CN108672706B - Preparation process of stainless steel fiber micro powder - Google Patents
Preparation process of stainless steel fiber micro powder Download PDFInfo
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- CN108672706B CN108672706B CN201810446694.XA CN201810446694A CN108672706B CN 108672706 B CN108672706 B CN 108672706B CN 201810446694 A CN201810446694 A CN 201810446694A CN 108672706 B CN108672706 B CN 108672706B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/062—Fibrous particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/045—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling
- B22F2009/046—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling by cutting
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Abstract
The invention provides a preparation process of stainless steel fiber micro powder, which comprises the following steps: pretreating a stainless steel wire, drawing by a bundling drawing method, shearing, cleaning, baking, screening and obtaining a finished product; according to the invention, after stainless steel wires are pretreated, and bundle drawing is adopted, the stainless steel fibers are not easy to break; according to the invention, after the stainless steel wire is pretreated, the prepared stainless steel has smaller crystal grains, so that the performance of the stainless steel is more excellent.
Description
Technical Field
The invention relates to the technical field of micro powder manufacturing, in particular to a preparation process of stainless steel fiber micro powder.
Background
The stainless steel fiber is a novel industrial material, not only has the performances of high electric conductivity, high heat conductivity, high strength, high temperature resistance, corrosion resistance and the like, but also has the characteristics of chemical fiber and synthetic fiber; the method is widely applied to the industrial fields of petroleum, chemical industry, chemical fiber, electronics, textile, military, aviation, high polymer materials, environmental protection and the like.
The stainless steel fiber is generally made by using 316L steel grade stainless steel as a base material and through a set of special processes of composite assembly, multiple bundling drawing, annealing, solution treatment and the like, wherein each strand is thousands or tens of thousands of stainless steel fibers. The stainless steel fiber has very large surface area, so that the stainless steel fiber has extraordinary performance in the aspects of internal structure, magnetism, heat resistance, melting point and the like. The stainless steel fiber diameter can reach 1-2 microns, the elongation is more than 1%, and the fiber strength can reach 1200-1800MPa and even exceeds the tensile strength of the material.
The bundling drawing is the main method for the present micron-sized metal fiber engineering preparation, dozens or even tens of thousands of metal wires are wrapped in a cylinder for drawing, so that simultaneous reducing of a plurality of metal wires is realized, and when the required fiber diameter is drawn, the wrapping tube is stripped to separate the fibers.
In actual production, as the grain size of the material is reduced, the higher the strength is, the lower the plasticity is, and the more difficult the processing is; meanwhile, as the silk warp becomes smaller, a great amount of silk breakage phenomenon occurs in the fiber.
In view of the above situation, the present invention provides a preparation process of stainless steel fiber micropowder to solve the above problems.
Disclosure of Invention
In view of the above situation, the present invention provides a preparation process of stainless steel fiber micropowder, comprising the steps of:
the method comprises the steps of stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product obtaining.
As an embodiment of the present invention, the step of pretreating the stainless steel wire comprises:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
As an embodiment of the present invention, the step S01 includes the following specific steps: polishing and cleaning the surface of the stainless steel wire as the raw material, and then placing the stainless steel wire in electrolyte for nano construction.
As an embodiment of the present invention, the step S02 includes the following specific steps: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
As one embodiment of the present invention, the electrolytic copper plating solution is an alkaline copper solution.
As an embodiment of the present invention, the main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
As an embodiment of the present invention, the secondary plating process in step S03 is to use the stainless steel wire after the electroplating process as a template, place the template in a carbon source environment, and perform a heat treatment to obtain a pretreated stainless steel wire.
In one embodiment of the present invention, the amount of deformation in the bundle drawing method is 50% to 60%.
In one embodiment of the present invention, the shearing is performed by shearing the copper wire in a length required for the fine powder.
In one embodiment of the present invention, the stainless steel fiber fine powder has a particle size of 1 to 3 μm.
