CN108660489B - Preparation method of three-dimensional porous metal material with non-deviation aperture and physical property - Google Patents
Preparation method of three-dimensional porous metal material with non-deviation aperture and physical property Download PDFInfo
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- CN108660489B CN108660489B CN201810580338.7A CN201810580338A CN108660489B CN 108660489 B CN108660489 B CN 108660489B CN 201810580338 A CN201810580338 A CN 201810580338A CN 108660489 B CN108660489 B CN 108660489B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/08—Perforated or foraminous objects, e.g. sieves
Abstract
The invention discloses a preparation method of a three-dimensional porous metal material with non-deviation aperture and physical properties, which comprises the steps of printing a substrate with uniform and consistent porous structure by using a 3D printer, wherein the substrate is at least provided with 1 blind hole to obtain the substrate with the blind hole; conducting treatment on the substrate with the blind holes to obtain a conductive substrate; immersing the conductive substrate in electroplating solution, inserting an ultrasonic vibration rod into the electroplating solution, inserting an injection needle matched with the blind hole into the blind hole, injecting the newly added electroplating solution into the blind hole, and obtaining a three-dimensional porous metal semi-finished product after electroplating is finished; and (3) airing the three-dimensional porous metal semi-finished product, putting the three-dimensional porous metal semi-finished product into an incinerator for incineration to remove the conductive matrix, and then putting the three-dimensional porous metal semi-finished product into reducing gas for high-temperature treatment. The invention has the advantages that the pore size and the surface density of the produced foam matrix can be kept consistent in an error range, and meanwhile, the consistency of the inner plating layer and the outer plating layer of the metal is kept to the maximum extent.
Description
Technical Field
The invention relates to the three-dimensional porous metal industry, in particular to a preparation method of a three-dimensional porous metal material with non-deviation of aperture and physical properties.
Background
The existing preparation of three-dimensional porous metal is generally finished by electroplating metal on a foam substrate, and the inconsistency of the aperture and the density on the foam substrate also causes the inconsistency of the physical properties of the three-dimensional porous metal, thereby influencing the surface density and the aperture of the foam metal. How to prepare the foam matrix with consistent pore diameter and density becomes a problem to be solved for manufacturing three-dimensional porous metal with consistent physical properties.
In addition to the pore size and density of the foam matrix, plating thickness is another important factor affecting the physical uniformity of the three-dimensional porous metal, and one important factor affecting plating thickness is the plating method. The preparation of the three-dimensional porous metal material generally adopts a continuous plating mode, and the continuous plating mode is suitable for wire rods and strips which are produced in batches. Because wires and strips produced by continuous plating are restricted by factors such as electrochemistry, geometry and the like, the thickness of the plating layer inside and outside the matrix is uneven, and the consistency of the performance of the foam body is influenced.
Document CN103147100A discloses a method for preparing a hybrid porous metal material, which comprises conducting treatment on a porous base material, pre-electroplating a porous base, adding burning particles for mixed electroplating, and finally burning the porous base and burning the particles and reducing to obtain the porous metal material. The physical properties of the porous metal material produced by the method are limited by the porous matrix and can not reach consistency, and the problem of plating uniformity is not solved.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a three-dimensional porous metal material without deviation of pore diameter and physical property, which can keep the pore diameter and the surface density of a produced foam matrix consistent within an error range and simultaneously keep the consistency of internal and external plating layers of the metal to the maximum extent.
The invention comprises the following steps:
(1) printing a base body with a uniform porous structure by using a 3D printer, wherein at least 1 blind hole is formed in the base body, and the depth of the blind hole is 1/2 of the thickness of the base body, so that the base body with the blind hole is obtained; by using the 3D printing technology, the porous matrix with consistent aperture and surface density can be printed, so that the electroplated porous metal can basically reach the consistency on the aperture and the surface density, and the electroplating inside the matrix is not limited by geometric factors any more.
