CN108692664A - A kind of test method of thickness of coating - Google Patents
A kind of test method of thickness of coating Download PDFInfo
- Publication number
- CN108692664A CN108692664A CN201710227457.XA CN201710227457A CN108692664A CN 108692664 A CN108692664 A CN 108692664A CN 201710227457 A CN201710227457 A CN 201710227457A CN 108692664 A CN108692664 A CN 108692664A
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- Prior art keywords
- coating
- thickness
- sample
- solution
- sample blocks
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
- G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The invention discloses a kind of test methods of thickness of coating, include the following steps:The sample blocks that plate areas can accurately calculate are made in sample to be tested, coating on sample blocks is cleared up completely with strong acid, the test solution of certain volume is made, the content of coated metal ingredient in solution is measured with inductive coupling plasma emission spectrograph, then the quality for calculating Coating composition, the thickness of coating is calculated in conjunction with the sample blocks area measured.Advantage of this approach is that accurate testing degree is high, representative strong, interference is less, error is small, test thickness of coating range is wide;General chemical laboratory can be tested, and the calibrator of profession is not needed.
Description
[Technical field]
The present invention relates to a kind of test method of thickness of coating, specially one kind by chemical digesting coating and utilizing inductance
The method that coupled plasma optical emission spectrometer measures thickness of coating and ingredient.
[Background technology]
Coating be in order to it is good-looking or change certain article characters and the one layer of thin metal plated on its surface or its
Its element, main function have:1, etch resistant properties of the metal parts in use environment are improved;2, the appearance of decoration parts, makes
It is bright beautiful;3, improve part working performance, such as hardness, wearability, electric conductivity, electromagnetically, heat resistance.
The thickness and ingredient of coating determine that the physical property of plating piece, blocked up coating can cause Deposit appearance coarse, easy
It peels off, plating piece is unable to undergo to carry and the collision in installation process.Coating is excessively thin to cause working performance to decline, and defencive function is not up to
To pre-provisioning request.So for plating piece, have suitable thickness of coating and ingredient extremely important.
There are three the current method for testing coating is main:
(1) metallographic method (also known as method of section or microscopic method);
(2) coulometry;
(3) x-ray fluorescence film thickness method.
Wherein metallographic method is that plating piece is carried out section cutting polishing, then coordinates precision scale to observe with high-power microscope
Measure the thickness of coating.But the method accuracy when thickness of coating is less than 1 micron plating thickness that is poor, and testing
Degree is the thickness of coating in certain section, which is possible to the accuracy of damage influence test result cutting the when of polishing.
Coulometry is to carry out local anode dissolving to being tested the coat of metal of part, reaches material by anodic solution coating
Potential change when matrix carries out the measurement of thickness of coating.But the method can only test surfaces be plane plating piece, and survey
Examination precision is affected by electricity, current efficiency and electrochemical equivalent.
X-ray fluorescence film thickness method measure overburden cover be based on a branch of strong and narrow heterogeneous x ray and matrix and
The interaction of coating.This interaction generates the secondary radiation of discrete wavelength and energy, these secondary radiations, which have, to be constituted
Coating and matrix element feature.Coating mass area ratio (if density it is known that if be coating linear thickness) and secondary
There are certain relationships between radiation intensity.The relationship is first by the coating calibration standard block correction of known unit area quality
It determines.If the density of covering layer material it is known that provide the density of reagent again simultaneously, such calibrated bolck can provide coating
Linear thickness.But the method is larger by instrument power and coating species influence, when the bigger coating of component atoms number in coating
When thickness is thicker, measurement result deviation is larger, or even can not penetrate coating causes test result deviation occur.
In addition chemical method test thickness of coating such as strips coating process, drop method and liquid flow method.And some are emerging fast
The method that speed measures coating.