Has the advantages that:
1. according to the invention, after stainless steel wires are pretreated, and bundle drawing is adopted, the stainless steel fibers are not easy to break;
2. according to the invention, after the stainless steel wire is pretreated, the prepared stainless steel has smaller crystal grains, so that the performance of the stainless steel is more excellent.
Drawings
FIG. 1: scanning electron microscopy spectra of stainless steel fibers of example 1.
FIG. 2: scanning electron microscopy spectra of stainless steel fibers of example 5.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The invention provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
the method comprises the steps of stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product obtaining.
Pretreatment of stainless steel wire
In the invention, the stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 30-45V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in sodium dihydrogen phosphate solution as electrolyte for secondary anodic oxidation with the voltage range of 10-35V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. During the anodic oxidation, the temperature of the electrolyte is passed through the ice-water mixtureMaintained at 0-10 ℃.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio of the complexing agent to the complexing agent is 0.4: 1.
the specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
Bundle drawing method
The metal fiber is an important functional material, the bundling drawing is a main method for the current micron-sized metal fiber engineering preparation, dozens or even tens of thousands of metal wires are wrapped in a cylinder for drawing, the simultaneous reducing of a plurality of metal wires is realized, and when the required fiber diameter is drawn, a wrapping pipe is stripped off to separate the fiber.
The stainless steel wires are pretreated and then are filled into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 2800 and 3200 cores; the drawing is to compact the loaded copper pipe, then draw, and anneal when the deformation reaches 50% -60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation amount reaches 50-60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
The mechanism is explained as follows: after the stainless steel is pretreated, the breakage of the prepared stainless steel fiber micro powder can be effectively avoided, the grain size of the stainless steel fiber micro powder is about 20nm, and the grain size of the prepared stainless steel fiber micro powder is about 1-3 mu m; the reason is that the cluster drawing method generates severe plastic deformation under the action of shearing force, the fibers are mutually bonded, and the treated stainless steel wire has excellent low surface energy under the drawing; meanwhile, after the crystal material is deformed, defects such as vacancies, dislocations and the like can be generated inside the crystal material, and the defects can cause the free energy of the material to be increased and be in an unstable state.
Embodiment 1. a preparation technology of stainless steel fiber micro powder, the preparation technology comprises the following steps:
the method comprises the steps of stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product obtaining.
In embodiment 2, further, in the preparation process of the stainless steel fiber micropowder, the step of the pretreatment of the stainless steel wire is as follows:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
Embodiment 3 further, in the preparation process of the stainless steel fiber micropowder, the specific step of the step S01 is: polishing and cleaning the surface of the stainless steel wire as the raw material, and then placing the stainless steel wire in electrolyte for nano construction.
Embodiment 4 further, in the preparation process of the stainless steel fiber micropowder, the specific step of the step S02 is: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
Embodiment 5 further, in the preparation process of the stainless steel fiber micro powder, the copper electroplating solution is an alkaline copper solution.
Embodiment 6 further, in the preparation process of the stainless steel fiber micro powder, the main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Embodiment 7, in the preparation process of the stainless steel fiber micropowder, the secondary coating process in the step S03 is to use the stainless steel wire after electroplating as a template, place the template in a carbon source environment, and perform heat treatment to obtain the pretreated stainless steel wire.
Embodiment 8 further provides a process for producing a stainless steel fiber fine powder, wherein the amount of deformation in the cluster drawing method is 50% to 60%.
Embodiment 9 further, in the process for preparing the stainless steel fiber micropowder, the shearing is to shear the copper wire according to the length required by the micropowder.
Embodiment 10 further provides the process for producing a fine stainless steel fiber powder, wherein the fine stainless steel fiber powder has a particle size of 1 to 3 μm.
The following will describe the process for preparing the stainless steel fiber micropowder provided by the present invention in detail with reference to specific examples, and the raw materials for the preparation provided by the present invention are all commercially available except for specific descriptions.
