CN109596651A - The analysis method of color spot in a kind of pair of modified polytetrafluoroethylresin resin gasket - Google Patents
The analysis method of color spot in a kind of pair of modified polytetrafluoroethylresin resin gasket Download PDFInfo
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- CN109596651A CN109596651A CN201710899983.0A CN201710899983A CN109596651A CN 109596651 A CN109596651 A CN 109596651A CN 201710899983 A CN201710899983 A CN 201710899983A CN 109596651 A CN109596651 A CN 109596651A
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Abstract
The present invention relates to the analysis methods of color spot in a kind of pair of modified polytetrafluoroethylresin resin gasket.Method provided by the invention is by importing the image methods such as scanning electron microscope system, characteristic point label, positioning target for optical microscope image, make scan image complete display, sample structure is injury-free, X-ray-energy-spectrum scanning the method combined by point, line, surface scanning, keep the qualitative and quantitative analysis of sample accurate, has important practice significance for the analysis of color spot unknown small and without surface topography difference in modified polytetrafluoroethylresin resin gasket.
Description
Technical field
The invention belongs to microexamination sample technical fields, are related to the image procossing and X-ray energy spectrum of a kind of scanning electron microscope
Quantitative analysis method, specifically to color spot unknown small and without surface topography difference in modified polytetrafluoroethylresin resin gasket
Identification and image procossing, and the method using this color spot surface atom composition of xps energy spectrum instrument quantitative detection.
Background technique
Modified Teflon (PTFE) resin gasket is after being modified PTFE, filler to be added in raw material, such as
Graphite, copper powder, pigment, glass fibre, bronze powder, carbon fiber etc. are formed through the uniform post moulding of mixed at high speed, then through high temperature sintering
And form, there is unique leakproofness, restorative and compressibility.Modified ptfe gasket has ultralow coefficient of friction, excellent
Compressive strength and brilliant antiwear characteristic, its exclusive leakproofness and torque retentivity, on the creep properties of cold flow and material,
The shortcomings that overcoming traditional polytetrafluoroethylene (PTFE) not only improves environment, but also has saved cost.It is examined in the quality of modified ptfe gasket
In survey, whether filler material is uniformly mixed with polytetrafluoroethylene (PTFE), and whether finished surface contains impurity, is one of the emphasis of detection.
There are many measuring method of sample surfaces detection, conventionally employed ocular estimate, optical microscopy, scanning electron microscope-power spectrum
Instrument (SEM-EDS) method, power spectrum Surface scan method etc..Wherein, ocular estimate and the distinguishable other color sample of optical microscopy and color spot, but
Qualitative and quantitative analysis can not be carried out to color spot and impurity component, SEM-EDS method is microcell detection technique emerging in recent years, is passed through
The electron beam of fine focusing irradiates sample, the various signals that test sample surface excitation goes out respectively, according to secondary electron and back scattering
The yield size of electronic signal, shows the topographical information of sample in the form of gray scale light and shade, according to the signal yield pair of X-ray
The element of sample carries out qualitatively or quantitatively, and this method is the side being widely used in the quality testing of modified ptfe gasket in recent years
Method, but the following limitations exist: can only identify that impurity that atomic number differs greatly or surface topography have the region of notable difference,
And it is uneven to filler mixing and caused by color spot can not identify, cause energy disperse spectroscopy can not by Electronic Speculum to color spot accurate positioning,
Therefore color spot interior element can not be carried out qualitative or quantitative.And power spectrum Surface scan method, it is only applicable to that color spot Primary Location is completed
And the biggish detection of mix ingredients content difference, the COMPLEX MIXED sample for completing positioning feature point not in Electronic Speculum are difficult
It finds target position and carries out constituent analysis.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of electricity that not only can recognize color but also can recognize pattern
The micro- scarnning mirror of son and image processing method are conducive to power spectrum positioning and carry out qualitative and quantitative analysis to the small color spot of sample.
