CN114563322B - Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material - Google Patents
Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material Download PDFInfo
- Publication number
- CN114563322B CN114563322B CN202210105747.8A CN202210105747A CN114563322B CN 114563322 B CN114563322 B CN 114563322B CN 202210105747 A CN202210105747 A CN 202210105747A CN 114563322 B CN114563322 B CN 114563322B
- Authority
- CN
- China
- Prior art keywords
- aluminum alloy
- surface treatment
- polymer
- porosity
- characterization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 215
- 238000000034 method Methods 0.000 title claims abstract description 68
- 229920000642 polymer Polymers 0.000 title claims abstract description 65
- 238000012512 characterization method Methods 0.000 title claims abstract description 39
- 238000005260 corrosion Methods 0.000 title claims abstract description 16
- 230000007797 corrosion Effects 0.000 title claims abstract description 15
- 239000002648 laminated material Substances 0.000 title claims abstract description 10
- 230000033228 biological regulation Effects 0.000 title abstract description 10
- 238000004381 surface treatment Methods 0.000 claims abstract description 105
- 238000003475 lamination Methods 0.000 claims abstract description 18
- 230000001105 regulatory effect Effects 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000011282 treatment Methods 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 229920000307 polymer substrate Polymers 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 24
- 206010040844 Skin exfoliation Diseases 0.000 description 12
- 238000010586 diagram Methods 0.000 description 12
- 238000005259 measurement Methods 0.000 description 11
- 238000002791 soaking Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000000956 alloy Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 6
- 239000004926 polymethyl methacrylate Substances 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229910000979 O alloy Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- -1 Polyethylene Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000078 claw Anatomy 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
-
- G—PHYSICS
- G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
- G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
- G16C10/00—Computational theoretical chemistry, i.e. ICT specially adapted for theoretical aspects of quantum chemistry, molecular mechanics, molecular dynamics or the like
-
- G—PHYSICS
- G16—INFORMATION AND COMMUNICATION TECHNOLOGY [ICT] SPECIALLY ADAPTED FOR SPECIFIC APPLICATION FIELDS
- G16C—COMPUTATIONAL CHEMISTRY; CHEMOINFORMATICS; COMPUTATIONAL MATERIALS SCIENCE
- G16C60/00—Computational materials science, i.e. ICT specially adapted for investigating the physical or chemical properties of materials or phenomena associated with their design, synthesis, processing, characterisation or utilisation
Landscapes
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Theoretical Computer Science (AREA)
- Computing Systems (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Bioinformatics & Computational Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Dispersion Chemistry (AREA)
- Laminated Bodies (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The invention discloses a characterization and regulation method of an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminated material, which calculates the mass reduction rate R of the aluminum alloy obtained after surface treatment by measuring mass and size information before and after surface treatment of an aluminum alloy sample m Or the surface porosity R is used as a quantitative characterization parameter for evaluating the microstructure of the aluminum alloy surface connected with the polymer, and is further used for guiding and regulating the surface treatment process parameter so as to optimize the bonding performance of the obtained aluminum alloy/polymer lamination interface. The characterization and regulation method is simple, convenient to operate, easy to obtain a measuring tool and high in accuracy; the test process has no pollution and damage to the sample, and the sample can still keep the original bonding performance with the polymer after the test; is convenient for popularization and application.
Description
Technical Field
The invention belongs to the technical field of material surface structure treatment and characterization, and particularly relates to a characterization and regulation method of an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminated material.
Background
With the development of industry, the aluminum alloy/polymer laminated material structure has a great deal of demands in the fields of weight reduction, anti-corrosion layers, insulating layers, packaging, transparent instrument manufacturing and the like; wherein the polymer can be directly combined by hot-press injection molding, friction heat welding, solution method and the like. To increase the bonding strength of the polymer and the aluminum alloy, the aluminum alloy is typically surface treated to provide a porous structure to form a microstructure with the polymer and increase the interfacial bonding strength. However, excessive surface treatment, especially excessive chemical corrosion treatment, causes problems of reduced strength of the aluminum alloy matrix, enrichment of active anions deep in surface pores, and the like; at the same time, the excessive surface treatment no longer gains its bonding strength with the polymer, since the pore area of the aluminum alloy surface is already saturated. Therefore, a simple and feasible method is needed to directly characterize the microstructure of the surface of the aluminum alloy, establish quantitative connection between the microstructure and the bonding performance, and be used for regulating and controlling the surface treatment of the aluminum alloy to avoid excessive or insufficient process conditions.
The process parameters (such as surface treatment time, treatment liquid concentration, temperature, etc.) of the surface treatment commonly used in production and experiments indirectly represent the surface treatment degree of the aluminum alloy, and are related with the connection performance of the aluminum alloy-polymer. Although the method is relatively direct and convenient, the process parameters are various, and strict control of multiple variables is often required to study one of the process parameters. Other physical quantities or methods for directly characterizing the surface of a material include: 1) The contact angle is used as the most common material surface characterization means and can be used for reflecting the surface roughness of the material, but aiming at the situation that the sizes of micropores on the surface are different, when the contact angle is measured, the liquid is easy to wet with the etching holes with larger sizes and is difficult to wet with the etching holes with smaller sizes, and the smaller etching holes can be overlapped and combined into the larger etching holes, so that the situation that the liquid is contacted with the surface of the aluminum alloy is complicated, the relation between the contact angle and the treatment degree of the surface of the aluminum alloy is difficult to determine, and therefore, the effective quantitative relation is difficult to be established with interface combination performance characterization data; 2) The microcosmic surface area of the material is used as another index capable of representing the surface microstructure, and can be obtained by respectively measuring the ideal smooth state and the contact angle between the rough state of the surface of the material and water at the molecular level; however, it is still necessary to measure the contact angle in a rough state, and in practical operation, it is difficult to obtain a smooth ideal surface at the molecular level; 3) As a method capable of simultaneously obtaining multiple surface characterization, an atomic force microscope can only scan a micron area of a solid surface, the measurement area is obviously insufficient to cover a metal surface microstructure in a macroscopic area range, and the test cost is high.
