CN101936712A - Method and device for measuring thickness of oil film on surface of metal plate - Google Patents
Method and device for measuring thickness of oil film on surface of metal plate Download PDFInfo
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- CN101936712A CN101936712A CN2009100543793A CN200910054379A CN101936712A CN 101936712 A CN101936712 A CN 101936712A CN 2009100543793 A CN2009100543793 A CN 2009100543793A CN 200910054379 A CN200910054379 A CN 200910054379A CN 101936712 A CN101936712 A CN 101936712A
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Abstract
The invention relates to the field of physicochemical detection, and in particular to a method and a device for measuring the thickness of an oil film. A device for measuring the thickness of an oil film on the surface of a metal plate comprises an oil removal device, an ellipsometer and a sample frame. A method for measuring the thickness of an oil film on the surface of a metal plate comprises the following steps of: (1) fixing a sample to be measured; (2) measuring the initial phase difference delta1 between a wave P and a wave S by the ellipsometer; (3) cleaning the oil film in situ; (4) measuring the final phase difference delta0 between the wave P and the wave S after the oil is removed by the ellipsometer; and (5) computing the relative delta value of the sample to be measured and analyzing the relative delta value to obtain the thickness of the oil film. The invention does not need the distilled water in the detection process and accords with the design concept of energy saving and consumption lowering; the detection precision, accuracy and detection efficiency are greatly improved and the time for each detection is within 1 minute; the invention satisfies the demand of mass production, particularly suits the production inspection of tin plate, can rapidly and correctly measure the thickness of the oil film on the surface of the tin plate, and has wide market prospect and application popularization value.
Description
Technical field
The present invention relates to the physics and chemistry detection range, relate in particular to a kind of oil film thickness assay method and device.
Background technology
In the tin plate production technology, generally the method with oil surface prevents to get rusty or scratch, and is coated with oil mass and is generally 3-8mg/M
2, be coated with the too much or very few production that all can influence next procedure of oil mass.Therefore being coated with oil mass is the key factor that influences product quality, and cold rolling mill will be coated with the important indicator of oil mass as quality control, and test result is instructed, adjusts oiling technology in real time.Measure test result if can't in time obtain oiling, may have influence on the production logistics of tin plate.
Patent CN92221096.9 has introduced a kind of lubrication medium film thickness measurement equipment, when oil film thickness very hour, steel ball surface will absorb the energy of a part of light wave, and intensity of reflected light is died down.Definite funtcional relationship is arranged between oil film thickness and the intensity of reflected light, after apparatus structure is determined, just can measure oil film thickness by the variation of intensity of reflected light.Described measuring instrument is made up of steel ball, glass disc, light source, driving mechanism, microscope, photo-detector, computing machine and picture monitor, and tested lubrication medium film places between steel ball and the glass disc; Described glass disc and driving mechanism relative fixed are installed, and described light source places a side of glass disc; Described microscope places the glass disc opposite side, and described photo-detector places the microscope rear, and the light intensity signal in the microscope is delivered to computing machine and picture monitor successively; Its principle is to utilize the variation of emitted luminescence intensity to detect oil film thickness.
Patent CN93104866.4 has introduced the method for oil film thickness between a kind of measurement point, the line, belongs to the measuring method of film thickness.This method with light by semi-transparent semi-reflecting film and the oil film that will survey, produce the reflection of different light paths, form interference ring, the different ring of light of light and shade is arranged on the interference ring, measure the interference light intensity of each point on the ring of light, draw the maximum interference light intensity, the interference light intensity of minimum interference light intensity and interference ring center, record simultaneously the only logical semi-transparent semi-reflecting film of light again, the interference light intensity at interference ring center during the apply oil film not can by formula be tried to achieve the thickness of lubricating oil film; Principle is to utilize the variation that detects lubricating oil film interpolation front and back interference light intensity to measure oil film thickness.
The technology of the mensuration tin plate oil film thickness that uses now has two kinds in addition: physics method and light extinction method.
