CN110146364B - Evaluation method of plating assistant agent for metal hot dipping - Google Patents
Evaluation method of plating assistant agent for metal hot dipping Download PDFInfo
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- CN110146364B CN110146364B CN201910566055.1A CN201910566055A CN110146364B CN 110146364 B CN110146364 B CN 110146364B CN 201910566055 A CN201910566055 A CN 201910566055A CN 110146364 B CN110146364 B CN 110146364B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
Abstract
The invention relates to the technical field of metal hot dipping, in particular to an evaluation method of a plating assistant agent for metal hot dipping. The method provided by the invention can effectively judge whether the plating assistant agent is matched with the corresponding metal hot-dip plating process or not by measuring the thickness of the plating assistant layer, analyzing the coating uniformity of the plating assistant agent and further analyzing the stripping mechanism of the plating assistant layer and taking the stripping temperature interval and the stripping duration as the evaluation indexes of the plating assistant agent for metal hot-dip plating, thereby providing necessary technical support for selecting the plating assistant agent with optimal performance for the metal hot-dip plating process and improving the quality of metal hot-dip plating products.
Description
Technical Field
The invention relates to the technical field of metal hot dipping, in particular to an evaluation method of a plating assistant agent for metal hot dipping.
Background
The usage amount of the metal material in modern industry accounts for more than 97% of that of engineering materials, but with the technological progress, the use condition of the metal material is more and more rigorous, and in many cases, the requirements of strength and toughness required by working conditions are met, and meanwhile, the requirements of multiple aspects such as light weight, corrosion resistance, electric conduction, magnetic conduction and the like are met. Traditionally used single type metals such as steel, aluminum, copper and the like are difficult to meet the requirements in various aspects, but the alloy capable of meeting the use requirement faces the problems that the production process is complex, the use cost is too high, and the large-scale application cannot be realized. In view of the above circumstances, researchers have studied composite bimetal to solve these problems, wherein metal hot dip plating has a low cost and a great environmental protection advantage, and is a metal composite process with wide application.
Hot dip plating, hot dip plating for short, is a surface modification process in which a metal substrate (plated article) is immersed in a molten metal liquid after being subjected to appropriate pretreatment to form a metal coating on the surface of the metal substrate. Before hot dipping, a plating assistant agent is usually coated on the surface of a metal matrix, and the plating assistant agent can not only protect the metal matrix against oxidation, but also improve the surface activity of the metal matrix, reduce the surface tension of a plating solution and be beneficial to improving the hot dipping effect. In the actual production process, in addition to the requirement that the plating assistant agent can form a stable protective film on the surface of the base metal, the plating assistant agent also needs to disappear rapidly after playing a role in the hot dip plating process so as not to influence the hot dip plating effect. Therefore, the selection of the plating assistant has a great influence on the formulation of the hot dip plating process (including the hot dip plating time, the plating solution renewal frequency, the arrangement of external gas treatment devices, and the like), but there is no method for evaluating the plating assistant for metal hot dip plating.
Disclosure of Invention
The invention aims to provide an evaluation method of a plating assistant agent for metal hot dip plating, which can effectively judge whether the plating assistant agent is matched with a corresponding metal hot dip plating process or not, and provides necessary technical support for selecting the plating assistant agent with optimal performance and improving the quality of a metal hot dip plating product in the metal hot dip plating process.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an evaluation method of a plating assistant agent for metal hot dipping, which comprises the following steps:
(1) coating the plating assistant agent to be evaluated on the surface of the metal matrix sample to form a plating assistant layer to obtain a coated plating assistant agent sample;
(2) detecting the thickness of the plating assistant layer in the sample coated with the plating assistant agent; and if the error value of the thickness of the plating assistant layer meets the preset uniformity error, heating the sample coated with the plating assistant agent to carry out stripping mechanism analysis, recording the time and the temperature from the beginning of deformation to complete stripping of the plating assistant layer, obtaining a stripping temperature interval and stripping duration of the plating assistant layer, and taking the stripping temperature interval and the stripping duration as evaluation indexes of the plating assistant agent for metal hot dipping.
Preferably, the thickness of the plating assistant layer is less than or equal to 3mm, and the uniformity error is less than or equal to 10% of the thickness of the plating assistant layer.
Preferably, when the thickness of the plating assistant layer is detected, the sample coated with the plating assistant agent is rotated in situ, and whether the error value of the thickness of the plating assistant layer meets the preset uniformity error is judged by measuring the thickness of the plating assistant layer in different areas of the sample coated with the plating assistant agent; wherein, the in-situ rotation frequency is 4-18, and the rotation is 180 degrees.