Example 1: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 40V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in a sodium dihydrogen phosphate solution as an electrolyte for secondary anodic oxidation with the voltage range of 25V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. Temperature of the electrolyte during anodic oxidationMaintained at 0-10 ℃ by an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 2: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 30V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in a sodium dihydrogen phosphate solution as an electrolyte for secondary anodic oxidation with the voltage range of 10V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. In the anodic oxidationIn the process, the electrolyte solution is stirred by the rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. During the anodization process, the temperature of the electrolyte was maintained at 0-10 ℃ by an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 2800 cores; the drawing is to compact the installed copper pipe, then draw, and when the deformation reaches 50%, carry out annealing treatment to soften the stainless steel wire for preparing the drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 50%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 3: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 45V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; then placing the dried sample in sodium dihydrogen phosphate solution as electrolyte to make secondary anodic oxidation, voltage range is 35V, then placing the above-mentioned sample in acetone and acetone respectivelyUltrasonically cleaning in water ethanol and secondary distilled water, and drying in air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. During the anodization process, the temperature of the electrolyte was maintained at 0-10 ℃ by an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3200 cores; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 55%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 55%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 4: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, electroplating the stainless steel wire;
the electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3With trimethylolpropane triacrylateThe molar ratio is 0.4: 1.
the stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 5: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, electroplating the stainless steel wire;
the copper electroplating solution is an acidic copper solution, the acidic copper solution is copper sulfate, and the concentration of copper ions is 3%. The ratio of copper to steel after electroplating is 20: 100.
the stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 6: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02 the raw stainless steel wire of step S01 is subjected to a plating process.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 40V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in a sodium dihydrogen phosphate solution as an electrolyte for secondary anodic oxidation with the voltage range of 25V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. During the anodization process, the temperature of the electrolyte was maintained at 0-10 ℃ by an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 7: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, electroplating the stainless steel wire;
s02, the stainless steel wire after being electroplated in the step S01 is subjected to secondary plating treatment.
The specific steps of step S01 are: and putting the stainless steel wire into the copper electroplating solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the specific steps of step S02 are: the sample treated in step S01 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 8: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 40V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in a sodium dihydrogen phosphate solution as an electrolyte for secondary anodic oxidation with the voltage range of 25V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2Between two electrodesThe distance is about 6 cm. During the anodization process, the temperature of the electrolyte was maintained at 0-10 ℃ by an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and when the deformation reaches 62%, carry out annealing treatment to soften the stainless steel wire for preparing the drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 62%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 9: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 40V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in a sodium dihydrogen phosphate solution as an electrolyte for secondary anodic oxidation with the voltage range of 25V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The above-mentioned process is implemented in two-electrode electrochemical anodic oxidation equipmentAnd the power supply equipment is a programmable direct current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. During the anodization process, the temperature of the electrolyte was maintained at 0-10 ℃ by an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is sodium hydroxide.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 2.2, and the concentration of copper ions is 2%.
The specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
Example 10: the embodiment provides a preparation process of stainless steel fiber micro powder, which comprises the following steps:
stainless steel wire pretreatment, bundle drawing method drawing, shearing, cleaning, baking, screening and finished product
The stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, the stainless steel wire after being electroplated in the step S02 is subjected to secondary plating treatment.
The specific steps of step S01 are as follows: sequentially grinding the surface of a raw material stainless steel wire by using sand paper and polishing by using diamond polishing paste, sequentially placing the stainless steel wire treated in the above processes into acetone, absolute ethyl alcohol and secondary distilled water for ultrasonic cleaning for ten minutes, taking out the stainless steel wire and drying in the air; after the pretreatment, the sample is placed in a perchloric acid-ethylene glycol solution system for the first anodic oxidation, wherein perchloric acid (HClO)470%) of 5 vol%, applying voltage of 40V for 3 minutes, then respectively placing the above-mentioned sample in acetone, absolute ethyl alcohol and secondary distilled water in turn to make ultrasonic cleaning, then drying in air; and then placing the dried sample in a sodium dihydrogen phosphate solution as an electrolyte for secondary anodic oxidation with the voltage range of 25V, then respectively placing the sample in acetone, absolute ethyl alcohol and secondary distilled water in sequence for ultrasonic cleaning, and then drying in the air.
