CN106645095A - Method for measuring contents of silicon and aluminum in aluminum silicon plate plating - Google Patents
Method for measuring contents of silicon and aluminum in aluminum silicon plate plating Download PDFInfo
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- CN106645095A CN106645095A CN201710077758.9A CN201710077758A CN106645095A CN 106645095 A CN106645095 A CN 106645095A CN 201710077758 A CN201710077758 A CN 201710077758A CN 106645095 A CN106645095 A CN 106645095A
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- silicon
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- 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
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Abstract
The invention discloses a method for measuring the contents of silicon and aluminum in aluminum silicon plate plating, and belongs to the technical field of metal material detection. The method comprises the following steps: establishing a method applicable to glow surface analysis of an aluminum silicon plate sample: setting operating parameters: discharge parameters are as follows: analysis voltage is 600 to 800V, analysis voltage is 20 to 30mA, and integral time is 600 to 1500s; preparation of a calibration operating curve and treatment of sample; preparing a polygon with the diameter phi of greater than or equal to 20mm and smaller than or equal to 100mm or the continuous area of greater than 800mm<2>; analyzing the aluminum silicon plate sample through a grow surface analysis method, so as to obtain a relation curve in which elements of aluminum, silicon and iron in each layer are changed with the thickness of the plating; computing the mass fractions of the silicon and aluminum elements in the plating. The method has the advantages that the method is convenient to operate, the result is accurate, and the problem that an aluminum silicon plate standard sample does not exist can be properly solved.
Description
Technical field
The invention belongs to technical field of detection of metal, more particularly to a kind of to determine silicon, aluminium content in silicon aluminum plate coating
Method.More particularly to one kind utilizes glow discharge emission spectrum to silicon, aluminum content tests method in silicon aluminum plate coating.
Background technology
Silicon aluminum plate has excellent heat resistance and corrosion resistance, environmental protection, is relatively used for automobile exhaust system, resistance to
Hot utensil, construction material etc..Because silicon aluminum plate is compared to galvanized sheet more preferably heat resistance, Shoudu Iron and Steel Co Jing Tang iron companies intend configuration
Hot dip sial board assembly line, the detection method that correlation need to be carried out to silicon aluminum plate coating is developed.
The production process of silicon aluminum plate is that silicon, aluminium are equably plated on the surface of steel plate, the accounting of silicon, aluminium in overlay coating
The performance of silicon aluminum plate will be affected, the silicon in coating, aluminium content are determined exactly, undoubtedly tool is of great significance.
What silicon, aluminium content were measured in silicon aluminum plate coating not yet has the country of formal issue or professional standard, relevant right
The method report that silicon, aluminium content are measured in silicon aluminum plate coating is less, and the measure report of similar coating analysis, paper mainly exist
The coating context of detection of galvanized sheet, tin plate etc..Retrieve British Standard " BS EN10346:2009 Continuously
Standard in hot-dip coated steel flat products-Technical delivery conditions "
Appendix B " Annex B (normative) Reference method for determination of the aluminium-
The reference method determined to silicon aluminum plate quality of coating is defined in silicon coating mass ", the method is former using chemistry
Sample surfaces are processed by reason dissolving coating repeatedly using hydrochloric acid or sodium hydroxide solution, of poor quality after before processing
Obtain the quality of silicon aluminum plate coating, the method that the standard does not specify element mass fraction in coating, can only obtain in coating silicon and
Total quality of aluminium；Retrieve and also lead in SN/T2951-2011 " zinc-plated and Al-Zn coated steel coating chemical composition analysis method "
Cross chemical means to process specimen surface, afterwards surveyed sample strip solution introducing inductively coupled plasma spectrometer
It is fixed, the mass fraction of element in coating is obtained, the measure element of the method only has silicon, nickel, copper and iron, the measurement range of element silicon
For 0.001%～5.00%, silicon aluminum plate is not suitable for；" steel surface zinc-base and (or) aluminium base are plated to retrieve GB/T24514-2009
Layer unit area quality of coating and chemical constituents determination gravimetric method, ICP-AES and flame are former
Sub- absorption spectrometry ", the standard modification adopts ISO17925-2004, and hydrochloric acid solution of the method containing corrosion inhibiter is to sample
Surface is processed, the as quality of coating of poor quality after before processing, the plating solution Jing dilutions that surface treatment is stripped out,
Surveyed using induced coupled plasma atomic emission spectrometry (ICP-AES) or flame atomic absorption spectrometry (FAAS) after filtration and constant volume
It is fixed, you can to obtain the element mass fraction in coating.It is 0.02%～60.0% that applicability of standard is coating aluminium content, coating
Silicone content is 0.2%～10%, wherein the inapplicable silicon aluminum plate of aluminium content scope, and silicone content scope reaches the upper limit；Retrieve GB/T
29559-2013 " analysis of surface chemist reaction glow discharge atomic emission spectrum zinc and/or acieral coating ", the standard etc.
