CN104330069A - Method for quickly measuring thickness of metal coating - Google Patents
Method for quickly measuring thickness of metal coating Download PDFInfo
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- CN104330069A CN104330069A CN201410609442.6A CN201410609442A CN104330069A CN 104330069 A CN104330069 A CN 104330069A CN 201410609442 A CN201410609442 A CN 201410609442A CN 104330069 A CN104330069 A CN 104330069A
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- 239000002184 metal Substances 0.000 title claims abstract description 109
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 109
- 239000011248 coating agent Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000001514 detection method Methods 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims description 34
- 230000000593 degrading effect Effects 0.000 claims description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 23
- 238000004458 analytical method Methods 0.000 claims description 17
- 239000011701 zinc Substances 0.000 claims description 17
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 16
- 238000005259 measurement Methods 0.000 claims description 16
- 229910052725 zinc Inorganic materials 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000005070 sampling Methods 0.000 claims description 14
- 241000931526 Acer campestre Species 0.000 claims description 10
- 230000003287 optical effect Effects 0.000 claims description 10
- 230000000630 rising effect Effects 0.000 claims description 9
- 238000012935 Averaging Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 7
- 230000004907 flux Effects 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- 238000006467 substitution reaction Methods 0.000 claims description 7
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 5
- 239000010953 base metal Substances 0.000 abstract 2
- 230000001066 destructive effect Effects 0.000 abstract 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 abstract 1
- 229910001369 Brass Inorganic materials 0.000 description 6
- 229910001335 Galvanized steel Inorganic materials 0.000 description 6
- 239000010951 brass Substances 0.000 description 6
- 230000003628 erosive effect Effects 0.000 description 6
- 239000008397 galvanized steel Substances 0.000 description 6
- 239000013049 sediment Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001336 glow discharge atomic emission spectroscopy Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000624 total reflection X-ray fluorescence spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000005250 beta ray Effects 0.000 description 1
- 238000003869 coulometry Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
- G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Length Measuring Devices By Optical Means (AREA)
Abstract
The invention discloses a method for quickly measuring the thickness of a metal coating. The method for quickly measuring the thickness of the metal coating includes that using a picosecond pulse laser to corrode a sample under such special conditions of single-point corrosion, 20 Hz of pulse frequency and 875 micrometers of defocusing distance, obtaining a time-resolved figure capable of intuitively distinguishing coating metal from base metal through an inductively coupled plasma mass spectrometry, confirming the junction point of the coating metal and base metal in the time-resolved figure so as to confirm the corroding time for corroding the coating metal, using the standard piece of the same coating as a standard to calculate the unit pulse corrosion quantity of the metal coating, and calculating according to the unit pulse corrosion quantity and corrosion time to obtain the coating thickness. The method for quickly measuring the thickness of the metal coating realizes the quick and non-destructive detection for the coating thickness, is not limited by the conductivity of the metal coating and does not require sample shape, and moreover, the method for quickly measuring the thickness of the metal coating is capable of precisely distinguishing the boundary of two layers of metal and high in detection precision.
Description
Technical field
The present invention relates to a kind of coat of metal determination techniques, especially relate to a kind of method of Fast Measurement metal layer thickness.
Background technology
The coat of metal can change the outward appearance of material, improve corrosion resistance, abrasion resistance and machinability etc., thus be used widely in the industries such as automobile, five metals bathroom, printed-wiring board (PWB), securing member, stationery, gold, silver and jewelry ornaments, the thickness of the coat of metal also becomes the important parameter characterizing its quality quality, therefore, usually to measure metal layer thickness in product quality detection, technology controlling and process and scientific research.
