CN114384002B - Method for detecting corrosion resistance of ceramic film and method for detecting quality of ceramic film - Google Patents
Method for detecting corrosion resistance of ceramic film and method for detecting quality of ceramic film Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 59
- 238000005260 corrosion Methods 0.000 title claims abstract description 39
- 230000007797 corrosion Effects 0.000 title claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 58
- 238000001514 detection method Methods 0.000 claims abstract description 49
- 239000012528 membrane Substances 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 12
- 238000007796 conventional method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 238000003279 ceramming Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 150000003608 titanium Chemical class 0.000 description 2
- 150000003754 zirconium Chemical class 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- General Physics & Mathematics (AREA)
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Molecular Biology (AREA)
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- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention belongs to the field of surface treatment, and particularly relates to a method for detecting corrosion resistance of a ceramic film, which comprises the following steps: the detection liquid is dripped on the surface of the standard ceramic film and simultaneously started for timing, when small bubbles are densely distributed in the liquid drops, the timing is finished, and the time is recorded as t 0 The method comprises the steps of carrying out a first treatment on the surface of the The method comprises the steps of dripping detection liquid on the surface of a ceramic film to be detected, starting timing at the same time, ending timing when small bubbles are densely distributed in the liquid drops, and recording the time as t; if t is greater than or equal to t 0 The corrosion resistance of the ceramic film to be tested meets the standard, otherwise, the ceramic film to be tested does not meet the standard; wherein the detection liquid comprises hydrochloric acid solution and potassium dichromate. The invention also relates to a method for detecting the quality of the ceramic membrane. The method has simple operation, can rapidly and accurately detect the corrosion resistance of the ceramic film, and has good repeatability.
Description
Technical Field
The invention belongs to the field of surface treatment, and particularly relates to a method for detecting corrosion resistance of a ceramic film and a method for detecting quality of the ceramic film.
Background
The ceramic process is used as a surface treatment process and has the advantages of environmental protection, energy conservation, high efficiency and the like. Compared with the phosphating process, the ceramming process omits the surface and passivation procedures, shortens the process flow, reduces the equipment quantity and is gradually and widely used. The ceramic process mainly uses titanium salt or zirconium salt as a main agent, and the ceramic process in the engineering machinery industry generally uses steel as a base material. The principle of the ceramic technology is as follows: the titanium salt or zirconium salt is subjected to hydrolysis reaction on the surface of the substrate and is combined with the substrate to form a compact ceramic film, and the ceramic film has strong barrier property and good adhesive force to subsequent organic coatings.
The quality of the ceramic film is generally judged by controlling the quality of the ceramic liquid or according to the color of the ceramic film. However, the quality of the ceramming solution cannot reflect the influence of the process operation on the quality of the ceramming film; the ceramic film is usually colorless or metallic, and is not easily distinguished from the color of the base material, so that the quality of the ceramic film is difficult to evaluate accurately according to the color. Moreover, the thickness of ceramic films is typically only a few hundred nanometers, which is difficult to measure accurately. Therefore, the quality of the ceramic film cannot be directly judged at the present stage.
The corrosion resistance is an important quality index of the ceramic film, and the quality of the ceramic film can be substantially reflected by detecting the corrosion resistance of the ceramic film. At present, the method for detecting the corrosion resistance of the ceramic film is to plate the ceramic film, then soak the ceramic film in sodium chloride solution for a long time, and then observe the surface state of the ceramic film. However, the method has long detection time and complicated operation steps, and cannot meet the requirements of rapid inspection of industrial products.
Disclosure of Invention
The invention aims to provide a method for detecting the corrosion resistance of a ceramic film, which has the advantages of simple operation, short detection time and high efficiency, and can accurately detect whether the corrosion resistance of the ceramic film meets the standard or not, and the method has good repeatability, so that whether the quality of the ceramic film meets the standard or not can be accurately detected. On the basis, the invention further aims to provide a method for detecting the quality of the ceramic membrane.
To achieve the above object, one aspect of the present invention relates to a method for detecting corrosion resistance of a ceramic film, comprising the steps of:
the detection liquid is dripped on the surface of the standard ceramic film, the timing is started at the same time, and when the liquid drop (of the detection liquid) is full of small bubbles, the timing is ended, and the time is recorded as t 0 ；
The method comprises the steps of dripping detection liquid on the surface of a ceramic film to be detected, starting timing at the same time, ending timing when small bubbles are distributed in the liquid drops (of the detection liquid), and recording the time as t;
if t is greater than or equal to t 0 The corrosion resistance of the ceramic film to be tested meets the standard, otherwise, the ceramic film to be tested does not meet the standard;
wherein the detection solution comprises hydrochloric acid (water) solution and potassium dichromate.
