CN114932218A - Method for reducing evaporation of 3D printing zinc powder to form zinc-silver alloy through chemical silver plating - Google Patents

Method for reducing evaporation of 3D printing zinc powder to form zinc-silver alloy through chemical silver plating Download PDF

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Publication number
CN114932218A
CN114932218A CN202210596553.2A CN202210596553A CN114932218A CN 114932218 A CN114932218 A CN 114932218A CN 202210596553 A CN202210596553 A CN 202210596553A CN 114932218 A CN114932218 A CN 114932218A
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zinc
silver
zinc powder
powder
silver alloy
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CN114932218B (en
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王小健
王成哲
李卫
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Jinan University
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Jinan University
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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
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/04—Metals or alloys
    • A61L27/047—Other specific metals or alloys not covered by A61L27/042 - A61L27/045 or A61L27/06
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
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    • A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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    • B22F10/20—Direct sintering or melting
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    • B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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    • 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
    • B33Y80/00—Products made by additive manufacturing
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0483—Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
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Abstract

The invention belongs to the field of surface modification of zinc powder, and discloses a method for reducing evaporation of 3D printing zinc powder to form a zinc-silver alloy by chemical silver plating. The invention uses low concentration (5g/L) SnCl 2 Sensitizing the zinc powder by the solution to ensure that a layer of Sn is discretely and randomly distributed on the surface of the zinc powder 2+ Therefore, silver ammonia solution with ultralow concentration (1g/L silver nitrate) can be used, so that a layer of dispersed silver layer is coated on the zinc powder, the thermal conductivity of the zinc powder is obviously improved, the highest temperature in a molten pool is lower than the boiling point of zinc, and the selective laser melting zinc-silver alloy prepared from the zinc-silver powder can fundamentally inhibit the evaporation of the zinc powder in the selective laser melting process.

Description

Method for reducing evaporation of 3D printing zinc powder to form zinc-silver alloy through chemical silver plating
Technical Field
The invention belongs to the field of surface modification of zinc powder, and particularly relates to a method for reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy through chemical silver plating.
Background
The zinc and the zinc alloy are widely applied to the biological fields of bone repair, vascular stents and the like due to the characteristics of good biocompatibility, proper degradation rate and the like. The conventional processing method is mostly used for preparing zinc-based materials, and parts with various complex structures cannot be prepared, so that the application of the zinc-based materials in bone implants and stent structures is limited.
The selective laser melting technology is one of metal additive manufacturing technologies, and the working process of the selective laser melting technology is a process of selectively melting and solidifying single-layer powder on a forming plane by focusing a high-energy laser beam on the forming plane to move at a certain speed and path, and finally stacking layer by layer to obtain a three-dimensional solid part. The selective laser melting technology has the characteristics of layered manufacturing and layer-by-layer superposition, and can regulate and control the porosity, the geometric shape and the microstructure of the part. Compared with the traditional casting method, the selective laser melting technology is not limited by the complex structure of the part, the selective laser melting technology can be used for conveniently preparing parts with various topological structures and customizing specific implants for patients, and therefore the requirements of individuation and precision of future medical treatment can be better met.
However, because pure zinc has lower melting point (419.5 ℃) and boiling point (907 ℃), zinc powder is easy to evaporate when pure zinc parts are prepared by using a selective laser melting technology, a large amount of smoke is generated, the smoke is gathered in a forming chamber and can weaken the input of laser energy, a large amount of evaporation can cause more key holes in a sample and influence the forming quality of the parts, most of the existing researches reduce the influence of evaporation on sample processing by designing a reasonable circulating airflow system, and when the flow rate and the flow rate of circulating airflow are proper, the evaporated smoke can be well removed, but the method does not fundamentally solve the problem of evaporation in the processing process of selective laser melting of pure zinc, how to improve the temperature field in the molten pool in the processing process of melting pure zinc by selective laser and ensure that the highest temperature in the molten pool does not exceed the boiling point of zinc has great significance for fundamentally inhibiting the evaporation of zinc powder.