Disclosure of Invention
The invention mainly aims to provide a characterization and regulation method for an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminated material, aiming at the problems and defects existing in the prior art, and solving the problems that effective data cannot be measured and calculated, a test area is limited, the size and the morphology of a test sample are limited, the test cost is high and the like in the existing characterization method; the method can effectively realize the predictive evaluation of the interface bonding performance of the aluminum alloy/polymer lamination and the regulation and control of the surface treatment process parameters of the aluminum alloy.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for characterizing an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminate, comprising the steps of:
1) Peeling the surface of the aluminum alloy sample, cleaning, drying and coolingMeasuring the initial mass M of the aluminum alloy 0 Or initial mass M of aluminium alloy 0 And initial size information I;
2) Surface treatment is carried out on the surface of the aluminum alloy, then cleaning, drying and cooling are carried out, and the mass M of the aluminum alloy obtained after the surface treatment is measured 1 Or mass M 1 And size information II;
3) According to the initial mass M of the aluminum alloy 0 And mass M 1 Calculating the mass reduction rate R of the aluminum alloy obtained after the surface treatment m ；
Or according to the initial mass M of the aluminum alloy 0 And initial dimension information I, and mass M of the aluminum alloy obtained after surface treatment 1 And size information II, calculating the surface porosity R of the aluminum alloy obtained after the surface treatment; wherein the apparent volume V of the aluminum alloy is calculated based on the measured dimensional information 0 Apparent volume V 1 And apparent surface area S 1 The method comprises the steps of carrying out a first treatment on the surface of the Using the initial mass M obtained 0 Mass M 1 Apparent volume V 0 Apparent volume V 1 And apparent surface area S 1 Calculating the surface porosity R;
4) By calculating mass reduction rate R of the aluminum alloy m Or surface porosity R as a quantitative characterization parameter for evaluating the microstructure of the surface of the aluminum alloy to which the polymer is attached.
In the above scheme, the mass reduction rate R m ＝(M 1 -M 0 )/M 0 。
In the above scheme, the surface porosity r= [ (M) 1 -M 0 )/M 0 -(V 1 -V 0 )/V 0 ]/S 1 。
In the scheme, the thickness of the aluminum alloy which is a base plate part is 0.5-3 mm, and the area is not less than 30mm 2 。
In the above scheme, the surface peeling step includes: completely soaking the surface of the aluminum alloy in a sodium hydroxide aqueous solution with the temperature of 35-50 ℃ and the concentration of 1-4 wt% for 8-20 min; the peeling process is not included in the "surface treatment" range.
In the scheme, the cleaning step is to add water for ultrasonic cleaning for more than or equal to 2 minutes.
In the scheme, the drying temperature is 40-50 ℃, and after drying, the apparent volume and the apparent surface area can be calculated by cooling to room temperature (15-25 ℃).
In the above scheme, the surface treatment process includes: the aluminum alloy is fully soaked in hydrochloric acid aqueous solution with the temperature of 35-50 ℃ and the concentration of 2-4 mol/L for 0-4 h.
Preferably, when the surface corrosion microstructure of the aluminum alloy sample connected by the same polymer is characterized or evaluated, the concentration of the hydrochloric acid aqueous solution (such as 2 mol/L) is fixed, and after testing different surface treatment time, the quality and size information of the aluminum alloy are obtained.
In the above scheme, the method is used for measuring the mass (M 0 And mass M 1 ) The minimum index value of the data obtained by the device measurement of (a) should not be greater than 1/10000 of the sample mass.
In the above scheme, the dimension information I and II in step 1) and step 2) includes length, width and thickness (one-dimensional dimension), wherein each dimension selects a plurality of geometric positions uniformly distributed in the aluminum alloy sample, and the measurement is performed by a screw micrometer (precision 0.001 mm); when the size exceeds the range of the screw micrometer, a vernier caliper with an graduation value below 0.01mm is used for measurement; when the size further exceeds the range of the vernier caliper, the measuring tool with larger range and convenient fixed position is used for measuring; the measured dimensions at different geometric positions are averaged to obtain the corresponding length, width and thickness, respectively.
Preferably, if the aluminum alloy sample is a product obtained by machining with a mechanical cutter or laser cutting, the sample measuring points on the contact surface of the cutter should be distributed in a matrix on the surface when measuring the outer contour dimension thereof.
Preferably, the aluminum alloy sample possesses a shape (preferably rectangular) that is regular in the normal plane of thickness and allows calculation of area by simple geometric relationships, otherwise it may not be possible to verify the effect of surface porosity on characterizing the aluminum alloy surface microstructure by preparing an aluminum alloy/polymer laminate lap sample to pass interfacial shear test results (results including bond strength and interfacial work-to-failure).
The invention also provides a regulating and controlling method for the surface treatment process of the aluminum alloy surface corrosion microstructure connected with the polymer based on the characterization method, which comprises the following steps: according to the calculated mass reduction rate R m Or the surface porosity R establishes a quantitative relation between the surface porosity R and the technological parameters of the aluminum alloy surface treatment, and regulates and controls the technological parameters of the aluminum alloy surface treatment.
Preferably, the process parameter of the surface treatment is the time of the surface treatment in step 2); according to the calculated mass reduction rate R m Or the surface porosity R, judging the void structure of the surface of the aluminum alloy after surface treatment, and obtaining a reasonable surface treatment time range.
Preferably, the quantitative relation determining method includes:
1) Measuring the mass reduction rate R of the aluminum alloy sample after different surface treatment time under the same other conditions m Or a surface porosity R value;
2) Respectively compounding the aluminum alloy samples subjected to different time surface treatments with a polymer to prepare an aluminum alloy lamination lap joint sample, and then measuring the corresponding interface bonding strength or interface failure work;
3) Establishing interface bonding strength or interface failure work and mass reduction rate R m Or a fit equation (quantitative relationship) between the surface porosity R values;
4) And regulating and controlling the technological parameters of the surface treatment according to the obtained fitting equation.
In the above scheme, the preparation steps of the aluminum alloy lamination lap joint sample comprise:
1) Stirring and dissolving polymer powder with the same composition as that of the polymer substrate to be bonded in an organic solvent to obtain a polymer solution;
2) Horizontally placing the aluminum alloy plate workpiece subjected to surface treatment on a horizontal operation table, and dripping the obtained polymer solution onto the surface of the aluminum alloy plate workpiece until the position to be bonded is completely wetted;
3) And (3) directly lapping the polymer substrate on the aluminum alloy plate obtained in the step (2), preventing the polymer substrate from rotating by using a limiting device, and standing to obtain the aluminum alloy lamination lapping sample.
In the above scheme, the organic solvent may be ethyl acetate, acetone, chloroform, paraxylene or the like.
In the above-mentioned scheme, the mass ratio of the solvent to the solute in the polymer solution is (16-13): 1.
In the scheme, the stirring and dissolving step adopts a magnetic stirring (tetrafluoroethylene magneton) method, and the time is 6-24 hours.
In the scheme, the standing treatment time is 12-48 hours.
In the above scheme, the polymer can be polymethyl methacrylate (PMMA), acrylonitrile-butadiene-styrene (ABS) or Polyethylene (PE) and the like.
