CN109490193A - A kind of binding force evaluation method of chrome plating surface coating - Google Patents
A kind of binding force evaluation method of chrome plating surface coating Download PDFInfo
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- CN109490193A CN109490193A CN201811426952.4A CN201811426952A CN109490193A CN 109490193 A CN109490193 A CN 109490193A CN 201811426952 A CN201811426952 A CN 201811426952A CN 109490193 A CN109490193 A CN 109490193A
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- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
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Abstract
The invention discloses a kind of binding force evaluation methods of chrome plating surface coating.Step is boric acid-borate buffer solution that (1) configuration pH is 8~9, (2) in electrochemical workstation, Mott-Schottky curve test is carried out using three-electrode system different chrome platings identical to size, (3) according to Mott-Schottky equation formulations, the ratio N of charge carrier density and receptor and donor is calculateda/Nd.(4) to using cross-hatching to be combined power test after different chrome plating surface coatings, work as Na/NdGood bonding strength when > 1, between chromium plating plate surface and film；Work as Na/NdWhen < 1, the binding force between chromium plating plate surface and film is poor.This method can effectively prejudge the binding force between chromium plating plate surface and film, provide foundation for the improvement production of film-covered iron.It is easy to operate, error is small, can characterize the binding force otherness between different chromium plating plate surfaces and film, the qualification rate of overlay film iron product can be improved, there is important practical significance to the expansion of film-covered iron application.
Description
Technical field
The present invention relates to the production control technologies of film-covered iron, are related to a kind of binding force evaluation side of chrome plating surface coating
Method.Binding force between chromium plating plate surface and film is related with chromium plating plate surface film of chromium oxide, is aoxidized with chromium plating plate surface chromium
The semiconductor property of object film evaluates the binding force between chromium plating plate surface and film.
Technical background
Film-covered iron is that (also referred to as chrome plating refers to and carries out at electrolytic chromate in surface of steel plate in cold-reduced sheet/tin free steel sheet
Reason makes surface of steel plate deposit 50~100mg/m2Metallic chromium layer and 5~20mg/m2The steel of chromium aqua oxidation nitride layer) two sides covering
Multilayer polyester laminated film (thickness is about 20-25 μm) in bonding has plastic film and sheet metal dual characteristics concurrently for one kind
Metallic Functional Materials, structure is as shown in Figure 1.Film-covered iron has excellent corrosion resistance, rustless property, and manufacturing process
And process cleaning, efficient, low energy consumption, low volatilization, environmentally protective etc., therefore, film-covered iron is widely used in DRD punching press tank, DI punching
The packaging materials such as the two-piece cans such as cupping, irregular can, easy-open end and Easy tearing lid field.Film-covered iron structure chart as shown in Figure 1.
By the difference of production technology, film-covered iron can be divided into melting film-covered iron and bonding film-covered iron.Bonding film-covered iron needs make
With binder, there are deviations for deficiency and package development in environmental-friendly and moulding process, are just gradually melted film-covered iron
Replace.So-called melting film-covered iron is exactly using the technologies such as high temperature overlay film and chilling recrystallization, in certain temperature range, by one
Fixed proportion rolls special, dedicated polyester film a kind of novel multiple on cold-reduced sheet (tin plate or chrome plating TFS)
Condensation material.Melting overlay film iron substrate can be divided into cold-reduced sheet (or other metal plates) and chromium plating steel plate (or other coating plates).
Film-covered iron using the thin steel substrate of cold rolling is known as film-covered iron of leaving a blank, and since can body commissure is also easy to produce corrosion, and bonding force is loosely,
Therefore making substrate using chrome plating (TFS) becomes the mainstream developed at present, and Europe, the United States, the various countries Deng film-covered iron technology are all made of plating
Chromium plate (TFS) makees substrate, and should not referred to as leave a blank film-covered iron.
For film-covered iron in addition to substrate, required important materials are macromolecule membrane, and performance had both been needed with thermoplasticity fitting
Ability, it is compatible from the physicochemical property of different canned contents again, to ensure that it checks plating chrome substrate and the good of content；
Meanwhile the original local flavor of packaging food must be kept in the shelf life of canned various contents, in food high temperature cooking disinfection
It is non-discolouring and fall off in the process, to keep high airtightness；During jug forming processed, it is amenable to high temperature, high frictional force and curved
The effect of the composite forces such as song has preferable adhesive force.The common film of film-covered iron is mostly PP (polypropylene) and PET at present
(polyethylene terephthalate).
