CN112858162A - Method for evaluating binding force of film layer on surface of coated iron - Google Patents
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Abstract
The invention provides an evaluation method for the binding force of a film layer on the surface of a coated iron. The epoxy resin and the PET film have similarity in structure, so that the invention simulates the combination of the PET film and the chromium plating plate by coating the epoxy resin on the surface of the chromium plating plate, and adopts the thermal vibration test to measure the combination capacity of the surface of the chromium plating plate and the organic film, thereby detecting and comparing the difference of the film layer combination force. The evaluation method is simple to operate, can visually find the bonding force difference between the chromium plating plate surfaces and the thin films of different plating solution systems and different structures according to the experimental result, and has the advantages of rapidness, effectiveness, accuracy and environmental friendliness.
Description
Technical Field
The invention relates to the technical field of production control of coated iron, in particular to an evaluation method for the binding force between the surface of a chromium-plated steel plate and a film.
Background
The coated iron is a novel composite material which is obtained by coating a certain number of plastic films (generally polyester composite films with the thickness of 20-25 mu m) on two surfaces of a cold-rolled thin steel plate (also called a chromium-plated plate, which is a thin steel plate with a layer of metal chromium and chromium hydroxide deposited on the surface by an electrochemical method) in a bonding or hot melting mode and the like, so that the characteristics of the plastic films and the characteristics of metal plates are achieved. The production process of the coated iron is simple, the production process is good, the coated iron has the advantages of corrosion resistance, rust resistance, stable chemical property and the like, the raw materials are environment-friendly and nontoxic, no waste gas is contained in the production process, no pollution is generated, the production cost is greatly reduced compared with tinplate, the coated iron gradually becomes a substitute for tinplate products at present, and the coated iron has a good development prospect.
The laminated iron adopts an electromagnetic induction heating roller to heat the surface, when the temperature of the substrate passing through a heating area reaches more than 250 ℃, the substrate is immediately pressurized, and the laminated iron is quickly attached to the surface of the chromium-plated iron after an organic polyester film with a multi-layer structure reaches the melting point thereof in a multi-layer co-extrusion mode and is cooled to form a laminated iron product. The structure of the coated iron is shown in figure 1. The main component of the coated iron is an organic thin film coated on the surface, and the thin films adopted by the coated iron mostly comprise a PP film, a PC film, a PE film and a PET film, and the surface of the coated iron is usually the PET film because the PET film has good formability, good wear resistance, easy painting and printing and the like.
At present, the more mature technology for producing the coated iron is mastered in the countries such as Germany, American, English, Japan, and the like, wherein the technology for producing the coated iron in Japan is the most mature, and the number of production lines is the most. The research of the production technology of the film-coated iron in China is still in the initial stage, for example, although a company without tin develops a method for adhering a polyester film on a chromium-plated plate under a low-temperature condition, the produced film-coated iron has a certain gap in performance compared with the film-coated iron produced abroad, and cannot be completely applied to the field of food and beverage packaging. Baoku group Bao Steel products company has domestic production line special for chromium plating plates with fastest production speed and thinnest plate thickness, and a plastic film is covered on the surface of the chromium plating plate by adopting a high-temperature and high-pressure extrusion process. The core process of the film-coated iron is a good match of the heating uniformity of the chromium-coated substrate, the film-coating temperature, the film-coating pressure and the like, the film-coating speed and the substrate specification, and the key performance index is the bonding strength problem between a PET film and a chromium-coated plate.
Due to the limitation of the production technology level, the problem that the bonding force between the organic film on the surface of the coated iron and the substrate is not strong becomes a bottleneck in the development of the coated iron in China. In addition, the prior art cannot represent the binding force of the coated iron timely, effectively and quickly, and also limits the technical progress and the production efficiency of the coated iron. Therefore, an evaluation method capable of quickly and effectively evaluating the bonding force between the organic film and the chromium-plated substrate is needed to be found, so that the inferior product with the bonding force not meeting the standard can be quickly and accurately found out in the actual production process, the qualification rate of the formed product is increased, the production efficiency of a production line is improved, and the evaluation method has profound significance for enhancing the product competitiveness of the coated iron in the actual application field. The existing methods for evaluating the binding force of the chromium-plated plate and the film mainly focus on electrochemical tests, the methods are complex to operate, the adhesion parameters of the chromium-plated plate to the film cannot be quickly and effectively obtained, and particularly, the continuity of production is influenced in industrial production.