Experiments show that the electroplating efficiency is gradually reduced when the base body extends from outside to inside, so that the thicknesses of the electroplated layers inside and outside the base body are influenced. In the continuous electroplating, because the thickness of the substrate is thinner, generally 1-3mm, the attenuation of the electroplating efficiency from outside to inside is not obvious, so the thickness difference of the inner and outer plating layers of the material prepared by the continuous electroplating is not great; the thickness of the porous metal material prepared by rack plating is generally larger than 8mm and even reaches 100mm, the attenuation of the electroplating efficiency from outside to inside is obvious, and the inside is difficult to plate through. The blind holes are arranged for injecting electroplating solution into the base body in the electroplating process, so that the electroplating inside the base body is not limited by the electroplating solution any more, an internal electroplated layer is thinner than an external electroplated layer, and the consistency of the performance of the porous structure is influenced.
When electroplating solution is injected into the base body through the blind holes, the injected electroplating solution can be diffused at the position 1/2 in the base body in 360 degrees, but the influence range of the diffusion is limited, and the electroplating solution is generally injected into the blind holes which are uniformly distributed, so that the uniform electroplating of the whole base body can be completed.
(2) Conducting treatment on the substrate with the blind holes to obtain a conductive substrate;
(3) immersing the conductive substrate in electroplating solution, inserting an ultrasonic vibration rod into the electroplating solution, inserting a liquid injection needle matched with the blind hole into the blind hole, injecting a newly added electroplating solution into the blind hole, wherein the volume concentration of the newly added electroplating solution is at least 1.5 times of the volume concentration of the original electroplating solution, and then starting electroplating and starting the ultrasonic vibration rod; the electroplating solution is adjusted according to different metals to be electroplated, the electroplating temperature is preferably controlled to be 45-60 ℃, the substrate can be burnt when the temperature is too high, the uniformity of an inner electroplating layer and an outer electroplating layer of the substrate can be influenced, the electroplating speed can be accelerated along with the rise of the temperature, and when the temperature is too high, the consumption speed of metal ions in the substrate can be greater than the supplement speed, so that the non-uniformity of the inner electroplating layer and the outer electroplating layer is enlarged;
in the electroplating process, the consumption of metal ions in the matrix is supplemented by the entrance of metal ions outside the matrix, the metal ions are continuously attracted by charges on the matrix and consumed when entering the matrix through pores, and if the electroplating speed is too high or the matrix is too thick, the metal ions in the matrix are insufficient in many times, so that the inside of the matrix cannot be plated through, and the consistency of the porous structure performance is influenced; by arranging the blind hole reaching the middle part of the matrix on the matrix and injecting the electroplating solution into the blind hole, metal ions in the matrix can be supplemented, and the internal and external deposition amounts of the matrix are balanced; the application of ultrasonic vibration is beneficial to the exchange of the electroplating liquid inside and outside the matrix; the volume concentration of the newly added electroplating solution is at least 1.5 times of the volume concentration of the original electroplating solution, so that the newly added electroplating solution has a relatively obvious diffusion effect to make up the concentration difference of metal ions inside and outside the matrix.
The current density when the electroplating is started is the calculated current density, the current density is adjusted to 1/3-1/2 of the calculated current density after 2-3 minutes, and after the current adjustment is finished for 30 minutes, the newly added electroplating solution is stopped from being injected, the electroplating current is closed, and the ultrasonic vibration rod is closed, so that a three-dimensional porous metal semi-finished product is obtained; the current density ASF can be calculated according to the thickness to be plated, and the formula is as follows:
current density (ASF) ═ plating layer thickness (um)/(plating time (min) × plating efficiency × constant C)
Wherein the constant C varies from metal to metal, such as C0.0202 for copper, 0.0182 for nickel, and 0.0456 for tin. Before actual electroplating, determining the thickness of an electroplating layer, calculating current density ASF, pre-plating for 2-3 minutes in the electroplating process, and keeping the current density as the calculated current density in the pre-plating process; after the pre-plating was completed, the current density was adjusted to 1/3 to 1/2 of the calculated current density for 30 minutes. Wherein, the outermost electroplating efficiency of the substrate can be different due to different electroplating metals, and the electroplating efficiency of the substrate can be gradually reduced along with the extension of the pores into the substrate.
