CN106970097A - A kind of metal surface non-metallic coatings uniformity detecting method - Google Patents
A kind of metal surface non-metallic coatings uniformity detecting method Download PDFInfo
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- CN106970097A CN106970097A CN201710210760.9A CN201710210760A CN106970097A CN 106970097 A CN106970097 A CN 106970097A CN 201710210760 A CN201710210760 A CN 201710210760A CN 106970097 A CN106970097 A CN 106970097A
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- 238000000576 coating method Methods 0.000 title claims abstract description 47
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 45
- 239000002184 metal Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000002389 environmental scanning electron microscopy Methods 0.000 claims abstract description 16
- 239000005030 aluminium foil Substances 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 239000000523 sample Substances 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 229910021538 borax Inorganic materials 0.000 claims description 12
- 239000004328 sodium tetraborate Substances 0.000 claims description 12
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 9
- 238000001228 spectrum Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000008199 coating composition Substances 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000004020 conductor Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000010183 spectrum analysis Methods 0.000 abstract description 3
- 238000009500 colour coating Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000007 visual effect Effects 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses the invention provides a kind of metal surface non-metallic coatings uniformity detecting method, including the metal sample by non-metallic coatings are scribbled, polished flat parallel to the non-detection face in detection faces direction, expose metallic matrix, sample non-detection face is pasted onto on aluminium foil with conducting resinl；Then the sample pasted is put on ESEM objective table, and sample is in high vacuum state, backscatter mode is selected in ESEM, ESEM parameter needed for adjustment, whether consistent observe the coating color depth, solid colour coating uniformity is good, and color has depth coating uniformity poor.The present invention determines coating composition by the energy spectrum analysis of ESEM, so that testing result accuracy is higher.The present invention uses aluminium foil as electric conductor, and base bottom need not be especially smooth, while facilitating the fixation of sample, multiple samples being pasted onto on aluminium foil can be observed simultaneously and sample state is fixed, and sample preparation is convenient, reproducible.
Description
Technical field
The present invention relates to a kind of detection method of metal surface non-metallic coatings, and in particular to a kind of metal surface is nonmetallic
Coating uniformity detection method.
Background technology
With the development of drawing process, the development of especially dry drawing process, Steel Wire Surface needs a kind of lubricant to improve
Drawing speed and compression ratio, but many lubricants can not directly be contacted with metal at present, otherwise contact effect is bad, and this is just
The carrier of lubricant and steel wire can be merged by needing one, and the borax layer of Steel Wire Surface is greatly improved as the carrier of lubricant
Drawing efficiency and drawing quality, if without this layer of carrier, steel wire is difficult the deformed area that the lubricating fluid of powdery is brought into drawing die,
It is used as the carrier of lubricating fluid, it is desirable to be firmly combined with matrix, is not fallen off in deformation process, so this layer of non-metal carrier is in base
Uniformity on body is just particularly important.
But, up to the present the detection method for the coat of metal is more, and Coating composition can be determined with chemical method, or
Optical microscopy determines coating uniformity, but light microscope has great limitation for the detection of non-metallic coatings
Property：One is that the light microscope depth of field is small, and fuzzy for on-plane surface sample fringe field of view, two be non-metallic coatings and metal fund color
It is close, it is not easily distinguishable, it is difficult to observe uniformity, therefore often detect cross section but bring the too small representativeness of inspection surface is not strong to ask
Topic, but ESEM Momentum profiles can solve these problems, one is that the ESEM depth of field is high, and observation scope is wide, i.e.,
Cylinder sample edge is remained to blur-free imaging, can directly observe cylinder sample surface, it is often more important that be different under backscatter mode
The deep mixed sample of element display color, the bigger display color of atomic number is more shallow, and the smaller display color of atomic number is got over
It is deep, and the atomic number of general common metal is larger, non-metallic coatings（Such as boron）Atomic number is smaller, there is substantially poor in color
It is different, and power spectrum can be used to carry out mode and basic metallic element Fe distributions that Surface scan determines exclusive element Na, O in borax