Preferably, the heating temperature range of the peeling mechanism analysis is from room temperature to T3The temperature rise rate is 5-10 ℃/s, and the temperature T is3The temperature at which the plating assistant layer is completely stripped.
Preferably, when the method for hot dip metal plating includes a step of preheating a metal matrix, a thermal stability analysis is further included before the peeling mechanism analysis, and the thermal stability analysis includes the steps of:
carrying out first-stage heating treatment on the coated plating assistant agent sample with the error value of the thickness of the plating assistant layer meeting the requirement of uniformity error to obtain a first heated sample; wherein the temperature range of the first-stage heating treatment is from room temperature to T1The temperature rise rate is 7-10 ℃/s, and the temperature T is1The lower limit temperature is the preheating temperature of the metal matrix in the metal hot dipping method;
if the appearance of the plating assistant layer in the first heating sample is not changed, carrying out second-stage heating treatment on the first heating sample to obtain a second heating sample; wherein the temperature range of the second stage heat treatment is T1～T2(ii) a The temperature rise rate is 2-4 ℃/s, and the temperature T is2Is the upper limit temperature of the preheating temperature of the metal matrix in the metal hot dipping method.
Preferably, the peeling isThe off-machine analysis heating temperature range is T2～T3The temperature rise rate is 5-10 ℃/s, and the temperature T is3The temperature at which the plating assistant layer is completely stripped.
Preferably, the metal matrix test specimen comprises a steel matrix test specimen.
Preferably, the metal matrix sample is cylindrical, the diameter of the metal matrix sample is 4-6 mm, and the height of the metal matrix sample is 8-12 mm.
Preferably, the detection device adopted in the step (2) comprises a control computer, and a spotlight light source, a sample support, a heating electric furnace, a double magnifier and a high-speed camera which are sequentially arranged, wherein the sample support transversely extends into the heating electric furnace, and the high-speed camera and the heating electric furnace are in communication connection with the control computer.
Preferably, the frame frequency of the high-speed camera is 1000 frames/second, and the electric heating furnace comprises a corundum tube and a platinum-rhodium wire wound on the surface of the corundum tube.
The invention provides an evaluation method of a plating assistant agent for metal hot dipping, which comprises the following steps: (1) coating the plating assistant agent to be evaluated on the surface of the metal matrix sample to form a plating assistant layer to obtain a coated plating assistant agent sample; (2) detecting the thickness of the plating assistant layer in the sample coated with the plating assistant agent; and if the error value of the thickness of the plating assistant layer meets the preset uniformity error, heating the sample coated with the plating assistant agent to carry out stripping mechanism analysis, recording the time and the temperature from the beginning of deformation to complete stripping of the plating assistant layer, obtaining a stripping temperature interval and stripping duration of the plating assistant layer, and taking the stripping temperature interval and the stripping duration as evaluation indexes of the plating assistant agent for metal hot dipping. The method provided by the invention can effectively judge whether the plating assistant agent is matched with the corresponding metal hot-dip plating process or not by measuring the thickness of the plating assistant layer, analyzing the coating uniformity of the plating assistant agent and further analyzing the stripping mechanism of the plating assistant layer and taking the stripping temperature interval and the stripping duration as the evaluation indexes of the plating assistant agent for metal hot-dip plating, thereby providing necessary technical support for selecting the plating assistant agent with optimal performance for the metal hot-dip plating process and improving the quality of metal hot-dip plating products.
Drawings
FIG. 1 is a schematic structural diagram of a thermal imaging detection device of the present invention, in which 1-a spotlight source, 2-a sample holder, 3-a heating furnace, 4-a double magnifier, 5-a high speed camera, and 6-a control computer;
FIG. 2 is a schematic diagram of the position of a constant temperature region of a heating electric furnace of the thermal imaging detection apparatus according to the present invention;
FIG. 3 is a diagram showing the change of the morphology of a sample during the detection process according to the present invention.
Detailed Description
The invention provides an evaluation method of a plating assistant agent for metal hot dipping, which comprises the following steps:
(1) coating the plating assistant agent to be evaluated on the surface of the metal matrix sample to form a plating assistant layer to obtain a coated plating assistant agent sample;
(2) detecting the thickness of the plating assistant layer in the sample coated with the plating assistant agent; and if the error value of the thickness of the plating assistant layer meets the preset uniformity error, heating the sample coated with the plating assistant agent to carry out stripping mechanism analysis, recording the time and the temperature from the beginning of deformation to complete stripping of the plating assistant layer, obtaining a stripping temperature interval and stripping duration of the plating assistant layer, and taking the stripping temperature interval and the stripping duration as evaluation indexes of the plating assistant agent for metal hot dipping.