The physics ratio juris is that sample is cleaned up and down in rectangular tank, makes oil film break away from sample surfaces and swims on the water surface.Drive specific device oil film is pooled to a zone, when being pooled to the thickness of a setting, sensor meeting output response signal, this moment is by measuring oil film calculates oil film in the length of tank volume (tank width and oil film thickness are known quantity), divided by the surface area of sample, can calculate oil film thickness.This method of testing can obtain suitable precision and accuracy, but its shortcoming also is quite tangible: the pre-treatment work more complicated of sample, detection efficiency is low, be about 10 minutes the analysis time of every sample, because the technology of production line will be adjusted according to test result, therefore analysis speed there is strict requirement, the examination requirements that detects three samples in left, center, right end to end with output and every roll bending material of present cold rolling mill, this method generally only is used for the correction and the interim emergent usefulness of analyzing of instrument, not too is suitable for the big production occasion of inspected number; And each analysis all can consume a large amount of distilled water, does not meet the theory of environmental protection and energy saving consumption reduction.
The light extinction method principle is to utilize the Extinction Characteristic of elliptically polarized light.Promptly have under the state of oil film at sample surfaces, the rotation polarizer and analyzer, it is strong to make photomultiplier behind the analyzer obtain full black light.Clean the oil film of sample surfaces then, rotate the polarizer once more, complete it is strong to make that photomultiplier obtains black light once more, the angle of polarizer rotation is different with the difference of sample surfaces oil film thickness.According to the calibration curve of making in advance, can obtain the thickness of oil film.This kind method is owing to be subjected to factor affecting such as light path resolution is not high, the easy error in extinction position, cause the thickness error of calculation, so measuring accuracy and accuracy are not satisfactory, can't reach the detection requirement, because this inborn defective can't be eliminated, and has stopped the further research and development and the production of this instrument.
Summary of the invention
Technical matters to be solved by this invention provides a kind of metal sheet surface oil film thickness assay method and device, and existing physics method detection efficiency is low to be unfavorable for large-scale production, the defective of light extinction method accuracy in detection difference to solve.
A kind of metal sheet surface oil film thickness assay method may further comprise the steps:
1) fixing testing sample;
2) use the ellipsometer measurement testing sample, obtain the initial phase difference Δ of P ripple and S ripple
1
3) original position is cleaned oil film, keeps testing sample to maintain static, and is injected in sample surfaces with oil removal plant after with oil film clean-out system heating and gasifying, and keeps the regular hour, thoroughly removes the oil film on testing sample surface;
4) use the final phase difference of P ripple and S ripple after the oil removing of ellipsometer measurement testing sample again
0
5) analysis obtains oil film thickness, by calculating the relative Δ value of testing sample, i.e. Δ=Δ
1-Δ
0, substitution correlativity curve finally draws oil film thickness.
A kind of metal sheet surface oil film thickness determinator, comprise oil removal plant, ellipsometer, specimen holder and control computer, testing sample is fixed on the specimen holder, described ellipsometer comprises ellipsometer detecting unit and ellipsometer light source cell, the position and the specimen holder of two unit match, the testing sample on the nozzle location counter sample frame of described oil removal plant.
Described specimen holder is six sample rotating mechanisms, by the fixing testing sample of electromagnet.
The light source of described ellipsometer is the 50W quartz halogen lamp, beam diameter 3～5mm, and spectral range 370nm～1000nm, polarized light go into, 70 ° of shooting angles.
Described oil removal plant comprises fluid reservoir, discharge pump, heating tank, nozzle solenoid valve and the nozzle that is connected in turn by pipeline, in the described fluid reservoir clean-out system is housed, level switch and heating rod are housed in the described heating tank, the cleaning air exhauster is equipped with in the oil removal plant below, the inlet duct that cleans air exhauster links to each other with the cavity that cleans sample, and outlet conduit is discharged outdoor.
Described nozzle is the constant temperature nozzle.
Described clean-out system is methylene chloride or triclene.
Described heating tank pressure limit is 0.6～1Kg/cm
2
Detection method of the present invention and pick-up unit thereof adopt ellipse inclined to one side technology, the polarizing light irradiation sample surfaces, its catoptrical phase differential can change, definite funtcional relationship is arranged between the changing value of oil film thickness and phase differential, can measure oil film thickness by the changing value that detects relative phase difference, need not to locate the extinction position during this measurement device, thereby overcome the thickness error of calculation that causes because of best extinction position error, improved measuring accuracy and accuracy greatly; This assay method sample pre-treatments is simple simultaneously, and average every sample analysis time can reach in 1 minute; The sample analysis process need not to consume any distilled water, meets energy-saving and cost-reducing design concept; Determinator of the present invention in addition adopts 6 sample self-turning mechanisms, once can analyze 6 samples continuously, has greatly improved labour productivity.Accuracy of detection of the present invention in sum, accuracy, detection efficiency all improve greatly, satisfied requirement of large-scale production, be specially adapted to the tin plate production testing, can measure the tin plate sheet surface oil film thickness rapidly and accurately, have vast market prospect and application and popularization value.