The process is carried out in a two-electrode electrochemical anodic oxidation device, and the power supply device is a programmable direct-current power supply. During the anodic oxidation process, the electrolyte solution is stirred by rotating magnetons to ensure the uniformity of the electrolyte solution. The graphite electrode used for the cathode has an area of about 9cm2The distance between the two electrodes was about 6 cm. During anodic oxidation, electrolysisThe temperature of the liquid was maintained at 0-10 ℃ by means of an ice-water mixture.
The specific steps of step S02 are: and (4) putting the stainless steel wire obtained in the step (S01) into an electroplating copper solution for electroplating.
The electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is basic copper carbonate; the auxiliary complexing agent is trimethylolpropane triacrylate compound.
Wherein the pH value of the alkaline copper solution is 11.5, the complexing ratio is 1.8, and the concentration of copper ions is 2%.
The preparation method of the trimethylolpropane triacrylate compound comprises the following steps:
firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring at room temperature for 30min, adjusting the reaction temperature of the system to 0 ℃, and then starting to introduce BF3Gas, controlled introduction of BF3The gas time is 3 hours, wherein BF3The molar ratio to trimethylolpropane triacrylate was 0.4: 1.
the specific steps of step S03 are: the sample treated in step S02 is immersed in dopamine hydrochloride solution (concentration is 2mg/mL, solvent is Tris-HCl buffer solution, pH is 8.5), kept for two hours at room temperature while stirring, taken out, ultrasonically cleaned in deionized water for ten minutes, and finally dried in air. Then annealing the cleaned stainless steel sample in a tube furnace, introducing argon for three times before annealing, and pumping out the argon by using a vacuum pump so as to remove air in the tube furnace as much as possible; in the annealing treatment process, argon flow is introduced into the annealing furnace to isolate air, the temperature is firstly increased to 650 ℃ at the temperature increase rate of 15 ℃/min, then the temperature is kept for 2h, and finally the annealing furnace is cooled.
The stainless steel wires are pretreated and then are loaded into a copper pipe with the diameter of 20mm, and the number of the stainless steel wire cores in the copper pipe is controlled to be 3000; the drawing is to compact the installed copper pipe, then draw, and anneal when the deformation reaches 60%, so that the stainless steel wire is softened to prepare for drawing of the next process; carrying out annealing treatment again when the secondary drawing is carried out and the deformation reaches 60%; the diameter of the required fiber is achieved by repeated drawing and annealing.
The shearing is to shear the stainless steel wire according to the length required by the micro powder.
And after copper and steel separation is carried out on the sheared stainless steel wire, cleaning, baking and screening are carried out to prepare a finished product.
And (3) performance testing:
1. testing the shape of the stainless steel fiber by a scanning electron microscope;
2. performance testing of shielding performance:
the prepared stainless steel fiber and cotton raw materials are blended, and the specific content is 5% of metal stainless steel fiber/95% of cotton.
The method comprises the following steps: a. cotton fibers are subjected to blowing, cotton carding, combing and multiple mixing processes, then are subjected to roving, spinning and spooling processes, and stainless steel fibers are gradually mixed in the multiple mixing processes; b. weaving; comprises the steps of sizing, drafting and weaving; c. printing and dyeing; mercerizing and dyeing are adopted; d. after finishing; comprises the steps of softening, sizing and preshrinking.
Test result for shielding mobile phone signal
The above examples are merely illustrative and serve to explain some of the features of the invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims not be limited by the choice of examples illustrating features of the invention, and that technological advances will form possible equivalents or sub-substitutes not presently contemplated for reasons of inaccuracy of the linguistic expressions, and that such variations are to be construed as being covered by the appended claims where possible.