Method provided by the invention is by importing scanning electron microscope system, characteristic point label, positioning for optical microscope image
The image methods such as target make scan image complete display, and sample structure is injury-free, are penetrated by the X that point, line, surface scanning combines
Line-energy-spectrum scanning method, keeps the qualitative and quantitative analysis of sample accurate, for unknown small in modified polytetrafluoroethylresin resin gasket
And the analysis of the color spot without surface topography difference has important practice significance.
Specifically, method provided by the invention the following steps are included:
(1) the modified polytetrafluoroethylresin resin pad sample to be analyzed containing color spot is clapped with optical microscopy
According to, it is ensured that the color spot is located at central region, obtains high definition light microscope photo；
(2) light microscope photo is imported into mapping software, describes color spot profile, and any position is got ready outside the profile
As characteristic point；
(3) under conditions of amplification factor identical as use of taking pictures described in step (1), with scanning electron microscope to described
Sample is taken pictures, it is ensured that the color spot is located at central region, obtains high definition electromicroscopic photograph；It is described using method identical with step (2)
Color spot profile, and get ready in position identical with step (2) as characteristic point；
(4) light microscope photo and electromicroscopic photograph are imported in scanning electron microscopic picture software, the spy that two pictures are marked
Sign point is interrelated, obtains the coincidence image of two photos；
(5) the coincidence image is observed under a scanning electron microscope, obtains the appearance information of color spot.
In order to further detect the specific element composition of color spot, the method also includes: (6) are scanned with X-ray energy disperse spectroscopy
The coincidence image, acquires the spectrogram of each element in the interior zone of the color spot, quantitatively calculates each element according to the spectrogram
Weight percentage.The element includes C and F, further includes modified coherent element, such as one of Sn, Cu, Si or a variety of.
The adoptable conventional method in this field can be used in the quantitative calculating, such as: algorithm eZAF is carried using energy disperse spectroscopy TEAM system
It is calculated.
In order to improve the accuracy of detection, the present invention preferably pre-processes sample.Specifically: what is be analysed to contains
The modified polytetrafluoroethylresin resin pad sample of color spot is cut into 1~2cm × 1~2cm bulk, is fixed on sample carrier with conducting resinl
On, sample surfaces, natural air drying to drying are cleaned with alcohol.
When the use scanning electron microscope, sample ion sputtering film coating instrument metal spraying is uniformly plated in sample surfaces
A layer thickness is the golden film of 5~15nm, places into scanning electron microscope example room and observes, takes pictures.It is preferably electric when scanning electron microscope is taken pictures
Mirror acceleration voltage is 3~5KV, line is 6~8, beam spot size < 500nm.
In order to ensure gained photo is easy to be overlapped, and ensures to be overlapped gained image and be easy to observation and elemental analysis, the present invention
In preferred steps (1) in the amplification factor of optical microscopy and step (3) amplification factor of scanning electron microscope be 10~
60 times.
When step (5) is observed, adjustable amplification factor to label range is paved with field of view, it is ensured that any position in the visual field
It is color spot interior zone.The appearance information of the obtained color spot includes its realistic colour.
In order to further increase the accuracy of detection, detection error is reduced, the present invention is carried out in step (6) using energy disperse spectroscopy
When scanning, preferably energy disperse spectroscopy Electronic Speculum acceleration voltage is 10~15KV, and line is 10~14, takes out 30~40 ° of angle, exports counting rate
>4000；It is highly preferred that energy disperse spectroscopy Electronic Speculum acceleration voltage is 14~15KV, line is 13~14, takes out 35 ° of angle, exports counting rate
6800~7000.
As a preferred solution of the present invention, the test object is copper powder modified polytetrafluoroethylresin resin gasket.This
By largely practice discovery, energy disperse spectroscopy Electronic Speculum acceleration voltage use Electronic Speculum acceleration voltage for 14~15KV for invention, line for 13~
14, when taking out 35 ° of angle, exporting the preferred parameter of counting rate 6800~7000, when can significantly reduce to element percentage composition detection
Standard deviation, to element (including C, F, Sn and Cu) contained in copper powder modified polytetrafluoroethylresin resin gasket, especially
The examination criteria deviation reducing effect of Cu constituent content is fairly obvious.
