CN118501390A - Quantitative detection method for zinc impregnation amount of metal material based on element content - Google Patents
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- 239000011701 zinc Substances 0.000 title claims abstract description 375
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 265
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 265
- 239000007769 metal material Substances 0.000 title claims abstract description 114
- 238000005470 impregnation Methods 0.000 title claims abstract description 112
- 238000001514 detection method Methods 0.000 title claims abstract description 45
- 238000005507 spraying Methods 0.000 claims abstract description 63
- 238000007747 plating Methods 0.000 claims abstract description 57
- 238000012360 testing method Methods 0.000 claims abstract description 50
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 33
- 238000004364 calculation method Methods 0.000 claims abstract description 21
- 238000005259 measurement Methods 0.000 claims abstract description 13
- 229910000838 Al alloy Inorganic materials 0.000 claims description 64
- 239000000463 material Substances 0.000 claims description 33
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 25
- 239000000956 alloy Substances 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 23
- 239000011248 coating agent Substances 0.000 claims description 22
- 239000007921 spray Substances 0.000 claims description 18
- 238000009616 inductively coupled plasma Methods 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000013077 target material Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000007888 film coating Substances 0.000 claims description 6
- 238000009501 film coating Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- -1 argon ion Chemical class 0.000 claims description 3
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 abstract description 7
- 238000001764 infiltration Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 36
- 230000000052 comparative effect Effects 0.000 description 14
- 230000007797 corrosion Effects 0.000 description 12
- 238000005260 corrosion Methods 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 4
- 230000029087 digestion Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000009681 x-ray fluorescence measurement Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 229910000611 Zinc aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009675 coating thickness measurement Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
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- 238000005086 pumping Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
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- 238000004876 x-ray fluorescence Methods 0.000 description 1
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Abstract
The application discloses a quantitative detection method for zinc impregnation amount of a metal material based on element content, which comprises the following steps: testing the mass fraction of Zn element in the metal material before zinc spraying or zinc plating; after zinc spraying or zinc plating is carried out on the metal material, the metal material subjected to zinc impregnation obtained through heat treatment is used as an object to be detected, and the mass fraction of Zn element in the object to be detected is tested; basic parameter measurement: measuring quality and length parameters of an object to be detected, and calculating the perimeter of the detected object; and (3) data calculation: and calculating the ratio of the mass of zinc in the unit to the surface area of the object to be detected as the zinc impregnation amount, and obtaining the zinc impregnation amount in the metal material. According to the application, the zinc content is measured and calculated integrally, and the analysis of the zinc infiltration amount can be realized by establishing the relation between the diffused zinc element content and the infiltration amount and combining an analysis model. The method overcomes the influence of non-uniformity, heat treatment and processing deformation of the zinc layer on the zinc layer, and has the advantages of wide applicability and high accuracy.
Description
Technical Field
The invention relates to the technical field of metal material surface treatment and data calculation, in particular to a quantitative detection method for zinc impregnation amount of a metal material based on element content.
Background
Recent researches show that the surface of metal materials such as aluminum alloy, steel and the like is galvanized or galvanized, so that the local corrosion risk of the materials can be obviously improved. Meanwhile, the metal material is often accompanied by a heat treatment zincating process, because after zinc element is dissolved into a metal matrix, the corrosion potential can be reduced by 25-30mV. The zinc-containing surface layer is used as low-potential preferential corrosion, so that the pitting corrosion can be converted into surface corrosion, and the corrosion resistance can be improved. However, the effect of inhibiting pitting corrosion cannot be achieved by the excessively low zinc infiltration amount, the material corrosion can be obviously accelerated by the excessively high zinc infiltration amount, and the Zn infiltration amount in the alloy is important to master in order to achieve excellent corrosion performance of the zinc-containing surface layer.
Currently, a common method for zinc spraying amount testing is "GB/T16921-2005X-ray spectrometry for metal coating thickness measurement". The method can determine the zinc content by measuring and calculating the zinc layer thickness after zinc spraying. However, in the existing corrosion-resistant process, after zinc spraying, a heat treatment process is required, and a surface zinc layer penetrates into the matrix to form a zinc-containing diffusion layer. Meanwhile, the zinc spraying layer on the surface is lost in the heat treatment process. At this time, accurate measurement of the zinc penetration amount cannot be realized by the film thickness method.
Disclosure of Invention
In order to overcome the difficulty in the existing assessment of the zinc content, the application provides a quantitative detection method for the zinc content of a metal material based on element content, which utilizes the whole measurement and calculation of the zinc content, and can realize the analysis of the zinc infiltration by establishing the relationship between the diffused zinc element content and the zinc infiltration and combining an analysis model. The method overcomes the influence of non-uniformity, heat treatment and processing deformation of the zinc layer on the zinc layer, and has the advantages of wide applicability and high accuracy.