(4) Cleaning the three-dimensional porous metal semi-finished product, airing for 2-3 days, and putting the semi-finished product into an incinerator to incinerate to remove the conductive matrix; and (3) placing the three-dimensional porous metal semi-finished product in reducing gas for reduction treatment, wherein the reduction reaction temperature is 900 ℃, and obtaining the three-dimensional porous metal material with non-deviation aperture and physical property. The three-dimensional porous metal semi-finished product needs to be aired for 2-3 days and cannot be directly put into an incinerator for incineration, and a certain period of stabilization period is needed because the electroplated layer is just plated on the substrate and is not stable. The base body is put into an incinerator for incineration, so that the conductive substance and the conductive base body can be incinerated, and the organic matter is removed to improve the flexibility of the electroplated layer. Because the combustion is an oxidation reaction, the reduction treatment is needed after the combustion is finished, the reduction reaction temperature is different from 710-950 ℃, when the temperature is higher than 900 ℃, the reduction reaction efficiency is not increased any more, therefore, the temperature of the reduction reaction is preferably 900 ℃, and finally the three-dimensional porous metal material without aperture deviation and physical property deviation is obtained.
Theoretically speaking, even if a porous substrate with consistent pore size and surface density is printed by using a 3D printing technology, the deposition amounts of metals inside and outside the substrate cannot be completely consistent, especially when large-size porous metals are hung and plated. The invention aims to reduce the influence of other factors, such as the internal and external conductivity of a substrate and the concentration difference of metal ions inside and outside the substrate, on the deposition amount of metals inside and outside the substrate, so that the overall physical properties of the substrate are consistent as much as possible, and the deviation of an electroplated layer is kept within an acceptable range.
The printing material used by the 3D printer in the step (1) is bioplastic polylactic acid, the polylactic acid belongs to renewable plant resources in the 3D printing material, is prepared by using starch raw materials extracted from plants, is very environment-friendly, does not generate harmful gas during combustion, and is not easily corroded by acidic substances during electroplating; in addition, polylactic acid has a melting point of not high, 155 ℃ and 185 ℃, and can be incinerated at a temperature of 400 ℃.
The diameter of the blind holes in the step (1) is 2-10mm, and the distance between the blind holes is 30 mm; the diameter of the blind hole is not suitable to be too large, otherwise the physical property of the porous metal is influenced, if the diameter is too small, the injection amount of newly-added electroplating solution is less, and the diffusion effect of the electroplating solution is not obvious; the distance between the blind holes is preferably 30mm, and the distance between the blind holes can be adjusted according to the concentration of the newly added electroplating solution.
The conducting treatment in the step (2) is implemented by adopting one or a combination of PVD (physical vapor deposition) electroplating, chemical plating and carbon glue coating treatment.
The carbon coating treatment comprises the steps of immersing the matrix with the blind holes in the carbon coating adhesive, and drying the matrix with the blind holes through ultrasonic vibration treatment to obtain the conductive matrix. The conductive treatment comprises coating conductive liquid on the substrate with blind holes for at least 3 times, and drying for at least 3 times each time, wherein the step is to increase the conductivity of the substrate with blind holes;
in addition, because the pores of the conductive substrate are small, when the conductive liquid enters the substrate through the pores on the substrate, the conductive liquid cannot fully enter the substrate due to the viscosity of the liquid, so that the conductive liquid is unevenly distributed in the substrate, and the conductivity in the substrate is affected. The ultrasonic vibration can enable the conductive liquid to get rid of the influence of liquid viscosity, and the conductive liquid can be uniformly distributed in the matrix, so that the internal electroplating of the matrix is not limited by the internal uneven conduction.
In the step (3), the rate of injecting the newly added electroplating solution into the blind hole is 0.2-0.5 m/min; the liquid injection rate is not too fast, otherwise, the newly added electroplating liquid has obvious spraying effect, is not beneficial to diffusion and can influence the electroplating in the matrix; in addition, the injection rate should not be too slow, otherwise the diffusion efficiency will be affected, and the rate is preferably 0.2-0.5 m/min.
The incineration temperature of the incinerator in the step (4) is 400 ℃, and the time is 5 minutes; the speed of the reduction of the specific surface area is related to the incineration temperature and time, when the surface area reaches the limit, the specific surface area is reduced by continuing incineration, so that the incineration temperature is reduced, the incineration time is shortened, the size of the specific surface area can be controlled, and the incineration condition is that the incineration temperature is 400 ℃ and the incineration time is 5 minutes.
In the step (4), the reducing gas is hydrogen, and the reduction reaction time is 15 minutes; the reducing gas can also be ammonia gas, the reduction time is adjusted according to the reduction temperature, and when the reduction temperature is 900 ℃, the reduction reaction time is preferably 15 minutes; if the temperature is too high or the reduction reaction time is too long, the generated three-dimensional porous metal can generate a phenomenon of arching.