The present invention uses optical microscopy-method associated with scanning electron microscope-energy disperse spectroscopy, can quickly and easily detection and localization
The elemental composition of non-uniform color spot in modified polytetrafluoroethylresin resin gasket.Compared with prior art, both can recognize color or
It can recognize pattern, and color spot unknown small and without surface topography difference can be quickly and accurately positioned；The deviation quantitative to element
It can be reduced to 0.03% by 12.13% before no-fix, greatly promote the confidence level of quantitative result；Accurate positioning, favorable reproducibility,
It is more intuitive, convenient for analysis.
Detailed description of the invention
Fig. 1 is modified polytetrafluoroethylresin resin pad sample under optical microscopy in embodiment 1.
Fig. 2 is the optical microscopy sample pictures after marking in embodiment 1.
Fig. 3 is modified polytetrafluoroethylresin resin pad sample under scanning electron microscope in embodiment 1.
Fig. 4 is that light microscopic and Electronic Speculum are overlapped image in embodiment 1.
Fig. 5 is the color spot that size all over the screen is amplified in embodiment 1, is at this time the accurate positioning effect of color spot.
Fig. 6 is that the element of energy disperse spectroscopy inside color spot in embodiment 2 acquires spectrogram.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The identification of copper powder modified polytetrafluoroethylresin resin gasket surface color spot and image procossing
Instrument: scanning electron microscope TESCAN MIRA3
Instrument parameter condition specifically:
Electronic Speculum acceleration voltage: 5KV；
Electronic beam current BI:7；
Operating distance WD:35cm；
Sweep speed: speed7；
Sample stage inclination angle: 0 °；
Beam spot size: < 500nm.
Concrete operation step are as follows:
(1) target sample is cut into the bulk of 1cm*1.3cm, is fixed on sample carrier with conducting resinl, cleans sample with alcohol
Product surface, natural air drying to drying；The sample made is put and is observed under an optical microscope, color spot position to center is adjusted, is clapped
Lower high definition photo (such as Fig. 1)；
(2) photo is imported into mapping software, marked color spot profile (such as Fig. 2), and any position gets mark ready outside profile
It is denoted as being characterized a little；
(3) by sample ion sputtering film coating instrument electric current 15mA metal spraying 100s, then it is put into scanning electron microscope example room Zhong Guan
It examines, scan and stores the high definition electron microscopic picture (such as Fig. 3) under 50 times of sample；
(4) optical microscope picture marked and scanning electron microscopic picture are imported in X-Position simultaneously, respectively will
The characteristic point of two pictures label is interrelated, at this point, being shown as the coincidence image of two pictures at Electronic Speculum real time scan window
(such as Fig. 4)；
(5) the color spot image under realistic colour is observed in real time under Electronic Speculum；Sample stage is increased, adjustment operating distance WD is
12.5mm adjusts amplification factor to label range and is paved with field of view (such as Fig. 5), at this point, any position is color spot in the visual field
Interior zone.
Embodiment 2
Copper powder modified polytetrafluoroethylresin resin gasket surface color spot is former molecular qualitative and quantitative
Instrument: X-ray energy disperse spectroscopy EDAX
Instrument parameter condition:
Electronic Speculum acceleration voltage: 15KV；
Electronic beam current BI:14；
Operating distance WD:12.5cm；
Sweep speed: speed7；
Taking-up angle: 35 °；
Output counting rate: > 4000；
Dead time: < 50；
Acquisition time: 100s；
Operating procedure:
Step (1)~(5) are the same as embodiment 1；
(6) by the color spot image synchronization for having positioned completion in embodiment 1 into energy disperse spectroscopy, changing Electronic Speculum acceleration voltage is
15KV, electronic beam current BI are 14, and operating distance WD is maintained at 12.5cm, and exporting counting rate at this time is 6830, dead time < 50, if
Setting acquisition time is 100s.Acquisition color spot interior zone element information obtains spectrogram (as shown in Figure 6).With EDAX energy disperse spectroscopy TEAM
System carries algorithm eZAF and carries out quantitative calculating to element, and quantitative result is repeated 3 times acquisition, standard deviation knot as shown in table 1,2
Fruit is as shown in Table 3, 4.