With using ISO 16962：2005, wherein regulation element determination scope 0.01%～10.00%, is not suitable for silicon aluminum plate, and should
Standard is versatility standard, wherein not there is the computational methods for silicon aluminum plate sample.
In addition, not retrieving the article with regard to sial assay in silicon aluminum plate coating.
The content of the invention
It is an object of the invention to provide a kind of determine silicon, the method for aluminium content in silicon aluminum plate coating, current life is solved
Produce in detection without the available problem of standard method.
A kind of to determine silicon, the method for aluminium content in silicon aluminum plate coating, concrete steps and parameter are as follows：
1st, set up and be applied to silicon aluminum plate sample, the aura surface analysis method comprising silicon, aluminium：
(1) setting of glow spectrometer running parameter：The discharge parameter of direct current glow discharge spectrometer is analysis voltage 600
～800V, analyzes 20～30mA of electric current, 600～1500s of the time of integration.Element-intensities are with analysis voltage, the increase of analysis electric current
And increase, but analysis voltage, the excessive increase that will also result in background signal intensities of analysis electric current, and make sample hole excite hole not
Flat, sample easily beats paste.For analysis spectral lines such as silicon 288.158nm, aluminium 396.152nm, optimized test obtains being best suitable for this
The instrument parameter of analysis method.
(2) making of calibration operation curve：Excite 35～45 pieces of standard samples, the wherein content range of Fe elements：0.005
The content range of～99.78wt%, Al element：The content range of 0.006～97.93wt%, Si element：0.004～
12.47wt%, sputtering raste：0.097～1.66 μ g/s, under the shooting condition of setting, each standard sample is excited more than 3 times,
The correction of element-intensities and quality weight fraction in different matrix is carried out using sputtering raste.It is determined that each mark surveyed in this fashion
The each element average mass fraction of quasi- sample determination is consistent with known standard value, and deviation should be in the range of rational mathematical statistics.
(3) sample treatment：Sample specification requires that diameter 20mm≤Φ d≤100mm or continuous area are more than 800mm2's
Polygon, wherein each polygonal summit of continuous area is not less than 20mm with the distance on opposite side summit.Any machinery can not be used
Means rubbed sample surface, with washes of absolute alcohol surface and dries.
2nd, silicon aluminum plate sample is analyzed using aura surface analysis method, obtains the elemental compositions such as each layer of aluminium, silicon, iron with plating
The relation curve of thickness degree, determines thickness of coating and silicon, aluminium element content depth quantitative relationship：Put testing sample as negative electrode
On light source, 10 ± 0.1Pa is evacuated down in light source, is filled with argon gas and maintains 500～1500Pa of pressure；Plus earth, sample
Upper plus 500～1500V of negative high voltage, argon gas is breakdown, forms stable plasma；In the presence of negative high voltage, by electric field
The high-energy argon ion bombardment sample surfaces of acceleration, sample is successively sputtered and excited, and launches elemental characteristic spectral line, Jing spectrometers
Detection and computer are calculated；Using glow discharge optical emission spectrometry successively peel sample surface, each layer of composition is detected, when the unit for measuring
When change is less than 1% in plain composition 3s, stop measurement, according to depth and the relation of composition of each measurement, draw composition with depth
Degree variation relation curve.By aluminium, iron content with the quantitative relationship of change in depth, the depth thickness of coating is determined, by silicon, aluminium
Constituent content with coating change in depth quantitative relationship, and definition depth bounds in integrate, obtain silicon in coating, aluminium it is total
Quality.