The invention has the beneficial effects that:
(1) by using the 3D printing technology, the porous matrix with consistent aperture and surface density can be printed, so that the electroplated porous metal can basically reach the consistency on the aperture and the surface density, and the electroplating inside the matrix is not limited by geometric factors any more.
(2) The electroplating solution is injected into the matrix in the electroplating process, so that the electroplating inside the matrix is not limited by the concentration difference of the electroplated metal ions inside and outside the electroplating solution, and the condition of insufficient electroplated metal ions occurs inside the matrix, thereby influencing the consistency of the performance of the porous structure.
(3) The ultrasonic vibration can enable the conductive liquid to get rid of the influence of liquid viscosity, and the conductive liquid can be uniformly distributed in the matrix, so that the electroplating charges in the matrix are uniformly distributed.
(4) When electroplating, the ultrasonic vibration rod is arranged in the electroplating solution, so that the ultrasonic vibration can accelerate the exchange of the electroplating solution inside and outside the matrix and promote the uniform distribution of metal ions.
(5) Polylactic acid belongs to renewable plant resources in 3D printing materials, is prepared by using starch raw materials extracted from plants, does not generate harmful gas during combustion, is not easily corroded by acidic substances during electroplating, and can be incinerated at the temperature of 400 ℃.
(6) The liquid injection rate is not too fast, otherwise, the newly added electroplating liquid has obvious spraying effect, is not beneficial to diffusion and can influence the electroplating in the matrix; in addition, the injection rate should not be too slow, otherwise the diffusion efficiency will be affected, and the rate is preferably 0.2-0.5 m/min.
(7) The base body is put into an incinerator for incineration, so that the conductive substance and the conductive base body can be incinerated, and the organic matter is removed to improve the flexibility of the electroplated layer.
(8) The speed of the reduction of the specific surface area of the porous metal is related to the incineration temperature and time, and the specific surface area is reduced by continuing the incineration when the specific surface area reaches the limit, and the incineration condition is that the incineration temperature is 400 ℃ and the time is 5 minutes.
(9) When the temperature is higher than 900 ℃, the reduction reaction efficiency is not increased any more, and the temperature of the reduction reaction is preferably 900 ℃.
Detailed Description
Example 1:
to test the effect of using a 3D printed substrate and a foamed substrate on the physical properties of three-dimensional porous metals, a comparative experiment was now performed using two different substrates with respect to the physical properties of three-dimensional porous metals.
3D printing substrate
Specification: the porosity is 95%, the average pore diameter is 1.5mm, the thickness of the matrix is 15mm, and the size of the matrix is 30mm multiplied by 30 mm;
the experimental steps are as follows:
(1) printing a base body with a uniform porous structure by using a 3D printer, wherein at least 1 blind hole is formed in the base body, and the depth of the blind hole is 1/2 of the thickness of the base body, so that the base body with the blind hole is obtained;
(2) immersing the substrate with the blind holes in conductive liquid carbon-coated glue, and performing ultrasonic vibration treatment, wherein the conductive liquid is immersed for at least 3 times, and the conductive liquid is dried for at least 3 times each time to obtain a conductive substrate;
(3) immersing a conductive substrate in electroplating solution, wherein the electroplating solution comprises 60-70g/L of nickel sulfate, 10-14g/L of sodium hypophosphite, 4-8g/L of sodium acetate, 3-5g/L of boric acid and 2-4g/L of sodium chloride, inserting an ultrasonic vibration rod into the electroplating solution, inserting an injection needle matched with the blind hole into the blind hole, injecting a newly added electroplating solution into the blind hole, wherein the volume concentration of the newly added electroplating solution is at least 1.5 times of the volume concentration of the original electroplating solution, then starting electroplating and starting the ultrasonic vibration rod, the current density when electroplating is started is the calculated current density, after 2-3 minutes, adjusting the current to adjust the current density to 1/3-1/2 of the calculated current density, after 30 minutes of current adjustment, stopping injecting the newly added electroplating solution, closing the electroplating current and closing the ultrasonic vibration rod, obtaining a three-dimensional porous metal semi-finished product;
(4) and after airing for 2-3 days, putting the three-dimensional porous metal semi-finished product into an incinerator at 400 ℃ for incineration for 5 minutes to remove the conductive matrix, then putting the three-dimensional porous metal semi-finished product without the conductive matrix into hydrogen for reduction reaction at 900 ℃ for 15 minutes to finally obtain a three-dimensional porous metal finished product, and then detecting the physical properties of the three-dimensional porous metal. Comparative example 1:
foam matrix
Specification: the porosity is 95-97%, the average pore diameter is 1.4-1.6mm, the thickness of the matrix is 15mm, and the size of the matrix is 30mm multiplied by 30 mm;
the experimental procedure of comparative example 1 was identical to that of example 1.