In order to solve the problems, the technical scheme adopted by the application is as follows:
the embodiment of the application provides a quantitative detection method for the zinc impregnation amount of a metal material based on element content, which comprises the following steps of
And (3) component detection: testing the mass fraction of Zn element in the metal material before zinc spraying or zinc plating; after zinc spraying or zinc plating is carried out on the metal material, the metal material subjected to zinc impregnation obtained through heat treatment is used as an object to be detected, and the mass fraction of Zn element in the object to be detected is tested;
Basic parameter measurement: measuring quality and length parameters of an object to be detected, and calculating the perimeter of the detected object;
And (3) data calculation: and calculating the ratio of the mass of zinc in the unit to the surface area of the object to be detected as the zinc impregnation amount, and obtaining the zinc impregnation amount in the metal material.
As a further preferable scheme, in the data calculation process of the embodiment of the application, the zinc impregnation amount is calculated as P and the unit is g/m 2 by adopting the following formula:
（1）；
In the formula (1), M Zn is the mass of zinc, and the unit is g; m Zn can be calculated by the following formula:
MZn=（ω1-ω0）×m（2）；
In the formula (2), omega 1 is the mass fraction of Zn element in the object to be detected, and the unit is wt%; omega 0 is the mass fraction of Zn element in the metal material before zinc spraying, and the unit is wt%; m is the mass of an object to be detected;
In the above formula (1), S is a zincification surface area, unit m 2, calculated by the following formula (3): s=c×l (3);
in the formula (3), C is the perimeter of the object to be detected, and the unit is m; l is the length of an object to be detected, and the unit is m;
Based on the basic parameters of the object to be detected and the component detection result, the zincification amount of the surface of the material after heat treatment can be calculated:
（4）。
As a further preferable scheme, the zinc spraying process according to the embodiment of the application comprises the following steps:
Melting pure zinc into liquid zinc, placing the liquid zinc in spraying equipment, keeping the fluidity of the liquid zinc, and placing a metal material to be treated in front of a spray head, wherein the distance between the surface of the metal material and the spray head is 2-10 cm; starting the spraying equipment, setting the pressure of the spraying equipment between 5 and 6Kg/cm 2, extruding liquid Zn to cover the surface of the metal material in front of the spray head, controlling the amount of sprayed Zn by spraying the mass and the maximum surface area of the liquid Zn, and naturally cooling to room temperature after the zinc spraying is finished to obtain the metal material with the zinc coated surface.
As a further preferable scheme, the galvanization process adopts a magnetron sputtering mode, and the target material is a Zn target material with the purity of more than 90 percent, and comprises the following steps:
vacuumizing: a Zn target is arranged in a coating cavity, a metal material is arranged in the coating cavity and opposite to the target, equipment is started, a molecular pump is started, and argon gas serving as a protective gas is filled after vacuumizing;
pre-plating: then starting pre-plating, blocking the surface of the metal material by using a baffle plate during pre-plating, plating for five minutes, and removing oxides and impurities on the surface of the Zn target material;
formal film plating: after the baffle is removed, formal film coating is started, the film coating speed is 6-7A/S, and the Zn spraying amount is controlled through the density of Zn and the thickness of magnetron sputtering Zn plating; and closing argon after Zn plating is completed, and deflating the cavity to obtain the metal material with the zinc coated surface.
As a further preferable scheme, the heat treatment according to the embodiment of the application comprises the following steps: and (3) placing the metal material with the zinc coated surface into a heat treatment furnace, setting the temperature to 550-650 ℃, preserving the heat for 2-8min after the temperature reaches the set temperature, and then cooling along with the furnace to finish the heat treatment.
As a further preferable scheme, the quantitative detection method for the zinc impregnation amount of the metal material based on the element content adopts an inductively coupled plasma technology to test the mass fraction of Zn element in the metal material before zinc spraying or zinc plating and the object to be detected.
The metal material before zinc spraying or zinc plating and the object to be detected are respectively twisted into particles or scraps, the particles or scraps are digested by using a zinc ICP-MS standard solution to obtain a clear solution, the clear solution is placed in ICP equipment for testing, an argon ion body is used for testing, after the sample is converted into ions, a mass spectrometer is used for measuring, and the mass fraction of Zn is directly obtained.