The silver has the advantages of good thermal conductivity, good biocompatibility, strong oxidation resistance and the like, so that when a zinc-silver alloy is processed by using a selective laser melting technology, the high thermal conductivity of the silver is favorable for heat transfer, the highest temperature in a molten pool is far lower than the evaporation temperature of zinc, and the effect of inhibiting the evaporation of the zinc powder can be achieved. The most important method for alloying metal powder is ball milling to prepare powder, however, the alloy powder prepared by the ball milling method often has the problem of poor sphericity, and the poor sphericity can reduce the fluidity of the powder and influence the powder paving process in the selective laser melting process, thereby influencing the precision and quality of the formed parts.
Chemical plating is a novel metal surface treatment technology, and is a surface treatment method for reducing metal ions in a plating solution into metal by using a reducing agent under the condition of no external current and depositing the metal ions on the surface of a part. Mainly comprises chemical nickel plating, chemical copper plating, chemical silver plating, chemical gold plating and the like.
Therefore, there is a need to develop a processing method for reducing the evaporation tendency of zinc powder in the selective laser melting process of pure zinc, so as to fundamentally inhibit the evaporation of zinc powder.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a method for reducing evaporation of 3D printing zinc powder to form a zinc-silver alloy by chemical silver plating.
The invention also aims to provide the zinc-silver alloy prepared by the method.
The invention also aims to provide the application of the zinc-silver alloy in bone repair and vascular stents implanted into human bodies.
The purpose of the invention is realized by the following scheme:
a method for reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating, mainly comprising the following steps:
(1) performing chemical silver plating on zinc powder: by SnCl 2 Sensitizing the surface of the zinc powder by the solution, and uniformly adsorbing a layer of discrete Sn on the surface of the zinc powder 2+ Then washing with water; activating the pretreated zinc powder by using a silver ammonia solution, and cleaning and drying the zinc powder after the activation is finished; then slowly dripping the silver ammonia solution into a beaker containing a reducing agent, stirring until the solution is uniform, finishing chemical silvering, centrifuging, cleaning, carrying out suction filtration, dehydrating and drying to obtain zinc-silver alloy powder;
(2) screening the zinc-silver alloy powder obtained in the step (1), screening 15-45 mu m powder meeting the requirement of the laser melting particle size in a selection area by using a screen, then putting the powder into a metal 3D printer, introducing gas to reduce the oxygen content, then processing a zinc-silver alloy part by using the 3D printer, removing the part after the part is processed, and cutting the part from a substrate by using a wire cut electrical discharge machine to obtain the part.
SnCl described in step (1) 2 The solution is preferably 5 g/L; 1ml of SnCl is used per 1g of zinc powder 2 Soaking the solution for 30min for sensitization; the zinc powder is preferably pure zinc powder meeting the selective laser melting requirement, and the size of the zinc powder is within the range of 15-45 mu m;
the silver-ammonia solution in the step (1) is prepared by silver nitrate, ammonia water and sodium hydroxide, and the ratio of reagents required for preparing the silver-ammonia solution is AgNO 3 0.1～5g：NH 3 ·H 2 O20-120 mL, and adjusting the pH value of the reaction system to 12-14 by using 0.1mol/LNaOH solution, wherein AgNO is preferred 3 The mass concentration is 1 g/L;
the activation in the step (1) is to add the pretreated zinc powder into a beaker filled with silver-ammonia solution and place the zinc powder in an ultrasonic generator for ultrasonic treatment for 15 to 30 min; activating each 1g of pretreated zinc powder by using 1mL of silver ammonia solution;
the volume ratio of the silver ammonia solution to the reducing agent in the step (1) is 1: 1; the reducing agent is prepared from glucose, water and ethanol, and the dosage ratio of each substance in the reducing solution is 800mL of water: 200mL of absolute ethanol: 0.5mol glucose;
the step (1) of suction filtration and dehydration is to remove water in the silver-plated zinc powder by using a suction filter and then use absolute ethyl alcohol for dehydration for 2-3 times;
the drying in the step (1) is drying in a vacuum drying oven at the temperature of 100-120 ℃;
the drying in the step (2) refers to drying in a vacuum drying oven at the temperature of 100-120 ℃ for 6-8 h;
the step (2) of introducing gas to reduce the oxygen content refers to introducing high-purity argon with the concentration of 99.999 percent to reduce the oxygen content in a machine to 80 ppm;
the processing parameter range of the metal 3D printer in the step (2) is 40-100W, the speed is 300-400mm/s, the layer thickness is 30 μm, and the scanning pitch is 70 μm.
A zinc-silver alloy prepared by the method.