The plating assistant agent to be evaluated is coated on the surface of the metal matrix sample to form a plating assistant layer, so that the coated plating assistant agent sample is obtained. In the present invention, the metal matrix test piece preferably comprises a steel-based test piece; the specific type of the steel-based test sample is not particularly limited, and the steel-based test sample can be made of materials well known by the technical personnel in the field; in the examples of the present invention, Q195 steel, 10 steel and 08Al steel were specified as steel-based test pieces. In the invention, the metal matrix sample is preferably cylindrical, the diameter is preferably 4-6 mm, and the height is preferably 8-12 mm; the metal matrix test piece is preferably prepared by a wire cutting machine according to a predetermined size.
In the invention, the plating assistant agent to be evaluated specifically refers to any plating assistant agent needing evaluation. In the embodiment of the invention, when the plating assistant agent is evaluated for Q195 steel base hot-dip galvanizing, the plating assistant agent to be evaluatedThe agent being in particular NH4Cl and ZnCl2In an aqueous solution of (1), wherein, NH4Cl concentration of 140g/L, ZnCl2The concentration of (A) is 120 g/L; when the plating assistant agent for 10 steel base hot-dip aluminum plating is evaluated, the plating assistant agent to be evaluated is specifically an aqueous solution of NaCl, KCl and KF, wherein the total mass concentration of the solute is 6%, and the mass ratio of the NaCl, the KCl and the KF is 47.25: 47.25: 5.5; when the 08Al steel base hot-dip copper plating assistant agent is evaluated, the assistant agent to be evaluated is specifically an aqueous solution of borax, boric acid and KF, wherein the total mass concentration of solutes is 5%, and the mass ratio of the borax to the boric acid to the KF is 50: 35: 15. the preparation method of the plating assistant agent to be evaluated is not specially limited, and all the components are fully and uniformly mixed.
In the present invention, the preparation method of the plating assistant agent coated sample preferably comprises the following steps:
soaking a metal matrix sample in an alkaline washing solution for alkaline washing, then rinsing by using hot water, soaking in an acid washing solution for acid washing, washing by using cold water, and then quickly soaking in a plating assistant agent to be evaluated for coating; and after coating, taking out the obtained sample, drying until no water stain exists on the surface, and forming a plating assistant layer to obtain a coating plating assistant agent sample.
In the present invention, the alkali wash solution is preferably NaOH and Na2CO3The concentration of NaOH is preferably 35-45 g/L, more preferably 40 g/L; na (Na)2CO3The concentration of (b) is preferably 15 to 25g/L, more preferably 20 g/L. In the invention, the temperature of the alkaline washing solution during alkaline washing is preferably 45-55 ℃, and more preferably 50 ℃; the soaking time is preferably 4-6 min, and more preferably 5 min. The invention removes oil from the metal matrix sample by alkali cleaning.
In the invention, the temperature of the hot water is preferably 65-75 ℃, and more preferably 60 ℃; the specific operation mode of the rinsing in the present invention is not particularly limited, and the alkaline cleaning solution on the surface of the sample can be removed by a method known to those skilled in the art.
In the invention, the acid washing solution is preferably hydrochloric acid, and the mass concentration of the hydrochloric acid is preferably 10-20%, and more preferably 15%. In the present invention, the temperature of the pickling solution during the pickling is preferably normal temperature, i.e., no additional heating or cooling is required; the soaking time is preferably 1-3 min, and more preferably 2 min. The invention removes the oxide on the surface of the sample by acid cleaning.
In the present invention, the temperature of the cold water is preferably normal temperature, i.e., no additional heating or cooling is required; in the present invention, the number of times of flushing with cold water is preferably two; the specific operation mode of the washing in the present invention is not particularly limited, and impurities such as an acid washing solution on the surface of the sample can be sufficiently removed by a method known to those skilled in the art.
In the invention, the temperature of the plating assistant agent to be evaluated during coating is preferably 55-65 ℃, and more preferably 60 ℃; the soaking time is preferably 4-6 min, and more preferably 5 min.
In the invention, the drying temperature is preferably 100-200 ℃, and more preferably 130-170 ℃; the drying time is not specially limited, the test surface is ensured to be free of water stain, and a layer of crystallized salt, namely the plating assistant layer, is formed on the surface of the sample. The present invention preferably dries the sample in an electric resistance furnace.
In the invention, the coating thickness of the plating assistant agent depends on the concentration of the plating assistant agent and the material, the size and the like of the metal matrix sample, and the coating thickness of the plating assistant agent is preferably controlled to ensure that the thickness of the obtained plating assistant layer meets the subsequent detection requirement.
