CN113624937B - Method for detecting fish scaling resistance of hot-rolled pickled enameled steel plate - Google Patents

Method for detecting fish scaling resistance of hot-rolled pickled enameled steel plate Download PDF

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CN113624937B
CN113624937B CN202010370908.7A CN202010370908A CN113624937B CN 113624937 B CN113624937 B CN 113624937B CN 202010370908 A CN202010370908 A CN 202010370908A CN 113624937 B CN113624937 B CN 113624937B
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刘欣
陶翀
刘友荣
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Shanghai Meishan Iron and Steel Co Ltd
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Abstract

The invention discloses a method for detecting the fish scaling resistance of a hot-rolled acid-washed enameled pressed steel, which mainly solves the technical problem that the fish scaling resistance of the existing hot-rolled acid-washed enameled pressed steel cannot be accurately detected. The invention discloses a method for detecting the fish scaling resistance of a hot-rolled pickled enameled pressed steel, which comprises the following steps: 1) preparing a sample; 2) coating an enamel glaze on a sample by a wet coating method, coating a colloidal enamel glaze on the surface of the sample, wherein the thickness of the colloidal enamel glaze coated on each pass is 0.05-0.10 mm, and the thickness of one side surface of the sample and the thickness of four cross-section enamel glaze layers are controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm; 3) carrying out enamel firing treatment on the sample; 4) and evaluating the fish scaling resistance of the hot-rolled pickled enameled steel plate. The method has the advantages of high detection efficiency, high detection precision and low detection cost.

Description

Method for detecting fish scaling resistance of hot-rolled pickled enameled steel plate
Technical Field
The invention relates to a method for detecting the performance of a hot-rolled pickled enameled pressed steel, in particular to a method for detecting the fish scaling resistance of a hot-rolled pickled enameled pressed steel, and belongs to the field of testing the performance of steel materials.
Background
Enamel has the advantages of easy cleaning, corrosion resistance, environmental protection and the like, and is widely applied to the aspects of light industry, household appliances, building engineering, metallurgy, chemical industry and the like, and has the figure of enamel from kitchen utensils, sanitary ware, barbecue ovens to water heater inner containers, subway decoration panels and chemical reaction tanks.
The steel sheet for enamel may be classified into hot-rolled acid-washed enamel steel, cold-rolled enamel steel and clad enamel steel according to the production process. Among them, the hot-rolled pickled plate has high strength before and after the enameling firing, good formability and good enameling performance, and is recently widely used in the aspects of water heater inner containers and the like, and is expanded to other uses such as heat exchangers and the like.
One of the important defects of the enameled steel after being enameled is the scale explosion, the scale explosion is mainly caused by that hydrogen is gathered between an enamel layer and a steel plate, pressure is generated, the pressure is gradually increased, and finally the hydrogen breaks through the enamel layer to cause the rupture of the enamel layer; in order to ensure the product quality, the scale explosion sensitivity performance of the enameled hot-rolled pickled steel plate needs to be accurately detected.
GB/T29515-.
No. CN202649161U discloses a testing device for the anti-fishscaling performance of a cold-rolled steel plate, which evaluates the anti-fishscaling performance of the cold-rolled steel plate by testing the hydrogen storage capacity of the steel plate.
Patent application publication No. CN103210103A discloses a surface defect-free enameled steel sheet and a manufacturing method thereof, which improves enameling properties by eliminating surface defects of the steel sheet.
The prior art lacks a method for quickly and accurately detecting the fish scaling resistance of a hot-rolled acid-washed enameled pressed steel.
Disclosure of Invention
The invention aims to provide a method for detecting the fish-scale explosion resistance of a hot-rolled pickled enameled pressed steel, which mainly solves the technical problem that the fish-scale explosion resistance of the existing hot-rolled pickled enameled pressed steel cannot be accurately detected.
