CN115044943A - Method for manufacturing metal alloy layer stack - Google Patents
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/003—3D structures, e.g. superposed patterned layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
Abstract
The invention relates to a method for manufacturing a metal alloy layer stack, belonging to the field of material coatings. Provided is a method for manufacturing a metal alloy laminate, comprising: preparing a first laminated subunit through electrodeposition, wherein the first laminated subunit has a positive electrode potential and is formed on a substrate or a subunit with a negative electrode potential; a second laminate sub-unit is prepared by electrodeposition, the second laminate sub-unit being at a more negative electrode potential and formed over an electrode potential-more positive sub-unit. The first lamination body and the second lamination body have obvious electrode potential difference, the thickness is in a nanometer level, the abrasion resistance and the corrosion resistance of the lamination body are improved, the process flow is simplified, and the production efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of material coatings, and relates to a manufacturing method of a metal alloy layer stack.
Background
In recent years, with the increase of the manufacturing level and the processing level of materials, various materials are beginning to be used in severer environments, or the requirements on the material performance of the traditional service environment are stricter and more severe, such as a high-pressure high-salt deep sea environment, an aviation environment with high temperature and high load, a high-temperature high-radiation nuclear industry environment and the like. Materials in service in these environments inevitably suffer degradation and failure due to the various environmental conditions mentioned above, and the most important failure mode is wear and corrosion of the materials.
At present, one of the measures taken to prevent the wear, corrosion and failure of materials is to use an electrodeposited wear-resistant and corrosion-resistant coating to protect a base material so as to prolong the service life of the base material. For example, electrodeposition of hexavalent chromium is used in metallurgical crystallizers, electrodeposition of cadmium is used in aircraft, and electrodeposition of zinc-nickel alloys is used in automotive parts. However, hexavalent chromium, metallic cadmium, has polluting and toxic properties; the electrodeposited zinc and nickel are relatively environment-friendly, but the wear resistance of the existing process is poor, and the comprehensive performance needs to be further improved.
Disclosure of Invention
In view of the above, the present invention is directed to a method for manufacturing a metal alloy laminate, which can solve the problem of preventing the material from corrosion failure due to wear.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for manufacturing a metal alloy layer stack, comprising:
preparing a first laminated subunit through electrodeposition, wherein the first laminated subunit has a positive electrode potential and is formed on a substrate or a subunit with a negative electrode potential;
a second laminate sub-unit is prepared by electrodeposition, the second laminate sub-unit being at a more negative electrode potential and formed over an electrode potential-more positive sub-unit.
Alternatively, different metal ions in the dielectric solution used for electrodeposition possess a significant electrode potential difference.
Optionally, the volume fraction of the ceramic particles in the dielectric solution used for electrodeposition is 0-25%.
Optionally, the ceramic particles comprise at least one of: oxides, carbides, nitrides.
Optionally, the step of preparing by electrodeposition comprises: outputting periodic variable current, and controlling the current density in the electrodeposition preparation process to be 0.5-15A/dm 2 。
Optionally, after the step of preparing a second laminate subunit by electrodeposition and placing the second laminate subunit on top of the first laminate subunit to form a metal alloy laminate unit, the method further comprises:
and carrying out sealing and passivating treatment on the metal alloy laminated body.
Optionally, the step of preparing by electrodeposition further comprises: the stirring device controls the time length and the strength of the clockwise and anticlockwise rotation period of the solution, and the turning period is 40-100 seconds.
Optionally, the constituent material of the laminate includes two or more of Ni, Cu, Co, P, Cr, Fe, or Zn.
Optionally, after the step of preparing a second stack subunit by electrodeposition, and placing the second stack subunit on the first stack subunit to form the metal alloy laminate unit, the method further includes:
and stacking from bottom to top to form a plurality of metal alloy laminated body units.
Optionally, the number of the metal alloy laminated units is 3 to 100.
The invention has the beneficial effects that:
the metal laminated body with obvious electrode potential difference between adjacent subunits is prepared by electrodeposition, so that the wear resistance and corrosion resistance are improved, the process flow is simplified, and the production efficiency is improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof.