Disclosure of Invention
According to the technical problems, the invention provides a rapid, effective and accurate detection mode for evaluating the binding force between the PET film and the chromium-plated plate.
The invention uses epoxy resin to simulate a PET film to carry out a bonding force test on the surface of the chromium-plated plate. Polyethylene terephthalate (PET) is a high polymer and is obtained by the dehydration condensation reaction of the PET; epoxy resins are organic high molecular compounds containing two or more epoxy groups in the molecule, and their relative molecular masses are not high except individually. The molecular structure of the epoxy resin is characterized in that a molecular chain contains active epoxy groups, and the epoxy groups can be positioned at the tail ends, in the middle or in a ring structure. The epoxy resin and the PET film have similarity in structure, so that the invention simulates the combination of the PET film and the chromium plating plate by coating the epoxy resin on the surface of the chromium plating plate, thereby comparing the difference of the binding force of the film layers. The method is characterized in that the binding capacity of the surface of a chromium plated plate and an organic film is measured by adopting a thermal vibration test, wherein the thermal vibration is a test method after the surface of a material is treated, a test sample to be tested is heated at a certain temperature and then is cooled suddenly, and the binding force of a coating can be measured, which is caused by the deformation difference due to the different thermal expansion coefficients of a base material and the coating.
The invention adopts the following specific technical means:
a method for evaluating the binding force of a film layer on the surface of a coated iron comprises the steps of adopting epoxy resin to simulate an organic film to test the binding force of the surface of a chromium-plated plate, carrying out thermal vibration treatment on the chromium-plated plate after coating, and judging the binding force of the surface film layer of the chromium-plated plate according to the final thermal vibration frequency; the thermal vibration treatment is a primary thermal vibration treatment in which a test sample is heated and then cooled immediately.
Further, the method specifically comprises the following steps:
(1) preparing a chromium plating plate test sample plate: cutting a chromium plating plate to be detected into a sample size for later use;
(2) preparing an organic film solution: 3-6 g of epoxy resin, 0.3-0.6 ml of diluent and tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2) 1-2 g, and fully mixing for later use;
(3) film coating process: dripping 0.3-0.6 g of organic film solution droplets on each chromium plating plate by using a dropper, and standing for 10-16 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the samples in a water bath, then transferring the samples into a water bath at room temperature for cooling, wherein the process is a thermal vibration process, repeating the process for a plurality of times, recording the thermal vibration times of each sample, and recording the final thermal vibration times after the organic film falls off;
(5) comparing the thermal vibration times of different chromium-plated plates, wherein the more the thermal vibration times, the greater the binding force between the chromium-plated plate and the organic film;
(6) the binding force of the coated iron is measured based on the result of a pull-open method (national standard GB/T5210-2006, namely that the test combination of the adhesion is placed on a suitable tensile testing machine, and the tensile force required for damaging the adhesion between the coating and the substrate is measured), so that the binding force standard of the film layer and the chromium-plated plate is established:
the number of times of thermal vibration is less than 60, and the binding force is poor;
the number of thermal vibration times is 60-90 times, and the binding force is moderate;
the times of thermal vibration are more than 90 times, and the binding force is good.
Further, the epoxy resin is bisphenol A type epoxy resin or bisphenol F type epoxy resin; the diluent is polypropylene glycol diglycidyl ether, alkylene glycidyl ether, ethylene glycol diglycidyl ether or C12-14 fatty glycidyl ethers.