At present film-covered iron at China in the starting stage, have it is domestic it is fastest, specification is most thin, the most advanced chromium plating of technique
The Co., Ltd, Baogang Stocks Trading Co., Bao Wu group of plate special production line is substrate using high temperature, high-pressure extrusion technique using chrome plating
Film-covered iron production line is in the heat run debugging stage, during which exposes more quality problems, wherein organic film and chrome plating table
It is loosely exactly a major issue that face, which combines,.
Binding force between substrate and film depends on the physicochemical properties on their surfaces.In thin polymer film or paint table
There are some polar bonds or polarizable functional groups, such as-C ≡ N ,-C-O-H ,-C=O ,-C-OOH in face, they have acid-base property, are
Realize the basis of good combination between substrate and film.In addition, there is the donor with acid-base property on substrate surface thin oxide film
Or receptor, surface have chemical inhomogeneity and different oxide semiconductor property, these semiconductor properties and substrate are thin
Binding force between film also has very big relationship.Chrome plating sectional schematic diagram as shown in Figure 2, chrome plating is generally by substrate, metal
Layers of chrome, film of chromium oxide and 4 layers of oil film composition.Film of chromium oxide is extremely important for the performance of product, different chrome platings
Surface, chromated oxide membrane structure, property are different, also different from functionalization PET film combining form, so as to cause the presence of its binding force
Notable difference.Some researches show that realize partly leading for surface oxide film by increasing chromium passivation film on tin plate surface
Volume property transformation, to improve paint film adhesion, i.e. the semiconductor property of the pairs of material surface of the group of chromium influences very big.Chromium plating
The main component of plate surface film of chromium oxide is CrOOH, Cr (OH)3、Cr2O3, the XPS fitting of chromium plating plate surface film of chromium oxide
Curve is as shown in Figure 3.Due to the difference of process conditions, constituent and ratio be will be different, same its surface chromium oxidation
Object film semiconductor property also can be different.Therefore, the Mott- of the different chromium plating plate surface film of chromium oxide of test can be passed through
Schottky curve determines the semiconductor type of its surface film of chromium oxide, calculates and carries further according to Mott-Schottky equation
Sub- density and receptor/donor are flowed, and then evaluates the binding force between chrome plating and film.Fig. 3 chromium plating plate surface film of chromium oxide
XPS matched curve.
Summary of the invention
The present invention provides the binding force evaluation method between a kind of chromium plating plate surface and film, in process of production hair in time
Existing substandard product simultaneously takes treatment measures, to reduce the disqualification rate of product, controls the production of film-covered iron, improves its product
The market competitiveness has important practical significance.
A kind of binding force evaluation method of chrome plating surface coating of the invention, includes the following steps:
1) boric acid solution is mixed with borax soln with certain volume ratio, and suitable sodium citrate or compound phosphorus is added
Hydrochlorate obtains boric acid-borate buffer solution that pH is 8~9, and the Mott-Schottky as chromium plating plate surface film of chromium oxide is bent
Line tests solution.
2) prepare chrome plating test sample: the sample that different chrome platings is cut into same size is stand-by.
3) experimental condition: using CHI660B electrochemical workstation, is ginseng with saturated calomel electrode using three-electrode system
Than electrode, chrome plating sample is working electrode, and graphite is to electrode.Test parameters are as follows: voltage -1.0~1.0V, amplitude 5~
10mV, 1~5kHz of frequency.
4) according to the data and following Mott-Schottky equation (1) measured, it is close data processing: to calculate electric charge carrier
Degree and Na/Nd(receptor/donor).
5) power test is combined using cross-hatching to after different chrome plating surface coatings.When oxidation film is presented significantly
P-type semiconductor property (Na/Nd> 1) good bonding strength when, between chromium plating plate surface and film；When oxidation film is presented significantly
N-type semiconductor property (Na/Nd< 1) when, the binding force between chromium plating plate surface and film is poor；Na/NdIt is worth bigger, chrome plating
Binding force between surface and film is better.