In the scheme, the interface bonding strength is measured by adopting an interface bonding strength quasi-static loading experiment; and then further obtaining the interface failure work through the integral area of the displacement-load curve.
In the above scheme, the mass reduction rate R m When there is a scatter relationship between bond strength/interfacial failure work that can be fitted with a regular function, it is expected that R in the approximate scatter relationship is present m In the value interval, the maximum value of the bonding strength/interface failure work can be obtained through the prediction of a scattered point fitting equation; and in the absence of R in the above-mentioned regularity relationship m And in the value interval, the bonding strength of the lamination interface of the polymer/metal material system and the convergence range of the interface failure work can be estimated and judged through the test result.
In the above scheme, when a scattered point relation which can be fitted by a regular function exists between the surface porosity R and the bonding strength value/interface failure work value, it can be expected that the maximum value of the bonding strength/interface failure work can be obtained through prediction of a scattered point fitting equation in an R value interval where the approximate scattered point relation exists; in the R value interval without the regularity, the bonding strength of the lamination interface of the polymer/metal material system and the convergence range of the interface failure work can be estimated and judged through the test result; the convergence range of the surface porosity R can be judged through the scattered point relation of the R value and the large range of the bonding strength/interface failure work, so that excessive surface treatment is avoided.
In the scheme, the regular interval and the discrete interval of the data are judged through the combination strength-surface porosity, the interface failure work-surface porosity, the combination strength-quality reduction rate and the interface failure work-quality reduction rate scattered point data; judging the convergence range of the bonding strength, the interface failure work and the surface porosity of the polymer-aluminum alloy material system in a whole interval; and reading the corresponding interval of the surface porosity or mass reduction rate according to the actual requirements (such as the maximum bonding strength and the maximum interface failure work) of the bonding strength and the interface failure work, limiting the corresponding range of the surface treatment time according to the corresponding interval, and taking the reduced time interval as the range of the sample selection representation.
In the process of the invention for the surface of the aluminum alloy, the total mass of the substrate and the possible apparent volume are reduced; percentage R of total mass reduction m Subtracting the percentage R of macroscopic outer contour volume reduction v The percentage of the surface pore volume after the surface treatment of the substrate to the total volume before the surface treatment is simulated, namely R m -R v The method comprises the steps of carrying out a first treatment on the surface of the The percentage is then divided by the surface area S 1 The surface porosity R defined in the present invention is obtained.
Wherein the surface porosity R is compared with the mass reduction rate R m The change of the external outline size of the measurement sample piece is considered while the surface pore volume ratio is considered, which is also the reason that the surface porosity converges to a certain specific value; measurement of the surface porosity index also helps to find the saturation range of the sample surface porosity; with the continuous surface treatment, the quality of the aluminum alloy plate is reduced without limit, the pore on the surface of the aluminum alloy is based on the apparent outline of the sample, the depth of pitting micropores is limited (0-50 μm), the area ratio of the pore to the surface of the outer outline is less than 1 from a mathematical angle (when the ratio of the pore to the surface of the outer outline is=1, the baseline of the outer outline of the sample moves downwards, the volume of the outer outline needs to be recalculated), so the value of the surface porosity is convergent; this interfaces with the polymer/aluminum alloy stackThe detection result of the bonding strength with the numerical limit is also corresponding, and further illustrates that the surface porosity can be used as a quantitative characterization, and is suitable for the association and evaluation of the interface bonding performance of the laminated structure of a multi-material system.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention calculates the mass reduction rate R of the aluminum alloy before and after surface treatment m Apparent volume reduction rate R v Obtaining the surface porosity R of the substrate to measure the surface microstructure, so as to estimate the bonding performance of the aluminum alloy/polymer lamination interface; compared with the means of establishing data connection between the technological indexes such as surface treatment time and the interface bonding performance of the aluminum alloy/polymer lamination and the like, the invention relates to the surface porosity R or the mass reduction rate R m As the characterization reflecting the microstructure of the surface of the aluminum alloy after the surface treatment, the surface microstructure is more directly related with the subsequent lamination bonding performance data, and the R and R are obtained m The values are distinguished among the samples, so that the scattered point distribution trend of the data can be analyzed;
2) The characterization method disclosed by the invention is applicable to a wide range of aluminum alloy sizes, and samples with specific sizes or shapes do not need to be additionally prepared to meet the special requirements of test equipment; the test process has no pollution and damage to the sample, and the sample can still keep the original bonding performance with the polymer after the test; the data of the obtained surface porosity R can represent the surface microstructure of the aluminum alloy and the capability of forming a mechanical interlocking structure between the aluminum alloy and the polymer; and the related measuring tool is easy to obtain, the principle and flow are easy to understand and operate, and the popularization and the application are convenient.