After obtaining a coating plating assistant agent sample, detecting the thickness of a plating assistant layer in the coating plating assistant agent sample; and if the error value of the thickness of the plating assistant layer meets the preset uniformity error, heating the sample coated with the plating assistant agent to carry out stripping mechanism analysis, recording the time and the temperature from the beginning of deformation to complete stripping of the plating assistant layer, obtaining a stripping temperature interval and stripping duration of the plating assistant layer, and taking the stripping temperature interval and the stripping duration as evaluation indexes of the plating assistant agent for metal hot dipping.
After obtaining the coating plating assistant agent sample, the invention firstly detects the thickness of the plating assistant layer in the coating plating assistant agent sample. In the invention, when the thickness of the plating assistant layer is detected, the sample coated with the plating assistant agent is preferably rotated in situ, and whether the error value of the thickness of the plating assistant layer meets the preset uniformity error is judged by measuring the thickness of the plating assistant layer in different areas of the sample coated with the plating assistant agent; the in-situ rotation frequency is preferably 4-18 times, more preferably 10-18 times, and the rotation frequency is 180 degrees in total.
In the invention, the thickness of the plating-assistant layer is preferably less than or equal to 3mm, more preferably 0.01-0.5 mm, and further preferably 0.02-0.2 mm; the uniformity error is preferably less than or equal to 10% of the thickness of the plating assistant layer; the thickness of the plating assistant layer (or the thickness of the plating assistant layer) in the invention specifically refers to the average thickness of the plating assistant layer. In the invention, the average value of the thickness of the plating assistant layer is subtracted from the maximum value and the minimum value of the actually measured thickness of the plating assistant layer respectively, and the obtained difference is divided by the average value of the thickness of the plating assistant layer, so that the obtained result is required to be less than or equal to 10 percent; if the obtained result is more than 10%, the error value of the plating assistant layer thickness does not meet the preset uniformity error, which indicates that the plating assistant agent is not suitable for the corresponding metal hot dipping method and does not need to be subjected to subsequent tests.
In the invention, if the error value of the thickness of the plating assistant layer meets the preset uniformity error, the sample coated with the plating assistant agent is heated to carry out stripping mechanism analysis, the time and the temperature from the beginning of deformation to complete stripping of the plating assistant layer are recorded, the stripping temperature interval and the stripping duration of the plating assistant layer are obtained, and the stripping temperature interval and the stripping duration are used as the evaluation indexes of the plating assistant agent for metal hot dipping. In the present invention, the heating temperature range for the peeling mechanism analysis is preferably from room temperature to T3The heating rate is preferably 5-10 ℃/s, and more preferably 6-8 ℃/s; the T is3The temperature at which the plating assistant layer is completely stripped.
According to the invention, the stripping temperature interval and the stripping duration are used as evaluation indexes of the plating assistant for metal hot dip plating, and specifically, according to the comparison of relevant operating parameters in the metal hot dip plating method with the stripping temperature interval and the stripping duration, the stripping temperature interval is required to be lower than the plating temperature, and the stripping duration does not exceed the plating duration, so that the plating assistant is suitable for the corresponding metal hot dip plating method.
In the present invention, when the method for hot dip coating metal includes the step of preheating the metal matrix, the method preferably further includes a thermal stability analysis before the peeling mechanism analysis, and the thermal stability analysis preferably includes the steps of:
carrying out first-stage heating treatment on the coated plating assistant agent sample with the error value of the thickness of the plating assistant layer meeting the requirement of uniformity error to obtain a first heated sample; wherein the temperature range of the first-stage heating treatment is from room temperature to T1The temperature rise rate is 7-10 ℃/s, and the temperature T is1The lower limit temperature is the preheating temperature of the metal matrix in the metal hot dipping method;
if the appearance of the plating assistant layer in the first heating sample is not changed, carrying out second-stage heating treatment on the first heating sample to obtain a second heating sample; wherein the temperature range of the second stage heat treatment is T1～T2(ii) a The temperature rise rate is 2-4 ℃/s, and the temperature T is2Is the upper limit temperature of the preheating temperature of the metal matrix in the metal hot dipping method.
In the invention, if the appearance of the plating assistant layer in the first heating sample is changed, such as softening, flowing or peeling, the plating assistant agent is not suitable for the corresponding metal hot dipping method, and subsequent tests are not required.
In the invention, if the plating assistant layer in the second heating sample is stripped, the plating assistant agent is not suitable for the corresponding metal hot dipping method, and subsequent tests are not needed; and if the appearance of the plating assistant layer in the second heating sample is not changed or slightly changed, such as volume expansion, but the stripping phenomenon does not occur, carrying out subsequent stripping mechanism analysis on the second heating sample.