The inventors of the present invention surprisingly found that: the detection liquid can penetrate through the pores of the ceramic membrane and react with the base material to generate gas; the denser the ceramic film is, the stronger the corrosion resistance is, and the less the detection liquid is likely to penetrate through the pores of the ceramic film to react with the substrate; therefore, the method can rapidly and accurately detect the corrosion resistance of the ceramic film.
In some embodiments of the present invention, the mass ratio of HCl to potassium dichromate in the detection solution is 5:1 to 20:1 (preferably 8:1 to 16:1, more preferably 9:1 to 13:1, for example 10:1, 11:1, 12:1, 15:1), wherein HCl is a hydrogen chloride substance in the hydrochloric acid solution.
In some embodiments of the invention, the concentration of the hydrochloric acid solution in the detection solution is 30% W/W to 40% W/W, preferably 36% W/W to 38% W/W.
In some embodiments of the invention, the detection liquid further comprises water; preferably, the volume of water is 1 to 5 times, for example 3 times, the volume of the hydrochloric acid solution.
In some embodiments of the invention, at least one drop, preferably one drop, of detection liquid is dropped onto the surface of the standard ceramic membrane and/or the ceramic membrane to be tested.
In some embodiments of the invention, the detection liquid forms a droplet area of 0.8-3 cm on the surface of the standard ceramic membrane and/or the ceramic membrane to be detected 2 Preferably 1 to 2cm 2 For example about 1.77cm 2 。
In some embodiments of the invention, the detection liquid forms droplets having a diameter of 1 to 2cm, for example about 1.5cm, on the surface of the standard ceramic membrane and/or the ceramic membrane to be tested.
In some embodiments of the invention, the standard ceramic film is a ceramic film having a corrosion resistance that meets standards.
In some embodiments of the invention, the standard ceramic film meets the corrosion resistance standard as detected by conventional methods. Conventional methods for detecting corrosion resistance of ceramic films are well known to those skilled in the art and include, but are not limited to, the following methods: and (3) soaking the ceramic film plate in sodium chloride solution for a long time, taking out, and observing whether the surface of the sample is corroded, if not, reaching the standard.
In some embodiments of the present invention, from the start of the timing, the droplets of the detection liquid on the surface of the standard ceramic film and/or the ceramic film to be detected sequentially undergo an initial state, a state in which small bubbles appear at the edges of the droplets, a state in which a small number of small bubbles appear in the middle of the droplets, a state in which small bubbles are densely distributed in the droplets, a state in which large bubbles are densely distributed in the droplets, and a state in which large bubbles are densely distributed in the droplets and the droplets are green over time.
In some embodiments of the present invention, six states that the droplets of the detection liquid on the surface of the standard ceramic membrane and/or the ceramic membrane to be measured sequentially go through with time from the start timing are shown in fig. 1 to 6.
In some embodiments of the invention, the middle of the droplet is yellow and the edges are green, except in the initial state and in the rest of the states in which large bubbles are densely packed within the droplet and the droplet is green.
In some embodiments of the present invention, the state of dense large bubbles within the droplets is larger than the green edge area of the droplets in the other three states, except the initial state and the state in which the dense large bubbles within the droplets are dense and the droplets are green.
In some embodiments of the invention, in a state where a small number of small bubbles appear in the middle of the droplet, the edges of the droplet still have (small) bubbles.
In some embodiments of the present invention, the volume of the bubbles is greater in a state where large bubbles are densely packed in the liquid droplets and the liquid droplets are green than in a state where large bubbles are densely packed in the liquid droplets.
In some embodiments of the invention, the substrate of the ceramic membrane comprises a reducing metal.
In some embodiments of the invention, the substrate comprises at least one selected from the group consisting of steel and aluminum alloys.
In a further aspect the invention provides a method of detecting the quality of a ceramic film comprising the step of detecting the corrosion resistance of a ceramic film according to the method of the first aspect of the invention.
