CN108535298A - A kind of micro slide and application method for the bad powder of SEM electric conductivities - Google Patents
A kind of micro slide and application method for the bad powder of SEM electric conductivities Download PDFInfo
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- CN108535298A CN108535298A CN201810244298.9A CN201810244298A CN108535298A CN 108535298 A CN108535298 A CN 108535298A CN 201810244298 A CN201810244298 A CN 201810244298A CN 108535298 A CN108535298 A CN 108535298A
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- Prior art keywords
- groove
- particle
- micro slide
- conducting resinl
- sem
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- 239000000843 powder Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 57
- 239000005357 flat glass Substances 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 239000007921 spray Substances 0.000 claims abstract description 4
- 239000004020 conductor Substances 0.000 claims abstract 2
- 238000012545 processing Methods 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000992 sputter etching Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- -1 biology Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Abstract
The invention discloses a kind of micro slides and application method for the bad powder of SEM electric conductivities.The micro slide uses conductive material, and subtracts material processing above or increase material attachment conductive metal mesh, forms groove.When use, conduction is adhesive on micro slide, the groove for ensureing conducting resinl covering slide surface spills powder particle on conducting resinl upper berth, and removal adheres to unstable particle, then it is suppressed with sheet glass, particle is set to be pressed into groove, wherein conducting resinl is in and is pressed among particle and groove, finally removes sheet glass, unstable particle is removed again, and SEM vacuum test samples can be carried out after carrying out metal spraying or spray carbon.
Description
Technical field
The present invention relates to a kind of micro slides and application method for the bad powder of SEM electric conductivities, belong to scanning electron
Microscope testing field.
Background technology
Scanning electron microscope（SEM）It is a kind of analytical instrument of large size, is mainly used for micro- point of the pattern of solid matter
Analysis and the micro-zone analysis to conventional ingredient, there is that resolution is high, amplification factor is big, the depth of field is big, three-dimensional sense is strong, sample preparation is simply excellent
Point is widely used in the fields such as chemical industry, material, medicine, biology, mineral products, the administration of justice.Since it is expensive and special work is former
Reason, it has higher requirement, the quality of sample preparation to directly affect whether sample analysis succeeds sample preparation.SEM is surveyed
When trying non-conductive sample, following situations can occur because of charged influence：1）Analysis site deviates, it is difficult to pinpoint accurate quantitative analysis；2）
Practical accelerating potential, which reduces, which influences quantitative correction result, absorbs electric current becomes smaller, and X-ray intensity is made to reduce；3）Poor image quality, or
Person can not be imaged.So EDS cannot be carried out in high vacuum sample room, under normal accelerating potential for non-conductive sample（Energy
Spectrum）Qualitative and quantitative analysis can not also obtain high quality graphic.
The sample of sem analysis must be solid, and want nontoxic, "dead", pollution-free, without magnetic, no moisture, and ingredient is steady
Fixed, bulk sample size wants moderate, and powder sample will carry out specially treated, to non-conductive and poor electric conductivity powder or block
Sample will carry out plating conductive film.But plated film can prevent conductive film from powder is completely covered because of itself spherical shape of powder
Grain, so that powder cannot generate conductive path, is susceptible to electric charging effect.In addition to this, if tested powder is fixed loosely
Solid then subparticle can be made to be detached from sample stage, pollution Electronic Speculum pole shoe even light path system, if powder is fixed more steady, researcher
It is general that powder particle is inlayed into epoxy resin, is then mechanically polished using edge sample, so that Particle attrition is exposed boundary section,
Then conductive film is plated, but this mode can destroy the integrality of particle, in addition can also increase experimental procedure and waste time.
Invention content
In view of the defects existing in the prior art, the purpose of the present invention is to provide a kind of micro slides, solve electric conductivity not
Good powder SEM test requests, and the reuse rate for improving micro slide will not destroy the integrality of particle again, also reduce powder
It is detached from the possibility of sample stage.
The technical solution adopted by the present invention is as follows：
A kind of micro slide for the bad powder of SEM electric conductivities is machined to sheet using the material of conductive matter,
Subtract material processing on surface or increase material and adhere to conductive metal mesh, forms the groove of different shapes that can accommodate particle, groove
Width is 50nm ~ 1000 μm.
The micro slide application method for the bad powder of SEM electric conductivities includes the following steps：
（1）Slide surface is cleaned, it is dry；
（2）Conduction is adhesive on micro slide, ensures the groove of conducting resinl covering slide surface；
（3）Powder particle is spilt on conducting resinl upper berth, then the unstable particle of adherency is blown away with hair-dryer, then uses sheet glass again
Compacting, the powder particle being guaranteed above groove can be pressed into groove by sheet glass, and wherein conducting resinl is in and is pressed particle
Among groove；Finally remove sheet glass compacting, is once dried again with hair-dryer, remove unstable particle；
（4）Powder particle to being pressed into groove carries out metal spraying or spray carbon operation, can carry out SEM vacuum tests after the completion
Sample.