Drawings
FIG. 1 shows the surface of 5052 aluminum alloy prior to peeling;
FIG. 2 shows the surface of 5052 aluminum alloy after peeling;
FIG. 3 is a schematic view of the microstructure and structure of the interface formed by the surface treated aluminum alloy and the polymer according to the present invention;
FIG. 4 is a schematic diagram showing the thickness measurement process of the aluminum alloy in examples 1 to 4;
FIG. 5 is a schematic diagram showing the width measurement process of the aluminum alloy in examples 1 to 4;
FIG. 6 is a schematic diagram showing the length measurement process of the aluminum alloy in examples 1 to 4;
FIG. 7 is a schematic diagram of the principle of the surface characterization step of the present invention in a short surface treatment time (. Ltoreq.50 min);
FIG. 8 is a schematic diagram of the surface characterization step of the present invention over a longer surface treatment time (> 50 min);
FIG. 9 is a plot of the bulk reduction rate and apparent volume reduction rate of an aluminum alloy obtained by subjecting a batch of the aluminum alloy to various surface treatment times as a function of the surface treatment time in example 1 of the present invention; (b) Scattered point relation of surface porosity with surface treatment time; (c) Bulk point relationship of aluminum alloy/polymer laminate interfacial bond strength to surface porosity; (d) The scattered point relation between the interfacial shear failure work and the surface porosity; (e) the scattered point relation of the interface failure work and the bonding strength; (f) Scattered point relation between interface bonding strength and aluminum alloy mass reduction rate; (g) Scattered point relation between interface failure work and aluminum alloy material reduction rate;
FIG. 10 is a schematic diagram of a quasi-static mechanical specimen preparation process for testing the interfacial bond strength and interfacial work-to-failure of an aluminum alloy and polymer laminate sample according to the present invention;
FIG. 11 is a schematic diagram showing the positional relationship between an aluminum alloy and a polymer substrate in a quasi-static mechanical sample for testing the interfacial bonding strength and interfacial failure work of an aluminum alloy and polymer laminate sample according to the present invention;
FIG. 12 is a schematic diagram of a quasi-static mechanical test method according to the present invention;
FIG. 13 is a plot of the bulk reduction ratio and apparent volume reduction ratio of an aluminum alloy obtained by subjecting a batch of the aluminum alloy to various surface treatment times as a function of the surface treatment time in example 2 of the present invention; (b) Scattered point relation of surface porosity with surface treatment time; (c) Bulk point relationship of aluminum alloy/polymer laminate interfacial bond strength to surface porosity; (d) The scattered point relation between the interfacial shear failure work and the surface porosity; (e) the scattered point relation of the interface failure work and the bonding strength; (f) Scattered point relation between interface bonding strength and aluminum alloy mass reduction rate; (g) Scattered point relation between interface failure work and aluminum alloy material reduction rate;
FIG. 14 is a plot of the bulk reduction ratio and apparent volume reduction ratio of an aluminum alloy obtained by subjecting a batch of the aluminum alloy to various surface treatment times as a function of the surface treatment time in example 3 of the present invention; (b) Scattered point relation of surface porosity with surface treatment time; (c) Bulk point relationship of aluminum alloy/polymer laminate interfacial bond strength to surface porosity; (d) The scattered point relation between the interfacial shear failure work and the surface porosity; (e) the scattered point relation of the interface failure work and the bonding strength; (f) Scattered point relation between interface bonding strength and aluminum alloy mass reduction rate; (g) Scattered point relation between interface failure work and aluminum alloy material reduction rate;
FIG. 15 is a plot of the mass reduction rate and apparent volume reduction rate of all aluminum alloys subjected to different surface treatment times as a function of the surface treatment time for the scattered points in example 4; (b) Integrating the scattered point relation of the surface porosity along with the surface treatment time; (c) Integrating the scattered point relation between the bonding strength of the aluminum alloy/polymer lamination interface and the surface porosity; (d) Integrating the scattered point relation between the shearing failure work of the interface and the surface porosity; (e) Integrating the scattered point relation of the interface failure work and the bonding strength; (f) Integrating the scattered point relation between the interface bonding strength and the aluminum alloy mass reduction rate; (g) Integrating the scattered point relation between the interface failure work and the aluminum alloy material reduction rate;
in the above figures, 1-aluminum alloy surface before peeling, 2-macroscopic scratch on aluminum alloy surface before peeling, 3-aluminum alloy surface after peeling, 4-aluminum alloy, 5-polymer, 6-aluminum alloy surface with micro holes after surface treatment, 7-aluminum alloy and polymer interface mechanical locking structure, 8-aluminum alloy/polymer lamination integration, 9-screw micrometer ranging screw, 10-aluminum alloy, 11-thickness value measuring point, 12-width value measuring point, 13-vernier caliper measuring outer claw, 14-length value measuring point, 15-polymer powder swelling solution, 16-polymer powder swelling solution after paving, 17-polymer substrate, 18-force-displacement curve, 19-interface breaking load, 20-force-displacement curve area (interface failure work), 21-quasi-static loading pressure head, 22-uniform loading load, 23-clamp, 24-lamination interface quasi-static shear strength sample.
Detailed Description
For a better understanding of the present invention, the following description will further illustrate the present invention with reference to specific examples, but the present invention is not limited to the following examples.
In the following examples, the aluminum alloy used was 5052 aluminum alloy of different batches, and the morphology diagrams before and after peeling treatment were respectively shown in fig. 1 and fig. 2; a schematic representation of the interfacial microscopic lock and structure formed by the surface treated aluminum alloy and the adhesive or polymer is shown in fig. 3.
The test methods for the apparent systems of the following examples included: the thickness and width dimensions were measured by taking measurement points in the thickness direction and the width direction by using a screw micrometer (precision 0.001 mm) in the method shown in fig. 4 and 5, the length dimension was measured by taking measurement points in the length direction by using a vernier caliper (minimum graduation value 0.01 mm) in the method shown in fig. 6, and the apparent volume was calculated by multiplying the three dimensions of length, width and thickness after averaging all the measured dimensions.
The mass of the aluminum alloy was measured using an analytical balance (precision 0.1. Mu.g).
Example 1
A characterization and regulation method of an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminated material relates to 17 aluminum alloy (5052) pieces in total, and nominal original dimensions are 30mm multiplied by 10mm multiplied by 2mm; the aluminum alloy substrates before and after the surface treatment are respectively measured and calculated in size and apparent volume, so that the surface porosity of the aluminum alloy substrates after the surface treatment is obtained, and the capability of forming a microscopic locking structure between the aluminum alloy substrates and a polymer interface is measured; the method specifically comprises the following steps:
1) Peeling and cleaning pretreatment: soaking the aluminum alloy in a NaOH aqueous solution with the concentration of 1wt% at 40 ℃ for 10min, immediately cleaning the aluminum alloy in deionized water for 2min by using ultrasonic waves, drying the aluminum alloy in a blast drying oven at 40 ℃, taking out, and cooling the aluminum alloy to the room temperature of 25 ℃; measuring and calculating initial apparent volume V 0 And aluminum alloy mass M 0 ；
2) Surface treatment: soaking aluminum alloy with HCl aqueous solution with concentration of 2mol/L at 40 ℃ for each substrate soaking time shown in table 1, and then immediately cleaning in deionized water by ultrasonic waves for 2min; using the same method to calculate and obtainInitial apparent volume V 1 And an initial mass M 1 Then, the surface area S after the final surface treatment is calculated according to the measured size 1 ；
3) Calculation of surface porosity R and mass reduction R m : calculating a characterization result according to the following relation: r= [ (M) 1 -M 0 )/M 0 -(V 1 -V 0 )/V 0 ]/S 1 ，R m ＝(M 1 -M 0 )/M 0 The method comprises the steps of carrying out a first treatment on the surface of the The specific calculation process is shown in fig. 7 or fig. 8.
The surface characterization results of the aluminum alloy obtained in this example after surface treatment are shown in fig. 9 (a) and 9 (b). From the test results, the aluminum alloy reduction rate and the surface treatment time show an increasing relationship; the apparent volume remained essentially unchanged with increasing surface treatment time, but after 70min there was a tendency to begin to decrease; the surface porosity has an increasing trend along with the increase of the surface treatment time, and after 70min, the surface porosity has no trend of continuous increase and converges to 0-6.05E-5+/-0.02E-5/mm 2 Within a range of (2).