The invention has the beneficial effects that:
1. the method disclosed by the invention is simple to operate, can be used for rapidly detecting the corrosion resistance of the ceramic film, and is accurate in detection result and good in method repeatability.
2. The method can accurately detect the quality of the ceramic film.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings, in which
FIG. 1 is an initial state of droplets of a detection liquid for the surface of a ceramic membrane in example 1;
FIG. 2 shows a state in which small bubbles appear at the edge of a droplet of the detection liquid on the surface of the ceramic film in example 1;
FIG. 3 is a diagram showing a state in which a small amount of small bubbles appear in the middle of the droplet of the detection liquid on the surface of the ceramic film in example 1;
FIG. 4 shows a state in which small bubbles are densely distributed in droplets of the detection liquid for the surface of the ceramic film in example 1;
FIG. 5 shows a state in which large bubbles are densely packed in droplets of the detection liquid for the surface of the ceramic membrane in example 1;
FIG. 6 shows a state in which large bubbles are densely distributed in droplets of the detection liquid for the surface of the ceramic film in example 1 and the droplets are green.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which it is shown, however, that the examples are shown, and in which the invention is practiced. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1 method for detecting Corrosion resistance of ceramic film
(1) 25ml of 36% W/W-38% W/W HCl solution (containing 29.5g of HCL), 3g of potassium dichromate and 75ml of distilled water were uniformly mixed to obtain a detection solution.
(2) Preparing standard ceramic film with standard corrosion resistance detected by conventional method, dropping the detection liquid on the surface of the standard ceramic film, and simultaneously starting timing, wherein the area of the liquid drop formed on the standard ceramic film is about 1.77cm 2 (about 1.5cm in diameter). From the beginning of the timing, the drops of the detection liquid on the surface of the standard ceramic membrane appear in the following 6 states (as shown in fig. 1-6) in sequence with the time: in the initial state, small bubbles appear at the edge of the liquid drop, a small amount of small bubbles appear in the middle of the liquid drop, small bubbles are densely distributed in the liquid drop, and the liquid drop is densely distributedLarge bubbles are distributed, large bubbles are densely distributed in the liquid drops, and the liquid drops are green. Taking the state of dense small bubbles in the liquid drop as a timing end point, and recording the elapsed time as t 0 。
(3) Dropping one drop of the detection liquid on the surface of the ceramic film to be detected, starting timing at the same time, and forming a drop area of about 1.77cm on the ceramic film to be detected 2 (about 1.5cm in diameter). From the beginning of the timing, the time is prolonged, and the liquid drops of the detection liquid on the surface of the ceramic film to be detected also appear in 6 states in the (2) in sequence. The time elapsed is denoted by t, with the state of dense small bubbles in the droplets being the end point of the time counting. When t is greater than or equal to t 0 The corrosion resistance of the ceramic film to be tested meets the standard, otherwise the corrosion resistance of the ceramic film to be tested does not meet the standard.
Example 2 accuracy and repeatability
Conventional methods for detecting corrosion resistance of ceramic films: and (3) immersing the ceramic membrane in an aqueous solution of NaCl with the mass fraction of 3.5% for 1 hour, taking out, and observing if the surface of the ceramic membrane is rust-free, wherein the corrosion resistance of the ceramic membrane is proved to reach the standard, or else the corrosion resistance of the ceramic membrane is not reached.
The corrosion resistance of the ceramic film obtained on a certain ceramic film production line, which is detected by the conventional method, reaches the standard, and is used as a standard ceramic film. T of the Standard ceramic film was measured as in example 1 0 30s.
And taking the ceramic films 1-10 to be detected on the production line, and detecting the corrosion resistance of the ceramic films to be detected according to the conventional method and the method of the embodiment 1, wherein the detection result is the same as that of the conventional method, and the detection result is considered to be accurate. The experiment was repeated three times.
(1) The accuracy of the example 1 detection method in three experiments was calculated according to the following formula.
Wherein A is 1 The number of samples with accurate detection results in the method of example 1 in each experiment is shown, and A represents the total number of samples detected in the method of example 1 in each experiment.
(2) All samples from three experiments were calculated as% study variation (% SV) by the method of example 1 using Minitab software. The industry generally considers that the% research variation (% SV) is less than 10%, which shows that the repeatability of the detection method is good and meets the practical application requirement.
The results are shown in Table 1.