The zinc-silver alloy is used for being implanted into the bone repair of a human body and the application of a blood vessel bracket.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the zinc-silver alloy powder prepared by the chemical silver plating method has the following characteristics: (1) the sphericity of the zinc powder cannot be damaged, and the sphericity meets the requirement of selective laser melting of the powder; (2) the silver layers on the surfaces of the zinc powder are dispersed and randomly distributed uniformly, so that the metal silver is melted without increasing the laser power, and meanwhile, the silver has strong oxidation resistance, thereby being beneficial to inhibiting the oxidation phenomenon in the storage and transportation process of the zinc powder; (3) the evaporation of zinc powder is well inhibited; (4) the melting point of silver is far higher than that of zinc, so that the effect of refining solidification structure grains is achieved due to heterogeneous nucleation in the solidification process; (5) the silver has good antibacterial performance, so that the antibacterial performance of the zinc-silver alloy prepared by the selective laser melting technology is improved to a certain extent, and the zinc-silver alloy can play a role in reducing inflammation after being implanted into a human body in the future.
2. The invention uses low concentration (5g/L) SnCl 2 The solution is used for sensitizing the zinc powder, so that a layer of Sn is discretely and randomly distributed on the surface of the zinc powder 2+ Therefore, the silver ammonia solution with ultra-low concentration (1g/L silver nitrate) can be used, and the components are saved. Using reduction of SnCl 2 The solution and the silver ammonia solution can overcome the defects that the zinc powder cannot be melted due to over-thick silver layer and the SnCl with lower concentration 2 The solution and the silver ammonia solution enable the zinc powder to be coated with a dispersed silver layer which is not compact, the zinc powder can be melted easily, and meanwhile, the cost is saved.
3. The invention is to chemically plate silver on the surface of zinc powder, and simultaneously chemically plate copper on the surface of zinc powder, and the like, and the method is similar and simple in process, and can effectively save cost.
4. The invention plates a layer of metal silver distributed in a discrete and random way on the surface of the zinc powder by a chemical plating method, which can not destroy the sphericity of the zinc powder and overcomes the defect that the sphericity of the powder is easy to destroy by other methods.
5. Aiming at the problem that zinc powder is easy to evaporate in the processing process of selective laser melting pure zinc, the method plates a layer of metal silver which is distributed discretely on the surface of the zinc powder by a chemical silver plating method, the prepared zinc-silver alloy powder has the advantages of good sphericity, accordance with the requirements of selective laser melting powder, improvement of the oxidation resistance of the zinc powder and the like, the method is simple, the operation is simple and convenient, and the selective laser melting zinc-silver alloy prepared from the zinc-silver powder has the advantages of inhibition of powder evaporation, fine crystal grains and improvement of antibacterial capability.
6. The chemical silver plating is carried out on the surface of the zinc powder, the heat conductivity coefficient of the zinc is 112W/mK, the heat conductivity coefficient of the silver is 411W/mK, the heat conductivity of the zinc powder is obviously improved by adding the silver, the highest temperature in a molten pool is lower than the boiling point of the zinc, and therefore the evaporation of the zinc powder in the selective laser melting process is fundamentally inhibited.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The reagents used in the examples are commercially available without specific reference.
Example 1
(1) The zinc powder is subjected to chemical silvering by the following method: zinc powder → sensitization (SnCl) 2 ·H 2 O) → deionized water rinse → activation (AgNO) 3 ) → deionized water washing → vacuum drying → reduction → centrifugation → deionized water washing → suction filtration dehydration → vacuum drying.