Patent document (application number:201410609442.6 a kind of method of quick measurement metal layer thickness) in introduce profit
The method for measuring the coat of metal with pulse laser series inductive coupling plasma mass spectrograph, according to unit pulse denudation and
Degrading the time is calculated thickness of coating, although this method is quick, needing to make high-precision standard component could be surveyed
The case where measuring, while being also the measurement of single-point or several points, cannot integrally reflect thickness of coating, can not measure coating
Ingredient;
Patent document (application number:201410609442.6 a kind of assay method of substrate surface coating) utilize electron microscopic
Mirror surveys thickness of coating, while the ingredient of coating is measured using energy disperse spectroscopy, and this method also suffers from certain drawbacks, in energy disperse spectroscopy
There are some elemental characteristic spectral lines are close, the case where interfering with each other, it is unfavorable for the accurate qualitative of ingredient.
Also just like Gong Shuqing (method of atomic absorption detecting tinplate thickness of coating, physical and chemical inspection (chemistry fascicle), 1995
03 phase of year) using the method for atomic absorption detecting tinplate thickness of coating, this method only surveys a kind of coat of metal method
It is fixed, it is unable to measure various metals coating simultaneously;
[Invention content]
The object of the present invention is to provide a kind of while testing thickness of coating and the method for ingredient.And the instrument used in the present invention
It is also the common equipment in most of laboratory, general chemical laboratory need not buy the thickness of coating measuring apparatus of profession,
Also the thickness and ingredient of coating can be measured.
The present invention detecting step include:
1, sample with the method for shearing, cutting, saw or mill is made to the sample blocks of rule, the cut surface of coating surrounding is used
Tool is modified such as file, is kept the smooth of the edge of coating smooth, but cannot be damaged to the surface of coating.
2, the length of side etc. of coating is measured with the accurate survey tool such as vernier caliper, sample is then calculated according to area formula
The surface area of coating in block.
3, by sample blocks coating strong acid or chloroazotic acid all dissolve, be made the solution containing Coating composition, transfer is fixed
Hold in the volumetric flask of certain volume.
4, the solution in volumetric flask is tested on inductive coupling plasma emission spectrograph, to determine its ingredient
And concentration.
5, the levels of Coating composition and ingredient, the constant volume for testing solution, plating in the solution measured according to instrument
The density of element, acquires the thickness of coating in the area and Coating composition of layer.
Calculation formula is:
Wherein:
D:The thickness (μm) of coating;
C1:Test the concentration (mg/L) of solution;
C0:The concentration (mg/L) of blank sample;
V:Test the constant volume (ml) of solution;
S:Surface area (the cm of coating on sample block2);
ρ:Density (the g/cm of Coating composition3);
100:Units conversion factor.
Note:The density of Coating composition is commonly considered as the density of the elemental composition, and such as copper-plated density may be considered pure
The density of copper is 8.90g/cm3, can be by consulting reference materials to obtain.
First with inductive coupling plasma emission spectrograph measure solution various composition, then calculate coating in each at
Divide levels, the thickness of each ingredient in coating is calculated according to the above detecting step, the thickness addition of all the components is exactly
The total thickness of coating of sample.
The advantage of the invention is that accuracy is high, the thickness range of test is wide, interference less, can measure thickness of coating and at
Point, need not in addition buy profession test thickness of coating instrument, general chemical laboratory can promote.With it is same both at home and abroad
Class method is compared, and innovation of the invention has the following aspects:
(1) method of chemical analysis is used to measure thickness of coating and ingredient, this is different from other using such as ultrasound
The methods of wave, potential difference, microscopic method and X-ray conventional method.
(2) using sample being made regular sample blocks, the side of its area is measured with fine measuring instruments such as vernier calipers
Method, to reduce the error of final testing result.
(3) it is measured using the measuring instrument and measurement method of inductive coupling plasma emission spectrograph comparative maturity molten
Coating composition and its concentration, the quality of Coating composition can be accurately calculated further according to the constant volume of solution, makes last coating in liquid
The result of thickness is more accurate.