Further, in the step (4), the heating temperature is 45-55 ℃, and the heating time is 4-6 min.
Further, in the step (4), the cooling time is 4-6 min.
The organic film solution must be prepared at the end, and due to the addition of the curing agent, if the organic film solution is placed in the air for too long, the organic film solution is solidified into blocks, and cannot be in a liquid drop shape, and subsequent experiments cannot be carried out.
Compared with the prior art, the invention has the following advantages:
1. the invention provides an evaluation method for the binding force between the surface film layer of a chromium-plated plate and a matrix, which can accurately, quantitatively and effectively pre-judge the binding force between the surface of the chromium-plated plate and a film so as to improve the qualification rate of a film-coated product.
2. The evaluation method is simple to operate, and the bonding force difference between the chromium plating plate surfaces and the thin films of different plating solution systems and different structures can be visually seen according to the experimental result.
3. The material used by the evaluation method is environment-friendly and has little pollution to the environment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural view of a coated iron.
FIG. 2 shows the molecular structure of PET.
Fig. 3 shows the molecular structure of the epoxy resin.
FIG. 4 shows a thermal shock exfoliation panel.
FIG. 5 shows XPS analysis of the surface layer of a chromium plating plate.
Detailed Description
In the following embodiments, a steel enterprise (A, B, C, D) in China is used to produce different chromium-plated plates.
Example 1
(1) Preparing a No. 1 chromium-plated plate test sample produced by an enterprise A: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: bisphenol A epoxy resin 5.2g, polypropylene glycol diglycidyl ether (X-632)0.5ml, tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.1g, and fully mixing for later use;
(3) film coating process: dripping 0.5g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 12 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. When the organic film of the No. 1 chromium-plated plate produced by the Enterprise A fell off, the final number of times of thermal vibration was 82, as shown in FIG. 4 (a).
Example 2
(1) Preparing a No. 2 chromium-plated plate test sample produced by an enterprise B: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: bisphenol A epoxy resin 4.8g, polypropylene glycol diglycidyl ether (X-632)0.6ml, tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.6g, and fully mixing for later use;
(3) film coating process: dripping 0.5g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 13 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. When the 2# chromium plating plate produced by the B corporation had an organic film peeled off, the final number of thermal shocks was 102, as shown in fig. 4 (B).
Example 3
(1) Preparing a No. 3 chromium-plated plate test sample produced by a C enterprise: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: bisphenol A epoxy resin 5.1g, polypropylene glycol diglycidyl ether (X-632)0.5ml, tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.8g, and fully mixing for later use;
(3) film coating process: dripping 0.6g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 15 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. When the organic film of the 3# chromium-plated plate produced by the company C fell off, the final number of thermal oscillations was 112, as shown in fig. 4 (C).
Example 4
(1) Preparing a No. 4 chromium-plated plate test sample produced by an enterprise D: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: 3.5g of bisphenol A epoxy resin, polypropylene glycol dimer0.4ml of glycerol ether (X-632), tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.7g, and fully mixing for later use;
(3) film coating process: dripping 0.5g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 11 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. When the organic film of the No. 4 chromium-plated plate produced by the Enterprise D fell off, the final number of times of thermal vibration was 107, as shown in FIG. 4 (D).
The chromium plating plates used in the following examples were each a plating solution containing NH4F、H2SiF6、Na2SiF6The hot vibration test is respectively carried out on the chromium plating plates of the three plating solution systems.
Example 5
(1) Preparation of NH4F plating bath system 5# chromium plate (determination of Cr (OH) in surface layer of 5# chromium plate based on peak area of three substances fitted from XPS result of chrome plate surface in FIG. 5)3Content 33.94%) test panel: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: bisphenol A type epoxy resin 4.1g, polypropylene glycol diglycidyl ether (X-632)0.3ml, tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.1g, and fully mixing for later use;
(3) film coating process: dripping 0.4g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 13 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. NH (NH)4When the No. 5 chromium plating plate organic film of the plating solution system F is peeled off, the final number of times of thermal vibration is 91.