The technical scheme adopted by the invention is that the method for detecting the fish scaling resistance of the hot-rolled pickled enameled pressed steel comprises the following steps:
1) preparing a sample, namely cutting a rectangular sample from a hot-rolled acid-washed enameled steel plate for enamel to be detected, wherein the length of the sample is 100-200 mm, the width of the sample is 50-100 mm, and the thickness of the sample is 1.80-4.00 mm; degreasing and cleaning the surface of the sample;
2) coating an enamel glaze on a sample by a wet coating method, and preparing colloidal enamel glaze from enamel glaze dry powder by deionized water, wherein the mass ratio of the enamel glaze dry powder to the deionized water in the colloidal enamel glaze is 200: 50-200: 80; coating colloidal enamel glaze on the surface of a sample, wherein the thickness of the colloidal enamel glaze coated on each pass is 0.05-0.10 mm, and the thickness of one side surface and four cross-section enamel glaze layers of the sample is controlled to be 0.30-0.35 mm, namely the thickness of the sample reference surface enamel glaze layer is controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm, namely controlling the thickness of the enamel glaze layer on the observation surface of the sample to be 0.10-0.20 mm;
3) carrying out enamel firing treatment on the sample, and firstly, slowly heating the sample coated with enamel glaze from 15-25 ℃ to 100-150 ℃ at a heating speed of 5-10 ℃/min to ensure that the sample is dried; carrying out high-temperature enameling on the sample at 800-860 ℃ for 5-10 min to generate an enamel layer; air cooling the sample to 15-25 ℃;
4) evaluating the scale explosion resistance of the hot-rolled pickled enameled steel plate, observing the observation surface of the sample after the enameling firing is finished for 8-24 hours, and if no scale explosion occurs on the observation surface of the sample, the scale explosion resistance of the hot-rolled pickled enameled steel plate is qualified; and conversely, if scale explosion occurs on the observation surface of the sample, the scale explosion resistance of the hot-rolled and pickled enameled steel plate is unqualified.
Further, the preferable scheme of the invention is that the surface cleanliness of the sample in the step 1) is controlled to be more than or equal to 90%.
Further, the preferred scheme of the invention is that the enamel glaze dry powder is sieved by a 300-mesh screen.
The invention discloses a method for detecting the fish scaling resistance of a hot-rolled pickled enameled pressed steel, which is based on the following research of an applicant:
enamel scaling is mainly due to hydrogen accumulation. There are three main sources of hydrogen: firstly, in the firing process, the reaction of water and an iron matrix occurs on the interface of the enamel layer and the steel plate, and hydrogen is replaced; hydrogen dissolved in the steel plate in the production process; thirdly, hydrogen entering the steel sheet during the pickling of the pretreatment. The generation of hydrogen is unavoidable in the production process of the enamel. During high-temperature enameling, the steel plate is in an austenite region, the main crystal grains are austenite, and the solubility of hydrogen in the steel plate is relatively high. After the enameling firing and cooling, the steel plate is in a ferrite area, the main crystal grains are ferrite, the solution degree of hydrogen is obviously reduced, and the hydrogen in the steel plate needs to diffuse outwards at the moment. The enamel layer is a continuous sub-regular network structure which is not beneficial to the diffusion of hydrogen, the hydrogen is gathered between the steel plate and the enamel layer in a gas form, and when the pressure is large enough, the enamel layer is broken to generate scale explosion.
The single-side enamel process can diffuse hydrogen from the non-enamelled surface, is favorable for the diffusion of hydrogen, can reduce the occurrence of scale explosion, deduces the diffusion condition of the hydrogen, and can be carried out according to the Fick first diffusion law:
Figure BDA0002478087950000021
in the formula I, J is the diffusion flux and has the unit kg/(m)2S) or number of atoms/(m)2S); d is a proportionality constant called diffusion coefficient, unit m2S; c is the concentration volume of diffusible hydrogen in kg/m3Or the number of atoms/m3
Figure BDA0002478087950000022
Is a concentration gradient; the minus sign indicates that the diffusion direction is opposite to the concentration gradient direction, and the diffusion proceeds from the high concentration gradient to the low concentration gradient.