(4) it is different from the methods of coulometry, metallographic method and x-ray fluorescence film thickness method, the present invention can be according to being made sample
The size of the surface area of block, come judge a certain range of sample coating average thickness.
(4) it is different from the methods of coulometry, metallographic method and x-ray fluorescence film thickness method, the present invention can not only measure coating
Thickness, the ingredient of coating can also be measured.
(5) present invention be because Multiple components in coating can be measured accurately, thus can measure simultaneously in coating it is a variety of at
The thickness and overall thickness divided.
(6) because inductive coupling plasma emission spectrograph has lower detection limits and wider detection model
It encloses, the test of thickness of coating can accurately measure thickness of coating less than 1 μm and with wider test scope.
The present invention needs the coating of sample uniform, because the limitation of sampling, uneven coating can cause test result cannot
The integral level of effective reflection sample coating;Can be produced on sample can accurately calculate the sample blocks of area, the sample produced
The error of the area of product block can directly result in the deviation of thickness of coating test result;Inductive coupling plasma emission spectrograph is surveyed
Examination solution in Coating composition content directly affect sample thickness of coating as a result, so with the Quality Controls hand such as mark-on, standard substance
Section ensures the accuracy of instrument test result.
[Description of the drawings]
Fig. 1 sample blocks sample schematic diagram
[Specific implementation mode]
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
The non-concrete operations for limiting the present invention.
Embodiment 1
1, sample blocks are produced
Two representative positions are chosen on shrapnel sample, two rectangular samples of interception are fast.To sample blocks
Coated position of covering place under repair, so that its smoothing regulation is not had burr.
2, plate areas is measured
Accurate measurement carried out to sample blocks coating position with vernier caliper, the length of side difference 0.729cm of two sample blocks,
0.758cm and 0.646cm, 0.728cm find out the area S of sample blocks coating according to area formula.
3, sample blocks are cleared up
Two sample blocks are respectively put into the clean beakers of 100ml, 5ml concentrated nitric acids and 1ml concentrated hydrochloric acids is added, beaker is put
(electric plate temperature is at 150 DEG C or so) are heated on electric hot plate, until sample blocks are cleared up completely.It removes and is cooled to room temperature, use ISO
Level-one water as defined in 3696 rinses beaker inner wall, transfers the solution into 50ml volumetric flasks, level-one water is used in combination to be settled to graduation mark,
It shakes up to be measured.Constant volume is V.Do sample solution blank simultaneously.
4, Coating composition concentration is measured
ICP multielement standard working solutions are prepared, with inductive coupling plasma emission spectrograph to standard working solution
It is measured, obtains standard working solution curve.Sample solution is measured, sample is measured according to standard working solution curve
Ingredient in coating is zinc, the zinc concentration C in solution1Respectively 13.0124mg/L and 12.8510mg/L, while measuring solution
Blank C0For 0.0002mg/L.
5, thickness of coating is calculated.
Thickness of coating D is acquired according to following formula.
D:The thickness (μm) of coating;
C1:Test the concentration (mg/L) of solution;
C0:The concentration (mg/L) of blank sample;
V:Test the constant volume of solution;(ml)
S:Area (the cm of coating on sample block2);
ρ:The density of zinc is 7.14g/cm3;
100:Units conversion factor.
The thickness for the two sample blocks zinc coatings asked according to formula is respectively 1.65 μm and 1.91 μm.
6 replications are carried out to this sample and are compared with x-ray fluorescence film thickness method,
As a result as follows:
While carrying out thickness of coating test, certified reference material GBW01679 heat resisting steel 3# is tested, test knot
Fruit is 0.0049%, standard value 0.0050%, experiments have shown that our measurement for Zn content in metal, can meet experiment and want
It asks.