Example 6
(1) Preparation H2SiF6Plating bath System No. 6 chromium plating plate (surface layer Cr (OH))3Content 49.28%) test panel: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: 5.7g of bisphenol A type epoxy resin, 0.6ml of polypropylene glycol diglycidyl ether (X-632), tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.9g, and fully mixing for later use;
(3) film coating process: dripping 0.5g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 16 hours at room temperature until the organic film and the chromium plating plate are fully adhered; .
(4) The test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. H2SiF6When the No. 6 chromium plating plate organic film of the plating solution system is peeled off, the final thermal vibration frequency is 113 times.
Example 7
(1) Preparation of Na2SiF6Plating bath System No. 7 chromium plating plate (surface layer Cr (OH))3Content 38.16%) test panel: cutting a to-be-detected chromium plating plate into samples with the size of 40 multiplied by 40mm for later use;
(2) preparing an organic film solution: 5.0g of bisphenol A epoxy resin, 0.3 to 0.6ml of polypropylene glycol diglycidyl ether (X-632), and tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2)1.9g, and fully mixing for later use;
(3) film coating process: dripping 0.5g of organic film liquid drops on the chromium plating plate by using a dropper, and standing for 14 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the sample in a water bath at 50 deg.C for 5min, transferring into water bath at room temperature, cooling for 5min, and repeating the process. Na (Na)2SiF6When the No. 7 chromium plating plate organic film of the plating solution system is peeled off, the final thermal vibration frequency is 105 times.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. A method for evaluating the binding force of a film layer on the surface of a coated iron is characterized in that epoxy resin is adopted to simulate an organic film to test the binding force of the surface of a chromium plate, the chromium plate coated with a film is subjected to thermal vibration treatment, and the binding force of the film layer on the surface of the chromium plate is judged according to the final thermal vibration frequency; the thermal vibration treatment is a primary thermal vibration treatment in which a test sample is heated and then cooled immediately.
2. The evaluation method according to claim 1, specifically comprising the steps of:
(1) preparing a chromium plating plate test sample plate: cutting a chromium plating plate to be detected into a sample size for later use;
(2) preparing an organic film solution: 3-6 g of epoxy resin, 0.3-0.6 ml of diluent and tetraethylenepentamine (H)2NC2H4(NHC2H4)3NH2) 1-2 g, and fully mixing for later use;
(3) film coating process: dripping 0.3-0.6 g of organic film solution droplets on each chromium plating plate by using a dropper, and standing for 10-16 hours at room temperature until the organic film and the chromium plating plate are fully adhered;
(4) the test conditions are as follows: heating the samples in a water bath, then transferring the samples into a water bath at room temperature for cooling, wherein the process is a thermal vibration process, repeating the process for a plurality of times, recording the thermal vibration times of each sample, and recording the final thermal vibration times after the organic film falls off;
(5) comparing the thermal vibration times of different chromium-plated plates, wherein the more the thermal vibration times, the greater the binding force between the chromium-plated plate and the organic film;
(6) based on the result of measuring the binding force of the coated iron by a drawing method, the binding force standard of the film layer and the chromium plate is established:
the number of times of thermal vibration is less than 60, and the binding force is poor;
the number of thermal vibration times is 60-90 times, and the binding force is moderate;
the times of thermal vibration are more than 90 times, and the binding force is good.
3. The evaluation method according to claim 2, wherein the epoxy resin is a bisphenol a type epoxy resin or a bisphenol F type epoxy resin; the diluent is polypropylene glycol diglycidyl ether, alkylene glycidyl ether, ethylene glycol diglycidyl ether or C12-14 fatty glycidyl ethers.
4. The method according to claim 2, wherein the heating temperature in the step (4) is 45 to 55 ℃ and the heating time is 4 to 6 min.
5. The method according to claim 2, wherein the cooling time in the step (4) is 4 to 6 min.
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Application publication date: 20210528 |