Claims (5)
1. The preparation process of the stainless steel fiber micro powder is characterized by comprising the following steps:
the method comprises the following steps of stainless steel wire pretreatment, drawing by a bundling drawing method, shearing, cleaning, baking, screening and finished product preparation, wherein the stainless steel wire pretreatment comprises the following steps:
s01, carrying out nano construction on the surface of the stainless steel wire serving as the raw material;
s02, electroplating the raw material stainless steel wire in the step S01;
s03, carrying out secondary coating treatment on the stainless steel wire subjected to the electroplating treatment in the step S02;
the specific steps of step S01 are: polishing and cleaning the surface of the stainless steel wire as the raw material, and then placing the stainless steel wire in electrolyte for nano construction, wherein the specific steps of the step S02 are as follows: putting the stainless steel wire obtained in the step S01 into an electrolytic copper plating solution for electroplating, wherein the electrolytic copper plating solution is an alkaline copper solution, and a main complexing agent of the alkaline copper solution is triethanolamine; the main salt is copper sulfate; the auxiliary complexing agent is a trimethylolpropane triacrylate compound, and the preparation method of the trimethylolpropane triacrylate compound is as follows: firstly, adding trimethylolpropane triacrylate into a reactor, then adding cetyl polyoxyethylene ether, stirring for 30min at room temperature, adjusting the reaction temperature of the system to 0 ℃, starting to introduce BF3 gas, and controlling the time of introducing BF3 gas to be 3 hours, wherein the molar ratio of BF3 to trimethylolpropane triacrylate is 0.4: 1.
2. the process for preparing stainless steel fiber micropowder of claim 1, wherein the secondary coating in step S03 is carried out by taking the stainless steel wire after electroplating as a template, placing in a carbon source environment, and carrying out heat treatment to obtain the pretreated stainless steel wire.
3. The process for preparing a stainless steel fiber micropowder according to claim 1, wherein the amount of deformation by the bundle drawing method is 50 to 60%.
4. A process for preparing stainless steel fiber micropowder according to claim 1, wherein the shearing is carried out by shearing the copper wire in the length required for micropowder.
5. The preparation process of the stainless steel fiber micro powder, according to claim 2, is characterized in that the particle size of the stainless steel fiber micro powder is 1-3 μm.
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Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54107835A (en) * | 1978-02-14 | 1979-08-24 | Furukawa Electric Co Ltd:The | Surface activating method for metal wire |
| US6045677A (en) * | 1996-02-28 | 2000-04-04 | Nanosciences Corporation | Microporous microchannel plates and method of manufacturing same |
| CN1589987A (en) * | 2003-08-26 | 2005-03-09 | 株式会社神户制钢所 | Method of producing solid wire for welding |
| CN1900345A (en) * | 2006-07-21 | 2007-01-24 | 周建华 | Metal fiber wire and its producing process |
| CN101220449A (en) * | 2008-01-25 | 2008-07-16 | 湖南惠同新材料股份有限公司 | Fire resistant iron chromium aluminum filament and production technique |
| CN101521988A (en) * | 2009-03-27 | 2009-09-02 | 浙江大学 | Preparation method of metal base copper-clad plate and copper-clad sectional material |