The measuring method of metal layer thickness, the methods such as conventional gravimetric method, coulometry, X-ray spectral analysis method, eddy-current method, method of magnetic, metaloscope method, scanning electron microscopy, section plotter method, β ray backscattering method and X-ray diffraction method.The method can carrying out ANALYSIS ON DEPTH PROFILES that development in recent years is got up, as glow discharge optical emission spectrometry (GD-OES), Auger electron spectroscopy (AES), secondary ion mass spectrum (SIMS), total Reflection X-ray Fluorescence Spectrometry (TXRF) and laser ablation inductively coupled plasma (LA-ICP-MS) etc., the measurement for metal layer thickness provides new approach.LA-ICP-MS is a kind of technology of solid sample Direct Analysis, and sample degrades and excite/and testing conditions can separately optimizing, and the signal of generation only relies on the quality of degrading out; Need sample size few, substantially can accomplish nondestructive analysis; Substantially do not have requirement to sample shape, sample preparation is simple; High spatial resolution, has the function of micro-zone analysis, can carry out in-situ study, depth analysis and surperficial imaging analysis; Be applicable to all solid matters (comprising insulating material), thus LA-ICP-MS is a kind of new method of potential thickness measure.
The measurement that LA-ICP-MS carries out metal layer thickness to the stability of pulsed laser energy and the focusing requirement of laser beam higher; Be metal material, base material for coating be also the product of metal material, because coating and base material can interpenetrate at intersection, also be difficult to the border accurately determining coating and base material at present, coating and base material cannot be distinguished intuitively, cause measurement result deviation larger.In view of this, how to determine that coating and base material are on the border of intersection, coating and base material are carried out accurate and visual differentiation, how effectively to improve the stability of pulsed laser energy and the focus condition of laser beam, make this technology can be successfully applied to the detection of thickness of coating, the Fast nondestructive evaluation realizing thickness of coating is significant.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method of Fast Measurement metal layer thickness, the method degrades pattern by picosecond pulse laser at single-point, under the specific condition such as 20Hz pulsed frequency and 875 μm of defocus distance, sample is degraded, the time resolution figure that coated metal and substrate metal intuitively can be distinguished is obtained by icp ms, determine the point of interface of coated metal and substrate metal in time resolution figure, that determines to degrade coated metal thus degrades the time, then the unit pulse denudation of the coat of metal is calculated, according to unit pulse denudation with degrade Time Calculation and obtain thickness of coating, realize the harmless of thickness of coating to detect fast, and distinguish double layer of metal border accurately, accuracy of detection is high.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of method of Fast Measurement metal layer thickness, is characterized in that comprising the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean;
2. sample being placed in purity is under the argon atmosphere of 99.996%, picosecond pulse laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 ~ 20 μ J, and diaphragm opening diameter is 4 ~ 6mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents that (centre has part to be the time of degrading to acquisition time, relevant to erosion sediment thickness), the ordinate of time resolution figure represents mass signal intensity;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine unit pulse denudation (individual pulse degrades the thickness of the coating) W of the coat of metal, detailed process is:
5.-1 get one and have the standard film of identical coating with sample, the thickness of coating of this standard film is h;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
The coating of described sample is zinc coating, and optical maser wavelength is 266nm, and pulse width is 30ps, and pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, and defocus distance is 875 μm, and each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn.
The RF power of described icp ms is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth is 11.5mm, working gas to be purity be 99.996% argon gas, plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, and adopt time resolution analytical model image data, residence time is 30ms.
Described step 3. in the airshed of pressure be 1.25L/min.
Compared with prior art, the invention has the advantages that the method degrades pattern by picosecond pulse laser at single-point, under the specific condition such as 20Hz pulsed frequency and 875 μm of defocus distance, sample is degraded, the time resolution figure that coated metal and substrate metal intuitively can be distinguished is obtained by icp ms, determine the point of interface of coated metal and substrate metal in time resolution figure, that determines to degrade coated metal thus degrades the time, then the unit pulse denudation of the coat of metal is calculated, according to unit pulse denudation with degrade Time Calculation and obtain thickness of coating, realize the harmless of thickness of coating to detect fast, and distinguish double layer of metal border accurately, accuracy of detection is high.
When the coating of sample is zinc coating, optical maser wavelength is 266nm, and pulse width is 30ps, and pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, and defocus distance is 875 μm, and each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118during Sn, laser pulse frequency is 20Hz, can efficiently avoid the problem that pulsed laser energy instability makes unit pulse denudation change, make testing result more accurately and reliably; Adopt defocus distance 875 μm, significantly reduce the power density of laser pulse, the energy distribution be conducive in laser beam plane is even, be conducive to reducing unit pulse denudation, the focus condition impact of denudation depth on laser beam is reduced, unit pulse denudation more reaches unanimity, and improves the accuracy that thickness of coating measures.