TABLE 1 Effect of Using 3D printed or foamed substrates on the physical Properties of three-dimensional porous metals
Experiments show that the three-dimensional porous metal manufactured by using the 3D printing substrate is superior to the three-dimensional porous metal manufactured by using the foam substrate in physical property. The density deviation of a three-dimensional porous metal surface manufactured by using a 3D printing substrate is small, and the density change of the three-dimensional porous metal surface generated by the foam substrate is large due to the periodical change of the pore diameter of the foam substrate; meanwhile, the three-dimensional porous metal produced by the 3D printing matrix has more stable physical structure and is superior to the three-dimensional porous metal produced by the foam matrix in tensile strength and elongation; in addition, the larger the substrate specification is, the more obvious the advantages of the 3D printing substrate on the physical properties of the foam substrate will be.
Example 2:
in order to test the influence of different factors on the uniformity of the electroplated layer inside and outside the matrix in the electroplating process, relevant comparison tests are carried out on the influence factors.
Reference test
Selecting a 3D printing substrate with the specification of 95% of porosity, 1.5mm of average pore diameter, 15mm of substrate thickness and 30mm multiplied by 30mm of substrate size;
the steps of the benchmark test were:
(1) printing the base body with the specification and the uniform and consistent porous structure by using a 3D printer to obtain a 3D printed base body;
(2) immersing the 3D printing substrate in the conductive liquid carbon-coated adhesive for at least 3 times, and drying for at least 3 times each time to obtain a conductive substrate;
(3) immersing a conductive substrate in electroplating solution, wherein the electroplating solution comprises 60-70g/L of nickel sulfate, 10-14g/L of sodium hypophosphite, 4-8g/L of sodium acetate, 3-5g/L of boric acid and 2-4g/L of sodium chloride, and electroplating for 30 minutes to obtain a three-dimensional porous metal semi-finished product;
(4) and after airing for 2-3 days, putting the three-dimensional porous metal semi-finished product into an incinerator at 400 ℃ for incineration for 5 minutes to remove the conductive matrix, then putting the three-dimensional porous metal semi-finished product without the conductive matrix into hydrogen for reduction reaction at 900 ℃ for 15 minutes to finally obtain a three-dimensional porous metal finished product, and then detecting the physical properties of the three-dimensional porous metal. Comparative example 2:
using ultrasonic vibrating rods during conductive treatment
Selecting a 3D printing substrate with the specification of 95% of porosity, 1.5mm of average pore diameter, 15mm of substrate thickness and 30mm multiplied by 30mm of substrate size; the experimental procedure of this comparative example 2 was identical to that of example 2, except that in step (2), an ultrasonic vibration bar was used while the base was immersed in the conductive liquid carbon-coated gel, so that the conductive liquid was uniformly distributed inside the base.
Comparative example 3:
ultrasonic vibrating rod used in electroplating
Selecting a 3D printing substrate with the specification of 95% of porosity, 1.5mm of average pore diameter, 15mm of substrate thickness and 30mm multiplied by 30mm of substrate size; the experimental procedure of this comparative example 3 was identical to that of example 2, but in both the conducting treatment of step (2) and the plating process of step (3), an ultrasonic vibrator was inserted into the plating liquid to allow efficient exchange of the plating liquid inside the substrate with the plating liquid outside.