Embodiment 2
1, sample blocks are produced
Electronic product wire jumper is the rectangle small sample part of rule, and sample tow sides have coating, this sample is directly whole
Body examination tries, and need not cut sample preparation.
2, plate areas is measured
Accurate measurement carried out to sample blocks coating position with vernier caliper, the length of side difference 0.400cm of two sample blocks,
0.235cm and 0.411cm, 0.235cm, sample blocks tow sides have coating, and sample blocks coating is found out according to area formula
Area S.
3, sample blocks are cleared up
Two sample blocks are respectively put into the clean beakers of 100ml, 5ml concentrated nitric acids and 1ml concentrated hydrochloric acids is added, beaker is put
(electric plate temperature is at 150 DEG C or so) are heated on electric hot plate, until sample blocks are cleared up completely.It removes and is cooled to room temperature, use ISO
Level-one water as defined in 3696 rinses beaker inner wall, transfers the solution into 50ml volumetric flasks, level-one water is used in combination to be settled to graduation mark,
It shakes up to be measured.Constant volume is V.Do sample solution blank simultaneously.
4, Coating composition concentration is measured
ICP multielement standard working solutions are prepared, with inductive coupling plasma emission spectrograph to standard working solution
It is measured, obtains standard working solution curve.Sample solution is measured, sample is measured according to standard working solution curve
Ingredient in coating is zinc, tin and nickel, the zinc concentration C in solution1Respectively 190.8mg/L and 197.6mg/L;Tin in solution
Concentration C1Respectively 5.680mg/L and 5.854mg/L;Nickel concentration C in solution1Respectively 2.809mg/L and 2.760mg/L.Together
When measure solution blank, zinc, tin, nickel reagent blank C0Respectively 0.0006mg/L, 0.0000mg/L and 0.0010mg/L.
5, thickness of coating is calculated.
Thickness of coating D is acquired according to following formula.
D:The thickness (μm) of coating;
C1:Test the concentration (mg/L) of solution;
C0:The concentration (mg/L) of blank sample;
V:Test the constant volume of solution;(ml)
S:Area (the cm of coating on sample block2);
ρ:The density of zinc is 7.14g/cm3, the density of tin is 7.28g/cm3, the density of nickel is 8.90g/cm3;
100:Units conversion factor.
The thickness for the two sample blocks zinc coatings asked according to formula is respectively 71.1 μm and 71.6 μm;The thickness of tin coating point
It Wei not be 2.1 μm and 2.1 μm;The thickness of nickel coating is respectively 0.8 μm and 0.8 μm.The overall thickness of two samples is respectively 74.0 μm
With 74.5 μm.
6 replications are carried out to this sample, since this sample coating is thicker, x-ray fluorescence film thickness method can not be to this sample
Product measure, row this method test data, as follows:
While carrying out thickness of coating test, certified reference material GBW02116 ledrite chemical standard samples are surveyed
Examination, test result Sn0.111%, Ni0.383%, Zn 31.86%, in standard substance the content of element be Sn0.113%,
Ni0.400%, Zn 32.70%, experiments have shown that our measurement for tin, nickel, Zn content in metal, can meet experiment and want
It asks.
The foregoing is merely the preferred embodiments of the present invention, are not intended to limit the invention, all spirit and original in the present invention
Within then, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of test method of thickness of coating, it is characterised in that it includes the following steps:
(1) sample blocks and the sample that area can be determined by mathematical model that area can be measured accurately are made;
(2) sample blocks and reference area are accurately measured;
(3) it clears up the coating on sample blocks completely with strong acid, and the solution of certain volume is made;
(4) Coating composition and its content in solution are measured with inductive coupling plasma emission spectrograph;
(5) according to Coating composition and its content, Coating composition density, plate areas, the thickness of coating is calculated;Calculate thickness of coating
Computational methods be that the content of Coating composition in solution is multiplied by the constant volume of solution divided by the area of coating and Coating composition
Density.