In the present invention, when the metal hot dip coating method includes the step of preheating the metal matrix, the heating temperature range for the peeling mechanism analysis is preferably T2～T3The heating rate is preferably 5-10 ℃/s, and the temperature T is3Is the temperature when the plating assistant layer is completely strippedAnd (4) degree.
In the invention, when the metal hot dip plating method comprises the step of preheating a metal matrix, the stripping temperature interval and the stripping duration are used as evaluation indexes of the plating assistant for metal hot dip plating, specifically, according to the comparison of relevant operating parameters in the metal hot dip plating method with the stripping temperature interval and the stripping duration, the stripping temperature interval is required to be between the preheating temperature of the metal matrix and the temperature of a plating solution, and the stripping duration does not exceed the immersion plating time, so that the plating assistant is suitable for the corresponding metal hot dip plating method.
In the evaluation method of the plating assistant for metal hot dip plating provided by the invention, except for the step of preparing the sample coated with the plating assistant, the detection device used in the other steps is a thermal imaging detection device, as shown in fig. 1, the detection device comprises a control computer and a spotlight light source, a sample support, a heating electric furnace, a double magnifier and a high-speed camera which are sequentially arranged, wherein the sample support transversely extends to the interior of the heating electric furnace, and the high-speed camera and the heating electric furnace are in communication connection with the control computer.
As an embodiment of the present invention, the frame rate of the high-speed camera is 1000 frames/second; the invention detects the thickness of the plating-assisting layer (the detection error is +/-0.002 mm) by a high-speed camera and observes the state change of the plating-assisting layer.
As an embodiment of the invention, the electric heating furnace comprises a corundum tube and a platinum-rhodium wire wound on the surface of the corundum tube, wherein the platinum-rhodium wire is specifically platinum-rhodium 30; the surface of the corundum tube is provided with threads, a platinum-rhodium wire is wound on the threads, and the corundum tube is heated through the platinum-rhodium wire; in the actual use process, a sample is placed in a constant temperature area in the corundum tube, and the heating electric furnace is controlled by a control computer to heat, wherein the position of the constant temperature area is specifically shown in fig. 2.
In the invention, when the thermal imaging detection device is used for carrying out related test analysis, specifically, a coated plating assistant sample is placed on a corundum tray, the corundum tray containing the coated plating assistant sample is placed on a sample support, the coated plating assistant sample is positioned in a constant temperature area of a heating electric furnace, a detection device is started (the heating electric furnace is not started at the moment, namely the heating electric furnace is not heated), the coated plating assistant sample is rotated in situ for 4-18 times, the rotation is carried out for 180 degrees in total, the thickness of the plating assistant layer in different areas of the coated plating assistant sample is detected by using a high-speed camera, and the uniformity of the thickness of the plating assistant layer is contrastively analyzed;
after the uniformity of the thickness of the plating assistant layer meets the requirement, a heating electric furnace is started, and the coated plating assistant agent sample is heated for stripping mechanism analysis (the heating temperature range of the stripping mechanism analysis is from room temperature to T)3The temperature rise rate is 5-10 ℃/s, and the temperature T is3The temperature of the plating assistant layer when the plating assistant layer is completely stripped), in the temperature rise process, a high-speed camera is used for recording the state change of a sample coated with the plating assistant agent, the state change is transmitted to a control computer in real time, image analysis software is used for analyzing the stripping mechanism of the plating assistant layer (or analyzing the thermal stability and the stripping mechanism of the plating assistant layer), and the stripping temperature interval and the stripping duration time of the plating assistant layer are obtained by recording the time and the temperature from the beginning of deformation of the plating assistant layer to the complete stripping.