Assuming that the diffusion coefficient D is independent of the concentration C at a certain temperature, the formula one can be written as
Figure BDA0002478087950000031
The hydrogen in the steel plate after single-side enamel can be diffused to the enamel surface and the non-enamel surface. The hydrogen diffuses to the non-enamel surface and can directly contact with the atmosphere when reaching the surface of the steel plate, the concentration of the hydrogen is changed into 0, and the diffusion process conforms to the second formula. In the diffusion process of hydrogen to the enamel surface, hydrogen is gathered under the action of the enamel layer, and the combination part of the enamel surface and the steel plate is gathered, so that the concentration of the hydrogen is increased, and the concentration gradient is caused
Figure BDA0002478087950000032
The diffusion flux becomes small, resulting in difficulty in hydrogen diffusion.
And pushing to obtain a double-sided hydrogen-coated diffusion model according to the single-sided hydrogen-coated diffusion model. Due to double-sided enameling, hydrogen in the steel plate diffuses to the contact surface of the steel plate and the enamel layer and cannot diffuse due to the obstruction of the enamel layer, and the hydrogen is accumulated between the enamel layer and the steel plate, so that the concentration of the hydrogen is increased, and the concentration gradient is generated
Figure BDA0002478087950000033
The smaller the diffusion flux, the smaller the diffusion flux. At the moment, hydrogen is gathered between the steel plate and the enamel layer to form hydrogen, and when the hydrogen reaches critical pressure, scaling occurs.
As can be seen from the diffusion model of the hydrogen coated on the double surfaces, the hydrogen diffusion in the double-surface enameling is more difficult and the scale explosion is more likely to occur, so when the scale explosion condition of the single-surface enameling of the hot-rolled acid-washed enamel steel is predicted, the six-surface enameling is selected for a detection test.
The method comprises the steps of dividing a sample into a reference surface and an observation surface, using five surfaces of four sections and a horizontal plane of the sample as the reference surface of the sample, and enameling, wherein the thickness of an enamel layer is more than 0.3 mm. And coating enamel on the other horizontal plane as an observation surface, wherein the thickness of the enamel layer is 0.10-0.20 mm, and enameling. And (4) after the enameling, carrying out scale explosion detection on the scale explosion condition of the observation surface/detection surface.
The thickness of the enamel layer on the reference surface of the sample is 0.30-0.35 mm, the obtained enamel layer has compact surface, few defects such as pinholes and the like, and the probability of scale explosion of the enamel layer is very low. Due to the compactness of the enamel layer, hydrogen in the steel sheet cannot escape from the enamel surface.
The thickness of the enamel layer on the reference surface is 0.30-0.35 mm, the physical basis is the particularity of the enamel, the enamel surface is not completely continuous, and a certain void ratio exists. The porosity is not fixed and constant, the thickness of the enamel is increased, the porosity is reduced, and the difficulty coefficient of hydrogen diffusion is larger, so that the hydrogen is more difficult to diffuse. And with the increase of the thickness of the enamel layer, the hydrogen breaks through the enamel layer, so that the difficulty of scale explosion caused by the rupture of the enamel layer is increased, and the thickness of the enamel layer of the reference surface is controlled to be 0.30-0.35 mm. The enamel surface is considered to be impervious to hydrogen evolution.
The thickness of the enamel layer on the observation surface of the sample is 0.10-0.20 mm, the enamel layer has normal porosity, and hydrogen can be gathered, escaped and scaled in the enamel layer.
The invention is verified from the theoretical or practical test results, and fully proves that: according to the invention, the scale explosion occurrence condition of the hot-rolled acid-washing enamel steel enamel coating can be effectively predicted by the reference surface enamel layer with the thickness of 0.30-0.35 mm and the other surface enamel layer with the thickness of 0.10-0.20 mm.
Compared with the prior art, the invention has the following positive effects: 1. the scale explosion observation period of the method is less than or equal to 24 hours, the observation period is shortened, the scale explosion resistance of the enameled pressed steel can be quickly tested, and a special method is provided for testing the scale explosion resistance of the hot-rolled and pickled enameled pressed steel. 2. The method has reliable safety coefficient, overcomes the probability problem of scale explosion, does not need repeated tests, improves the detection precision and reduces the detection cost.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention is further illustrated below with reference to specific examples 1-4, as shown in table 1.