As a further preferable scheme, the quantitative detection method for the zinc impregnation amount of the metal material based on the element content further comprises the step of calculating the plating amount of the zinc layer:
The said （5）；
In the above formula (5), M ' Zn is the mass of zinc plating on the surface of the metal material, the mass of the metal material before zinc impregnation is M ', the circumference of the metal material before zinc impregnation is C ', the length is L ', and the calculated area S ' =c ' ×l '; the symbol of Zn content in the galvanized metal material is omega' 1.
As a further preferable scheme, the quantitative detection method for the zinc impregnation amount of the metal material based on the element content further comprises the step of calculating zinc loss:
The zinc loss meter is Zn, （6）。
In a further preferred scheme, in the quantitative detection method for the zinc impregnation amount of the metal material based on the element content, the metal material is one of an aluminum alloy material, a magnesium alloy material, a steel material and the like, and the mass of a detection object is 3-5g.
Compared with the prior art, the invention has the beneficial effects that:
1. According to the quantitative detection method for the zinc impregnation amount of the metal material based on the element content, disclosed by the embodiment of the application, the mass fraction of Zn element in the metal material before and after zinc impregnation is directly tested, and the mass of zinc in unit area, namely the zinc impregnation amount, can be accurately calculated by combining basic parameters (such as mass and length) of an object to be detected; errors possibly caused by indirect deduction are avoided, and the accuracy of zinc impregnation measurement is ensured.
2. In the quantitative detection method for the zinc impregnation amount of the metal material based on the element content, the measurement process is based on the actual content of Zn element, and is beneficial to providing reliable data support in the aspects of quality control, material selection, process optimization and the like.
3. The quantitative detection method of the zinc impregnation amount of the metal material based on the element content is not only suitable for the metal material after zinc spraying treatment, but also suitable for the metal material after zinc plating and other zinc impregnation processes; whether steel, nonferrous metal or alloy material, the quantitative detection of the zinc impregnation amount can be realized by measuring the mass fraction of Zn element by a proper test means.
4. According to the quantitative detection method for the zinc impregnation amount of the metal material based on the element content, the thickness and uniformity of the zinc impregnation layer can be known by measuring the zinc impregnation amount, so that the effect of zinc impregnation treatment is evaluated; has important significance for guiding the adjustment of technological parameters in the production process, optimizing the zincification treatment process and improving the product quality.
The present invention will be described in further detail with reference to the following embodiments.
Drawings
FIG. 1 is a calculation flow chart of a quantitative detection method of the zinc impregnation amount of the metal material based on the element content;
FIG. 2 is a graph comparing calculated data with XRF thickness measurement data of a quantitative detection method of zinc impregnation amount of a metal material based on element content.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described in the following in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The terms "comprises" and "comprising" and their equivalents, when used in this specification and claims, are intended to cover a non-exclusive inclusion, such that a process or element is not described, but is inherent to the product, method, or structure, but is included in the application that is expressly described in the specification and claims.
The embodiment of the application provides a quantitative detection method for the zinc impregnation amount of a metal material based on element content, which comprises the following steps of
And (3) component detection: testing the mass fraction of Zn element in the metal material before zinc spraying or zinc plating; after zinc spraying or zinc plating is carried out on the metal material, the metal material subjected to zinc impregnation is obtained through heat treatment and is used as an object to be detected, and the mass fraction of Zn element in the object to be detected is tested;
Basic parameter measurement: measuring quality and length parameters of an object to be detected, and calculating the perimeter of the detected object;
And (3) data calculation: and calculating the ratio of the mass of zinc in the unit to the surface area of the object to be detected as the zinc impregnation amount, and obtaining the zinc impregnation amount in the metal material.
As a further preferable scheme, in the data calculation process of the embodiment of the application, the zinc impregnation amount is calculated as P and the unit is g/m 2 by adopting the following formula:
（1）；
In the formula (1), M Zn is the mass of zinc, and the unit is g; m Zn can be calculated by the following formula:
MZn=（ω1-ω0）×m（2）；
In the formula (2), omega 1 is the mass fraction of Zn element in the object to be detected, and the unit is wt%; omega 0 is the mass fraction of Zn element in the metal material before zinc spraying, and the unit is wt%; m is the mass of an object to be detected; considering the mass fraction (omega 0) of Zn element in the metal material before zinc spraying, the method is helpful for more accurately evaluating the increase of Zn element content on the surface of the material by zinc impregnation treatment, and the calculated zinc mass can exclude the interference of Zn element in the matrix.
In the above formula (1), S is a zincification surface area, unit m 2, calculated by the following formula (3): s=c×l (3);
In the formula (3), C is the perimeter of the object to be detected, and the unit is m; l is the length of an object to be detected, and the unit is m; in the embodiment of the application, the zincification amount is calculated based on the zincification surface area (S), and the zincification surface area is calculated by the circumference (C) and the length (L) of the object to be detected, and the actual area of the surface of the material is considered, so that the calculation of the zincification amount is more in line with the actual situation.