3rd, in coating sial element mass fraction computational methods：
(1) process is integrated with time or thickness of coating to silicon, aluminium element mass fraction in coating depth direction, when
Between function be converted into the function of depth, obtain silicon aluminum plate depth direction analysis chart；
A. the mass fraction for determining coating Main elements aluminium is down to 10% depth from the 90% of peak value, determines that aluminium is down to
50% depth, marks these depth to be Al90%, Al 10%, Al50%, and peak value refers to from integration the quality point started to aluminium
Number is the mass fraction maximum between 50%.
B. definition interfaces depth W is down to the width of Al 10% for Al90%.
C. definition plating layer depth L is Al50% depth and interface depth W sums.
D. coating element integrated depth is plating layer depth L.
(2) silicon, the calculating of aluminium element mass fraction：Plus the quality of coating with silicon, aluminium in coating, obtain total matter of coating
Amount, by the quality of coating of silicon, aluminium element the gross mass of coating is respectively divided by, and obtains the average mass fraction in silicon aluminum plate coating,
Computing formula is as follows：
D is that coating integrates thickness in formula, and m is silicon, the quality of aluminium element in coating.
It is an advantage of the current invention that：Easy to operate, result is accurate, and can solve well without silicon aluminum plate standard sample
Problem.
Description of the drawings
Fig. 1 is each element sial the intensity of spectral line schematic diagram under different voltages.
Fig. 2 is sial the intensity of spectral line schematic diagram under different electric currents.
Fig. 3 is element silicon calibration graph.
Fig. 4 is aluminium element calibration graph.
Fig. 5 is that silicon aluminum plate coating quantitative depth dissects result example.
Fig. 6 is typical silicon aluminum plate aura analysis of spectra -1.
Fig. 7 is typical silicon aluminum plate aura analysis of spectra -2.
Specific embodiment
Embodiment 1
The specific embodiment of the present invention is illustrated below in conjunction with the accompanying drawings：
It is embodied as using LECO companies of U.S. GDS850A glow discharge spectrometries：Anode diameter 4mm, is equipped with a collection
In for 0.75 meter of polychromator (56 passages)：Polychromator optical system Paschen-Runge；Polychromator carves 3600/mm of number；
Polychromator grating resolution 0.017nm.Nanjing and Australia's MY-200 sand belt sample milling machines.One kind determines silicon, aluminium in silicon aluminum plate coating and contains
The method of amount, concrete steps and parameter it is as follows：
1st, set up and be applied to silicon aluminum plate sample, the aura surface analysis method comprising silicon, aluminium：
(1) setting of glow spectrometer running parameter：The discharge parameter of direct current glow discharge spectrometer is analysis voltage
750V, analyzes electric current 25mA, time of integration 1500s.Element-intensities increase with analysis voltage, the increase of analysis electric current, but point
Analysis voltage, analysis electric current are excessive to will also result in the increase of background signal intensities, and makes sample hole excite hole uneven, and sample is easy
Beat paste.For analysis spectral lines such as silicon 288.158nm, aluminium 396.152nm, optimized test obtains being best suitable for the instrument of this analysis method
Device parameter.
(2) making of calibration operation curve：Excite 38 pieces of standard samples, each standard sample to excite more than 3 times, adopt and splash
The rate of penetrating carries out the correction of element-intensities and quality weight fraction in different matrix.It is determined that each standard sample surveyed in this fashion
The each element average mass fraction of measure is consistent with known standard value, and deviation should be in the range of rational mathematical statistics.This method
Standard sample is listed in the table below 2：
Table 2, the list of calibration curve standard sample and each element content value, sputtering raste value
After by selected standard sample surface treated, under the Instrumental Analysis parameter of optimization each standard sample, Jing are excited
After relative sputtering rate correction, calibration curve Fig. 3, Fig. 4 of silicon, aluminium element are obtained.
(3) sample treatment：Sample size is 20mm width * 100mm length, it is impossible to any mechanical means rubbed sample surface,
With washes of absolute alcohol surface and dry.