Accompanying drawing explanation
Fig. 1 is the time resolution figure of No. 1 hot-dip galvanized steel sheet in embodiment one;
Fig. 2 is the time resolution figure of No. 2 hot-dip galvanized steel sheets in embodiment two;
Fig. 3 is the time resolution figure of white zine nut in embodiment three;
Fig. 4 is that embodiment four is prized the time resolution figure of zinc screw;
Fig. 5 is the time resolution figure of blue zinc screw in embodiment five.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment one: a kind of method of Fast Measurement metal layer thickness, comprises the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean, sample is No. 1 hot-dip galvanized steel sheet;
2. sample being placed in purity is under the argon atmosphere of 99.996%, pulsed laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, icp ms is to jump time resolution analytical model (TRA) image data of peak mode, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents that (centre has part to be the time of degrading to acquisition time, relevant to erosion sediment thickness), the ordinate of time resolution figure represents mass signal intensity; Icp ms is the Agilent 7500a icp ms that Agilent company of the U.S. produces: RF (radio frequency) power is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth 11.5mm, working gas is argon gas (purity is 99.996%), plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, adopt time resolution analytical model (TRA) image data, each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn, residence time 30ms;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine unit pulse denudation (individual pulse degrades the thickness of the coating) W of the coat of metal, detailed process is:
5.-1 get brass Zinc Coating Thickness standard film, the thickness of coating of this standard film is h, h=11.9 μm;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation, unit pulse denudation W is 67nmpulse
-1;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
Embodiment two: a kind of method of Fast Measurement metal layer thickness, comprises the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean, sample is No. 2 hot-dip galvanized steel sheets;
2. sample being placed in purity is under the argon atmosphere of 99.996%, pulsed laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, icp ms is to jump time resolution analytical model (TRA) image data of peak mode, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents that (centre has part to be the time of degrading to acquisition time, relevant to erosion sediment thickness), the ordinate of time resolution figure represents mass signal intensity; Icp ms is the Agilent 7500a icp ms that Agilent company of the U.S. produces: RF (radio frequency) power is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth 11.5mm, working gas is argon gas (purity is 99.996%), plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, adopt time resolution analytical model (TRA) image data, each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn, residence time 30ms;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine unit pulse denudation (individual pulse degrades the thickness of the coating) W of the coat of metal, detailed process is:
5.-1 get brass Zinc Coating Thickness standard film, the thickness of coating of this standard film is h, h=11.9 μm;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation, unit pulse denudation W is 67nmpulse
-1;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
Embodiment three: a kind of method of Fast Measurement metal layer thickness, comprises the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean, sample is white zine nut;
2. sample being placed in purity is under the argon atmosphere of 99.996%, pulsed laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, icp ms is to jump time resolution analytical model (TRA) image data of peak mode, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents that (centre has part to be the time of degrading to acquisition time, relevant to erosion sediment thickness), the ordinate of time resolution figure represents mass signal intensity; Icp ms is the Agilent 7500a icp ms that Agilent company of the U.S. produces: RF (radio frequency) power is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth 11.5mm, working gas is argon gas (purity is 99.996%), plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, adopt time resolution analytical model (TRA) image data, each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn, residence time 30ms;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine unit pulse denudation (individual pulse degrades the thickness of the coating) W of the coat of metal, detailed process is:
5.-1 get brass Zinc Coating Thickness standard film, the thickness of coating of this standard film is h, h=11.9 μm;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation, unit pulse denudation W is 67nmpulse
-1;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
Embodiment four: a kind of method of Fast Measurement metal layer thickness, comprises the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean, sample is color zinc screw;