Drawings
For a better understanding of the objects, aspects and advantages of the present invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic flow chart of a method for manufacturing a metal alloy layer stack;
FIG. 2 is a schematic structural view of a metal alloy laminate;
FIG. 3 is a schematic view of the composition distribution of a metal alloy laminate;
FIG. 4 is a graph comparing hardness of the samples.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the drawings provided in the following embodiments are only for illustrating the basic idea of the present invention in a schematic way, and the features in the following embodiments and examples may be combined with each other without conflict.
Wherein the showings are for the purpose of illustrating the invention only and not for the purpose of limiting the same, and in which there is shown by way of illustration only and not in the drawings in which there is no intention to limit the invention thereto; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by terms such as "upper", "lower", "left", "right", "front", "rear", etc., based on the orientation or positional relationship shown in the drawings, it is only for convenience of description and simplification of description, but it is not an indication or suggestion that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes, and are not to be construed as limiting the present invention, and the specific meaning of the terms may be understood by those skilled in the art according to specific situations.
Example 1
Referring to fig. 1, the present invention provides a method for manufacturing a metal alloy laminate, including:
s1: preparing a first laminated subunit by electrodeposition, wherein the first laminated subunit has a positive electrode potential and is formed on a substrate or a subunit with a negative electrode potential;
s2: a second laminate sub-unit is prepared by electrodeposition, the second laminate sub-unit being at a more negative electrode potential and formed over an electrode potential-more positive sub-unit.
The metal laminated body with obvious electrode potential difference between adjacent subunits is prepared by electrodeposition, so that the wear resistance and corrosion resistance are improved, the process flow is simplified, and the production efficiency is improved.
In some embodiments, the dielectric solution used for electrodeposition includes a metal salt containing a corresponding metal ion, nano-sized ceramic particles, a conductive salt enhancing ionic conductivity in the solution, a complexing agent maintaining stable dispersion of the metal ion in the solution, various additives improving the surface quality of the laminate, and the like. The PH of the solution may be adjusted by adding an acid or alkali solution having the effect of adjusting the PH, and a PH buffer such as boric acid may be added to stabilize the solution environment during the preparation of the laminate. Ceramic particles with nano-scale sizes can be added, and the comprehensive addition amount of the ceramic particles is 5-50 g/L. Preferably, the addition amount is 15-25 g/L. After the ceramic particles are added, in order to ensure that the ceramic particles are uniformly dispersed in the solution, an energy-gathering ultrasonic crusher is used for carrying out ultrasonic dispersion on the ceramic particles in the solution before preparation. The power is about 20-100W, and the time is about 1-5 h. Preferably, the power is 30-60W, and the time is 1.5-2 h.
In some embodiments, the ceramic particles comprise at least one of: oxides, carbides, nitrides. Aluminum oxide, silicon carbide, titanium carbide, silicon nitride, boron nitride may be selected.
Optionally, the step of preparing by electrodeposition comprises: outputting periodic variable current, and controlling the current density in the electrodeposition preparation process to be 0.5-15A/dm 2 . Preferably, the current density is 1 to 7A/dm 2 。
Optionally, after the step of preparing a second stack subunit by electrodeposition, and placing the second stack subunit on the first stack subunit to form the metal alloy laminate unit, the method further includes:
and sealing and passivating the first stack subunit and the second stack subunit.
Optionally, the step of preparing by electrodeposition further comprises: the stirring device controls the time length and the strength of the clockwise and anticlockwise rotation period of the solution, and the turning period is 40-100 seconds, preferably 50-60 seconds.
Optionally, after the step of preparing a second stack subunit by electrodeposition, and placing the second stack subunit on the first stack subunit to form the metal alloy laminate unit, the method further includes:
and stacking from bottom to top to form a plurality of metal alloy laminated body units.