Based on the basic parameters of the object to be detected and the component detection result, the zincification amount of the surface of the material after heat treatment can be calculated:
（4）。
The zinc impregnation amount (P) of the surface of the metal material after zinc impregnation can be accurately calculated through the calculation of the formulas (1) - (4), so that the zinc impregnation amount can be evaluated more accurately, and the quality control and process optimization in the production process can be facilitated. Accurate zinc impregnation measurement is helpful to ensure that the surface of the metal material has enough zinc layer thickness, thereby improving the corrosion resistance and the service life of the product, and is particularly important for the metal material which needs to be exposed to severe environments for a long time. The effect of the zincification treatment can be known by measuring the zincification amount, thereby guiding the adjustment of the technological parameters in the production process. For example, if insufficient zinc impregnation is found, parameters such as zinc spraying time, temperature and the like can be adjusted to improve the zinc impregnation effect.
In the research, the calculation result of the zinc impregnation amount is closely related to the zinc spraying process on the metal surface, and factors such as the thickness of spraying, the uniformity of spraying, the spraying mode and the like can influence whether the finally calculated zinc impregnation amount is accurate or not. For example, the larger the spray thickness, the more zinc layer mass is attached per unit area, and the amount of zinc impregnation increases accordingly. If the spraying is uneven, there is caused a deviation in the calculation result of the amount of zincification, because the amount of zincification is calculated on a per unit area basis. Different spray patterns (such as thermal spray, electrostatic spray, etc.) affect the adhesion of the zinc layer and the calculation of the zinc impregnation. In the present application, the zinc spraying process used in some embodiments includes the steps of:
Melting pure zinc into liquid zinc, placing the liquid zinc in high-temperature resistant spraying equipment, keeping the fluidity of the liquid zinc, and placing a metal material to be treated in front of a spray head, wherein the distance between the surface of the metal material and the spray head is 2-10 cm; starting the spraying equipment, setting the pressure of the spraying equipment between 5 and 6Kg/cm 2, rapidly extruding the liquid Zn to cover the surface of the metal material in front of the spray head, controlling the amount of sprayed Zn by spraying the mass and the maximum surface area of the liquid Zn, and naturally cooling to room temperature after the zinc spraying is finished to obtain the metal material with the zinc coated surface. For example, when Zn0.08g is sprayed and the spray area is 0.01m 2, the Zn spray amount is 8g/m 2.
Further, in other embodiments, zinc plating is used to coat zinc on the metal surface, and the zinc plating process also affects the calculation result of the zinc impregnation amount of the metal material. The thickness of the zinc coating directly influences the calculation result of the zinc impregnation amount, for example, the heat and the electroplating can cause the zinc impregnation result of the metal material to be different, and the measurement and calculation of the thickness of the coating need to consider the influence of the technological parameters.
The galvanization process of the embodiment of the application adopts a magnetron sputtering mode, and the target material is a Zn target material with the purity more than 90 percent, and comprises the following steps:
vacuumizing: a Zn target is arranged in a coating cavity, a metal material is arranged in the coating cavity and opposite to the target, equipment is started, a molecular pump is started, and argon gas serving as a protective gas is filled after vacuumizing;
pre-plating: then starting pre-plating, blocking the surface of the metal material by using a baffle plate during pre-plating, plating for five minutes, and removing oxides and impurities on the surface of the Zn target material;
formal film plating: after the baffle is removed, formal film coating is started, the film coating speed is 6-7A/S, and the Zn spraying amount is controlled through the density of Zn and the thickness of magnetron sputtering Zn plating; and closing argon after Zn plating is completed, and deflating the cavity to obtain the metal material with the zinc coated surface.
In the above scheme, in the specific embodiment of the application, when the vacuum degree reaches 10 -4 MPa, argon is filled as a protective gas, the vacuum degree is controlled to be 0.4-0.5 MPa when the argon is filled, and then pre-coating is started for five minutes; in the formal coating process, the coating speed is 6-7A/S, the Zn spraying amount is controlled by the density of Zn and the thickness of magnetron sputtering Zn, for example, the coating thickness is 1 mu m, the density of Zn is 7.14g/cm 3, and the Zn spraying amount is 7.14g/m 2.