Example 1, the hot-rolled pickled steel sheet for porcelain enamel was designated Q330 RT.
A method for detecting the fish scaling resistance of a hot-rolled pickled enameled steel plate comprises the following steps:
1) preparing a sample, namely cutting a rectangular sample from a hot-rolled acid-washed enameled steel plate for enamel to be detected, wherein the length of the sample is 100mm, the width of the sample is 60mm, and the thickness of the sample is 3.5 mm; degreasing and cleaning the surface of the sample, and controlling the surface cleanliness of the sample to be 95%;
2) coating an enamel glaze on a sample by using a wet coating method, and preparing the enamel glaze dry powder into a colloidal enamel glaze by using deionized water, wherein the mass ratio of the enamel glaze dry powder to the deionized water in the colloidal enamel glaze is 200: 70; coating and smearing colloidal enamel glaze on the surface of a sample, wherein the thickness of the colloidal enamel glaze smeared every time is 0.05-0.10 mm, and the thickness of one side surface and four cross-section enamel glaze layers of the sample is controlled to be 0.30-0.35 mm, namely the thickness of the enamel glaze layer on the reference surface of the sample is controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm, namely controlling the thickness of the enamel glaze layer on the observation surface of the sample to be 0.10-0.20 mm;
3) carrying out enamel firing treatment on the sample, and firstly, slowly heating the sample coated with enamel glaze from 15-25 ℃ to 100-150 ℃ at a heating speed of 5-10 ℃/min to ensure that the sample is dried; enameling the sample at 840 ℃ for 10min to generate an enamel layer; air cooling the sample to 15-25 ℃;
4) and the thicknesses of the enamel layer are measured, and the thicknesses of the reference surface and the observation surface are respectively 0.33mm and 0.16mm, so that the test requirements are met. And (3) evaluating the fish scaling resistance of the hot-rolled pickled enameled pressed steel, and observing the observation surface of the sample after 24 hours of enameling firing, wherein the sample has no fish scaling, and the fish scaling resistance of the hot-rolled pickled enameled pressed steel is qualified. And the method is put into batch production, and the batch production has no problem.
Example 2, the hot-rolled pickled steel sheet for enamel was designated as Q330 RT.
A method for detecting the fish scaling resistance of a hot-rolled pickled enameled pressed steel comprises the following steps:
1) preparing a sample, namely cutting a rectangular sample from a hot-rolled acid-washed enameled steel plate for enamel to be detected, wherein the length of the sample is 100mm, the width of the sample is 70mm, and the thickness of the sample is 1.5 mm; degreasing and cleaning the surface of the sample, and controlling the surface cleanliness of the sample to be 90%;
2) coating an enamel glaze on a sample by using a wet coating method, and preparing the enamel glaze dry powder into a colloidal enamel glaze by using deionized water, wherein the mass ratio of the enamel glaze dry powder to the deionized water in the colloidal enamel glaze is 200: 75; coating and smearing colloidal enamel glaze on the surface of a sample, wherein the thickness of the colloidal enamel glaze smeared every time is 0.05-0.10 mm, and the thickness of one side surface and four cross-section enamel glaze layers of the sample is controlled to be 0.30-0.35 mm, namely the thickness of the enamel glaze layer on the reference surface of the sample is controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm, namely controlling the thickness of the enamel glaze layer on the observation surface of the sample to be 0.10-0.20 mm;
3) carrying out enameling firing treatment on the sample, and firstly, slowly heating the sample coated with enamel glaze from 15-25 ℃ to 100-150 ℃ at a heating speed of 5-10 ℃/min to ensure that the sample is dried; carrying out high-temperature enameling on the sample at 850 ℃ for 8min to generate an enamel layer; air cooling the sample to 15-25 ℃;
4) and the thicknesses of the enamel layer are measured, and the thicknesses of the reference surface and the observation surface are respectively 0.35mm and 0.14mm, so that the test requirements are met. And (3) evaluating the scale explosion resistance of the hot-rolled pickled enameled steel plate, observing the observation surface of the sample after the enameling firing is finished for 24 hours, wherein the scale explosion does not occur in the sample, and the scale explosion resistance of the hot-rolled pickled steel plate is qualified. And the method is put into batch production, and the batch production has no problem.