Description of drawings
Fig. 1 looks synoptic diagram for the master of metal sheet surface oil film thickness determinator of the present invention;
Fig. 2 looks synoptic diagram for the left side of determinator of the present invention;
Fig. 3 looks synoptic diagram for the right side of determinator of the present invention;
Fig. 4 is a structural representation of the present invention.
Among the figure: 1 fluid reservoir, 2 discharge pumps, 3 clean air exhauster, 4 ellipsometer detecting units, 5 specimen holders, 6 ellipsometer light source cells, 7 heating rods, 8 heating tanks, 9 level switches, 10 nozzle solenoid valves, 11 nozzles, 12 testing samples.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's statement, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Referring to Fig. 1,2,3, shown in 4, a kind of metal sheet surface oil film thickness determinator, comprise oil removal plant, ellipsometer, specimen holder 5 and control computer, described specimen holder 5 is six sample rotating mechanisms, once can place 6 testing samples 12, adsorb fixedly testing sample 12 by electromagnet, the suction of electromagnet to guarantee testing sample 12 in jet cleaning oil film process not by displacement, six sample rotating mechanisms reach pinpoint purpose by the umber of pulse of setting step motor and the dual control measure that read the photoelectric sensor control signal, when in the analytic process during step motor step-out, photo-sensor signal will can conducting, rotating mechanism is got back to the position that needs analytic sample after with auto-initiation, guarantees the accurate location of specimen holder 5.Described ellipsometer comprises ellipsometer detecting unit 4 and ellipsometer light source cell 6, the position of two unit and specimen holder 5 match, the preferred implementation condition of ellipsometer is the 50W quartz halogen lamp for the light source that uses, beam diameter 3～5mm, spectral range 370nm～1000nm, polarized light go into, 70 ° of shooting angles, and the 50w Halogen lamp LED can obtain enough light intensity, improve power and will reduce serviceable life, the Δ sensitivity that the incident angle that evidence is 70 ° obtains is the highest.Testing sample 12 on the nozzle 11 position counter sample framves 5 of described oil removal plant.Described oil removal plant comprises the fluid reservoir 1 that is connected in turn by pipeline; discharge pump 2; heating tank 8; nozzle solenoid valve 10 and nozzle 11; in the described fluid reservoir 1 clean-out system is housed; level switch 9 and heating rod 7 are housed in the described heating tank 8; the oil removal plant below is equipped with and is cleaned air exhauster 3; the inlet duct of air exhauster 3 links to each other with the cavity that cleans sample; outlet conduit is discharged outdoor; clean-out system is selected methylene chloride or triclene usually for use; because methylene chloride or triclene are harmful; from the safeguard protection angle; cleaning the process of oil film finishes in an airtight relatively space; discharge outdoor rapidly with cleaning air exhauster 3 after finishing; consider that triclene is stronger to the toxicity of human body, so from the view of safety, do not recommend to use.
For guaranteeing that clean-out system keeps gaseous state, nozzle 11 selected constant temperature nozzles are to guarantee gasification result.Wherein heating tank 8 is tank bodies of heating oil film clean-out system, is responsible for heating oil film clean-out system by special-purpose heating rod 7, and its boiling point is set at target temperature, and is provided with safety valve, and heating tank 8 internal pressure scopes are 0.6～1Kg/cm
2In case overload can be opened release automatically, to guarantee safety; Level switch 9 is installed in the heating tank 8, in case liquid level is lower than desired value, heating rod 7 will quit work, and discharge pump 2 will be opened automatically this moment, and the clean-out system in the fluid reservoir 1 is added to heating tank 8.Pass through the constant temperature nozzle ejection behind the clean-out system heating and gasifying on testing sample 12 surfaces, and keep the regular hour, make the oil film on testing sample 12 surfaces thoroughly be eliminated, can not remain in testing sample 12 surfaces simultaneously and form new retes and the impact analysis result.