The change of the sample morphology when the technical scheme of the invention is adopted for detection and analysis is shown in fig. 3 (the high temperature detection corresponds to the peeling mechanism analysis process in fig. 3, or corresponds to the thermal stability analysis and peeling mechanism analysis process), as can be seen from fig. 3, after the plating assistant agent is coated and dried on the metal matrix sample, the plating assistant layer is formed, and then in the high temperature detection process, the plating assistant layer is peeled off, and the sample recovers the original morphology.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The evaluation is carried out on the plating assistant agent of Q195 steel base hot-dip galvanizing (the process parameters are shown in the table 1), and the evaluation comprises the following steps:
1) reacting NH4Cl、ZnCl2Is soluble in waterPreparing a plating assistant agent, wherein NH4Cl concentration of 140g/L, ZnCl2The concentration of (A) is 120 g/L;
2) preparing a steel-based Q195 steel sample, wherein the shape of the steel-based Q195 steel sample is a cylinder with the diameter of 5mm and the height of 9 mm;
3) coating the plating assistant agent on the surface of the steel-based sample in a hanging manner, then placing the steel-based sample in a drying box for drying, wherein the temperature of the drying box is 100 ℃, and forming a plating assistant layer on the surface of the steel-based sample to obtain a coated plating assistant agent sample;
4) placing the coated plating assistant agent sample on a corundum tray, and placing the tray in a constant temperature area of a heating electric furnace; starting a detection device (at the moment, the electric heating furnace is not started, namely, the electric heating furnace is not heated), uniformly rotating the coated plating assistant agent sample in situ for 10 times, wherein the angle of each rotation is the same, and the total rotation angle of 10 rotations is 180 degrees; the detection shows that the thickness of the plating assistant layer is 0.150mm, the uniformity error is 0.010mm, the coating is uniform, and the process requirement of Q195 steel base hot-dip galvanizing is met by preliminary judgment;
5) because the Q195 steel base hot-dip galvanizing process does not require preheating of the steel base, the thermal stability analysis of the plating assistant is not carried out;
6) the Q195 steel base hot-dip galvanizing process requires that the temperature of a plating solution is 430-480 ℃, a heating electric furnace is started to control the heating speed at 8 ℃/s for heating, a high-speed camera is used for observing and finding that when the temperature reaches 380 ℃, a plating assistant layer begins to deform, part of the plating assistant agent begins to gasify, and part of the plating assistant agent begins to peel off, and when the temperature reaches 400 ℃, the plating assistant layer is completely peeled off;
7) the detection result shows that the stripping temperature range of the plating assistant layer is 380-400 ℃, the stripping duration is 2.5s, and the average stripping rate is 0.600 multiplied by 10-4m/s, meets the process requirements of Q195 steel base hot-dip galvanizing.
TABLE 1 Process parameters for Q195 STEEL-BASED HOT-DIP ZINC PLATING
| Base bodyMaterial | Q195 size 40X 4(mm) |
| Immersion plating material | Pure zinc |
| Preheating temperature of substrate | Without preheating |
| Temperature of plating solution | 430～480℃ |
| Immersion plating time | 5～300s |
Example 2
The evaluation is carried out on the plating assistant agent for 10 steel base hot dip aluminum plating (the process parameters are shown in the table 2), and the evaluation comprises the following steps:
1) dissolving NaCl, KCl and KF in water, and preparing to obtain the plating assistant agent, wherein the total mass concentration of solutes in the plating assistant agent is 6%, and the mass ratio of the NaCl, the KCl and the KF is 47.25: 47.25: 5.5;
2) preparing a 10-steel-based test sample, wherein the shape of the test sample is a cylinder with the diameter of 6mm and the height of 10 mm;
3) coating the plating assistant agent on the surface of the steel-based sample in a hanging manner, then placing the steel-based sample in a drying box for drying, wherein the temperature of the drying box is 120 ℃, and forming a plating assistant layer on the surface of the steel-based sample to obtain a coated plating assistant agent sample;
4) placing the coated plating assistant agent sample on a corundum tray, and placing the tray in a constant temperature area of a heating electric furnace; starting a detection device (at the moment, the electric heating furnace is not started, namely, the electric heating furnace is not heated), uniformly rotating the coated plating assistant agent sample in situ 16 times, wherein the angle of the in situ rotation every time is the same, and the total rotation angle of the 16 rotations is 180 degrees; the detection shows that the thickness of the plating aid layer is 0.125mm, the uniformity error is 0.009mm, the coating is uniform, and the process requirement of 10 steel base hot-dip aluminum plating is met by preliminary judgment;
5) setting the thermal stability analysis temperature of the plating assistant agent to be 200-280 ℃ based on the preheating temperature requirement of 10 steel base hot-dip aluminum plating on a steel base, specifically, heating a sample coated with the plating assistant agent in two stages, wherein the heating temperature range of the first stage is room temperature-200 ℃, and the heating rate is 8 ℃/s; the heating temperature interval of the second stage is 200-280 ℃, and the heating rate is 4 ℃/s; monitoring the appearance change of a sample coated with the plating assistant agent by a high-speed camera, and judging that the thermal stability of the plating assistant agent meets the process requirement of 10 steel-based hot-dip aluminum plating if the detection shows that no obvious deformation occurs to the plating assistant layer;
6) the 10 steel base hot dipping aluminum plating process requires that the temperature of a plating solution is 680-710 ℃, a heating electric furnace is utilized to control the heating speed at 9 ℃/s for heating, a high-speed camera is utilized to observe and discover that when the temperature reaches 640 ℃, a plating assistant layer begins to deform, part of plating assistant agent begins to soften and flow, and when the temperature reaches 665 ℃, the plating assistant layer is completely stripped;
7) the detection result shows that the stripping temperature interval of the plating assistant layer is 640-665 ℃, the stripping duration is 2.8s, and the average stripping rate is 0.450 multiplied by 10-4m/s, meets the technological requirements of hot dip aluminizing of 10 steel base.