Example 3, the hot-rolled pickled steel sheet for porcelain enamel was given a designation of Q210 RT.
A method for detecting the fish scaling resistance of a hot-rolled pickled enameled steel plate comprises the following steps:
1) preparing a sample, namely cutting a rectangular sample from a hot-rolled acid-washed enameled steel plate for enamel to be detected, wherein the length of the sample is 150mm, the width of the sample is 70mm, and the thickness of the sample is 2.7 mm; degreasing and cleaning the surface of the sample, and controlling the surface cleanliness of the sample to be 95%;
2) coating an enamel glaze on a sample by using a wet coating method, and preparing the enamel glaze dry powder into a colloidal enamel glaze by using deionized water, wherein the mass ratio of the enamel glaze dry powder to the deionized water in the colloidal enamel glaze is 200: 80; coating and smearing colloidal enamel glaze on the surface of a sample, wherein the thickness of the colloidal enamel glaze coated each time is 0.05-0.10 mm, and the thickness of one side surface and four cross-section enamel glaze layers of the sample is controlled to be 0.30-0.35 mm, namely the thickness of the sample reference surface enamel glaze layer is controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm, namely controlling the thickness of the enamel glaze layer on the observation surface of the sample to be 0.10-0.20 mm;
3) carrying out enameling firing treatment on the sample, and firstly, slowly heating the sample coated with enamel glaze from 15-25 ℃ to 100-150 ℃ at a heating speed of 5-10 ℃/min to ensure that the sample is dried; enameling the sample at 850 ℃ for 8min to generate an enamel layer; air cooling the sample to 15-25 ℃;
4) and the thickness of the enamel layer is measured, and the thickness of the reference surface and the thickness of the observation surface are respectively 0.31mm and 0.12mm, so that the test requirement is met. And (3) evaluating the scale explosion resistance of the hot-rolled pickled enameled steel plate, observing the observation surface of the sample 8 hours after the enameling firing is finished, and determining that the scale explosion resistance of the sample is unqualified.
Example 4, the hot-rolled pickled steel sheet for porcelain enamel was designated as Q210 RT.
A method for detecting the fish scaling resistance of a hot-rolled pickled enameled steel plate comprises the following steps:
1) preparing a sample, namely cutting a rectangular sample from a hot-rolled acid-washed enameled steel plate for enamel to be detected, wherein the length of the sample is 120mm, the width of the sample is 70mm, and the thickness of the sample is 3.7 mm; degreasing and cleaning the surface of the sample, and controlling the surface cleanliness of the sample to be 90%;
2) coating an enamel glaze on a sample by a wet coating method, and preparing colloidal enamel glaze from enamel glaze dry powder by deionized water, wherein the mass ratio of the enamel glaze dry powder to the deionized water in the colloidal enamel glaze is 200: 75; coating and smearing colloidal enamel glaze on the surface of a sample, wherein the thickness of the colloidal enamel glaze smeared every time is 0.05-0.10 mm, and the thickness of one side surface and four cross-section enamel glaze layers of the sample is controlled to be 0.30-0.35 mm, namely the thickness of the enamel glaze layer on the reference surface of the sample is controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm, namely controlling the thickness of the enamel glaze layer on the observation surface of the sample to be 0.10-0.20 mm;
3) carrying out enamel firing treatment on the sample, and firstly, slowly heating the sample coated with enamel glaze from 15-25 ℃ to 100-150 ℃ at a heating speed of 5-10 ℃/min to ensure that the sample is dried; enameling the sample at 850 ℃ for 8min to generate an enamel layer; air cooling the sample to 15-25 ℃;
4) and measuring the thickness of the enamel layer, wherein the thickness of the reference surface and the thickness of the observation surface are respectively 0.32mm and 0.11mm, meeting the test requirement, evaluating the scale explosion resistance of the hot-rolled and pickled enameled steel plate, observing the observation surface of the sample after the enameling firing is finished for 24 hours, wherein the scale explosion resistance of the sample is not generated, and the scale explosion resistance of the hot-rolled and pickled enameled steel plate is qualified. And the material is put into batch production, and the batch production is free from problems.