The device have the advantages that：1）Groove shape is changeable, can accommodate different size of powder particle；2）Particle
It is adhered in the trench by glass compacting with together with conducting resinl, obtains adhering to close powdered sample；3）It is pressed into groove
The surface of grain exposure is less, is easy metal spraying and easily forms access with conducting resinl；4）It ensure that granule integrity；5）Groove size is not
One, adapt to varigrained particle；6）Groove describes easy machining, and prepared by micro slide is easy；7）Micro slide can repeat profit
With；8）After powder particle is embedded in groove, exposed surface is reduced, and can be reduced the metal spraying time, improves conventional efficient and experiment is economical
Performance.The present invention does not have found with the presence of similar approach and product, by searching for pertinent literature to leading in SEM test process
Prepared by electrically undesirable powder sample have very strong Auxiliary Significance, there is novel creative and certain application prospect.
Description of the drawings
Fig. 1：Groove for arc-shaped micro slide front view and uses schematic diagram in embodiment 1；
Fig. 2：Groove is arc-shaped micro slide vertical view in embodiment 1；
Fig. 3：The particle schematic diagram into arc-shaped groove is pressed in embodiment 1；
Fig. 4：Groove for rectangular micro slide front view and uses schematic diagram in embodiment 2；
Fig. 5：Groove is rectangular micro slide vertical view in embodiment 2；
Fig. 6：The particle schematic diagram into square trench is pressed in embodiment 2；
Fig. 7：In embodiment 3 metal mesh groove micro slide front view and use schematic diagram；
Fig. 8：Metal mesh groove micro slide vertical view in embodiment 3；
Fig. 9：Groove for rectangular micro slide front view and uses schematic diagram in embodiment 4；
Figure 10：Groove is rectangular micro slide vertical view in embodiment 4；
Wherein：1- micro slides, 2- conducting resinls, 3- powder particles, 4- sheet glass, 1-1- grooves, 1-2- metal meshes, L0, L1, L2,
L3, L4, L5- groove width, D0- metal mesh relief widths.
Specific implementation mode
In order to deepen the understanding of the present invention, with reference to embodiment and attached drawing, the invention will be further described, the reality
It applies example to be only used for explaining the present invention, be not intended to limit the scope of the present invention..
Embodiment 1
The material for choosing micro slide 1 first is 45 steel, is then machined out into 20mm × 10mm × 4mm.And above with
Ion etching equipment subtracts material and processes groove 1-1 that is in the arc-shaped and can accommodating particle, as shown in Figure 1, arc-shaped groove size
L0, L1, L2 etch width for 300 μm, 10 μm, 50nm, as shown in Figure 2.
Then, slide surface is cleaned using absolute alcohol, the impurity such as removal surface and oil contaminant are dry, then conducting resinl 2 is glued
On micro slide, ensure the arc groove of conducting resinl covering slide surface.
Further, scattered WC ceramic powder particles 3 are spilt on conducting resinl upper berth, then blows away adherency loosely with hair-dryer
Solid particle, then again use sheet glass 4 suppress, groove 1-1 can be pressed by sheet glass by being guaranteed at groove particles above,
Middle conducting resinl 2, which is in, to be pressed among particle 3 and groove 1-1, as shown in Figure 3.Finally remove the compacting of sheet glass 4, uses hair-dryer
It is once dried again, removes unstable particle.
Further, metal spraying operation is carried out to above-mentioned pressed particle.SEM vacuum test samples can be carried out after the completion.
Embodiment 2
The material for first choosing micro slide 1 is TC4 alloys, is then machined out into 20mm × 10mm × 4mm.And above with
Ion etching equipment subtracts material processing squarely and can accommodate the groove 1-1 of particle, as shown in figure 4, the size L0 of square trench,
L1, L2 etch width for 1000 μm, 50 μm, 100nm, as shown in Figure 5.
Then, cleaning slide surface is to be dried, then conducting resinl 2 is sticked on micro slide, ensures that conducting resinl covers loading
The square trench on piece surface.
Further, scattered Al is spilt on conducting resinl upper berth2O3Then ceramic powder particle 3 blows away adherency not with hair-dryer
Firm particle then uses sheet glass 4 to suppress again, and groove 1-1 can be pressed by sheet glass by being guaranteed at groove particles above,
Wherein conducting resinl 2, which is in, is pressed among particle 3 and groove 1-1, as shown in Figure 6.Finally remove the compacting of sheet glass 4, with blowing
Machine is once dried again, removes unstable particle.