Optionally, the number of the metal alloy laminated units is 3 to 100. The thicknesses of different sub-units in the plurality of metal alloy laminated body units can be the same or different. 20 to 2000nm, preferably 50 to 500nm, in the same case; in different cases, the electrode potential is more positive, i.e. the thickness of the more inactive subcell is thicker, which is 1.5 to 5 times, preferably 2 to 3 times, the thickness of the active subcell.
Example 2
This example uses Q-235 steel as the substrate for carrying the laminate structure. The dimensions are 25X 25mm and the thickness is 3 mm.
The specific operations in this example are as follows:
1. and in order to ensure that the laminated body is deposited on the substrate in a smooth manner, a grinding and polishing device is adopted to grind and polish the deposition surface of the substrate. And the grinding and polishing respectively adopt 180-mesh, 400-mesh and 800-mesh silicon carbide sand paper, so that the flatness of the surface of the ground substrate after grinding and polishing is less than Ra0.05 mu m.
2. In order to remove oil stain and an oxidation film of a Q-235 matrix, oil is removed in ethanol, alkali liquor and acid liquor respectively. Wherein the ethanol is used for removing abrasive grains remained on the matrix after polishing, and is matched with an ultrasonic cleaning machine for use, and the treatment time is 10 min. The alkali liquor consists of 15g/L of sodium hydroxide solution and 15g/L of sodium carbonate solution, the temperature is 80 ℃, and the treatment time is 10 min. The acid solution consists of 5% dilute sulfuric acid, the temperature is room temperature, and the treatment time is 10 s. After treatment in alkaline solution and acid solution, the substrate was thoroughly washed with deionized water.
3. And packaging the back of the substrate by using an insulating adhesive tape and a copper conduction band, so that all surfaces except the deposition surface of the substrate are coated with insulation.
4. After the package is degreased, electrodeposition is performed on the surface of the substrate for a corresponding time using the ingredients and process parameters in table 1.
TABLE 1
In this embodiment, different subunit structures with distinct differences in composition and electrode potential are deposited by periodically varying the current density applied to the electrolyte solution. Specifically, there are two sub-layers with significant differences, which are arranged in a periodic alternating manner.
The preparation method comprises the following steps: using the dielectric systems and parameters in Table 1, after energization, at 2A/dm 2 Electrodepositing for 180s under current density to finish the deposition of the subunit 1; then switched to 4A/dm 2 And (5) electrodepositing for 90s under the current density to finish the deposition of the subunit 2.
And controlling the output power supply through the process sequence, and repeatedly carrying out the operations until the target thickness is reached. In the examples, the deposition time was 225min, and 50 each of the subelement 1 and subelement 2 structures were obtained, each having a thickness of about 680nm, and a total thickness of about 34 μm in total, which was a copper-nickel alloy coating in a laminate structure.
And (3) performing section microscopic scanning on the deposited laminated body, wherein figure 2 is a section appearance diagram after slight corrosion is performed by using a ferric trichloride solution, and figure 3 is a component distribution result represented by EDS (electron-dispersive spectroscopy) scanning on the section when the section is not corroded. It can be seen that the as-deposited structure is made up of two different subcell layers that exhibit significant differences in Cu content, which overlap.
Comparative examples 1 to 3
Meanwhile, using the dielectric system and parameters in Table 1, 2A/dm was employed, respectively 2 、3A/dm 2 、4A/dm 2 The electrodeposition time was 300min, 225min and 150min, respectively, to obtain single-structure structures having a total thickness of about 34 μm, comparative examples 1, 2 and 3, respectively.
Evaluation of Performance
The examples and comparative examples were subjected to hardness and abrasion resistance tests.
The hardness of the structure was measured by a Vickers hardness tester with a load of 50N, and the same sample was subjected to averaging at 9 points of left, middle and right sides, respectively, and compared.
A comparison of the hardness of the different samples is thus obtained, as shown in fig. 4, where the abscissa represents the different samples and the ordinate represents the hardness.
And (3) detecting by using a reciprocating friction tester and a friction wear detector. Under the condition of no lubrication, silicon carbide ceramic balls are used
The load was 15N, the moving distance was 5mm, the temperature was 25 ℃ and sliding friction was performed for 60 min. And then, detecting the abrasion loss by using a frictional abrasion detector, and carrying out detection for 5 times to obtain an average value.