As no detection method for the scale explosion resistance of the special hot-rolled pickled enameled steel plate exists at present, the applicant tests the TH value of the sample according to the national standard GB/T29515-.
TABLE 1 test data of fishscale resistance of steel plates according to the examples of the invention
Figure BDA0002478087950000061
As shown in Table 1, the samples of examples 1, 2 and 4 were tested for the fishscale resistance TH of the steel plates in GB/T29515-2013, TH was 7.8min/mm2、8.2min/mm2、6.7min/mm2The scale explosion is not easy to occur, and the scale explosion resistance of the steel plate is qualified according to the detection method of the invention; in example 3, the samples are tested according to GB/T29515-2Scaling easily occurs; the fish scaling resistance of the steel plate is detected to be unqualified according to the method of the invention; the detection result of the method is consistent with the fish scaling resistance of the steel plate detected according to GB/T29515-2013, and the method is accurate and reliable.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.

Claims (3)

1. The method for detecting the fish scaling resistance of the hot-rolled pickled enameled steel plate is characterized by comprising the following steps of:
1) preparing a sample, namely cutting a rectangular sample from a hot-rolled acid-washed enameled steel plate for enamel to be detected, wherein the length of the sample is 100-200 mm, the width of the sample is 50-100 mm, and the thickness of the sample is 1.80-4.00 mm; degreasing and cleaning the surface of the sample;
2) coating an enamel glaze on a sample by a wet coating method, and preparing colloidal enamel glaze from enamel glaze dry powder by deionized water, wherein the mass ratio of the enamel glaze dry powder to the deionized water in the colloidal enamel glaze is 200: 50-200: 80; coating colloidal enamel glaze on the surface of a sample, wherein the thickness of the colloidal enamel glaze coated on each pass is 0.05-0.10 mm, and the thickness of one side surface and four cross-section enamel glaze layers of the sample is controlled to be 0.30-0.35 mm, namely the thickness of the sample reference surface enamel glaze layer is controlled to be 0.30-0.35 mm; controlling the thickness of the enamel glaze layer on the surface of the other side of the sample to be 0.10-0.20 mm, namely controlling the thickness of the enamel glaze layer on the observation surface of the sample to be 0.10-0.20 mm;
3) carrying out enamel firing treatment on the sample, and firstly, slowly heating the sample coated with enamel glaze from 15-25 ℃ to 100-150 ℃ at a heating speed of 5-10 ℃/min to ensure that the sample is dried; enameling the sample at the high temperature of 800-860 ℃ for 5-10 min to generate an enamel layer; air cooling the sample to 15-25 ℃;
4) evaluating the scale explosion resistance of the hot-rolled pickled enameled steel plate, observing the observation surface of the sample after the enameling firing is finished for 8-24 hours, and if no scale explosion occurs on the observation surface of the sample, the scale explosion resistance of the hot-rolled pickled enameled steel plate is qualified; on the contrary, if scale explosion occurs on the observation surface of the sample, the scale explosion resistance of the hot-rolled pickled enameled steel sheet is unqualified.
2. The method for detecting the fish scaling resistance of the hot-rolled pickled enameled pressed steel according to claim 1, wherein in step 1), the surface cleanliness of the sample is controlled to be not less than 90%.
3. The method for detecting the fish scaling resistance of the hot-rolled pickled enameled steel plate as claimed in claim 1, wherein the dry powder of the enamel glaze is sieved by a 300-mesh sieve.
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