2. a kind of test method of thickness of coating according to claim 1, it is characterised in that the sample blocks in step (1) are
It is made by the methods of shearing, cutting, saw or mill, there is regular shape and smooth edge.
3. a kind of test method of thickness of coating according to claim 1, it is characterised in that the face of sample blocks in step (2)
Product is measured by vernier caliper or other Precision measurement tools.
4. a kind of test method of thickness of coating according to claim 1, it is characterised in that this method can not only test
Single thickness of coating and ingredient can also test the overall thickness and heterogeneity of more coating.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109539998A (en) * | 2018-12-05 | 2019-03-29 | 陕西理工大学 | A kind of nanometer gap measuring device and method based on light-intensity test |
| CN110006351A (en) * | 2019-04-01 | 2019-07-12 | 江汉大学 | A kind of thickness of coating measurement method |
| CN110823158A (en) * | 2019-10-08 | 2020-02-21 | 广州兴森快捷电路科技有限公司 | Electroplating hole metal layer thickness measurement system |
| CN110926399A (en) * | 2019-12-10 | 2020-03-27 | 中国电子科技集团公司第四十六研究所 | Method for testing thickness of metal filament ultrathin metal coating |
| CN110987998A (en) * | 2019-12-12 | 2020-04-10 | 山东东岳高分子材料有限公司 | Method for testing inorganic coating amount on surface of polymer film material |
| CN112179895A (en) * | 2020-08-31 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Method for detecting pre-lithium amount of pole piece |
| CN113091662A (en) * | 2021-04-02 | 2021-07-09 | 中国计量科学研究院 | Self-supporting multi-material coating thickness standard suite and preparation method thereof |
| CN113281326A (en) * | 2021-05-21 | 2021-08-20 | 安泰科技股份有限公司 | Characterization method of thickness of galvanized passivation film |
| CN114018196A (en) * | 2021-10-15 | 2022-02-08 | 镇江锦兴表面工程技术有限公司 | Method for measuring thickness of metal coating |
| CN114324298A (en) * | 2021-12-16 | 2022-04-12 | 东风汽车集团股份有限公司 | Method for measuring sputtering rate |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109539998A (en) * | 2018-12-05 | 2019-03-29 | 陕西理工大学 | A kind of nanometer gap measuring device and method based on light-intensity test |
| CN110006351A (en) * | 2019-04-01 | 2019-07-12 | 江汉大学 | A kind of thickness of coating measurement method |
| CN110823158A (en) * | 2019-10-08 | 2020-02-21 | 广州兴森快捷电路科技有限公司 | Electroplating hole metal layer thickness measurement system |
| CN110823158B (en) * | 2019-10-08 | 2021-07-27 | 广州兴森快捷电路科技有限公司 | Electroplating hole metal layer thickness measurement system |
| CN110926399A (en) * | 2019-12-10 | 2020-03-27 | 中国电子科技集团公司第四十六研究所 | Method for testing thickness of metal filament ultrathin metal coating |
| CN110987998A (en) * | 2019-12-12 | 2020-04-10 | 山东东岳高分子材料有限公司 | Method for testing inorganic coating amount on surface of polymer film material |
| CN112179895A (en) * | 2020-08-31 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Method for detecting pre-lithium amount of pole piece |
| CN113091662A (en) * | 2021-04-02 | 2021-07-09 | 中国计量科学研究院 | Self-supporting multi-material coating thickness standard suite and preparation method thereof |
| CN113281326A (en) * | 2021-05-21 | 2021-08-20 | 安泰科技股份有限公司 | Characterization method of thickness of galvanized passivation film |
| CN114018196A (en) * | 2021-10-15 | 2022-02-08 | 镇江锦兴表面工程技术有限公司 | Method for measuring thickness of metal coating |
| CN114324298A (en) * | 2021-12-16 | 2022-04-12 | 东风汽车集团股份有限公司 | Method for measuring sputtering rate |
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