The boric acid solution: it weighs boric acid in the balance and (analyzes pure H3BO3) be added in beaker, after deionized water dissolving, turn
It moves on in 1000ml volumetric flask, and adds deionized water constant volume, being made into concentration is 0.1~0.3molL-1Boric acid solution.
The borax soln: it weighs borax in the balance and (analyzes pure Na2B4O7·10H2O it) is added in beaker, uses deionized water
It after dissolution, is transferred in 1000ml volumetric flask, and adds deionized water constant volume, being made into concentration is 0.02~0.06molL-1Boron
Sand solution.
Method of the invention can effectively prejudge the binding force between chromium plating plate surface and film, be that the improvement of film-covered iron produces
Provide foundation.This method is easy to operate, error is small, can characterize the binding force difference between different chromium plating plate surfaces and film
Property, the qualification rate of overlay film iron product can be improved, there is important practical significance to the expansion application of film-covered iron.
Detailed description of the invention
Fig. 1 is film-covered iron structure chart.
Fig. 2 is chrome plating sectional schematic diagram.
Fig. 3 is the XPS matched curve of chromium plating plate surface film of chromium oxide.
Fig. 4 is 1#, two kinds of chromium plating plate surface Mott-Schottky curves of 2#.
Fig. 5 is 3#, two kinds of chromium plating plate surface Mott-Schottky curves of 4#.
Specific embodiment
Embodiment 1
Two kinds of chrome platings for taking different manufacturers to produce, the Mott-Schottky for testing its surface film of chromium oxide respectively are bent
Line, and utilize its charge carrier density of Mott-Schottky equation calculation and Na/Nd。
(1) match preparing boric acid-borate buffer solution.The concentration for preparing boric acid solution is 0.1~0.3molL-1, borax soln
Concentration is 0.02~0.06molL-1, sodium citrate or composite phosphate (sodium tripolyphosphate, sodium pyrophosphate, calgon)
Concentration be 0.1~0.2molL-1, prepared boric acid solution is mixed with borax soln with certain volume ratio, and is added suitable
The sodium citrate or composite phosphate of amount obtain boric acid-borate buffer solution that pH is 8~9, as chromium plating plate surface chromated oxide
The Mott-Schottky curve test solution of film.
(2) prepare chrome plating test sample.Two different chrome platings (1#, 2#) are cut into the sample of same size.
(3) experimental condition.It is to join with saturated calomel electrode using three-electrode system using CHI660B electrochemical workstation
Than electrode, chrome plating sample is working electrode, and graphite is to electrode.In voltage -1.0~1.0V, 5~10mV of amplitude, frequency 1~
The Mott-Schottky curve of two kinds of chromium plating plate surface film of chromium oxide is tested under 5kHz respectively.
(4) data processing.According to the data and following Mott-Schottky equation measured, it is close to calculate electric charge carrier
Degree and Na/Nd(receptor/donor).
(5) power test is combined using cross-hatching to after two kinds of chrome plating surface coatings.As a result, it has been found that Na/NdValue and knot
It is corresponding, N between resultant forcea/NdIt is worth biggish 1# chrome plating, the good bonding strength between chromium plating plate surface and film.Fig. 4
Two kinds of chromium plating plate surface Mott-Schottky curves of 1#, 2#
Embodiment 2
Two kinds of chrome platings of identical producer's production are taken, the Mott-Schottky for testing its surface film of chromium oxide respectively is bent
Line, and utilize its charge carrier density of Mott-Schottky equation calculation and Na/Nd。
(1) match preparing boric acid-borate buffer solution.The concentration for preparing boric acid solution is 0.1~0.3molL-1, borax soln
Concentration is 0.02~0.06molL-1, sodium citrate or composite phosphate (sodium tripolyphosphate, sodium pyrophosphate, calgon)
Concentration be 0.1~0.2molL-1, prepared boric acid solution is mixed with borax soln with certain volume ratio, and is added
Proper amount of sodium citrate or composite phosphate obtain boric acid-borate buffer solution that pH is 8~9, as chromium plating plate surface chromated oxide
The Mott-Schottky curve test solution of film.
