and cyclic array that forms of visible PEO nanophase; (b) corresponding field emission electron scanning mirror picture does not show any structure feature; (c) through AgNO
3PEO after the dyeing
272-b-PMA (Az)
116The surface atomic force microscope height mode scanning figure, be unstained before compare, do not have significant change; (d) corresponding field emission electron scanning mirror picture shows that film presents orderly arrangement nanostructured.Confirmed the effect of dyeing.
Embodiment
Further describe the present invention below by specific embodiment.
Embodiment 1:
Di-block copolymer is to be made of two kinds of different components of chemical property, and as shown in Figure 1, structural formula is abbreviated as PEO
m-b-PMA (Az)
n, one section is the hydrophilic parts that poly-oxirene is formed, another section is the hydrophobic nature part that polymethacrylate constitutes.With copolymer p EO
272-b-PMA (Az)
116On the single crystalline Si substrate, form the film of thickness, after annealing in process, can obtain the regular nanostructured films of large tracts of land at 100nm by lacquering technique.Shown in Fig. 2 a afm scan image, the arrangement of PEO nano-pillar (point of light colour) formation rule in hydrophobic nature PMA (Az) medium.Subsequently, (S5200 Hitachi) observes down, owing to there are a large amount of electric charges to be accumulated in film surface, can not distinguish the microstructure of film at all, can not obtain significant image (Fig. 2 b) resulting sample directly to be placed an emission mode scanning electron microscope.
Prepare saturated AgNO again
3Solution places saturated solution 5min with film sample, and taking-up is dried.(NanoscopeIV, Veeco) observing samples surface (Fig. 2 c) find that the film surface structure does not have significant change, does not observe any variation in PEO nano-pillar position to use atomic force microscope.During imaging, shown in Fig. 2 d, the accelerating potential of surveying electron beam is observed the nanostructured of orderly arrangement when 5kV under field emission microscope, and the result who arrives with atomic force microscope observation is consistent.In fact, accelerating potential can clearly obtain the Pareto diagram picture of nanostructured all the time in 1kV to 30KV scope.
Embodiment 2:
Preparation 1mol/l HAuCl
4Ethanolic solution, then several solution are transferred to PEO
272-b-PMA (Az)
116On the film, leave standstill 2h.Remove the solution of polymer surfaces then with suction pipe, place the air air dry.When using field emission microscope to observe, its accelerating potential all can clearly be observed regular nanostructured in the 1-30KV scope.
Embodiment 3:
The KCl of preparation 5mol/l transfers to PEO with several solution then
454-b-PMA (Az)
115On the surface of film, leave standstill 24h again, and remove the remaining liquid of film surface with suction pipe.After the sample air dry removed moisture, re-use field emission microscope sample for reference surface appearance, find to observe during at 2KV the nanostructured of orderly arrangement at accelerating potential.
Claims (3)
1. one kind prepares the required method of scanning electron microscope macromolecule sample.It is characterized in that, adopt slaine as coloring agent, and this slaine can be dissolved in water, the organism equal solvent.
2. a class new dyeing method prepares the required sample of scanning electron microscope.Slaine can be dissolved in water or the organic solvent and form solution, and solution is with after pending sample contacts then, and the metal cation selectivity is trapped in high molecular certain or the several component of micro nano structureization, realizes dyeing course.
3. the sample after handling through above-mentioned 1 and 2 can be directly used in the sem observation imaging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910216708XA CN102095897A (en) | 2009-12-11 | 2009-12-11 | Method for preparing macromolecular samples of scanning electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910216708XA CN102095897A (en) | 2009-12-11 | 2009-12-11 | Method for preparing macromolecular samples of scanning electron microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102095897A true CN102095897A (en) | 2011-06-15 |
Family
ID=44129076
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910216708XA Pending CN102095897A (en) | 2009-12-11 | 2009-12-11 | Method for preparing macromolecular samples of scanning electron microscope |
Country Status (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111801565A (en) * | 2018-01-10 | 2020-10-20 | 堪萨斯大学 | Conduction fixation for electron microscopy |
-
2009
- 2009-12-11 CN CN200910216708XA patent/CN102095897A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| JING ZE LI ET AL: "Phase-selective staining of metal salt for scanning electron microscopy imaging of block copolymer film", 《ULTRAMICROSCOPY》 * |
| JINGZE LI ET AL: "Tailored Ag nanoparticle array fabricated by block copolymer photolithography", 《THIN SOLID FILM》 * |
| 程冬梅 等: "SDS聚丙烯酰胺凝胶电泳快速染色新方法的研究", 《西北植物学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111801565A (en) * | 2018-01-10 | 2020-10-20 | 堪萨斯大学 | Conduction fixation for electron microscopy |
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Application publication date: 20110615 |