1 color spot inner region atom quantitative result of table
| Element | Weight % | Atom % | Net intensity |
| C | 14.46 | 44.1 | 81.69 |
| F | 7.35 | 14.15 | 61.52 |
| Sn | 12.3 | 3.79 | 148.17 |
| Cu | 65.9 | 37.96 | 501.04 |
2 color spot exterior domain atom quantitative result of table
| Element | Weight % | Atom % | Net intensity |
| C | 26.51 | 43.9 | 131.61 |
| F | 38.54 | 40.41 | 264.25 |
| Sn | 2.26 | 5.74 | 41.2 |
| Cu | 32.69 | 9.95 | 242.33 |
3 color spot inner region atomic wts % quantitative result of table
Atomic wts % quantitative result outside 4 color spot region of table
| Element | It acquires for the first time | Second of acquisition | Third time acquires | Standard deviation |
| C | 26.51 | 26.33 | 26.55 | 0.10 |
| F | 38.54 | 38.66 | 38.48 | 0.07 |
| Sn | 2.26 | 2.39 | 2.33 | 0.05 |
| Cu | 32.69 | 32.62 | 32.64 | 0.03 |
Embodiment 3
X-ray energy spectrum analysis is carried out to the modified polytetrafluoroethylresin resin gasket surface color spot of accurate positioning in embodiment 1,
With embodiment 2, difference is only that specific implementation method, and electronic beam current BI is 10, and exporting counting rate at this time is 4690, and element is quantitative
The results are shown in Table 5, is repeated 3 times acquisition, and Cu standard deviation is 1.14%.
5 color spot inner region atomic wts % quantitative result of table
| Element | It acquires for the first time | Second of acquisition | Third time acquires | Standard deviation |
| C | 15.51 | 13.14 | 15.98 | 1.24 |
| F | 6.69 | 7.06 | 7.33 | 0.26 |
| Sn | 12.06 | 12.33 | 11.98 | 0.15 |
| Cu | 65.74 | 67.47 | 64.71 | 1.14 |
Embodiment 4
X-ray energy spectrum analysis is carried out to the modified polytetrafluoroethylresin resin gasket surface color spot of accurate positioning in embodiment 1,
With embodiment 2, difference is only that specific implementation method, and Electronic Speculum acceleration voltage is 10KV, and exporting counting rate at this time is 4130, element
Quantitative result is as shown in table 6, is repeated 3 times acquisition, and Cu standard deviation is 1.23%.
6 color spot inner region atomic wts % quantitative result of table
Comparative example 1
X-ray energy spectrum analysis, specific embodiment party are carried out to the modified polytetrafluoroethylresin resin gasket surface color spot of embodiment 1
With embodiment 2, difference is only that method, is not carried out light microscopic-Electronic Speculum combination to sample and is positioned to color spot, directly with energy disperse spectroscopy
Surface scan method carries out primary positioning to sample, carries out qualitative elementary quantitative analysis to color spot.Output counting rate is 6600 at this time, member
Plain quantitative result is as shown in table 7, is repeated 3 times acquisition, and Cu standard deviation is 12.13%.