Each is performed the action of device the control computer major control, comprises the rotation and the correction of heating, fluid infusion, injection, six sample rotating mechanisms; The supervising device state comprises heating-up temperature, pressure, six sample rotating mechanism positions etc.; The control ellipsometer also reads the ellipsometer detecting information, calculates the oil film thickness result by the calibration curve of making in advance; Functions such as data storage, inquiry and transmission.
Before the mensuration unknown sample, the reply instrument is proofreaied and correct.The method that obtains the correlativity curve is that the substrate of same roughness is got 5 kind or above sample by thick to thin by oil film thickness, and every kind of sample is got two (i.e. 5 groups of samples, 2 every group).2 samples of same group are tested on this device and hydrophilic balance respectively.The relative Δ value (Δ that records by device of the present invention
1-Δ
0) with hydrophilic balance on the oil film thickness (can obtain per sample 5 groups above data) that records calculate relevance formula, and use the correlativity curve representation.The substrate of different roughness has different correlativity curves, can call corresponding correlativity curve and obtain the result according to actual sample during mensuration.
A kind of metal sheet surface oil film thickness assay method may further comprise the steps:
1) fixing testing sample 12;
2), obtain the initial phase difference Δ of P ripple and S ripple with ellipsometer measurement testing sample 12
1
3) original position is cleaned oil film, keeps testing sample 12 to maintain static, and is injected in sample surfaces with oil removal plant after with oil film clean-out system heating and gasifying, and keeps the regular hour, thoroughly removes the oil film on testing sample 12 surfaces;
4) use the final phase difference of P ripple and S ripple after 12 oil removings of ellipsometer measurement testing sample again
0
5) analysis obtains oil film thickness, by calculating the relative Δ value of testing sample 12, i.e. Δ=Δ
1-Δ
0, substitution correlativity curve finally draws oil film thickness.
The mensuration process:
At first testing sample 12 is adsorbed on the electromagnet of specimen holder 5, can loads one to six testing sample 12 according to testing sample 12 amounts.After application software received the beginning analysis instruction, control computer was at first controlled ellipsometer and is read the initial phase difference Δ
1Automatically open nozzle solenoid valve 10 then, the gaseous cleaning agent during heating is irritated is ejected into testing sample 12 surfaces, can set injecting time in advance to guarantee deoiling effect according to actual conditions; Etc. several seconds, after the clean-out system on wait test sample product 12 surfaces volatilizees fully, control the final phase difference after ellipsometer reads the oil film cleaning once more
0Control computer goes out the difference DELTA of two phase differential by computed in software, and the correlativity curve by making in advance calculates the oil film thickness result, and result of calculation is come out in screen displayed, and automatically with the mean value storage with transmit.
Claims (8)
1. metal sheet surface oil film thickness assay method may further comprise the steps:
1) fixing testing sample (12);
2), obtain the initial phase difference Δ of P ripple and S ripple with ellipsometer measurement testing sample (12)
1
3) original position is cleaned oil film, keeps testing sample (12) to maintain static, and is injected in sample surfaces with oil removal plant after with oil film clean-out system heating and gasifying, and keeps the regular hour, thoroughly removes the oil film on testing sample (12) surface;
4) use the final phase difference of P ripple and S ripple after ellipsometer measurement testing sample (12) oil removing again
0
5) analysis obtains oil film thickness, by calculating the relative Δ value of testing sample (12), i.e. Δ=Δ
1-Δ
0, substitution correlativity curve finally draws oil film thickness.
2. metal sheet surface oil film thickness determinator, comprise oil removal plant, ellipsometer, specimen holder and control computer, it is characterized in that: testing sample (12) is fixed on the specimen holder, described ellipsometer comprises ellipsometer detecting unit (4) and ellipsometer light source cell (6), the position of two unit and specimen holder (5) match, the testing sample (12) on the nozzle of described oil removal plant (11) the position counter sample frame (5).
3. metal sheet surface oil film thickness determinator as claimed in claim 2 is characterized in that: described specimen holder (5) is six sample rotating mechanisms, by the fixing testing sample 12 of electromagnet.
4. metal sheet surface oil film thickness determinator as claimed in claim 2 is characterized in that: the light source of described ellipsometer is the 50W quartz halogen lamp, beam diameter 3～5mm, and spectral range 370nm～1000nm, polarized light go into, 70 ° of shooting angles.