A comparison of the wear resistance of the different samples is thus obtained, as shown in table 2.
TABLE 2
| Test specimen | Base material | Coefficient of friction | Amount of wear, mm 3 |
| Example 1 | Q-235 | 0.423 | 0.0092±0.0023 |
| Comparative example 1 | Q-235 | 0.612 | 0.0303±0.0069 |
| Comparative example 2 | Q-235 | 0.643 | 0.0282±0.0076 |
| Comparative example 3 | Q-235 | 0.598 | 0.0259±0.0036 |
The hardness and the wear amount reflect the wear resistance of the material, and generally, the greater the hardness, the more excellent the wear resistance of the material with the smaller wear amount. According to the comparison between the embodiment and the comparative example, the abrasion resistance of the structure can be obviously improved by adopting the laminated structure design.
Electrochemical tests were performed on the examples and comparative examples.
Paraffin wax and rosin 1: 1 the mixed sealant was sealed to the samples, each sample leaving a region of 1cm x 1cm in the middle for testing. The test is carried out according to the sequence of open circuit potential, polarization impedance, self-corrosion potential and corrosion current density. The measuring system is a three-electrode system, wherein the reference electrode is a saturated potassium chloride calomel electrode, and the working electrode is a corresponding sample.
TABLE 3
Polarization resistance versus corrosion current density can be evaluated for a material's ability to resist corrosion. The higher the polarization resistance, the lower the corrosion current density, which indicates that the material has a greater resistance to corrosion, and the lower the corrosion rate at which corrosion occurs, thus having better corrosion properties.
From the results in table 3, the laminate represented by the example shows a significant advantage of 1 to 2 times as compared with the single structure in both polarization resistance and corrosion current density. Meaning that the laminate construction possesses better corrosion resistance.
Finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A method for manufacturing a metal alloy layer stack, comprising:
preparing a first laminated subunit by electrodeposition, wherein the first laminated subunit has a positive electrode potential and is formed on a substrate or a subunit with a negative electrode potential;
a second laminate sub-unit is prepared by electrodeposition, the second laminate sub-unit being relatively negative in electrode potential and formed over the positive electrode potential sub-unit.
2. The method of claim 1, wherein the second laminate sub-unit electrode potential is more positive than the second laminate unit.
3. The method for producing a metal alloy laminate according to claim 1, wherein a volume fraction of ceramic particles in a dielectric solution for electrodeposition is 0 to 25%, and the ceramic particles include at least one of: oxides, carbides, nitrides.
4. The metal alloy laminate manufacturing method of claim 1, wherein the step of preparing by electrodeposition comprises: outputting periodic variable current, and controlling the current density in the electrodeposition preparation process to be 0.5-15A/dm 2 。
5. The metal alloy laminate manufacturing method of claim 1, wherein after the step of forming a metal alloy laminate unit by preparing a second stack sub-unit by electrodeposition and placing the second stack sub-unit over the first stack sub-unit, further comprising:
and sealing and passivating the first stack subunit and the second stack subunit.
6. The metal alloy laminate manufacturing method of claim 1, wherein the step of preparing by electrodeposition further comprises: the stirring device controls the time length and the strength of the clockwise and anticlockwise rotation period of the solution, and the turning period is 40-100 seconds.
7. The method of manufacturing a metal alloy laminate according to claim 1, wherein the constituent materials of the laminate comprise two or more of Ni, Cu, Co, P, Cr, Fe, or Zn.
8. The metal alloy laminate manufacturing method of claim 1, wherein after the step of forming a metal alloy laminate unit by preparing a second stack sub-unit by electrodeposition and placing the second stack sub-unit over the first stack sub-unit, further comprising:
and stacking from bottom to top to form a plurality of metal alloy laminated body units.
9. The method for producing a metal alloy laminate according to claim 8, wherein the number of metal alloy laminate units is 3 to 100.
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