(2) prepare test sample.Two different chrome platings (3#, 4#) are cut into same size sample.
(3) experimental condition.It is to join with saturated calomel electrode using three-electrode system using CHI660B electrochemical workstation
Than electrode, chrome plating sample is working electrode, and graphite is to electrode.In voltage -1.0~1.0V, 5~10mV of amplitude, frequency 1~
The Mott-Schottky curve of two kinds of chromium plating plate surface film of chromium oxide is tested under 5kHz respectively.
(4) data processing.According to the data and following Mott-Schottky equation measured, it is close to calculate electric charge carrier
Degree and Na/Nd(receptor/donor).
(5) power test, N are combined using cross-hatching to after two kinds of chrome plating surface coatingsa/NdBetween value and binding force
It is corresponding.As a result, it has been found that Na/NdValue differs lesser two kinds of chrome platings, the binding force between chromium plating plate surface and film
It differs smaller.Two kinds of plates are compared, Na/NdIt is slightly good to be worth slightly larger 3# chrome plating binding force.But compared with 1#, 2#, two kinds of 3#, 4# platings
Binding force between chromium plate surface and film is substantially reduced.Therefore, work as Na/NdCombination when > 1, between chromium plating plate surface and film
Power is preferable；Work as Na/NdWhen < 1, the binding force between chromium plating plate surface and film is poor；Na/NdBe worth it is bigger, chromium plating plate surface with it is thin
Binding force between film is better.Two kinds of chromium plating plate surface Mott-Schottky curves of Fig. 5 3#, 4#.
Claims (5)
1. a kind of binding force evaluation method of chrome plating surface coating, which is characterized in that steps are as follows:
(1) boric acid solution is mixed with borax soln, and sodium citrate or composite phosphate is added, and obtains the boric acid-that pH is 8~9
Borate buffer solution, the Mott-Schottky curve test solution as chromium plating plate surface film of chromium oxide；
(2) CHI660B electrochemical workstation is used, using three-electrode system, using saturated calomel electrode as reference electrode, chrome plating
Sample is working electrode, and graphite is to electrode；Mott- is carried out using three-electrode system different chrome platings identical to size
Schottky curve test；
(3) data measured by step (2), according to following Mott-Schottky equation formulations, calculate charge carrier density and
The ratio of receptor and donor
(4) to using cross-hatching to be combined power test after different chrome plating surface coatings, according to Na/NdValue with binding force it
Between corresponding relationship evaluated, when significant p-type semiconductor property N is presented in oxidation filma/NdWhen > 1, chromium plating plate surface with it is thin
Binding force between film is good；When significant n-type semiconductor property N is presented in oxidation filma/NdWhen < 1, chromium plating plate surface and film it
Between binding force it is poor；Na/NdValue is bigger, and the binding force between chromium plating plate surface and film is better.
2. binding force evaluation method according to claim 1, which is characterized in that boric acid-boron described in the step (1)
It is 0.1~0.3molL that sand buffer, which is by concentration,-1Boric acid solution and concentration are 0.02~0.06molL-1Borax soln is mixed
The concentration closed, and be added is 0.1~0.2molL-1Sodium citrate or 0.1~0.2molL-1Composite phosphate, allotment and
At.
3. binding force evaluation method according to claim 1 or 2, which is characterized in that described step (2) three-electrode system
It is using saturated calomel electrode as reference electrode, chrome plating sample is working electrode, and graphite is to electrode.
4. a kind of binding force evaluation method of chrome plating surface coating according to claim 1 or 2, which is characterized in that institute
The step of stating (2) test parameters are as follows: voltage -1.0~1.0V, 5~10mV of amplitude, 1~5kHz of frequency.
5. a kind of binding force evaluation method of chrome plating surface coating according to claim 3, which is characterized in that described
Step (2) test parameters are as follows: voltage -1.0~1.0V, 5~10mV of amplitude, 1~5kHz of frequency.
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Cited By (1)
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| CN111141797A (en) * | 2019-12-25 | 2020-05-12 | 东北大学 | Method for evaluating surface passivation film characteristics of tin plate based on semiconductor properties |
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