2nd, silicon aluminum plate sample is analyzed using aura surface analysis method, obtains the elemental compositions such as each layer of aluminium, silicon, iron with plating
The relation curve of thickness degree, determines thickness of coating and silicon, aluminium element content depth quantitative relationship：Put testing sample as negative electrode
On light source, 10 ± 0.1Pa is evacuated down in light source, is filled with argon gas and maintains pressure 1000Pa；Plus earth, it is on sample plus negative
High pressure 750V, argon gas is breakdown, forms stable plasma；In the presence of negative high voltage, by the high energy argon of electric field acceleration
Ions Bombardment sample surfaces, sample is successively sputtered and excited, and launches elemental characteristic spectral line, the detection of Jing spectrometers and computer
Calculate；Using glow discharge optical emission spectrometry successively peel sample surface, each layer of composition is detected, when becoming in elemental composition 3s for measuring
When changing less than 1%, stop measurement, according to depth and the relation of composition of each measurement, draw composition bent with change in depth relation
Line.By aluminium, iron content with the quantitative relationship of change in depth, the depth thickness of coating is determined, by silicon, aluminium element content with plating
The quantitative relationship of layer depth change, and integrate in the depth bounds of definition, obtain the gross mass of silicon in coating, aluminium.
3rd, in coating sial element mass fraction computational methods：
(1) process is integrated with time or thickness of coating to silicon, aluminium element mass fraction in coating depth direction, when
Between function be converted into the function of depth, obtain silicon aluminum plate depth direction analysis chart；
A. the mass fraction for determining coating Main elements aluminium is down to 10% depth from the 90% of peak value, determines that aluminium is down to
50% depth, marks these depth to be Al90%, Al 10%, Al50%, and peak value refers to from integration the quality point started to aluminium
Number is the mass fraction maximum between 50%.
B. definition interfaces depth W is down to the width of Al 10% for Al90%.
C. definition plating layer depth L is Al50% depth and interface depth W sums.
D. coating element integrated depth is plating layer depth L.
(2) silicon, the calculating of aluminium element mass fraction：Plus the quality of coating with silicon, aluminium in coating, obtain total matter of coating
Amount, by the quality of coating of silicon, aluminium element the gross mass of coating is respectively divided by, and obtains the average mass fraction in silicon aluminum plate coating,
Computing formula is as follows：
D is that coating integrates thickness in formula, and m is silicon, the quality of aluminium element in coating.
Typical silicon aluminum plate aura analysis of spectra such as Fig. 6, Fig. 7, according to the method for determination in 4.1 to two pieces of silicon aluminum plate samples
Determine 3 times respectively, while adopting BS EN 10346 to two pieces of samples:Method is processed surface specified in 2009, is obtained
The gross mass of silicon, aluminium in overlay coating, obtains result table 3.
Silicon, the quality of aluminium and mass fraction in table 3, silicon aluminum plate sample coating
* note：BS EN 10346:The deviation range of method is not referred in 2009.
As can be seen from Table 3, the precision of method is fine, hence it is evident that better than GB/T1839-2008 " product made from steel zinc coating qualities
Requirement of the repeatability for mean value ± 5% is determined to galvanizing production quality of coating in method of testing ", in the silicon aluminum plate coating for measuring
Silicon, the gross mass of aluminium with adopt BS EN 10346:2009 method measured result deviations are less.It can be seen that utilization the method realizes silicon
Aluminium sheet quality of coating is 20～80g/m2(wherein silicone content about 10%, aluminium content quick measure about 90%), easy to operate, knot
Fruit is accurate, and the needs of production detection are solved well, during production is had application at present.
Claims (3)
1. it is a kind of to determine silicon, the method for aluminium content in silicon aluminum plate coating, it is characterised in that concrete steps and parameter are as follows：
1) set up and be applied to silicon aluminum plate sample, the aura surface analysis method comprising silicon, aluminium：
1. the setting of glow spectrometer running parameter：The discharge parameter of direct current glow discharge spectrometer be analysis voltage 600～
800V, analyzes 20～30mA of electric current, 600～1500s of the time of integration；
2. the making of calibration operation curve：35～45 pieces of standard samples are excited, under the shooting condition of setting, each standard sample
Excite more than 3 times, the correction of element-intensities and quality weight fraction in different matrix is carried out using sputtering raste；
3. sample treatment：Sample specification requires that diameter 20mm≤Φ d≤100mm or continuous area are more than 800mm2Polygon,