TABLE 210 Process parameters for hot-dip aluminizing of the steel base
| Base material | 10 steel wire diameter 1mm |
| Immersion plating material | Guiyang Al99.80 |
| Preheating temperature of substrate | 200～280℃ |
| Temperature of plating solution | 680～710℃ |
| Immersion plating time | 4.8～6.4s |
Example 3
The evaluation is carried out on a plating assistant agent for 08Al steel-based hot-dip copper plating (the process parameters are shown in Table 3), and the evaluation comprises the following steps:
1) dissolving borax, boric acid and KF in water, and preparing to obtain the plating assistant agent, wherein the total mass concentration of solutes in the plating assistant agent is 5%, and the mass ratio of the borax to the boric acid to the KF is 50: 35: 15;
2) preparing a steel-based test sample of 08Al steel, wherein the shape of the steel-based test sample is a cylinder with the diameter of 6mm and the height of 10 mm;
3) coating the plating assistant agent on the surface of the steel-based sample in a hanging manner, then placing the steel-based sample in a drying box for drying, wherein the temperature of the drying box is 200 ℃, and forming a plating assistant layer on the surface of the steel-based sample to obtain a coated plating assistant agent sample;
4) placing the coated plating assistant agent sample on a corundum tray, and placing the tray in a constant temperature area of a heating electric furnace; starting a detection device (at the moment, the electric heating furnace is not started, namely, the electric heating furnace is not heated), uniformly rotating the coated plating assistant sample in situ for 18 times, wherein the angle of the in situ rotation for each time is the same, and the total rotation angle of the 18 times of rotation is 180 degrees; the detection shows that the thickness of the plating-assisting layer is 0.190mm, the uniformity error is 0.015mm, the coating is uniform, and the process requirement of 08Al steel-based hot-dip copper plating is met by preliminary judgment;
5) setting the thermal stability analysis temperature of the plating assistant agent to be 400-800 ℃ based on the preheating temperature requirement of 08Al steel-based hot-dip copper plating on a steel substrate, specifically, heating a sample coated with the plating assistant agent in two stages, wherein the heating temperature interval of the first stage is room temperature-400 ℃, and the heating rate is 10 ℃/s; the heating temperature interval of the second stage is 400-800 ℃, and the heating rate is 5 ℃/s; monitoring the appearance change of the sample coated with the plating assistant agent by a high-speed camera, and detecting to find that when the temperature reaches 650 ℃, the plating assistant layer begins to deform but does not soften and peel off, the temperature is continuously raised to 800 ℃, the volume of the plating assistant layer expands, but the steel-based sample is not peeled off, and then the thermal stability of the plating assistant agent is judged to basically meet the process requirement of 08Al steel-based hot-dip copper plating;
6) the 08Al steel base hot dipping copper plating process requires that the temperature of a plating solution is 1090-1150 ℃, a heating electric furnace is used for controlling the heating speed at 7 ℃/s for heating, a high-speed camera is used for observing and finding that when the temperature reaches 845 ℃, a plating assistant layer starts to soften and flow, and when the temperature reaches 850 ℃, the plating assistant layer is completely stripped.
7) The detection result shows that the stripping temperature range of the plating assistant layer is 845-850 ℃, the stripping duration is 0.71s, and the average stripping rate is 0.266 multiplied by 10-3m/s, which basically meets the process requirements of 08Al steel hot-dip copper plating.