Comparative example 4:
injecting the newly added electroplating solution
Selecting a 3D printing substrate with the specification of 95% of porosity, 1.5mm of average pore diameter, 15mm of substrate thickness and 30mm multiplied by 30mm of substrate size; the experimental procedure of the comparative example 4 is the same as that of the experimental example 2, but the substrate printed in the step (1) of the comparative example is provided with blind holes with the diameter of 2-10mm and the distance of 30mm, and in the electroplating process of the step (3), a new electroplating solution is injected into the substrate at the speed of 0.3m/min by using an injection needle matched with the blind holes with the diameter of 2mm, and the volume concentration of the new electroplating solution is at least 1.5 times of that of the original electroplating solution.
Comparative example 5:
the ultrasonic vibration rod and the newly added electroplating solution are used for conducting and electroplating
Selecting a 3D printing substrate with the specification of 95% of porosity, 1.5mm of average pore diameter, 15mm of substrate thickness and 30mm multiplied by 30mm of substrate size; the experimental procedure of this comparative example 5 was identical to that of example 2, except that the substrate printed in step (1) had blind holes with a diameter of 2-10mm and a pitch of 30mm, and both the conductive treatment in step (2) and the plating in step (3) were carried out using an ultrasonic vibrator, and the same additional plating solution as in comparative example 4 was injected into the substrate at a rate of 0.3m/min during the plating.
TABLE 2 influence of different factors on the thickness of the nickel layer inside and outside the substrate during electroplating
Experiments show that when the matrix is too thick, the uniformity of the nickel layer inside and outside the matrix is influenced most by insufficient nickel ions inside the matrix. The electroplating solution is injected into the matrix to promote the uniform arrangement of the nickel layer, but when the nickel ions inside and outside the matrix are sufficient, the largest factor limiting the uniformity of the nickel layer becomes the non-uniform arrangement of the charges inside and outside the matrix; when the substrate is subjected to conductive treatment, an ultrasonic vibrating rod is used in the conductive liquid, so that the conductive liquid can be fully immersed into the substrate, and the charges on the substrate are relatively uniformly distributed, thereby promoting the consistency of the inner nickel layer and the outer nickel layer of the substrate; in addition, an ultrasonic vibrating rod is arranged in the electroplating solution during electroplating, the ultrasonic vibration can accelerate the exchange between the inside and the outside of the electroplating solution, and a certain beneficial effect is uniformly distributed on the nickel layer; finally, the three methods are simultaneously used, so that the internal and external nickel layers of the three-dimensional porous metal can be kept consistent within an acceptable deviation range to the maximum extent, and the porous metal with relatively consistent surface density and physical properties is obtained.
Claims (8)
1. A preparation method of a three-dimensional porous metal material with non-deviation aperture and physical property is characterized by comprising the following steps: the method comprises the following steps:
(1) printing a base body with a uniform porous structure by using a 3D printer, wherein at least 1 blind hole is formed in the base body, and the depth of the blind hole is 1/2 of the thickness of the base body, so that the base body with the blind hole is obtained;
(2) conducting treatment on the substrate with the blind holes to obtain a conductive substrate;
(3) immersing a conductive substrate in electroplating solution, inserting an ultrasonic vibration rod into the electroplating solution, inserting an injection needle matched with the blind hole into the blind hole, injecting a newly added electroplating solution into the blind hole, wherein the volume concentration of the newly added electroplating solution is at least 1.5 times of the volume concentration of the original electroplating solution, then starting electroplating and starting the ultrasonic vibration rod, the current density at the beginning of electroplating is the calculated current density, after the current density is maintained for 2-3 minutes, adjusting the current to 1/3-1/2 of the calculated current density, and after the current adjustment is finished for 30 minutes, stopping injecting the newly added electroplating solution, closing the electroplating current and closing the ultrasonic vibration rod to obtain a three-dimensional porous metal semi-finished product;
(4) cleaning the three-dimensional porous metal semi-finished product, airing for 2-3 days, and putting the semi-finished product into an incinerator to incinerate to remove the conductive matrix; and (3) placing the three-dimensional porous metal semi-finished product in reducing gas for reduction treatment, wherein the reduction reaction temperature is 900 ℃, and obtaining the three-dimensional porous metal material with non-deviation aperture and physical property.
2. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 1, wherein: the printing material used by the 3D printer in the step (1) is bio-plastic polylactic acid.
3. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 1, wherein: the diameter of the blind holes in the step (1) is 2-10mm, and the distance between the blind holes is 30 mm.
4. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 1, wherein: the conducting treatment in the step (2) is implemented by one or a combination of PVD (physical vapor deposition) electroplating, chemical plating and carbon glue coating.
5. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 4, wherein: the carbon coating treatment comprises the steps of immersing the matrix with the blind holes in the carbon coating adhesive, and drying the matrix with the blind holes through ultrasonic vibration treatment to obtain the conductive matrix.
6. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 1, wherein: and (4) in the step (3), the rate of injecting the newly added electroplating solution into the blind hole is 0.2-0.5 m/min.
7. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 1, wherein: the incineration temperature of the incinerator in the step (4) is 400 ℃, and the time is 5 minutes.
8. The method for preparing a three-dimensional porous metal material having no variation in pore size and physical properties according to claim 1, wherein: in the step (4), the reducing gas is hydrogen, and the reduction reaction time is 15 minutes.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298686A (en) * | 2007-04-30 | 2008-11-05 | 比亚迪股份有限公司 | Method for preparing foamed metal |
| CN102094224A (en) * | 2011-03-03 | 2011-06-15 | 常德力元新材料有限责任公司 | Preparation method of porous metal material |
| CN102485965A (en) * | 2010-12-06 | 2012-06-06 | 中国科学院微电子研究所 | Electroplating method of deep blind hole |
| CN203007457U (en) * | 2012-11-30 | 2013-06-19 | 东莞市富默克化工有限公司 | PCB (Printed Circuit Board) electroplating tank |
| CN105189826A (en) * | 2013-03-15 | 2015-12-23 | 莫杜美拓有限公司 | Electrodeposited compositions and nanolaminated alloys for articles prepared by additive manufacturing processes |
| CN106011962A (en) * | 2016-07-13 | 2016-10-12 | 中南大学 | TSV electroplating method and TSV electroplating system under action of ultrasonic outfield |
| CN106793576A (en) * | 2016-12-27 | 2017-05-31 | 江门崇达电路技术有限公司 | A kind of filling perforation method of blind hole in PCB |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4398355B2 (en) * | 2004-12-22 | 2010-01-13 | 住友電気工業株式会社 | Metal porous body and method for producing the same |
| CN102534283A (en) * | 2010-12-10 | 2012-07-04 | 北京有色金属研究总院 | Multi-element alloy foam material and preparation method thereof |
| CN103147100B (en) * | 2013-04-02 | 2016-06-01 | 中南大学 | A kind of preparation method mixing porous metal material |
| CN105177338B (en) * | 2015-08-14 | 2017-12-29 | 华北电力大学 | A kind of preparation method of the adjustable nano porous metal material of yardstick |
| CN106680901B (en) * | 2015-11-11 | 2018-12-21 | 台湾创新材料股份有限公司 | 3-D ordered multiporous method for manufacturing microstructure |
| CN106756186A (en) * | 2015-11-25 | 2017-05-31 | 常德力元新材料有限责任公司 | The preparation method of porous foam nickel-iron-chromium alloy material |
| CN108660489B (en) * | 2018-06-07 | 2020-04-24 | 常德力元新材料有限责任公司 | Preparation method of three-dimensional porous metal material with non-deviation aperture and physical property |
-
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298686A (en) * | 2007-04-30 | 2008-11-05 | 比亚迪股份有限公司 | Method for preparing foamed metal |
| CN102485965A (en) * | 2010-12-06 | 2012-06-06 | 中国科学院微电子研究所 | Electroplating method of deep blind hole |
| CN102094224A (en) * | 2011-03-03 | 2011-06-15 | 常德力元新材料有限责任公司 | Preparation method of porous metal material |
| CN203007457U (en) * | 2012-11-30 | 2013-06-19 | 东莞市富默克化工有限公司 | PCB (Printed Circuit Board) electroplating tank |
| CN105189826A (en) * | 2013-03-15 | 2015-12-23 | 莫杜美拓有限公司 | Electrodeposited compositions and nanolaminated alloys for articles prepared by additive manufacturing processes |
| CN106011962A (en) * | 2016-07-13 | 2016-10-12 | 中南大学 | TSV electroplating method and TSV electroplating system under action of ultrasonic outfield |
| CN106793576A (en) * | 2016-12-27 | 2017-05-31 | 江门崇达电路技术有限公司 | A kind of filling perforation method of blind hole in PCB |
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