Further adopting a quasi-static test result to verify the reliability of the surface porosity and the quality reduction rate characterization aluminum alloy surface: a polymethyl methacrylate (PMMA) substrate (20 mm×10mm×2 mm) and a surface-treated aluminum alloy laminate lap joint sample (specific positional relationship is shown in fig. 11) were prepared in accordance with the procedure shown in fig. 10 so that the interface therebetween attains bonding strength, wherein the preparation method of the aluminum alloy laminate lap joint sample comprises the steps of: 1) Preparing an adhesive solution (polymer solution) with a mass ratio of the solvent to the solute of 15:1 by taking an acetone pure solution as a solvent and PMMA powder as a solute, and stirring for 12 hours by using polytetrafluoroethylene magnetons in the preparation process until no macroscopic particles exist in the solution; 2) Horizontally placing the aluminum alloy plate subjected to surface treatment on a horizontal operation table top, sucking 50 mu L of solution by using a dropper, extruding the solution, and completely wetting the positions of the substrate and the polymer to be bonded; 3) And (2) directly lapping the polymer substrate on the aluminum alloy plate piece obtained in the step (2), preventing the polymer substrate from rotating by using a proper limiting device, and standing for 48 hours without applying any external pressure above the overlapped position of the polymer substrate and the aluminum alloy plate to obtain a laminated lapping sample. Then, an interface bonding strength quasi-static loading experiment is carried out by the method shown in fig. 12, so that an interface failure load, namely bonding strength, is obtained, and an interface failure work is obtained by the integral area of a displacement-load curve.
As shown in fig. 9 (c), 9 (d) and 9 (E), the binding strength has an approximately parabolic relationship with the surface porosity within the range of 0 < R < 2.25E-5±0.05e-5, fitting an approximate equation y=1474x 0.5 Determining the coefficient R 2 In the same range, the interfacial failure work has an approximate linear relation with the surface porosity, and the approximate equation y=1.4473E7x is fitted to determine the coefficient R 2 =0.946; when the bonding strength is less than 6.6MPa, the relationship between the bonding strength and the interface failure work is similar to parabolic, and the relationship between the surface porosity and the bonding strength and the interface failure work is met mathematically; as can be seen from the data scatter diagrams of FIG. 9 (f) and FIG. 9 (g), R is smaller than 0 m Within the range of < 0.022+/-0.002, the binding strength has approximate parabolic relation with mass reduction rate, and the approximate equation y=46.62 x is fitted 0.5 Determining the coefficient R 2 =0.942, at 0 < R m Within the range of less than 0.029+/-0.002, the interface failure work has approximate linear relation with mass reduction rate, the fitting approximate equation y=11762x is adopted, and the coefficient R is determined 2 ＝0.947。
From the above relationship, it can be seen that the combination property of the surface porosity and the mass reduction rate with the aluminum alloy/polymer lamination interface formed by microscopic locking is at a certain R m Has good corresponding relation with the characterization data in the R value range. As is clear from the results of FIG. 9 of the present example, the porosity at the surface of the aluminum alloy was 2.25E-5.+ -. 0.05E-5/mm 2 Or when the mass reduction rate is 0.022+/-0.002, the bonding strength can reach about 6.5MPa, the highest bonding strength in the embodiment is closest to 7.6MPa in a fitted parabolic interval, and in the conclusion range of the embodiment, if the interface bonding strength is as high as possible, the surface of the aluminum alloy is not excessively subjected to surface treatment, and the corresponding surface treatment time screening range is 25-40 min.
Example 2
A characterization and regulation method of an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminated material relates to 13 aluminum alloy (5052) pieces, and nominal original dimensions are 30mm multiplied by 10mm multiplied by 2mm; the aluminum alloy substrates before and after the surface treatment are respectively measured and calculated in size and apparent volume, so that the surface porosity of the aluminum alloy substrates after the surface treatment is obtained, and the capability of forming a microscopic locking structure between the aluminum alloy substrates and a polymer interface is measured; the method specifically comprises the following steps:
1) Peeling and cleaning pretreatment: soaking the aluminum alloy in a NaOH aqueous solution with the concentration of 1wt% at 40 ℃ for 10min, immediately cleaning the aluminum alloy in deionized water for 2min by using ultrasonic waves, drying the aluminum alloy in a blast drying oven at 40 ℃, taking out, and cooling the aluminum alloy to the room temperature of 25 ℃; measuring and calculating initial apparent volume V 0 And aluminum alloy mass M 0 ；
2) Surface treatment: soaking aluminum alloy with HCl aqueous solution with concentration of 2mol/L at 40deg.C, wherein soaking time of each substrate is shown in Table 1, and immediately cleaning with ultrasonic wave in deionized water for 2min; the initial apparent volume V is calculated by the same method 1 And an initial mass M 1 At the same time, the surface area S after the formal surface treatment is calculated according to the measured size 1 ；
3) Calculation of surface porosity R and mass reduction R m : according to the measured results of the previous steps, calculating a characterization result according to the following relation: r= [ (M) 1 -M 0 )/M 0 -(V 1 -V 0 )/V 0 ]/S 1 ，R m ＝(M 1 -M 0 )/M 0 。
The surface characterization results of the aluminum alloy obtained in this example after surface treatment are shown in fig. 13 (a) and 13 (b). From the test results, the aluminum alloy reduction rate and the surface treatment time show an increasing relationship; the apparent volume remains substantially unchanged with increasing surface treatment time, but after 50min there is a tendency to begin to decrease; the surface porosity firstly shows a non-linear increasing trend along with the increase of the surface treatment time, after 70min, no further increasing trend exists, and the surface porosity is converged to 0-4.35E-5+/-0.05E-5/mm 2 Within a range of (2).
Verification of surface porosity and quality reduction Using the results of the quasi-static test as described in reference to example 1 to characterize aluminium alloysReliability of gold surface. As shown in fig. 13 (c), 13 (d) and 13 (E), the binding strength has an approximately parabolic relationship with the surface porosity within the range of 0 < R < 2.30E-5±0.05E-5, fitting an approximate equation y=1566x 0.5 Determining the coefficient R 2 In the same range, the interfacial failure work has an approximate linear relation with the surface porosity, an approximate equation y=1.623E7x is fitted, and a coefficient R is determined 2 =0.985; when the bonding strength is less than 7MPa, the relationship between the bonding strength and the interface failure work is similar to parabolic, and the relationship between the surface porosity and the bonding strength and the interface failure work is met mathematically; as can be seen from the data scatter diagrams of FIG. 13 (f) and FIG. 13 (g), R is smaller than 0 m Within < 0.023.+ -. 0.001, the binding strength has an approximately parabolic relationship with mass reduction rate, fitting an approximate equation y= 51.31x 0.5 Determining the coefficient R 2 In the same range, interface failure work and mass reduction rate have approximate linear relation, fitting approximate equation y=17783x, and determining coefficient R 2 =0.970. From the above relationship, it can be seen that the combination property of the surface porosity and the mass reduction rate with the aluminum alloy/polymer lamination interface formed by microscopic locking is at a certain R m Has good corresponding relation with the characterization data in the R value range.