2. sample being placed in purity is under the argon atmosphere of 99.996%, pulsed laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, icp ms is to jump time resolution analytical model (TRA) image data of peak mode, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents that (centre has part to be the time of degrading to acquisition time, relevant to erosion sediment thickness), the ordinate of time resolution figure represents mass signal intensity; Icp ms is the Agilent 7500a icp ms that Agilent company of the U.S. produces: RF (radio frequency) power is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth 11.5mm, working gas is argon gas (purity is 99.996%), plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, adopt time resolution analytical model (TRA) image data, each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn, residence time 30ms;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine unit pulse denudation (individual pulse degrades the thickness of the coating) W of the coat of metal, detailed process is:
5.-1 get brass Zinc Coating Thickness standard film, the thickness of coating of this standard film is h, h=11.9 μm;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation, unit pulse denudation W is 67nmpulse
-1;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
Embodiment five: a kind of method of Fast Measurement metal layer thickness, comprises the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean, sample is blue zinc screw;
2. sample being placed in purity is under the argon atmosphere of 99.996%, pulsed laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, icp ms is to jump time resolution analytical model (TRA) image data of peak mode, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents that (centre has part to be the time of degrading to acquisition time, relevant to erosion sediment thickness), the ordinate of time resolution figure represents mass signal intensity; Icp ms is the Agilent 7500a icp ms that Agilent company of the U.S. produces: RF (radio frequency) power is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth 11.5mm, working gas is argon gas (purity is 99.996%), plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, adopt time resolution analytical model (TRA) image data, each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn, residence time 30ms;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine unit pulse denudation (individual pulse degrades the thickness of the coating) W of the coat of metal, detailed process is:
5.-1 get brass Zinc Coating Thickness standard film, the thickness of coating of this standard film is h, h=11.9 μm;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation, unit pulse denudation W is 67nmpulse
-1;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
No. 1 hot-dip galvanized steel sheet of selection respectively of above-described embodiment one to embodiment five, No. 2 hot-dip galvanized steel sheets, white zine nut, color zinc screw, blue zinc screw are as sample, brass Zinc Coating Thickness standard film is as standard thickness sheet, under similarity condition, degrade sample and standard thickness sheet respectively, gather
66the time resolution figure (detection of other collection is isotopic will not be marked) of Zn and base material major component, carry out the mensuration of galvanized layer thickness, concrete test result row are as shown in table 1, and the asserting value system of table 1 sample adopts the measured value of GB/T 24514-2009 analysis.
Table 1 sample analysis result
As can be seen from Table 1, maximum result error is 0.4 μm, illustrates that method of the present invention has feasibility and accuracy thus.Although have the RSD of sample to have more than 10% in table, trace it to its cause relevant with the homogeneity of hot dipping Zinc coat and the micro-zone analysis of LA-ICP-MS, we take independent measure 3 times after the method for averaging obtain result, be conducive to eliminating the inequality of thickness of coating and the representative bad problem of micro-zone analysis thus.
It should be noted that in addition, in time resolution figure of the present invention, can rise fast after the signal appearance of general coated metal, after degrading certain hour, the signal of substrate metal there will be, if when not forming composite bed between coated metal and substrate metal, the signal of substrate metal occurs that rear horse back can rise rapidly, simultaneously the signal meeting decline fast of coated metal, then the epoch point of substrate metal is the quick rising point of mass signal intensity of substrate metal signal; If when being formed with composite bed between coated metal and substrate metal, not rise rapidly after the signal appearance of substrate metal, but have a mild transitional region, now the signal of coated metal also can not decline at once, in this case, should draw an oblique line based on the quick riser of substrate metal signal, with the intersection point of the transitional region point of interface as coating and base material, this point of interface is the quick rising point of mass signal intensity of substrate metal signal.