The heat treatment of the metal surface is an important factor influencing the zinc impregnation effect, the zinc impregnation layer is influenced by temperature in the heat treatment process, and the zinc element in the zinc impregnation layer and other elements in the base material react to form a new compound or alloy layer due to the excessively high temperature, so that the chemical composition and physical properties of the zinc impregnation layer can be changed, and the calculation result of the zinc impregnation amount is influenced. An excessively long heat treatment time may cause excessive diffusion of zinc element in the zinciferous layer into the substrate, thereby reducing the zinc content of the zinciferous layer. The choice of color medium in the heat treatment process may also affect the calculation result of the zinc impregnation amount, and different media may have different effects on the zinc impregnation layer, such as changing the chemical composition, structure or morphology of the zinc impregnation layer. The cooling process after heat treatment may also affect the calculation result of the zincification amount, and rapid cooling may cause an increase in stress in the zincification layer, thereby affecting the stability and corrosion resistance of the zincification layer. As a further preferable scheme, the heat treatment adopted in the embodiment of the application comprises the following steps: the heat treatment uses a medium temperature furnace, the temperature is set to 550-650 ℃, the temperature of the sample is raised along with the furnace, the temperature is kept for 2-8min after the temperature is reached, and then the temperature is reduced along with the furnace. Because of the high Zn concentration of the surface Zn layer and the low Zn concentration of the aluminum alloy, zn atoms can enter the aluminum alloy matrix according to the principle of diffusion from high concentration to low concentration in the Phake law under the conditions of concentration gradient difference and kinetic energy provided by heat treatment.
Inductively Coupled Plasma (ICP) technology detects elemental mass fractions in metals, and mainly uses plasma generated by a high frequency electromagnetic field to excite and ionize a sample, thereby generating a characteristic spectrum. The wavelength and intensity of these characteristic spectra are related to the type and content of the elements in the sample, so the content of the various elements in the sample can be determined by detecting and analyzing these spectra. As a further preferable scheme, the quantitative detection method for the zinc impregnation amount of the metal material based on the element content adopts an inductively coupled plasma technology to test the mass fraction of Zn element in the metal material before zinc spraying or zinc plating and the object to be detected. The mass fraction of Zn element in the metal material before zinc spraying or zinc plating and the object to be detected is tested by adopting the inductively coupled plasma technology, and the specific steps are as follows: the metal to be measured is twisted into small particles with the diameter smaller than 2mm or scraps are taken, a zinc ICP-MS standard solution (HNO 3+H2 O) is used for digestion to obtain a clear solution, the clear solution is placed in ICP equipment, an argon ion body is used for testing, after a sample is converted into ions, a mass spectrometer is used for measurement, and the Zn content is directly obtained.
As a further preferable scheme, the quantitative detection method for the zinc impregnation amount of the metal material based on the element content further comprises the step of calculating the plating amount of the gold layer:
The said （5）；
In the above formula (5), M ' Zn is the mass of zinc plating on the surface of the metal material, the mass of the metal material before zinc impregnation is M ', the circumference of the metal material before zinc impregnation is C ', the length is L ', and the circumference S ' =c ' ×l ' is calculated; the symbol of Zn content in the galvanized metal material is omega' 1.
As a further preferable scheme, the quantitative detection method for the zinc impregnation amount of the metal material based on the element content further comprises the step of calculating zinc loss:
The zinc loss meter is Zn, （6）。
In a further preferred scheme, in the quantitative detection method for the zinc impregnation amount of the metal material based on the element content, the detection object is an aluminum alloy material or a surface zinc-spraying/zinc-aluminum alloy material without a zinc layer on the surface, and the mass of the detection object is 3-5g.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Example 1
The zinc loss amount of the zinc impregnation heat treatment is calculated, the basic parameter test result of the aluminum alloy material before the zinc impregnation is that the material section perimeter C= 0.0452m, the length L ' = 0.0995m and the mass m ' = 4.5044g are calculated to obtain the surface area S ' =0.0045 m 2;
The zinc spraying process is adopted to carry out zinc spraying treatment on the aluminum alloy material, and the zinc spraying process comprises the following steps: melting pure zinc into liquid zinc, placing the liquid zinc in high-temperature resistant spraying equipment, keeping the fluidity of the liquid zinc, and placing the metal material to be treated in front of a spray nozzle, wherein the distance between the surface of the aluminum alloy and the spray nozzle is 5cm; starting a spraying device, wherein the pressure of the spraying device is set between 5 and 6Kg/cm 2, and rapidly extruding liquid Zn to enable the liquid Zn to cover the surface of a metal material in front of a spray nozzle, wherein the Zn spraying amount is 8g/m 2;