Supplementary mode determine the uniformity of metal surface nonmetallic coating.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to now provide it is a kind of can be effectively to nonmetallic coating
Uniformity is tested, and the high metal surface non-metallic coatings uniformity detecting method of testing result accuracy.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of metal surface non-metallic coatings are uniform
Property detection method, its innovative point is：By alcohol washes, polishing, paste and scanning step, complete the nonmetallic plating in metal surface
The detection of layer uniformity；It is described to comprise the following steps that：
（1）Alcohol washes：The metal sample for scribbling non-metallic coatings is chosen, the surface of non-metallic coatings is soaked using alcohol
Bubble cleaning, the alcohol is the analysis absolute alcohol of concentration >=99.7%, and the soak time is 1-5 minutes；
（2）Polishing：By the metal sample for scribbling non-metallic coatings after immersion, polished parallel to the non-detection face in detection faces direction
It is smooth, expose metallic matrix；
（3）Paste：By step（2）The sample non-detection face that polishing is obtained is pasted onto on aluminium foil with conducting resinl；
（4）Scanning：The sample pasted is put on the sample bench in ESEM storehouse, door is closed, will be evacuated in storehouse
State, adjusts the focusing multiple of ESEM, and is scanned；
（5）Parameter setting：By step（4）In scan pattern be set to backscatter mode, the accelerating potential for setting electron gun is
8KV；
（6）Observed and recorded：Sample bench is risen into Electronic Speculum probe lower section, multiplication factor, the surface of observing samples, dark colour is adjusted
The borax layer for metal surface, it is white for metallic matrix, then the coverage condition of metal surface borax layer is recorded
Analysis, carries out the observation of multistage sample successively.
Further, the step（4）In focusing multiple be 50 times, the scan method is power spectrum Surface scan method point
Exclusive element determines that metal surface is non-using the supplementary mode of basic metallic element distribution is determined simultaneously in analysis nonmetallic coating
The uniformity of metal coating.
Further, the step（6）In multiplication factor be 50 times, the hop count of the sample is more than or equal to 3, the examination
Sample platform is 9-11mm with the range difference that Electronic Speculum is popped one's head in.
Beneficial effects of the present invention are as follows：
（1）By the present invention in that cleaned with alcohol to metal sample surface, influence of the impurity to observation and not is eliminated
Coating can be influenceed.
（2）The mode that the present invention substitutes conventional optical microscope observation cross section with direct observation coating surface evaluates coating
Uniformity, accuracy is high, simple operation.
（3）Coating and the matrix color contrast of the present invention is obvious, and different element display colors is deep under backscatter mode
Shallow different, the bigger display color of atomic number is more shallow, and the smaller display color of atomic number is deeper, and general common metal
Atomic number it is larger, non-metallic coatings atomic number is smaller, there is notable difference in color, is easy to observer to be observed, note
Record and analysis.
（4）The present invention determines coating composition by the energy spectrum analysis of ESEM, so that testing result accuracy is higher.
（5）The present invention uses aluminium foil as electric conductor, and base bottom need not be especially smooth, while facilitating consolidating for sample
It is fixed, multiple samples being pasted onto on aluminium foil can be observed simultaneously and sample state is fixed, and sample preparation is convenient, reproducible.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
A kind of metal surface non-metallic coatings uniformity detecting method, by alcohol washes, polishing, pastes and scanning step
Suddenly, the detection of metal surface non-metallic coatings uniformity is completed；Comprise the following steps that：
（1）Alcohol washes：The metal sample for scribbling non-metallic coatings is chosen, the surface of non-metallic coatings is soaked using alcohol
Bubble cleaning, alcohol is the analysis absolute alcohol of concentration >=99.7%, and soak time is 1-5 minutes；
（2）Polishing：By the metal sample for scribbling non-metallic coatings after immersion, polished parallel to the non-detection face in detection faces direction
It is smooth, expose metallic matrix；
（3）Paste：By step（2）The sample non-detection face that polishing is obtained is pasted onto on aluminium foil with conducting resinl；
（4）Scanning：The sample pasted is put on the sample bench in ESEM storehouse, door is closed, will be evacuated in storehouse
State, adjusts the focusing multiple of ESEM, and is scanned；
（5）Parameter setting：By step（4）In scan pattern be set to backscatter mode, the accelerating potential for setting electron gun is
8KV；
（6）Observed and recorded：Sample bench is risen into Electronic Speculum probe lower section, multiplication factor, the surface of observing samples, dark colour is adjusted
The borax layer for metal surface, it is white for metallic matrix, then the coverage condition of metal surface borax layer is recorded
Analysis, carries out the observation of multistage sample successively.