Further, spray carbon operation is carried out to above-mentioned pressed particle.SEM vacuum test samples can be carried out after the completion.
Embodiment 3
The material for first choosing micro slide 1 is brass H90 alloys, is then machined out into 20mm × 10mm × 4mm.And above
Using the groove 1-1 that material equipment is processed into metal mesh 1-2 and formation can accommodate particle is increased, as shown in fig. 7, metal mesh relief width
D0 is 500 μm, as shown in Figure 8.
Then, cleaning slide surface is to be dried, then conducting resinl 2 is sticked on micro slide, ensures that conducting resinl covers loading
The polygon groove on piece surface.
Further, scattered Al is spilt on conducting resinl upper berth2O3Then it is insecure to blow away adherency with hair-dryer for powder particle 3
Particle, then again use sheet glass 4 suppress, groove 1-1 can be pressed by sheet glass by being guaranteed at groove particles above, wherein
Conducting resinl 2, which is in, to be pressed among particle 3 and groove 1-1.Finally remove the compacting of sheet glass 4, is once blown again with hair-dryer
Wind removes unstable particle.
Further, metal spraying operation is carried out to above-mentioned pressed particle.SEM vacuum test samples can be carried out after the completion.
Embodiment 4
The material for first choosing micro slide 1 is 3105 aluminium alloys, is then machined out into 20mm × 10mm × 4mm.And above
Subtract material processing squarely using ion etching equipment and the groove 1-1 of particle can be accommodated, as shown in figure 9, the ruler of square trench
Very little L0, L1, L2, L3, L4, L5 etch width for 1000 μm, 200 μm, 50 μm, 5 μm, 200nm, 50nm, as shown in Figure 10.
Then, cleaning slide surface is to be dried, then conducting resinl 2 is sticked on micro slide, ensures that conducting resinl covers loading
The square trench on piece surface.
Further, scattered Al is spilt on conducting resinl upper berth2O3Then ceramic powder particle 3 blows away adherency not with hair-dryer
Firm particle then uses sheet glass 4 to suppress again, and groove 1-1 can be pressed by sheet glass by being guaranteed at groove particles above,
Wherein conducting resinl 2, which is in, is pressed among particle 3 and groove 1-1.Finally remove the compacting of sheet glass 4, one is carried out again with hair-dryer
Secondary blowing removes unstable particle.
Further, metal spraying operation is carried out to above-mentioned pressed particle.SEM vacuum test samples can be carried out after the completion.
Claims (3)
1. a kind of micro slide for the bad powder of SEM electric conductivities processes slabbing using conductive material, subtracts material on surface and add
Work increases material attachment conductive metal mesh, forms groove（1-1）.
2. micro slide according to claim 1, which is characterized in that groove（1-1）Width be 50nm ~ 1000 μm.
3. the application method of micro slide described in claim 1, includes the following steps：
（1）Clean micro slide（1）Surface, it is dry；
（2）By conducting resinl（2）It is sticked to micro slide（1）On, make conducting resinl（2）Cover micro slide（1）The groove on surface（1-1）；
（3）In conducting resinl（2）Spill powder particle in upper berth（3）, then the unstable powder particle of removal adherency, uses sheet glass（4）
Compacting, makes powder particle（3）It is pressed into groove（1-1）, conducting resinl（2）In downtrodden powder particle（3）With groove（1-
1）Sheet glass is finally removed in centre（4）, unstable powder particle is removed again；
（4）To being pressed into the powder particle of groove（3）Carry out metal spraying or spray carbon operation, you can carry out SEM vacuum test samples
Product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810244298.9A CN108535298A (en) | 2018-03-23 | 2018-03-23 | A kind of micro slide and application method for the bad powder of SEM electric conductivities |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810244298.9A CN108535298A (en) | 2018-03-23 | 2018-03-23 | A kind of micro slide and application method for the bad powder of SEM electric conductivities |
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| CN108535298A true CN108535298A (en) | 2018-09-14 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110006937A (en) * | 2019-04-02 | 2019-07-12 | 深圳鸿鹏新能源科技有限公司 | Utilize the method for scanning electron microscope test sample under limiting resolution |
| CN111474200A (en) * | 2020-04-16 | 2020-07-31 | 宸鸿科技(厦门)有限公司 | Method for preparing microstructure sample of electronic element |
| 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110006937A (en) * | 2019-04-02 | 2019-07-12 | 深圳鸿鹏新能源科技有限公司 | Utilize the method for scanning electron microscope test sample under limiting resolution |
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Application publication date: 20180914 |