As shown in FIG. 13, the porosity of the aluminum alloy surface was 2.30E-5.+ -. 0.05E-5/mm 2 Or when the mass reduction rate is 0.023+/-0.001, the bonding strength can reach about 6.8MPa, the maximum value of the method is closest to 7.6MPa in the embodiment in a fitted parabolic interval, and in the conclusion range of the embodiment, if the interface bonding strength is as high as possible, the surface of the aluminum alloy is not excessively treated, and the corresponding time screening range is about 25-50 min.
Example 3
A characterization and regulation method of an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminated material relates to 18 aluminum alloys (5052) with nominal original dimensions of 30mm multiplied by 10mm multiplied by 2mm; the aluminum alloy substrates before and after the surface treatment are respectively measured and calculated in size and apparent volume, so that the surface porosity of the aluminum alloy substrates after the surface treatment is obtained, and the capability of forming a microscopic locking structure between the aluminum alloy substrates and a polymer interface is measured; the method specifically comprises the following steps:
1) Peeling and cleaning pretreatment: soaking the aluminum alloy in a NaOH aqueous solution with the concentration of 1wt% at 40 ℃ for 10min, immediately cleaning the aluminum alloy in deionized water for 2min by using ultrasonic waves, drying the aluminum alloy in a blast drying oven at 40 ℃, taking out, and cooling the aluminum alloy to the room temperature of 25 ℃; measuring and calculating initial apparent volume V 0 And aluminum alloy mass M 0 ；
2) Surface treatment: soaking aluminum alloy with HCl aqueous solution with concentration of 2mol/L at 40deg.C, wherein soaking time of each substrate is shown in Table 1, and immediately cleaning with ultrasonic wave in deionized water for 2min; the initial apparent volume V is calculated by the same method 1 And an initial mass M 1 At the same time, the surface area S after the formal surface treatment is calculated according to the measured size 1 ；
3) Calculation of surface porosity R and mass reduction R m : according to the measured results of the previous steps, the result is calculated according to the following relation: r= [ (M) 1 -M 0 )/M 0 -(V 1 -V 0 )/V 0 ]/S 1 ，R m ＝(M 1 -M 0 )/M 0 。
The surface characterization results of the aluminum alloy obtained in this example after surface treatment are shown in fig. 14 (a) and 14 (b). The test result shows that the aluminum alloy material reduction rate and the formal surface treatment time show an increasing relationship; the apparent volume remains substantially unchanged with increasing surface treatment time, but after 40min there is a tendency to begin to decrease; the surface porosity shows a trend of increasing with the increase of the surface treatment time, and after 70min, the surface porosity has no trend of increasing, and converges to 0-5.45E-5+/-0.10E-5/mm 2 Within a range of (2).
The reliability of the surface of the aluminum alloy was characterized by verifying the surface porosity and mass reduction using the quasi-static test results with reference to the method described in example 1. As shown in fig. 14 (c), 14 (d) and 14 (E), when R < 0 < 2.40E-5±0.05e-5, the bonding strength has an approximately parabolic relationship with the surface porosity, and the approximation equation y=1473 x is fitted 0.5 Determining the coefficient R 2 =0.870; interface failure work and surface when R is more than 0 and less than 2.35E-5+/-0.05E-5The porosity has approximate linear relation, the approximate equation y=1.574E7x is fitted, and the coefficient R is determined 2 =0.944; when the bonding strength is less than 7MPa, the relationship between the bonding strength and the interface failure work is similar to parabolic, and the relationship between the surface porosity and the bonding strength and the interface failure work is met mathematically; as can be seen from the data scatter diagrams of FIG. 14 (f) and FIG. 14 (g), R is smaller than 0 m Within the range of < 0.023+/-0.002, the binding strength has an approximate parabolic relationship with mass reduction rate, and the approximate equation y=46.25x is fitted 0.5 Determining the coefficient R 2 =0.898; in the same range, the interface failure work has approximate linear relation with the mass reduction rate, an approximate equation y=17910 x is fitted, and a coefficient R is determined 2 =0.964. From the above relationship, it can be seen that the combination property of the surface porosity and the mass reduction rate with the aluminum alloy/polymer lamination interface formed by microscopic locking is at a certain R m Has good corresponding relation with the characterization data in the R value range. As is clear from the results of FIG. 8, the porosity at the surface of the aluminum alloy was 2.40E-5.+ -. 0.05E-5/mm 2 Or the mass reduction rate is 0.023+/-0.002, the bonding strength can reach 7.1MPa, the maximum value of the method is closest to 7.9MPa in the embodiment in a fitted parabolic interval, and the corresponding time screening range is about 30-35 min in the conclusion range of the embodiment if the interface bonding strength is as high as possible and the surface of the aluminum alloy is not excessively subjected to surface treatment.
Example 4
Summarizing the characterization results obtained in examples 1-3, the reliability of the method for characterizing the aluminum alloy surface of the present invention was verified in a wider data range, and the specific results are shown in table 1 and fig. 15.
The results show that: the aluminum alloy mass reduction rate and the surface treatment time show a nonlinear increasing relation (non-convergence); the apparent volume does not change significantly with the surface treatment time, but has a tendency to decrease after 50 minutes; the surface porosity of the aluminum alloy shows an increasing trend before 70min along with the surface treatment time, but no increasing trend (convergence) exists after 70 min; the corresponding data results for all bond strengths with respect to surface porosity still present a distinct approximately parabolic scatter distribution, fitting the parabolic equation y=1501 x 0.5 Determining the coefficient R 2 ＝0.852The interfacial failure work and the surface porosity still keep an approximate linear relation, a linear equation y=1.610E7x is fitted, and a coefficient R is determined 2 =0.912; the mass reduction rate of the aluminum alloy and the bonding strength of the interface and the failure work of the interface have similar parabolic and approximately linear scattered point distribution relations respectively, and a fitted parabolic equation y=48.00 x 0.5 Determining the coefficient R 2 Linear equation y=16944 x, determining coefficient r=0.868 2 =0.900. In all embodiments, the coefficients in the fitting equation in the same scatter relationship are closer in each embodiment in the rest of the scatter relationships except for the mass reduction rate and interface failure power scatter relationship in embodiment 1.