With washes of absolute alcohol surface and can not be dried with any mechanical means rubbed sample surface；
2) silicon aluminum plate sample is analyzed using aura surface analysis method, obtains the elemental compositions such as each layer of aluminium, silicon, iron with plating thickness
The relation curve of degree, determines thickness of coating and silicon, aluminium element content depth quantitative relationship：Light is placed in using testing sample as negative electrode
On source, 10 ± 0.1Pa is evacuated down in light source, is filled with argon gas and maintains 500～1500Pa of pressure；Plus earth, adds on sample
500～1500V of negative high voltage, argon gas is breakdown, forms stable plasma；In the presence of negative high voltage, by electric field acceleration
High-energy argon ion bombardment sample surfaces, sample successively sputtered and excited, and launches elemental characteristic spectral line, the detection of Jing spectrometers
Calculate with computer；Using glow discharge optical emission spectrometry successively peel sample surface, detect each layer of composition, when the element for measuring into
When dividing the interior changes of 3s less than 1%, stop measuring, according to the depth of measurement every time and the relation of composition, draw composition with depth change
Change relation curve；By aluminium, iron content with the quantitative relationship of change in depth, the depth thickness of coating is determined, by silicon, aluminium element
Content with coating change in depth quantitative relationship, and definition depth bounds in integrate, obtain total matter of silicon in coating, aluminium
Amount；
3) in coating sial element mass fraction computational methods：
1. process is integrated with time or thickness of coating to silicon, aluminium element mass fraction in coating depth direction, the time
Function is converted into the function of depth, obtains silicon aluminum plate depth direction analysis chart；
A. the mass fraction for determining coating Main elements aluminium is down to 10% depth from the 90% of peak value, determines that aluminium is down to 50%
Depth, marks these depth to be Al90%, Al10%, Al50%, and peak value refers to from integration beginning and is to the mass fraction of aluminium
Mass fraction maximum between 50%；
B. definition interfaces depth W is down to the width of Al10% for Al90%；
C. definition plating layer depth L is Al50% depth and interface depth W sums；
D. coating element integrated depth is plating layer depth L；
2. silicon, the calculating of aluminium element mass fraction：Plus the quality of coating with silicon, aluminium in coating, the gross mass of coating is obtained, will
Silicon, the quality of coating of aluminium element are respectively divided by the gross mass of coating, obtain the average mass fraction in silicon aluminum plate coating, calculate public
Formula is as follows：
D is that coating integrates thickness in formula, and m is silicon, the quality of aluminium element in coating.
2. method according to claim 1, it is characterised in that described step 1) in the standard sample that excites, wherein Fe
The content range of element：The content range of 0.005～99.78wt%, Al element：0.006～97.93wt%, Si element contains
Amount scope：0.004～12.47wt%, sputtering raste：0.097～1.66 μ g/s.
3. method according to claim 1, it is characterised in that described step 1) in sample, wherein continuous area
Each polygonal summit is not less than 20mm with the distance on opposite side summit.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110823861A (en) * | 2019-10-19 | 2020-02-21 | 首钢集团有限公司 | Method for positioning analysis in glow analysis |
| RU2759632C1 (en) * | 2021-04-05 | 2021-11-16 | Акционерное общество "Уральский электромеханический завод" | Method for determining chemical composition and thickness of two-layer electroplated coating |
| CN114113291A (en) * | 2020-08-25 | 2022-03-01 | 江苏隆达超合金航材有限公司 | Method for determining content of main element in multi-element alloy by using proportional coefficient correction glow mass spectrometry |
| CN114295603A (en) * | 2022-01-13 | 2022-04-08 | 鞍钢股份有限公司 | Method for simultaneously determining contents of multiple elements in aluminum alloy |
| CN117907562A (en) * | 2024-03-19 | 2024-04-19 | 张家港扬子江冷轧板有限公司 | Method for simultaneously detecting contents of multiple elements in coating |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110823861A (en) * | 2019-10-19 | 2020-02-21 | 首钢集团有限公司 | Method for positioning analysis in glow analysis |
| CN114113291A (en) * | 2020-08-25 | 2022-03-01 | 江苏隆达超合金航材有限公司 | Method for determining content of main element in multi-element alloy by using proportional coefficient correction glow mass spectrometry |
| RU2759632C1 (en) * | 2021-04-05 | 2021-11-16 | Акционерное общество "Уральский электромеханический завод" | Method for determining chemical composition and thickness of two-layer electroplated coating |
| CN114295603A (en) * | 2022-01-13 | 2022-04-08 | 鞍钢股份有限公司 | Method for simultaneously determining contents of multiple elements in aluminum alloy |
| CN117907562A (en) * | 2024-03-19 | 2024-04-19 | 张家港扬子江冷轧板有限公司 | Method for simultaneously detecting contents of multiple elements in coating |
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