TABLE 1 Corrosion resistance results and accuracy for the conventional method and the example 1 method
The% study variation (% SV) resulted in 7.25%.
The data show that the method can rapidly detect the corrosion resistance of the ceramic film, has accurate detection result and good repeatability, and can meet the practical application requirements of the industry.
Comparative example 1
The detection method is different from that of example 1: taking the state that a small amount of small bubbles appear in the middle of the liquid drop as a timing end point to obtain t 0 And t.
The t of the standard ceramic membrane of example 2 was determined by the method described above 0 =20s the corrosion resistance of the ceramic films 1 to 10 to be tested in example 2 was examined according to the method described above.
The accuracy of the detection method of comparative example 1 was calculated with reference to the formula in example 2.
The results are shown in Table 2.
TABLE 2 Corrosion resistance results and accuracy for the conventional method and the comparative example 1 method
Comparative example 2
The detection method is different from that of example 1: taking a state that large bubbles are densely distributed in the liquid drops and the liquid drops are green as a timing end point to obtain t 0 And t.
The t of the standard ceramic membrane of example 2 was determined by the method described above 0 =62 s, the corrosion resistance of the ceramic films 1 to 10 to be tested in example 2 was examined according to the method described above.
The accuracy of the detection method of comparative example 2 was calculated with reference to the formula in example 2.
The results are shown in Table 3.
TABLE 3 Corrosion resistance results and accuracy for the conventional method and the comparative example 2 method
As can be seen in connection with tables 1-3, the accuracy of the methods of comparative examples 1-2 is significantly lower than the methods of the present invention. The accuracy of the methods of comparative examples 1-2 cannot meet the requirements of practical applications.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A method for detecting corrosion resistance of a ceramic film comprising the steps of:
the detection liquid is dripped on the surface of the standard ceramic film and the timing is started at the same time, when the liquid drops are densely distributed with small bubbles, the middle part of the liquid drops is yellow, the edge of the liquid drops is green, the timing is ended, and the time is recorded as t 0 ；
The method comprises the steps of dripping detection liquid on the surface of a ceramic film to be detected, starting timing at the same time, ending timing when small bubbles are densely distributed in the liquid drops, the middle part of the liquid drops is yellow, the edges of the liquid drops are green, and recording time as t;
if t is greater than or equal to t 0 The corrosion resistance of the ceramic film to be tested meets the standard, otherwise, the ceramic film to be tested does not meet the standard;
wherein the detection liquid comprises hydrochloric acid solution and potassium dichromate.
2. The method of claim 1, wherein at least one drop of detection liquid is dropped onto the surface of the standard ceramic membrane and/or the ceramic membrane to be tested.
3. The method according to claim 1, wherein one drop of detection liquid is dropped onto the surface of the standard ceramic membrane and/or the ceramic membrane to be tested.
4. The method according to claim 1, wherein the detection liquid forms a droplet area of 0.8 to 3cm on the surface of the standard ceramic film and/or the ceramic film to be measured 2 。
5. The method of claim 1, wherein the standard ceramic film is a corrosion resistant ceramic film.
6. The method according to claim 1, wherein from the start of the timing, the droplets of the detection liquid on the surface of the standard ceramic film and/or the ceramic film to be detected sequentially undergo an initial state, a state in which small bubbles appear at the edges of the droplets, a state in which small bubbles appear in the middle of the droplets, a state in which small bubbles are densely distributed in the droplets, a state in which large bubbles are densely distributed in the droplets, and a state in which large bubbles are densely distributed in the droplets and the droplets are green over time.
7. The method according to claim 6, wherein the middle part of the droplet is yellow and the edge is green, among a state in which small bubbles appear at the edge of the droplet, a state in which a small amount of small bubbles appear at the middle part of the droplet, and a state in which large bubbles are densely distributed in the droplet.
8. The method of claim 1, wherein the substrate of the ceramic film comprises a reducing metal.
9. The method of claim 1, wherein the substrate of the ceramic film comprises at least one selected from the group consisting of steel and aluminum alloys.
10. A method of detecting the quality of a ceramic film comprising the step of detecting the corrosion resistance of the ceramic film according to the method of any one of claims 1 to 9.
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| KR101886054B1 (en) * | 2016-08-23 | 2018-08-07 | 주식회사 한국화학 | Ceramic nano-coating agent for metal surface having improved corrosion resistance and the metal surface treating method using the same |
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