Feasible, step（4）In focusing multiple be 50 times, scan method is that power spectrum Surface scan method analyzes nonmetallic painting
Exclusive element determines metal surface nonmetallic coating using the supplementary mode of basic metallic element distribution is determined simultaneously in layer
Uniformity.
Feasible, step（6）In multiplication factor be 50 times, the hop count of sample is more than or equal to 3, and sample bench is popped one's head in Electronic Speculum
Range difference be 9-11mm.
Embodiment 1
The uniformity of borax layer on test diameter 3.08mm steel wires.
Three sections of diameter 3.08mm sample 2cm are taken, are transversely slightly polished after being soaked using alcohol, the non-gold in surface is removed
Belong to layer；
The sample sheared detection is face-up, it is adhesive on aluminium foil, is put on the objective table of Electronic Speculum with conduction；
It is put on the sample bench in ESEM storehouse, slowly closing door, is vacuumized after equipment is stable, after finishing, regulation 50
Multiple focus on and scan, the scan pattern of ESEM is changed to backscatter mode, the accelerating potential of electron gun is adjusted to
8KV；
Objective table is slowly risen at Electronic Speculum probe 10mm, adjusts multiplication factor, the image of sample is occupied whole visual field,
Auto contrast；
Multiplication factor is changed to 50 times, the surface of sample is observed, dark colour is the borax layer of Steel Wire Surface, white for steel wire
Matrix；
Three sections of Steel Wire Surfaces are observed successively, judge the coverage condition and record of Steel Wire Surface borax layer；
Coating edge to be detected is confirmed and recorded to result using power spectrum Surface scan.
The borax coverage rate difference of the metal surface under following experimental data the present embodiment can be obtained by above-described embodiment
For 75%, 75% and 90%.
By the present invention in that cleaned with alcohol to metal sample surface, influence of the impurity to observation and not is eliminated
Coating can be influenceed.The mode that the present invention substitutes conventional optical microscope observation cross section with direct observation coating surface evaluates coating
Uniformity, accuracy is high, simple operation.
Coating and the matrix color contrast of the present invention is obvious, and the different element display color depths is not under backscatter mode
Equally, the bigger display color of atomic number is more shallow, and the smaller display color of atomic number is deeper, and the original of general common metal
Sub- ordinal number is larger, and non-metallic coatings atomic number is smaller, there is notable difference in color, is easy to observer to be observed, record and
Analysis.
The present invention determines coating composition by the energy spectrum analysis of ESEM, so that testing result accuracy is higher.This
Invention uses aluminium foil as electric conductor, and base bottom need not be especially smooth, while facilitating the fixation of sample, can observe simultaneously
Multiple samples being pasted onto on aluminium foil and sample state is fixed, sample preparation is convenient, reproducible.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
The technical scheme that can be realized without creative work on the basis of above-described embodiment, is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (3)
1. a kind of metal surface non-metallic coatings uniformity detecting method, it is characterised in that：By alcohol washes, polishing, paste
And scanning step, complete the detection of metal surface non-metallic coatings uniformity；It is described to comprise the following steps that：
Alcohol washes：The metal sample for scribbling non-metallic coatings is chosen, the surface of non-metallic coatings is soaked using alcohol
Cleaning, the alcohol is the analysis absolute alcohol of concentration >=99.7%, and the soak time is 1-5 minutes；
Polishing：By the metal sample for scribbling non-metallic coatings after immersion, it is polished flat parallel to the non-detection face in detection faces direction
It is whole, expose metallic matrix；
Paste：By step（2）The sample non-detection face that polishing is obtained is pasted onto on aluminium foil with conducting resinl；
Scanning：The sample pasted is put on the sample bench in ESEM storehouse, door is closed, by the shape that is evacuated in storehouse
State, adjusts the focusing multiple of ESEM, and is scanned；
Parameter setting：By step（4）In scan pattern be set to backscatter mode, the accelerating potential for setting electron gun is 8KV；
Observed and recorded：Sample bench is risen into Electronic Speculum probe lower section, multiplication factor, the surface of observing samples, dark colour is adjusted
It is white for metallic matrix for the borax layer of metal surface, record point then is carried out to the coverage condition of metal surface borax layer
Analysis, carries out the observation of multistage sample successively.