Placing the aluminum alloy material into a heat treatment furnace after zinc spraying is completed, setting the temperature to 600 ℃, heating a sample along with the furnace, preserving heat for 3min after the temperature is reached, and then cooling along with the furnace; because the surface Zn layer has high Zn concentration, the aluminum alloy has low Zn concentration, under the conditions of concentration gradient difference and heat treatment providing kinetic energy, zn atoms can enter an aluminum alloy matrix according to the principle that substances are diffused from high concentration to low concentration in the Phake law; obtaining a zincified aluminum alloy material;
the basic parameter test result of the aluminum alloy material after zincification is that the material section perimeter C= 0.0452m, the length L=0.0100 m and the mass m= 4.3700g, and the surface area S=0.0045 m 2 is calculated; after the basic parameter test of the material is finished, digesting the galvanized aluminum alloy into molten metal liquid, then performing ICP test, and also performing digestion and ICP test on the aluminum alloy substrate with zinc-free surface, wherein the test results are shown in the following table:
Table 1: zinc content wt% of the aluminum alloy, the aluminum alloy before zincification, and the aluminum alloy after zincification in example 1
| Zn content omega in aluminum alloy 0 | 0.008 |
| Zn content omega 'in aluminum alloy before zinc impregnation' 1 | 0.54 |
| Zn content omega in aluminium alloy after zinc impregnation 1 | 0.25 |
According to the obtained basic parameters of the material and the detection result of the material components, the zinc layer plating rate of the aluminum alloy before the test object is galvanized in the embodiment is calculated to be 5.1g/m 2, and the zinc impregnation amount of the aluminum alloy after the zinc impregnation is 2.30g/m 2.
Example 2
In the embodiment, the zinc loss of the zinc impregnation heat treatment is calculated, the basic parameter test result of the aluminum alloy material before the zinc impregnation is that the material section perimeter C= 0.0452m, the length L ' = 0.0995m and the mass m ' = 4.5456g are calculated to obtain the surface area S ' =0.0045 m 2;
The aluminum alloy material is galvanized by adopting a magnetron sputtering mode, and the target material is Zn target material with purity more than 90 percent, and the method comprises the following steps: a Zn target is arranged in a coating cavity, a metal material is arranged in the coating cavity and opposite to the target, a device is started, a molecular pump is started, the vacuum pumping is carried out, protective gas argon is filled after the vacuum degree reaches 10 -4 MPa, and the vacuum degree is controlled to be 0.4-0.5 MPa when the argon is filled; then starting pre-plating, blocking the surface of the metal material by using a baffle plate during pre-plating, plating for five minutes, and removing oxides and impurities on the surface of the Zn target material; after the baffle is removed, formal film plating is started, the film plating speed is 6-7A/S, and the Zn plating amount is 7.14g/m 2; closing argon after Zn plating is completed, and deflating the cavity to obtain a metal material with a zinc coated surface;
Placing the aluminum alloy material into a heat treatment furnace after zinc spraying is completed, setting the temperature to 600 ℃, heating a sample along with the furnace, preserving heat for 3min after the temperature is reached, and then cooling along with the furnace; because the surface Zn layer has high Zn concentration, the aluminum alloy has low Zn concentration, under the conditions of concentration gradient difference and heat treatment providing kinetic energy, zn atoms can enter an aluminum alloy matrix according to the principle that substances are diffused from high concentration to low concentration in the Phake law; obtaining a zincified aluminum alloy material;
The basic parameter test result of the aluminum alloy material after the zinc impregnation is that the material length L=0.0100 m, the mass m= 4.5301g, the surface area S=0.0045 m 2 is calculated, the aluminum alloy before the zinc impregnation and the aluminum alloy after the zinc impregnation are digested into molten metal liquid after the basic parameter test of the material is finished, then ICP test is carried out, the aluminum alloy base material with the surface free of zinc is also digested and ICP test, and the test result is shown in the following table:
table 2: zinc content wt% of the aluminum alloy, the aluminum alloy before the zinc impregnation, the aluminum alloy after the zinc impregnation in example 2
| Zn content omega in aluminum alloy 0 | 0.008 |
| Zn content omega 'in aluminum alloy before zinc impregnation' 1 | 0.85 |
| Zn content omega in aluminium alloy after zinc impregnation 1 | 0.39 |
According to the obtained basic parameters of the material and the detection result of the material components, the zinc layer plating rate of the aluminum alloy before the test object is galvanized in the embodiment is calculated to be 8.45g/m 2, and the zinc impregnation amount of the aluminum alloy after the zinc impregnation is 3.82g/m 2.