The method specifically comprises the following steps: by using 5g/L SnCl 2 The solution is used for soaking the surface of the zinc powder for 30min for sensitization, and a layer of discrete Sn is uniformly adsorbed on the surface of the zinc powder 2+ Then washing with water; dissolving the mixture with silver ammoniaLiquid (AgNO) 3 The mass concentration is 1g/L, the pH value of a reaction system is adjusted to 12-14 by using 0.1mol/L NaOH solution), and the pretreated zinc powder is activated, namely, the pretreated zinc powder is added into a beaker filled with silver-ammonia solution and is placed in an ultrasonic generator for ultrasonic treatment for 15 min; after the activation is finished, cleaning and drying; then slowly dripping the silver ammonia solution into a beaker containing a reducing agent (800mL/L water, 200mL/L absolute ethyl alcohol, 0.5mol/L glucose), mechanically stirring for 30min to complete chemical silver plating, centrifuging, washing with deionized water, performing suction filtration, dehydrating and drying to obtain zinc-silver alloy powder;
(2) screening the zinc-silver alloy powder obtained in the step (1) (the powder may absorb moisture after being stored and can be dried for 6 hours at 120 ℃ in a vacuum drying oven before being used), screening 15-45 mu m powder meeting the requirement of the laser melting particle size in a selected area by using a screen, then putting the powder into a metal 3D printer, introducing high-purity argon with the concentration of 99.999% to reduce the oxygen content in the machine to 80ppm, then processing the zinc-silver alloy part by using the 3D printer, removing the part after the part is processed, and cutting the part from a substrate by using a wire cut electric discharge machine to obtain the part.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A method for reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating, characterized by mainly comprising the steps of:
(1) performing chemical silver plating on zinc powder: by SnCl 2 Sensitizing the surface of the zinc powder by the solution, and uniformly adsorbing a layer of discrete Sn on the surface of the zinc powder 2+ Then washing with water; activating the pretreated zinc powder by using a silver ammonia solution, and cleaning and drying the zinc powder after the activation is finished; then slowly dripping the silver ammonia solution into a beaker containing a reducing agent, stirring until the solution is uniform, and completing the solutionChemical silvering, centrifuging, cleaning, suction filtering, dehydrating and drying to obtain zinc-silver alloy powder;
(2) screening the zinc-silver alloy powder obtained in the step (1), screening 15-45 mu m powder meeting the requirement of the laser melting particle size in a selection area by using a screen, then putting the powder into a metal 3D printer, introducing gas to reduce the oxygen content, then processing a zinc-silver alloy part by using the 3D printer, removing the part after the part is processed, and cutting the part from a substrate by using a wire cut electrical discharge machine to obtain the part.
2. A method of reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: SnCl described in step (1) 2 The solution is preferably 5 g/L; 1mLSnCl is used for each 1g of zinc powder 2 Soaking the solution for 30min for sensitization; the zinc powder is preferably pure zinc powder meeting the selective laser melting requirement, and the size of the zinc powder is in the range of 15-45 mu m.
3. A method of reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: the silver-ammonia solution in the step (1) is prepared by silver nitrate, ammonia water and sodium hydroxide, and the ratio of reagents required for preparing the silver-ammonia solution is AgNO 3 0.1～5g,：NH 3 ·H 2 O20-120 mL, and adjusting the pH value of the reaction system to 12-14 by using 0.1mol/L NaOH solution, wherein AgNO is preferred 3 The mass concentration is 1 g/L.
4. A method of reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: the activation in the step (1) is to add the pretreated zinc powder into a beaker filled with silver-ammonia solution and place the zinc powder in an ultrasonic generator for ultrasonic treatment for 15 to 30 min; 1mL of silver ammonia solution was used for activation per 1g of pretreated zinc powder.
5. A method of reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: the volume ratio of the silver ammonia solution to the reducing agent in the step (1) is 1: 1; the reducing agent is prepared from glucose, water and ethanol, and the dosage ratio of each substance in the reducing solution is 800mL of water: 200mL of absolute ethanol: 0.5mol glucose.
6. A method of reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: the step (1) of suction filtration and dehydration is to remove water in the silver-plated zinc powder by using a suction filter and then use absolute ethyl alcohol for dehydration for 2-3 times;
the drying in the step (1) is drying in a vacuum drying oven at the temperature of 100-120 ℃.
7. A method of reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: the drying in the step (2) refers to drying in a vacuum drying oven at the temperature of 100-120 ℃ for 6-8 h;
the step of introducing gas to reduce the oxygen content in the step (2) refers to introducing high-purity argon with the concentration of 99.999 percent to reduce the oxygen content in a machine to 80 ppm.
8. A method for reducing evaporation of 3D printed zinc powder to form a zinc-silver alloy by electroless silver plating according to claim 1, wherein: the processing parameter range of the metal 3D printer in the step (2) is 40-100W, the speed is 300-400mm/s, the layer thickness is 30 μm, and the scanning pitch is 70 μm.
9. The zinc-silver alloy prepared by any one of the methods of claims 1 to 8.
10. Use of the zinc-silver alloy according to claim 9 for implantation in bone repair and vascular stents in the human body.
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