7 color spot inner region atomic wts % quantitative result of table
| Element | It acquires for the first time | Second of acquisition | Third time acquires | Standard deviation |
| C | 22.31 | 16.57 | 30.1 | 5.54 |
| F | 36.12 | 30.11 | 46.33 | 6.70 |
| Sn | 4.23 | 6.93 | 6.21 | 1.14 |
| Cu | 37.34 | 46.39 | 17.36 | 12.13 |
Conclusion: by above-described embodiment and comparative example it is found that provided by the invention be directed to modified polytetrafluoroethylresin resin gasket
The quantification and qualification method of color spot, this method simple process, easily operated and popularization, data reappearance is good, is suitable for tight
The confidence interval of lattice, has a good application prospect.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (10)
1. the analysis method of color spot in a kind of pair of modified polytetrafluoroethylresin resin gasket, which comprises the steps of:
(1) it is taken pictures with optical microscopy to the modified polytetrafluoroethylresin resin pad sample to be analyzed containing color spot, really
It protects the color spot and is located at central region, obtain high definition light microscope photo；
(2) light microscope photo is imported into mapping software, describes color spot profile, and any position gets conduct ready outside the profile
Characteristic point；
(3) under conditions of amplification factor identical as use of taking pictures described in step (1), with scanning electron microscope to the sample
It takes pictures, it is ensured that the color spot is located at central region, obtains high definition electromicroscopic photograph；Color spot is described using method identical with step (2)
Profile, and get ready in position identical with step (2) as characteristic point；
(4) light microscope photo and electromicroscopic photograph are imported in scanning electron microscopic picture software, the characteristic point that two pictures are marked
It is interrelated, obtain the coincidence image of two photos；
(5) the coincidence image is observed under a scanning electron microscope, obtains color spot appearance information.
2. the method according to claim 1, wherein further including step (6): described in the scanning of X-ray energy disperse spectroscopy
It is overlapped image, the spectrogram of each element in the interior zone of the color spot is acquired, the weight of each element is quantitatively calculated according to the spectrogram
Measure percentage composition.
3. according to the method described in claim 2, it is characterized in that, the Electronic Speculum acceleration voltage of the energy disperse spectroscopy be 10~15KV,
Line is 10~14, and taking out angle is 30~40 °, exports counting rate > 4000.
4. according to the method described in claim 2, it is characterized in that, the Electronic Speculum acceleration voltage of the energy disperse spectroscopy be 14~15KV,
Line is 13~14, and taking out angle is 34.5~35.5 °, and output counting rate is 6800~7000.
5. according to the method described in claim 2, it is characterized in that, the instrument parameter condition of the energy disperse spectroscopy includes:
Electronic Speculum acceleration voltage: 15KV；
Electronic beam current BI:14；
Operating distance WD:12.5cm；
Sweep speed: speed7；
Taking-up angle: 35 °；
Output counting rate: 6830；
Dead time: < 50；
Acquisition time: 100s.
6. method described in any one according to claim 1~5, which is characterized in that further include being located in advance to the sample
Reason；Specifically:
The modified polytetrafluoroethylresin resin pad sample containing color spot being analysed to is cut into 1~2cm × 1~2cm bulk, uses
Conducting resinl is fixed on sample carrier, cleans sample surfaces, natural air drying to drying with alcohol.
7. the method according to claim 1, wherein step (3) use scanning electron microscope when, by sample with from
Sub- sputter coating instrument metal spraying uniformly plates the golden film that a layer thickness is 5~15nm in sample surfaces, places into scanning electron microscope example
It observes, take pictures in room.
8. method according to claim 1 or claim 7, which is characterized in that when step (3) is taken pictures with scanning electron microscope, Electronic Speculum accelerates
Voltage is 3~5KV, line is 6~8, beam spot size < 500nm.
9. method according to claim 1 or claim 7, which is characterized in that the instrument for the scanning electron microscope that step (3) uses
Parameter Conditions include:
Electronic Speculum acceleration voltage: 5KV；
Electronic beam current BI:7；
Operating distance WD:35cm；
Sweep speed: speed7；
Sample stage inclination angle: 0 °；
Beam spot size: < 500nm.
10. method described in any one according to claim 1~9, which is characterized in that optical microscopy puts in step (1)
The amplification factor of scanning electron microscope is 10~60 times in big multiple and step (3).
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| CN112415036A (en) * | 2019-08-23 | 2021-02-26 | 中昊晨光化工研究院有限公司 | Method for detecting PTFE emulsion particles based on scanning electron microscope |
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