5. metal sheet surface oil film thickness determinator as claimed in claim 2, it is characterized in that: described oil removal plant comprises fluid reservoir (1), discharge pump (2), heating tank (8), nozzle solenoid valve (10) and the nozzle (11) that is connected in turn by pipeline, described fluid reservoir is equipped with clean-out system in (1), level switch (9) and heating rod (7) are housed in the described heating tank (8), the oil removal plant below is equipped with and is cleaned air exhauster (3), the inlet duct that cleans air exhauster (3) links to each other with the cavity that cleans sample, and outlet conduit is discharged outdoor.
6. metal sheet surface oil film thickness determinator as claimed in claim 5 is characterized in that: described nozzle (11) is the constant temperature nozzle.
7. metal sheet surface oil film thickness determinator as claimed in claim 5 is characterized in that: described clean-out system is methylene chloride or triclene.
8. metal sheet surface oil film thickness determinator as claimed in claim 5 is characterized in that: described heating tank (8) pressure limit is 0.6～1Kg/cm
2
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100543793A CN101936712B (en) | 2009-07-03 | 2009-07-03 | Method and device for measuring thickness of oil film on surface of metal plate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100543793A CN101936712B (en) | 2009-07-03 | 2009-07-03 | Method and device for measuring thickness of oil film on surface of metal plate |
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| Publication Number | Publication Date |
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| CN101936712A true CN101936712A (en) | 2011-01-05 |
| CN101936712B CN101936712B (en) | 2012-01-11 |
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102410967A (en) * | 2010-09-21 | 2012-04-11 | 上海宝钢工业检测公司 | Method for measuring oil film amount on surface of chrome-plating steel |
| CN104677784A (en) * | 2015-03-04 | 2015-06-03 | 苏州创恩机械设备有限公司 | Plate surface oil film measurement device and method adopting same |
| CN104731002A (en) * | 2013-12-18 | 2015-06-24 | 上海宝钢工业技术服务有限公司 | Full-automatic tinplate oiling amount detection instrument based on Wilhelmy plate method |
| CN107192857A (en) * | 2016-03-14 | 2017-09-22 | 中国科学院沈阳自动化研究所 | A kind of nano film thickness detection means and its method based on ultrasonic AFM |
| CN111380809A (en) * | 2020-05-06 | 2020-07-07 | 长春理工大学 | Method for testing oil film type based on polarization characteristic |
| CN112501622A (en) * | 2020-11-11 | 2021-03-16 | 浙江智海化工设备工程有限公司 | Aluminum alloy oil removing cleaning agent and oil removing and dirt removing cleaning method thereof |
| CN113029050A (en) * | 2021-03-02 | 2021-06-25 | 桂恩波 | High-precision pressing plate bias early warning protection system |
-
2009
- 2009-07-03 CN CN2009100543793A patent/CN101936712B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102410967A (en) * | 2010-09-21 | 2012-04-11 | 上海宝钢工业检测公司 | Method for measuring oil film amount on surface of chrome-plating steel |
| CN104731002A (en) * | 2013-12-18 | 2015-06-24 | 上海宝钢工业技术服务有限公司 | Full-automatic tinplate oiling amount detection instrument based on Wilhelmy plate method |
| CN104731002B (en) * | 2013-12-18 | 2019-01-04 | 上海宝钢工业技术服务有限公司 | A kind of tin plate painting full-automatic detector of oil mass based on Wilhelmy flat band method |
| CN104677784A (en) * | 2015-03-04 | 2015-06-03 | 苏州创恩机械设备有限公司 | Plate surface oil film measurement device and method adopting same |
| CN107192857A (en) * | 2016-03-14 | 2017-09-22 | 中国科学院沈阳自动化研究所 | A kind of nano film thickness detection means and its method based on ultrasonic AFM |
| CN111380809A (en) * | 2020-05-06 | 2020-07-07 | 长春理工大学 | Method for testing oil film type based on polarization characteristic |
| CN112501622A (en) * | 2020-11-11 | 2021-03-16 | 浙江智海化工设备工程有限公司 | Aluminum alloy oil removing cleaning agent and oil removing and dirt removing cleaning method thereof |
| CN113029050A (en) * | 2021-03-02 | 2021-06-25 | 桂恩波 | High-precision pressing plate bias early warning protection system |
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|---|---|
| CN101936712B (en) | 2012-01-11 |
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