TABLE 308 technological parameters of Al steel base hot-dip copper plating
| Base material | 08Al steel plate size 120X 1.5(mm) |
| Immersion plating material | No. 1 electrolytic copper (copper content 99%) |
| Preheating temperature of substrate | 400～800℃ |
| Temperature of plating solution | 1090～1150℃ |
| Immersion plating time | 0.2～4s |
As can be seen from the above embodiments, in the method provided by the present invention, by determining the thickness of the plating assistant layer, analyzing the coating uniformity of the plating assistant agent, and further analyzing the peeling mechanism of the plating assistant layer (or analyzing the thermal stability and peeling mechanism of the plating assistant layer), and taking the peeling temperature interval and the peeling duration as the evaluation indexes of the plating assistant agent for metal hot dip plating, it can be effectively determined whether the plating assistant agent is matched with the corresponding metal hot dip plating process, for example, the plating assistant agents in embodiments 1 to 3 are respectively suitable for the corresponding hot dip plating processes, while the plating assistant agents in embodiments 1 and 2 are not suitable for the hot dip plating process in embodiment 3. Therefore, the method provided by the invention provides necessary technical support for selecting the plating assistant agent with the optimal performance for the metal hot dip plating process and improving the quality of the metal hot dip plated product.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for evaluating a plating assistant for metal hot dip plating is characterized by comprising the following steps:
(1) coating the plating assistant agent to be evaluated on the surface of the metal matrix sample to form a plating assistant layer to obtain a coated plating assistant agent sample;
(2) detecting the thickness of the plating assistant layer in the sample coated with the plating assistant agent; if the error value of the thickness of the plating assistant layer meets the preset uniformity error, heating the sample coated with the plating assistant agent to carry out stripping mechanism analysis, recording the time and the temperature of the plating assistant layer from deformation to complete stripping, obtaining the stripping temperature interval and the stripping duration of the plating assistant layer, and taking the stripping temperature interval and the stripping duration as the evaluation indexes of the plating assistant agent for metal hot dipping; the heating temperature range of the stripping mechanism analysis is from room temperature to T3The temperature rise rate is 5-10 ℃/s, and the temperature T is3The temperature at which the plating assistant layer is completely stripped.
2. The evaluation method according to claim 1, wherein the thickness of the plating aid layer is 3mm or less, and the uniformity error is 10% or less of the thickness of the plating aid layer.
3. The evaluation method according to claim 1 or 2, wherein when the thickness of the plating assistant layer is detected, the sample coated with the plating assistant agent is rotated in situ, and the thickness of the plating assistant layer in different areas of the sample coated with the plating assistant agent is measured to judge whether the error value of the thickness of the plating assistant layer meets the preset uniformity error; wherein, the in-situ rotation frequency is 4-18, and the rotation is 180 degrees.
4. The evaluation method according to claim 1, wherein when the method for hot dip coating metal includes the step of preheating the metal matrix, a thermal stability analysis is further included before the peeling mechanism analysis, the thermal stability analysis including the steps of:
carrying out first-stage heating treatment on the coated plating assistant agent sample with the error value of the thickness of the plating assistant layer meeting the requirement of uniformity error to obtain a first heated sample; wherein the temperature range of the first-stage heating treatment is from room temperature to T1The temperature rise rate is 7-10 ℃/s, and the temperature T is1The lower limit temperature is the preheating temperature of the metal matrix in the metal hot dipping method;
if the appearance of the plating assistant layer in the first heating sample is not changed, carrying out second-stage heating treatment on the first heating sample to obtain a second heating sample; wherein the temperature range of the second stage heat treatment is T1～T2(ii) a The temperature rise rate is 2-4 ℃/s, and the temperature T is2Is the upper limit temperature of the preheating temperature of the metal matrix in the metal hot dipping method.
5. The evaluation method according to claim 4, wherein the heating temperature range for the peeling mechanism analysis is T2～T3The temperature rise rate is 5-10 ℃/s, and the temperature T is3The temperature at which the plating assistant layer is completely stripped.
6. The evaluation method according to claim 1, wherein the metal base test piece comprises a steel base test piece.
7. The evaluation method according to claim 1 or 6, wherein the metal matrix sample is cylindrical, has a diameter of 4 to 6mm and a height of 8 to 12 mm.
8. The evaluation method according to claim 1, wherein the detection device adopted in the step (2) comprises a control computer and a spotlight light source, a sample support, a heating electric furnace, a double magnifier and a high speed camera which are arranged in sequence, wherein the sample support transversely extends to the interior of the heating electric furnace, and the high speed camera and the heating electric furnace are in communication connection with the control computer.
9. The evaluation method according to claim 8, wherein the frame rate of the high-speed camera is 1000 frames/sec, and the electric heating furnace comprises a corundum tube and a platinum-rhodium wire wound around the surface of the corundum tube.
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Application publication date: 20190820 Assignee: TANGSHAN ZHENGYUAN PIPE INDUSTRY CO.,LTD. Assignor: NORTH CHINA University OF SCIENCE AND TECHNOLOGY Contract record no.: X2023980039443 Denomination of invention: Evaluation method of a plating aid for metal hot dip plating Granted publication date: 20220121 License type: Common License Record date: 20230811 |