2. a kind of metal surface non-metallic coatings uniformity detecting method according to claim 1, it is characterised in that：It is described
Step（4）In focusing multiple be 50 times, the scan method be power spectrum Surface scan method analysis nonmetallic coating in exclusive member
Element determines the uniformity of metal surface nonmetallic coating using the supplementary mode of basic metallic element distribution is determined simultaneously.
3. a kind of metal surface non-metallic coatings uniformity detecting method according to claim 1, it is characterised in that：It is described
Step（6）In multiplication factor be 50 times, the hop count of the sample is more than or equal to 3, the distance that the sample bench is popped one's head in Electronic Speculum
Difference is 9-11mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710210760.9A CN106970097A (en) | 2017-03-31 | 2017-03-31 | A kind of metal surface non-metallic coatings uniformity detecting method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710210760.9A CN106970097A (en) | 2017-03-31 | 2017-03-31 | A kind of metal surface non-metallic coatings uniformity detecting method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030605A (en) * | 2018-08-30 | 2018-12-18 | 武汉钢铁有限公司 | The determination method of chrome plating surface metal chromium content height |
| CN111426714A (en) * | 2020-05-15 | 2020-07-17 | 云南中烟工业有限责任公司 | Cut tobacco perfuming uniformity detection method based on scanning electron microscope energy spectrum |
| CN111896568A (en) * | 2020-07-27 | 2020-11-06 | 昆明贵研催化剂有限责任公司 | Method for measuring catalyst coating and ash distribution on automobile particulate matter trap |
| CN112924437A (en) * | 2019-12-06 | 2021-06-08 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN114636722A (en) * | 2022-03-01 | 2022-06-17 | 湖南华菱涟源钢铁有限公司 | A kind of sample preparation method for electron microscope detection of hard film layer on metal surface |
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| CN103411987A (en) * | 2013-07-22 | 2013-11-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Uniformity characterization method and dispersibility characterization method of titanium oxide surface coating |
| CN104133083A (en) * | 2014-07-09 | 2014-11-05 | 河冶科技股份有限公司 | Method for quantitative detection of MC carbide in high-V high-speed steel |
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| CN103411987A (en) * | 2013-07-22 | 2013-11-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Uniformity characterization method and dispersibility characterization method of titanium oxide surface coating |
| CN104133083A (en) * | 2014-07-09 | 2014-11-05 | 河冶科技股份有限公司 | Method for quantitative detection of MC carbide in high-V high-speed steel |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030605A (en) * | 2018-08-30 | 2018-12-18 | 武汉钢铁有限公司 | The determination method of chrome plating surface metal chromium content height |
| CN109030605B (en) * | 2018-08-30 | 2020-08-04 | 武汉钢铁有限公司 | Method for judging metal chromium content on surface of chromium plated plate |
| CN112924437A (en) * | 2019-12-06 | 2021-06-08 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN112924437B (en) * | 2019-12-06 | 2023-02-21 | 核工业西南物理研究院 | Laser-induced breakdown spectroscopy absolute quantitative analysis method |
| CN111426714A (en) * | 2020-05-15 | 2020-07-17 | 云南中烟工业有限责任公司 | Cut tobacco perfuming uniformity detection method based on scanning electron microscope energy spectrum |
| CN111426714B (en) * | 2020-05-15 | 2023-03-31 | 云南中烟工业有限责任公司 | Cut tobacco perfuming uniformity detection method based on scanning electron microscope energy spectrum |
| CN111896568A (en) * | 2020-07-27 | 2020-11-06 | 昆明贵研催化剂有限责任公司 | Method for measuring catalyst coating and ash distribution on automobile particulate matter trap |
| CN111896568B (en) * | 2020-07-27 | 2023-05-02 | 昆明贵研催化剂有限责任公司 | Method for measuring catalyst coating and ash distribution on automobile particulate matter catcher |
| CN114636722A (en) * | 2022-03-01 | 2022-06-17 | 湖南华菱涟源钢铁有限公司 | A kind of sample preparation method for electron microscope detection of hard film layer on metal surface |
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Application publication date: 20170721 |
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