Example 3
In the embodiment, the zinc loss of the zinc impregnation heat treatment is calculated, the basic parameter test result of the aluminum alloy material before the zinc impregnation is that the material section perimeter C= 0.0452m, the length L ' = 0.0995m and the mass m ' = 4.4533g are calculated to obtain the surface area S ' =0.0045 m 2; zinc spraying and heat treatment are carried out on the aluminum alloy material according to the process of the embodiment 1, so as to obtain the zinc-impregnated aluminum alloy material;
The basic parameter test result of the zinc-impregnated aluminum alloy material is that the material length L=0.0100 m, the mass m= 4.4267g, and the surface area S=0.0045 m 2 is calculated; after the basic parameter test of the material is finished, digestion is carried out on the aluminum alloy before zincification and the aluminum alloy after zincification into molten metal liquid, then ICP test is carried out, digestion and ICP test are also carried out on the aluminum alloy base material with the surface free of zinc, and the test results are shown in the following table:
table 3: zinc content wt% of the aluminum alloy, the aluminum alloy before the zinc impregnation, the aluminum alloy after the zinc impregnation in example 3
| Zn content omega in aluminum alloy 0 | 0.008 |
| Zn content omega 'in aluminum alloy before zinc impregnation' 1 | 1.13 |
| Zn content omega in aluminium alloy after zinc impregnation 1 | 0.57 |
According to the obtained basic parameters of the material and the detection result of the material components, the zinc layer plating rate of the aluminum alloy before the test object is galvanized in the embodiment is calculated to be 11.09g/m 2, and the zinc impregnation amount of the aluminum alloy after the zinc impregnation is 5.50g/m 2. The zinc loss during the zincification heat treatment is 5.59 g/m 2.
Comparative example 1
The comparative example uses XRF (X-ray fluorescence thickness gauge) to test the coating thickness, uses Zn standards for calibration before testing, and then tests the coating thickness without damaging the sample. The test object is the same batch of the same zinc-treated material in example 1. The surface zincification layer was not detected by XRF measurement of the aluminum alloy after the zincification heat at 0.01g/m 2.
Comparative example 2
The XRF was used to test the thickness of the coating for this comparative example, and the test object was the same batch of the same zincified material of example 2. The surface zincification layer was not detected by XRF measurement of the aluminum alloy after the zincification heat at 0.01g/m 2.
Comparative example 3
The XRF was used to test the thickness of the coating for this comparative example, and the test object was the same batch of the same zincified material of example 3. The surface zincification layer was not detected by XRF measurement of the aluminum alloy after the zincification heat at 0.01g/m 2.
Comparative example 4
The XRF was used to test the coating thickness for this comparative example, and the test object was the same batch of the same material as in example 1 prior to the zincification heat treatment. The zinc layer plating amount was 4.20g/m 2 as measured by XRF of the aluminum alloy before the zinc impregnation.
Comparative example 5
The comparative example uses XRF to test the coating thickness, and the test object is the same batch of example 1 before the same zinc impregnation heat treatment. The zinc layer plating amount was 7.07 g/m 2 as measured by XRF of the aluminum alloy before the zinc impregnation.
Comparative example 6
The XRF was used to test the coating thickness for this comparative example, and the test object was the same batch of the same material as in example 1 prior to the zincification heat treatment. The XRF of the aluminum alloy before the zincating heat measured a zinc coating plating amount of 9.54 g/m 2.
FIG. 2 is a graph comparing calculated data of the present application with XRF thickness measurement data, and it can be seen from comparative examples 4,5 and 6 that prior to zincification, the prior art XRF thickness measurement technique can more accurately test the zinc coating. However, in comparative examples 1,2 and 3 after zincification, the surface zinc layer disappeared due to diffusion of zinc into the inside and peeling of oxide formation, etc., and a zincification layer was formed, and the zincification amount could not be measured by using the conventional XRF thickness measuring technique, and it was difficult to determine the zincification amount. The embodiments 1,2 and 3 of the application can accurately calculate the zinc impregnation amount in the aluminum alloy after zinc impregnation.
The components listed in the present invention, and the upper and lower limits and interval values of the components of the present invention can all realize the present invention, and examples are not listed here. While the invention has been described with reference to certain specific embodiments, it should be understood that the description is only illustrative and not intended to limit the scope of the invention.
Claims (10)
1. A quantitative detection method for the zinc impregnation amount of a metal material based on element content is characterized by comprising the following steps,
And (3) component detection: testing the mass fraction of Zn element in the non-galvanized or non-galvanized metal material; after zinc spraying or zinc plating is carried out on the metal material, the metal material subjected to zinc impregnation obtained through heat treatment is used as an object to be detected, and the mass fraction of Zn element in the object to be detected is tested;
Basic parameter measurement: measuring quality and length parameters of an object to be detected, and calculating the perimeter of the detected object;
And (3) data calculation: and calculating the ratio of the mass of zinc in the unit to the surface area of the object to be detected as the zinc impregnation amount, and obtaining the zinc impregnation amount in the metal material.
2. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content, which is characterized in that in the data calculation process, the zinc impregnation amount is calculated by adopting the following formula, wherein the unit of the zinc impregnation amount is g/m 2:
（1）；
In the formula (1), M Zn is the mass of zinc, and the unit is g; m Zn can be calculated by the following formula:
MZn=（ω1-ω0）×m（2）；
In the formula (2), omega 1 is the mass fraction of Zn element in the object to be detected, and the unit is wt%; omega 0 is the mass fraction of Zn element in the metal material before zinc spraying, and the unit is wt%; m is the mass of an object to be detected;
In the above formula (1), S is a zincification surface area, unit m 2, calculated by the following formula (3): s=c×l (3);
in the formula (3), C is the perimeter of the object to be detected, and the unit is m; l is the length of an object to be detected, and the unit is m;
Based on the basic parameters of the object to be detected and the component detection result, the zincification amount of the surface of the material after heat treatment can be calculated:
（4）。
3. the quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 2, wherein the step of zinc spraying the metal material is as follows:
Melting pure zinc into liquid zinc, placing the liquid zinc in spraying equipment, keeping the fluidity of the liquid zinc, and placing a metal material to be treated in front of a spray head, wherein the distance between the surface of the metal material and the spray head is 2-10 cm; starting the spraying equipment, setting the pressure of the spraying equipment to be 5-6Kg/cm 2, extruding liquid Zn to cover the surface of the metal material in front of the spray head, controlling the amount of sprayed Zn by spraying the mass and the maximum surface area of the liquid Zn, and naturally cooling to room temperature after the zinc spraying is finished to obtain the metal material with the zinc coated surface.
4. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 2, wherein the metal material is galvanized by a magnetron sputtering mode, and the target is a Zn target with the purity of more than 90 percent, and the method comprises the following steps:
vacuumizing: a Zn target is arranged in a coating cavity, a metal material is arranged in the coating cavity and opposite to the target, equipment is started, a molecular pump is started, and argon gas serving as a protective gas is filled after vacuumizing;
pre-plating: then starting pre-plating, blocking the surface of the metal material by using a baffle plate during pre-plating, plating for five minutes, and removing oxides and impurities on the surface of the Zn target material;
formal film plating: after the baffle is removed, formal film coating is started, the film coating speed is 6-7A/S, and the Zn spraying amount is controlled through the density of Zn and the thickness of magnetron sputtering Zn plating; and closing argon after Zn plating is completed, and deflating the cavity to obtain the metal material with the zinc coated surface.
5. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 3 or 4, wherein the heat treatment comprises the following steps: and (3) placing the metal material with the zinc coated surface into a heat treatment furnace, setting the temperature to 550-650 ℃, preserving the heat for 2-8min after the temperature reaches the set temperature, and then cooling along with the furnace to finish the heat treatment.
6. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 2, wherein the mass fraction of Zn element in the metal material before zinc spraying or zinc plating and the object to be detected is tested by adopting an inductively coupled plasma technology.
7. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 6, wherein the specific steps of using an inductively coupled plasma technology to test the mass fraction of Zn elements in the metal material before zinc spraying or zinc plating and the object to be detected are as follows:
The metal material before zinc spraying or zinc plating and the object to be detected are respectively twisted into particles or scraps, the particles or scraps are digested by using a zinc ICP-MS standard solution to obtain a clear solution, the clear solution is placed in ICP equipment for testing, an argon ion body is used for testing, after the sample is converted into ions, a mass spectrometer is used for measuring, and the mass fraction of Zn is directly obtained.
8. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 2, further comprising the step of calculating the plating amount of the zinc layer:
The said （5）；
In the above formula (5), M ' Zn is the mass of zinc plating on the surface of the metal material, the mass of the metal material before zinc impregnation is M ', the circumference of the metal material before zinc impregnation is C ', the length is L ', and the surface area S ' =c ' ×l ' is calculated; the symbol of Zn content in the galvanized metal material is omega' 1.
9. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 8, further comprising the step of calculating zinc loss:
The zinc loss meter is Zn, （6）。
10. The quantitative detection method for the zinc impregnation amount of the metal material based on the element content according to claim 2, wherein the metal material is one of an aluminum alloy material, a magnesium alloy material and a steel material, and the mass of the detection object is 3-5g.
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