From the summary of the results of examples 1 to 3 shown in fig. 15, it is clear that: by the characterization method, excessive aluminum alloy surface treatment can be effectively avoided: when the surface porosity is controlled to be 2.55E-5+/-0.20E-5/mm 2 Or when the mass reduction rate is controlled to be 0.023+/-0.002, the highest interfacial bonding strength of the aluminum alloy with the polymer can reach 7.6MPa in the corresponding state range after surface treatment, and the highest bonding strength of the aluminum alloy is already close to 7.9MPa in the embodiment, so that the corresponding surface treatment time screening range is about 25-40 min if the interface bonding strength is as high as possible without excessive surface treatment on the surface of the aluminum alloy in the conclusion range of all the embodiments of the invention; the failure work of the interface is R & gt2.75E-5 or R m After more than 0.025, the interfacial failure work shows a more discrete change trend along with the surface porosity and mass reduction rate, and the value of the interfacial failure work can be further improved within the range.
By summarizing the data in examples 1-3, it is demonstrated with sufficient data points that the interfacial bond strength between the aluminum alloy and PMMA system is up to about 7.9MPa, and if only the highest bond strength is approached or reached, only the aluminum alloy surface porosity needs to be controlled at 2.55E-5.+ -. 0.20E-5/mm 2 Or the mass reduction rate is controlled to be 0.023 plus or minus 0.002, and the aluminum alloy sample conforming to the surface porosity or mass reduction rate range can be selected by characterization in the workpiece in the time interval (25-40 min) of the corresponding surface treatment; if the interface failure work is considered on the basis, the extension can be continuedSurface treatment time, the one with the greater surface porosity was selected from the resulting articles, but according to the experience of this example, the surface porosity converged to about 0 to 6.07E-5/mm 2 The corresponding surface treatment time is not more than 70min.
Table 1 results of the process parameters and performance tests of the aluminum alloy test pieces of examples 1 to 3
/>
Table 2 recording of quality before and after surface treatment of aluminum alloy test pieces according to examples 1 to 3
/>
Table 3 records of the dimensions of the aluminum alloy test pieces of examples 1 to 3 before and after the surface treatment
/>
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (8)
1. A method for characterizing an aluminum alloy surface corrosion microstructure in an aluminum alloy/polymer laminate, comprising the steps of:
1) Peeling the surface of the aluminum alloy sample, cleaning, drying and cooling the aluminum alloy sample to obtain the initial mass M of the aluminum alloy 0 And initial size information I;
2) Surface treatment is carried out on the surface of the aluminum alloy, then cleaning, drying and cooling are carried out, and the mass M of the aluminum alloy obtained after the surface treatment is measured 1 And size information II;
3) According to the initial mass M of the aluminum alloy 0 And initial dimension information I, and mass M of the aluminum alloy obtained after surface treatment 1 And size information II, calculating the surface porosity R of the aluminum alloy obtained after the surface treatment; wherein the apparent volume V of the aluminum alloy is calculated based on the measured dimensional information 0 Apparent volume V 1 And apparent surface area S 1 The method comprises the steps of carrying out a first treatment on the surface of the Using the initial mass M obtained 0 Mass M 1 Apparent volume V 0 Apparent volume V 1 And apparent surface area S 1 Calculating the surface porosity R;
4) Using the calculated surface porosity R of the aluminum alloy as a quantitative characterization parameter for evaluating the corrosion microstructure of the aluminum alloy surface in the aluminum alloy/polymer laminated material;
the surface porosity r= [ (M) 1 -M 0 )/M 0 -(V 1 -V 0 )/V 0 ]/S 1 ；
The surface treatment process comprises the following steps: the dimensional information I and II in the step 1) and the step 2) comprise length, width and thickness, wherein each dimension is measured by selecting a plurality of geometric positions on the surface of the aluminum alloy sample and taking an average value.
2. The characterization method according to claim 1, wherein the aluminum alloy is a substrate product, the thickness is 0.5-3 mm, and the area is 30mm 2 The above.
3. The method of characterization according to claim 1, wherein the surface peeling step comprises: the surface of the aluminum alloy is completely soaked in sodium hydroxide aqueous solution with the temperature of 35-50 ℃ and the concentration of 1-4 wt% for 8-20 min.
4. The characterization method of claim 1, wherein the surface treatment process comprises: the aluminum alloy is fully soaked in hydrochloric acid aqueous solution with the temperature of 35-50 ℃ and the concentration of 2-4 mol/L for 0-4 h.
5. A method for controlling the corrosion microstructure of an aluminum alloy surface connected with a polymer based on the characterization method as claimed in any one of claims 1 to 4, wherein the surface porosity R is calculated, a quantitative relationship between the surface porosity R and the process parameters of the aluminum alloy surface treatment is established, and the process parameters of the aluminum alloy surface treatment are controlled.
6. The method according to claim 5, wherein the process parameter of the surface treatment is the time of the surface treatment in step 2).
7. The method of claim 5, wherein the quantitative relationship determination method comprises:
1) Respectively measuring the surface porosity R values of the aluminum alloy samples after different surface treatment times under the condition that other conditions are the same;
2) Respectively compounding the aluminum alloy samples subjected to different time surface treatments with a polymer to prepare an aluminum alloy lamination lap joint sample, and then measuring the corresponding interface bonding strength or interface failure work;
3) Establishing a fitting equation between the interface bonding strength or the interface failure work and the surface porosity R value;
4) And regulating and controlling the technological parameters of the surface treatment according to the obtained fitting equation.