Claims (4)
1. a method for Fast Measurement metal layer thickness, is characterized in that comprising the following steps:
1. air-dry after being adopted on the surface of sample the pure absolute ethyl alcohol of analysis clean;
2. sample being placed in purity is under the argon atmosphere of 99.996%, picosecond pulse laser is adopted to degrade sample under single-point degrades pattern, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 ~ 20 μ J, and diaphragm opening diameter is 4 ~ 6mm, defocus distance is 875 μm, and pulsed laser mode of operation is fixed pulse mode of operation;
3. the specimen material degrading out is analyzed with in argon gas input icp ms, the time resolution figure obtaining each element contained in specimen material exports, the horizontal ordinate of time resolution figure represents acquisition time, and the ordinate of time resolution figure represents mass signal intensity;
4. using the time of occurrence point of the quick rising point of mass signal intensity of substrate metal signal in time resolution figure as substrate metal signal, the time of degrading of coated metal is designated as T, the time of occurrence point of coated metal signal is designated as T1, the time of occurrence of substrate metal signal point is designated as T2, and what calculate coated metal according to formula T=T2-T1 degrades the time;
5. determine the unit pulse denudation W of the coat of metal, detailed process is:
5.-1 get one and have the standard film of identical coating with sample, the thickness of coating of this standard film is h;
5.-2 adopt picosecond pulse laser independently to degrade 3 times at the diverse location of standard film, the time of degrading coating for three times is designated as t1, t2 and t3 respectively, and averaging time is designated as t, t=(t1+t2+t3)/3;
5.-3 h, t substitution formula W=h/ (20 × t) can be calculated unit pulse denudation;
6. T is substituted into formula H=W × T, can thickness of coating H be calculated.
2. the method for a kind of Fast Measurement metal layer thickness according to claim 1, it is characterized in that the coating of described sample is zinc coating, optical maser wavelength is 266nm, pulse width is 30ps, pulsed frequency is 20Hz, and pulsed laser energy is 10 μ J, and diaphragm opening diameter is 4mm, defocus distance is 875 μm, and each Element detection isotope is
56fe,
63cu,
66zn and
27al,
52cr,
60ni,
118sn.
3. the method for a kind of Fast Measurement metal layer thickness according to claim 1, it is characterized in that the RF power of described icp ms is 1150W, torch tube hub pore footpath ф 2.0mm, Ni sampling spiroid and intercepting cone, sampling depth is 11.5mm, working gas to be purity be 99.996% argon gas, plasma flow amount is 15.0L/min, assisted gas flow is 1.0L/min, carrier gas flux is 1.25L/min, adopt time resolution analytical model image data, residence time is 30ms.
4. the method for a kind of Fast Measurement metal layer thickness according to claim 1, is characterized in that during described step 3., the airshed of pressure is 1.25L/min.
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| CN106225692A (en) * | 2016-06-29 | 2016-12-14 | 内蒙古第机械集团有限公司 | A kind of measuring method of aluminium alloy compound plate coating thickness |
| CN109709201A (en) * | 2018-12-28 | 2019-05-03 | 北京大学深圳研究生院 | A kind of high time resolution mass spectrometry detection equipment and its application |
| CN110519925A (en) * | 2019-07-23 | 2019-11-29 | 福州瑞华印制线路板有限公司 | A kind of method of quick reckoning PCB via hole hole copper thickness |
| CN119437125A (en) * | 2025-01-13 | 2025-02-14 | 玛斯特(中山)汽车表面技术有限公司 | Method and system for detecting uniformity of barrel plating of deep and blind hole fasteners |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106225692A (en) * | 2016-06-29 | 2016-12-14 | 内蒙古第机械集团有限公司 | A kind of measuring method of aluminium alloy compound plate coating thickness |
| CN109709201A (en) * | 2018-12-28 | 2019-05-03 | 北京大学深圳研究生院 | A kind of high time resolution mass spectrometry detection equipment and its application |
| CN109709201B (en) * | 2018-12-28 | 2021-06-08 | 北京大学深圳研究生院 | High-time-resolution mass spectrum detection equipment and application |
| CN110519925A (en) * | 2019-07-23 | 2019-11-29 | 福州瑞华印制线路板有限公司 | A kind of method of quick reckoning PCB via hole hole copper thickness |
| CN110519925B (en) * | 2019-07-23 | 2022-01-25 | 福州瑞华印制线路板有限公司 | Method for rapidly calculating thickness of copper in PCB (printed circuit board) via hole |
| CN119437125A (en) * | 2025-01-13 | 2025-02-14 | 玛斯特(中山)汽车表面技术有限公司 | Method and system for detecting uniformity of barrel plating of deep and blind hole fasteners |
| CN119437125B (en) * | 2025-01-13 | 2025-05-13 | 玛斯特(中山)汽车表面技术有限公司 | Method and system for detecting barrel plating uniformity of deep hole blind hole fastener |
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