| CN102181898A (en) * | 2011-04-20 | 2011-09-14 | 江苏法尔胜泓昇集团有限公司 | On-line pretreatment device for copper-coated stainless steel wires |
| CN102477577A (en) * | 2010-11-22 | 2012-05-30 | 湖南汇博金属材料有限责任公司 | Preparation process for metal fibers |
| CN102825096A (en) * | 2012-03-23 | 2012-12-19 | 常州市武进恒通金属钢丝有限公司 | New process for producing micron-order stainless steel fiber |
| CN103388174A (en) * | 2013-08-02 | 2013-11-13 | 娄底市通达金属材料有限公司 | Process for preparing stainless steel fiber micro powder |
| CN103611757A (en) * | 2013-12-10 | 2014-03-05 | 西部新锆核材料科技有限公司 | Method for preparing zirconium metal filaments |
| CN103882442A (en) * | 2014-04-16 | 2014-06-25 | 武汉科技大学 | Stainless steel surface three-dimensional nanocarbon film and preparation method thereof |
| CN104831192A (en) * | 2015-05-22 | 2015-08-12 | 丹阳凯富达过滤器材有限公司 | Meta wire and production process thereof |
| CN106757279A (en) * | 2016-12-01 | 2017-05-31 | 三达奥克化学股份有限公司 | Steel wire drawing electrolytic phosphating liquid and production method |
| CN106835258A (en) * | 2016-12-15 | 2017-06-13 | 华北电力大学（保定） | A kind of dot matrix type etches the preparation method and applications of stainless steel fibre |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694847A (en) * | 2013-12-04 | 2014-04-02 | 铜陵三佳变压器有限责任公司 | Wire enamel for copper-clad aluminum for transformer and preparation method thereof |
| CN105131797A (en) * | 2015-09-22 | 2015-12-09 | 太仓市金鹿电镀有限公司 | Plastic electroplating technology for automobile trim strips |
-
2018
- 2018-05-11 CN CN201810446694.XA patent/CN108672706B/en active Active
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS54107835A (en) * | 1978-02-14 | 1979-08-24 | Furukawa Electric Co Ltd:The | Surface activating method for metal wire |
| US6045677A (en) * | 1996-02-28 | 2000-04-04 | Nanosciences Corporation | Microporous microchannel plates and method of manufacturing same |
| CN1589987A (en) * | 2003-08-26 | 2005-03-09 | 株式会社神户制钢所 | Method of producing solid wire for welding |
| CN1900345A (en) * | 2006-07-21 | 2007-01-24 | 周建华 | Metal fiber wire and its producing process |
| CN101220449A (en) * | 2008-01-25 | 2008-07-16 | 湖南惠同新材料股份有限公司 | Fire resistant iron chromium aluminum filament and production technique |
| CN101521988A (en) * | 2009-03-27 | 2009-09-02 | 浙江大学 | Preparation method of metal base copper-clad plate and copper-clad sectional material |
| CN102477577A (en) * | 2010-11-22 | 2012-05-30 | 湖南汇博金属材料有限责任公司 | Preparation process for metal fibers |
| CN102181898A (en) * | 2011-04-20 | 2011-09-14 | 江苏法尔胜泓昇集团有限公司 | On-line pretreatment device for copper-coated stainless steel wires |
| CN102825096A (en) * | 2012-03-23 | 2012-12-19 | 常州市武进恒通金属钢丝有限公司 | New process for producing micron-order stainless steel fiber |
| CN103388174A (en) * | 2013-08-02 | 2013-11-13 | 娄底市通达金属材料有限公司 | Process for preparing stainless steel fiber micro powder |
| CN103611757A (en) * | 2013-12-10 | 2014-03-05 | 西部新锆核材料科技有限公司 | Method for preparing zirconium metal filaments |
| CN103882442A (en) * | 2014-04-16 | 2014-06-25 | 武汉科技大学 | Stainless steel surface three-dimensional nanocarbon film and preparation method thereof |
| CN104831192A (en) * | 2015-05-22 | 2015-08-12 | 丹阳凯富达过滤器材有限公司 | Meta wire and production process thereof |
| CN106757279A (en) * | 2016-12-01 | 2017-05-31 | 三达奥克化学股份有限公司 | Steel wire drawing electrolytic phosphating liquid and production method |
| CN106835258A (en) * | 2016-12-15 | 2017-06-13 | 华北电力大学（保定） | A kind of dot matrix type etches the preparation method and applications of stainless steel fibre |
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