8. The method of claim 7, wherein the step of preparing the aluminum alloy laminate lap joint sample comprises:
1) Stirring and dissolving polymer powder with the same composition as that of the polymer substrate to be bonded in an organic solvent to obtain a polymer solution;
2) Dripping the obtained polymer solution onto the surface of the aluminum alloy plate piece after surface treatment until the position to be bonded is completely wetted;
3) And (2) directly lapping the polymer substrate on the aluminum alloy plate obtained by the treatment in the step (2), preventing the polymer substrate from rotating by using a limiting device, and standing to obtain the aluminum alloy lamination lapping sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210105747.8A CN114563322B (en) | 2022-01-28 | 2022-01-28 | Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210105747.8A CN114563322B (en) | 2022-01-28 | 2022-01-28 | Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114563322A CN114563322A (en) | 2022-05-31 |
| CN114563322B true CN114563322B (en) | 2023-12-19 |
Family
ID=81713319
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210105747.8A Active CN114563322B (en) | 2022-01-28 | 2022-01-28 | Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114563322B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101256134A (en) * | 2008-04-17 | 2008-09-03 | 电子科技大学 | Method for measurement of printed circuit gold-plating layer porosity |
| WO2010072104A1 (en) * | 2008-12-23 | 2010-07-01 | 南京工业大学 | Porous material surface orifice's diameter distribution measuring method |
| CN102116730A (en) * | 2010-12-09 | 2011-07-06 | 中兴通讯股份有限公司 | Method for testing porosity of electric connector gold-plating layer |
| CN105424574A (en) * | 2015-11-10 | 2016-03-23 | 国网吉林省电力有限公司电力科学研究院 | Quantitative characterization method for foam aluminum alloy porosity and dispersity |
| CN108226007A (en) * | 2017-12-29 | 2018-06-29 | 大连理工大学 | A kind of carbon fiber enhancement resin base composite material porosity characterizing method two-parameter based on ultrasound |
| CN112033874A (en) * | 2019-06-04 | 2020-12-04 | 中国航发商用航空发动机有限责任公司 | Method for obtaining porosity and interface strength of composite material cementing interface |
| CN112962132A (en) * | 2021-02-02 | 2021-06-15 | 山东省科学院新材料研究所 | Magnesium alloy ultrahigh-porosity micro-arc oxidation coating and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7776604B2 (en) * | 2003-04-01 | 2010-08-17 | Cabot Corporation | Methods of selecting and developing a particulate material |
-
2022
- 2022-01-28 CN CN202210105747.8A patent/CN114563322B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101256134A (en) * | 2008-04-17 | 2008-09-03 | 电子科技大学 | Method for measurement of printed circuit gold-plating layer porosity |
| WO2010072104A1 (en) * | 2008-12-23 | 2010-07-01 | 南京工业大学 | Porous material surface orifice's diameter distribution measuring method |
| CN102116730A (en) * | 2010-12-09 | 2011-07-06 | 中兴通讯股份有限公司 | Method for testing porosity of electric connector gold-plating layer |
| CN105424574A (en) * | 2015-11-10 | 2016-03-23 | 国网吉林省电力有限公司电力科学研究院 | Quantitative characterization method for foam aluminum alloy porosity and dispersity |
| CN108226007A (en) * | 2017-12-29 | 2018-06-29 | 大连理工大学 | A kind of carbon fiber enhancement resin base composite material porosity characterizing method two-parameter based on ultrasound |
| CN112033874A (en) * | 2019-06-04 | 2020-12-04 | 中国航发商用航空发动机有限责任公司 | Method for obtaining porosity and interface strength of composite material cementing interface |
| CN112962132A (en) * | 2021-02-02 | 2021-06-15 | 山东省科学院新材料研究所 | Magnesium alloy ultrahigh-porosity micro-arc oxidation coating and preparation method and application thereof |
Non-Patent Citations (6)
| Title |
|---|
| AZ91D镁合金微弧氧化膜的致密性及其对耐蚀性的影响;董海荣;马颖;郭惠霞;张玉福;郝远;;中国有色金属学报(04);全文 * |
| Effect of initial surface treatment on obtaining a superhydrophobic surface on 5052 aluminum alloy with enhanced anticorrosion properties;Rafael G.C. da Silva et al.;Surface & Coatings Technology;第311-322页 * |
| Rafael G.C. da Silva et al..Effect of initial surface treatment on obtaining a superhydrophobic surface on 5052 aluminum alloy with enhanced anticorrosion properties.Surface & Coatings Technology.2019,第311-322页. * |
| 微孔陶瓷管孔隙率的测定及表面润湿性研究;张利娜;徐秉声;陈军伟;吴燕;徐红艳;袁章福;;有色金属科学与工程(06);全文 * |
| 苑芳友.建筑材料与检测技术(第3版).北京理工大学出版社,2020,第168页. * |
| 铜电解精炼不锈钢阴极板的结合强度研究;薛方勤等;有色金属(冶炼部分)(第6期);第10-12页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114563322A (en) | 2022-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kajihara et al. | Joining strength dependence on molding conditions and surface textures in blast-assisted metal-polymer direct joining | |
| Newman et al. | Short-crack growth behaviour in an aluminum alloy: an AGARD cooperative test programme | |
| Rech et al. | Different cold spray deposition strategies: single-and multi-layers to repair aluminium alloy components | |
| US20140034233A1 (en) | Composites having improved interlayer adhesion and methods thereof | |
| CN114563322B (en) | Characterization and regulation method for aluminum alloy surface corrosion microstructure in aluminum alloy/polymer laminated material | |
| Gao et al. | Facile fabrication of a superhydrophobic titanium surface with mechanical durability by chemical etching | |
| Zhang et al. | A method for bond strength evaluation for laminated structures with application to ultrasonic consolidation | |
| Van Tooren et al. | Experimental verification of a stress singularity model to predict the effect of bondline thickness on joint strength | |
| Subramanya et al. | A three-dimensional numerical study of mixed mode (I and II) crack tip fields in elastic–plastic solids | |
| CN112199632B (en) | Laser-textured aluminum alloy surface hardness prediction method | |
| Chen et al. | Crack path selection in adhesively-bonded joints: the role of material properties | |
| Freund et al. | Relationship between laser-generated micro-and nanostructures and the long-term stability of bonded epoxy-aluminum joints | |
| Tay et al. | Analysis of delamination growth in laminated composites with consideration for residual thermal stress effects | |
| CN108896411B (en) | Shearing experimental device for sandwich plate core layer and experimental method thereof | |
| Annoni et al. | Microcutting force prediction by means of a slip-line field force model | |
| EP3670694A1 (en) | Additively manufactured article and method of coating same | |
| Ying et al. | Investigation of the effect of the cut parameter on the machining performance of PTFE cutting | |
| Arola et al. | Surface texture, fatigue, and the reduction in stiffness of fiber reinforced plastics | |
| CN105758792A (en) | Method and device for measuring interface average peel strength of metal laminated composite material | |
| Leong et al. | Effect of through-thickness compression on the microstructure of carbon fiber polymer-matrix composites, as studied by electrical resistance measurement | |
| Cedeno-Campos et al. | Towards mould free composites manufacturing of thermoset prepregs. Incremental curing with localised pressure-heat (ICULPH) | |
| Zhang et al. | Properties and cutting performance of tialsin coating prepared by cathode ARC ion plating | |
| Zhang | A thermomechanical analysis of an ultrasonic bonding mechanism | |
| Poveromo et al. | Development of percussion diagnostics in evaluating ‘kiss’ bonds between composite laminates | |
| Williams et al. | Epoxy adhesive behaviour on ceramic surfaces in commercial optoelectronic assemblies |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |