CN101298686A - Method for preparing foamed metal - Google Patents
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- CN101298686A CN101298686A CNA2007101020229A CN200710102022A CN101298686A CN 101298686 A CN101298686 A CN 101298686A CN A2007101020229 A CNA2007101020229 A CN A2007101020229A CN 200710102022 A CN200710102022 A CN 200710102022A CN 101298686 A CN101298686 A CN 101298686A
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Abstract
The invention relates to a preparation method of a foam metal, which comprises the conductivity attachment of a foam plastic substrate, the metal galvanization on the foam plastic substrate that is attached with conductivity and the removing of the foam plastic substrate; the method of metal galvanization on the foam plastic substrate that is attached with conductivity comprises following steps: the foam plastic substrate that is attached with conductivity is used as a cathode so as to contact with electroplate liquid and implement galvanization under the galvanization condition, and the electroplate liquid is an aqueous solution of a salt of a galvanized metal; wherein, in the galvanization process, an insoluble anode is adopted, the content of the salt of the galvanized metal in the electroplate liquid is maintained between 100 and 500 grams per liter, and pH value is maintained between 2 and 5. The foam metal produced by adopting the preparation method of a foam metal provided by the invention has excellent uniformity of planar density.
Description
Technical field
The present invention relates to a kind of preparation method of foamed metal.
Background technology
Alkaline cell is to be assembled in battery steel shell by positive plate, negative plate, ionogen and barrier film.Positive and negative plate generally is to be coated on the conducting base by the mixture with active substance, additive and binding agent to make.Conducting base generally adopts for example materials such as steel band of nickel foam or foam copper, perforated metal band, perforation plated metal of foamed metal and since foamed metal for example nickel foam or foam copper special tridimensional network, big specific surface area, high porosity, good perviousness and very big fillable energy and preferentially be elected to be conducting base.The special microvoid structure of foamed metal can make the active substance of electrode be fully used, and reduces battery internal resistance, the augmenting response area, thus improve battery performance.
The production technique of common foamed metal is earlier with after the porous plastics matrix conductionization, to carry out the galvanic deposit of metal, then thermal treatment scumming plastic substrate.Galvanic deposit in this technology is to adopt metal to be plated as anode, porous plastics matrix after the conductionization is as negative electrode, electroplate, the size that generally metal is cut into 25 * 25mm is contained in the titanium basket as anode, metal block on the anode constantly consumes, and enters in the solution and is plated on the porous plastics matrix, causes in the titanium basket built on stilts, make strength of electric field unbalanced, finally make the area density (weight of metal on the foamed metal of unit surface) of foamed metal inhomogeneous.
As mentioned above, foamed metal is when particularly nickel foam is as the conducting base of battery positive and negative electrode, the negative or positive electrode slurry (active substance) of battery is filled in the vesicular structure of nickel foam, if the area density of nickel foam conducting base is inhomogeneous, then make the loading level of positive pole, negative electrode active material inhomogeneous, directly have influence on the capacity of battery, cause cell container inhomogeneous.
Summary of the invention
The objective of the invention is to overcome the uneven defective of the area density of foamed metal in the prior art, a kind of preparation method who makes the uniform foamed metal of area density of foamed metal is provided.
The invention provides a kind of preparation method of foamed metal, this method comprises porous plastics matrix conductionization, is leading plated metal on the electrochemical porous plastics matrix, and plastic substrate then defoams; Comprise in the method for leading plated metal on the electrochemical porous plastics matrix, to lead electrochemical porous plastics matrix contacts with electroplate liquid as negative electrode, under galvanized condition, electroplate, described electroplate liquid is the aqueous solution of the salt of plated metal, it is characterized in that, in electroplating process, adopt insoluble anode, keeping the content of the salt of plated metal in the electroplate liquid is the 100-500 grams per liter, and the pH value is 2-5.
Adopt the preparation method of foamed metal provided by the invention, make the foamed metal area density of acquisition even, thereby it is even to make the foamed metal that is obtained by the present invention make the performance of battery such as cell container and internal resistance, capability retention is better simultaneously.
In addition since metallic compound especially the price of nickel or copper compound is more much lower than the price of price of metal especially nickel or copper, therefore adopt method provided by the invention to greatly reduce the cost of preparation foamed metal.
Embodiment
The preparation method of foamed metal provided by the invention comprises that this method comprises porous plastics matrix conductionization, is leading plated metal on the electrochemical porous plastics matrix, and plastic substrate then defoams; Comprise in the method for leading plated metal on the electrochemical porous plastics matrix, to lead electrochemical porous plastics matrix contacts with electroplate liquid as negative electrode, under galvanized condition, electroplate, described electroplate liquid is the aqueous solution of the salt of plated metal, it is characterized in that, in electroplating process, adopt insoluble anode, keep the content of the salt of plated metal in the electroplate liquid to be the 100-500 grams per liter, be preferably the 200-400 grams per liter, the pH value is 2-5, be preferably 2.5-3.8.
According to method provided by the invention, the reaction that is taken place in electroplating process is,
Anode main reaction: 4OH
--4e=2H
2O+O
2
Negative electrode main reaction: A
X++ xe=A (A is a plated metal)
Owing to constantly consume OH at anode
-Ion, and constantly consume the plated metal ion at negative electrode, therefore need in electroplate liquid, add to form OH
-Ion and plated metal ionic compound are to keep the content and the pH value of the salt of plated metal in the electroplate liquid.
So content and pH value in order to keep plated metal salt in the electroplate liquid, in electroplating process, can select in electroplate liquid, to add the oxyhydroxide and/or the oxide compound of plated metal, perhaps also can select in electroplate liquid, to add the salt of plated metal and add alkali simultaneously.In the preferred case, select in electroplate liquid, to add the oxyhydroxide of plated metal and/or the mode of oxide compound, both can keep the content of the salt of plated metal, also can regulate the pH value.The oxyhydroxide of described metal and/or oxide compound are the oxyhydroxide and/or the oxide compound of nickel, copper, tin, palladium, gold or rhodium.
The mode that the mode of above-mentioned interpolation can be selected interpolation continuously or intermittently add.Under the preferable case,, select the mode that adds continuously for the concentration of the salt of the pH value that keeps electroplate liquid and plated metal keeps constant.
According to method provided by the invention, the insoluble anode that is adopted is for well known to a person skilled in the art various insoluble anodes, for example iridium titanium net, tantalum iridium titanium net, ruthenium-iridium-tantalum net, platinum or graphite.
According to method provided by the invention, in order to cushion the change of pH value in the electroplate liquid, in the preferred case, described electroplate liquid also contains the pH value buffer reagent of 10-50 grams per liter.Described pH value buffer reagent be described pH value buffer reagent for well known to a person skilled in the art various pH value buffer reagents, for example one or more in boric acid, thionamic acid, sulfuric acid and the hydrochloric acid are preferably boric acid.
According to method provided by the invention, under the preferable case, the salt of described plated metal is the salt of nickel, copper, tin, palladium, gold or rhodium.
According to method provided by the invention, the salt of described plated metal can be various water-soluble salt, one or more in vitriol, carbonate, muriate and the organic acid salt for example, and described organic acid salt is preferably sulfamate.The preferred vitriol that adopts in the above-mentioned various salt.
According to method provided by the invention, described galvanized condition is for well known to a person skilled in the art, for example this condition comprises, current density is 5-15A/dm
2, be preferably 8-12A/dm
2, the temperature of electroplate liquid is 40-70 ℃, is preferably 50-60 ℃ that the galvanized time is 20-60 minute, preferred 10-50 minute.
According to method provided by the invention, the porous plastics matrix is led electrochemical method can be adopted and well known to a person skilled in the art the whole bag of tricks, for example can adopt the method for coated with conductive glue, electroless plating or vacuum plating, preferably on the porous plastics matrix coated with conductive glue so that porous plastics matrix conductionization.
Generally speaking, the process of coated with conductive glue comprises flooded described porous plastics matrix 3-10 minute in conductive resin, then the porous plastics matrix was taken out and extrude unnecessary conductive resin, and dry under temperature is 90-110 ℃.Described conductive resin contains graphite, resene caking agent and water, is benchmark with the weight of conductive resin, and the content of graphite in conductive resin is 5-16 weight %, and the content of resene caking agent is 1-5 weight %, and the content of water is 80-90 weight %.Can also contain ammoniacal liquor in the conductive resin, the amount of ammoniacal liquor makes the pH value of conductive resin be 10-11.Described resene caking agent can be acrylamide or phenolic caking agent.
Generally speaking, the method for electroless plating comprises the porous plastics matrix is contacted with the chemical plating fluid that contains nickel salt and reductive agent.Nickel salt is preferably nickelous chloride and/or single nickel salt.Reductive agent is selected from one or more in hypophosphite, formaldehyde and the hydroborate, and described hypophosphite is preferably sodium hypophosphite and/or potassium hypophosphite.The reaction conditions of electroless plating comprises that the temperature of chemical plating fluid is 40-90 ℃, is preferably 40-80 ℃; Chemical plating fluid pH value is 4-12; The time of electroless plating is 0.05-0.5 hour, is preferably 0.1-0.2 hour; The concentration of reductive agent described in the chemical plating fluid is the 0.2-1.0 mol, and the concentration of nickel salt is the 0.1-0.25 mol.Wherein, before carrying out electroless plating, can the surface of porous plastics matrix be activated, the activatory method can be existing various activation methods, for example can use the colloidal palladium activation method, under 35-45 ℃ the porous plastics matrix being handled 4 minutes in LH8305A activation solution (Guangzhou international chemical company produce), is the processing 100 seconds under 35-45 ℃ of the sulphuric acid soln of 40-60 grams per liter with concentration then.
Generally speaking, the method for vacuum plating is included in (absolute pressure is the 2-10 handkerchief) under the vacuum condition, hits the nickel target with electron beam, and nickle atom is dropping on the porous plastics matrix under the effect in magnetic field.
According to method provided by the invention, the method for the plastic substrate that defoams can adopt the whole bag of tricks conventional in the prior art.For example, earlier the porous plastics behind the plated metal is burnt down at 300-700 ℃ in oxidizing atmosphere, the preferred burn time is burned the removing and decarburization of porous plastics that made in 0.1-0.5 hour wherein, in hydrogen reducing atmosphere, reduce down then at 500-1100 ℃, the preferred recovery time is to make oxidized metallic reducing in 0.5-2 hour, and described reducing atmosphere is preferably hydrogen atmosphere.
According to method provided by the invention, in the preferred case, electroplated metal is nickel, copper, tin, palladium, gold or rhodium on the electrochemical porous plastics matrix leading.
According to method provided by the invention, described porous plastics can be preferably polyurethane sponge or non-woven fabrics, more preferably polyurethane sponge for the conventional various porous plastics that use in the prior art.
Below by embodiment the present invention is further elaborated.
Embodiment 1
1, preparation nickel foam
Select for use 50 square metres of continuous polyurethane sponges (hole density 110PPI (quantity in hole on the inchage), 1000 millimeters of width, 1.9 millimeters of thickness) as the porous plastics matrix.
The polyurethane sponge matrix was flooded 8 minutes in conductive resin (contain 8 weight % graphite and 2 weight % acrylamide caking agents, pH is 10), then the polyurethane sponge matrix is taken out and extrude unnecessary conductive resin, dry down at 100 ℃ then.
The polyurethane sponge matrix that is coated with conductive resin is immersed in electroplate liquid (200 grams per liter single nickel salts, 50 grams per liter boric acid, pH are 2.5) as negative electrode, with tantalum iridium titanium net as anode.Connect direct supply, current density is 10A/dm
2, electroplated 50 minutes down at 50 ℃, the interpolation speed with 20 gram/minute adds nickel hydroxide continuously in galvanized process simultaneously.
Polyurethane sponge matrix after the nickel plating was burnt 0.3 hour in air under 600 ℃, the polyurethane sponge burning is removed and decarburization, under hydrogen atmosphere, reducing 60 minutes under 1000 ℃, obtain nickel foam then oxidized metallic reducing.
2, make the SC-1700mAh nickel-cadmium cell
Adopt the above-mentioned nickel foam that obtains to make anode, use common nickel plated steel strip to make battery cathode, produce 30 SC-1700mAh nickel-cadmium cells.
Anodal is made.Above-mentioned nickel foam compressing tablet, the cut-parts that obtain are made into 200 * 61 * 1.4 millimeters 15 of nickel foam substrates, at the nickel strap (being flow collection band) of 200 * 3 * 0.2 millimeter of the mid-way of nickel foam substrate roller weldering.Anode sizing agent being coated in above-mentioned roller having welded on the nickel foam substrate of nickel strap, is 160 ℃ of oven dry down in temperature, and scraping blade and roller-compaction are produced 15 200 * 61 * 0.6 millimeter battery anode slice then.Anode sizing agent is 60: 4: 8 by weight ratio: 3: 25 nickel hydroxide, cobalt oxide, nickel, tackiness agent Xylo-Mucine (CMC) and water are formulated.Above-mentioned battery anode slice is cut grow up 30 of 200 millimeters, wide 30 millimeters positive plate from the mid-way of roller weldering nickel strap, as the positive pole of battery.Each positive pole contains nickel hydroxide active substance 8 grams.
The making of negative pole.(aperture is 36.63 millimeters to adopt continuous perforated SPCC nickel plating Punching steel strip, thickness is 0.08 millimeter, width is 210 millimeters) as the cadmium oxide negative electrode matrix, cathode size is coated on this negative pole matrix, under 160 ℃ temperature, dry, scraping blade and roller-compaction are produced 30 250 * 32 * 0.6 millimeter battery cathode sheet, as the negative pole of battery then.Cathode size is 60: 10: 10 by weight ratio: 20 Cadmium oxide, cadmium, binding agent Xylo-Mucine (CMC) and water are formulated.Each negative pole contains Cadmium oxide active substance 10 grams.
Above-mentioned positive pole, diaphragm paper and above-mentioned negative pole lamination are reeled, put into battery case, carry out the end face weldering, (electrolytic solution is KOH and LiOH mixed aqueous solution to inject electrolytic solution 1.1g/Ah, the LiOH that contains 30 weight %KOH and 15 grams per liters in the mixed aqueous solution), be made into 30 of SC-1700mAh nickel-cadmium cells.
Comparative Examples 1
1, preparation nickel foam
Prepare nickel foam according to the method for describing among the embodiment 1, different is, in electroplating process, adopt nickel block as anode, and contain the single nickel salt of 200 grams per liters, the boric acid of 30 grams per liters and the nickelous chloride of 10-50 grams per liter in the electroplate liquid, the pH value of electroplate liquid is 4, and the interpolation speed with 0.05ml/Ah adds sulfuric acid continuously in galvanized process simultaneously.
Obtain nickel foam thus.
2, make the SC-1700mAh nickel-cadmium cell
Make battery according to the method for describing among the embodiment 1, different is that the nickel foam that adopts this Comparative Examples 1 to obtain is made the positive pole of battery.Obtain 30 of SC-1700mAh nickel-cadmium cells.
Embodiment 2
Prepare nickel foam and make battery according to the method for describing among the embodiment 1, different is in electroplating process, the single nickel salt, the boric acid of 20 grams per liters, the pH that contain 400 grams per liters in the electroplate liquid are 3.8, and the interpolation speed with 60 gram/minute adds single nickel salt continuously, with the interpolation speed adding sodium hydroxide of 20 gram/minute.
Obtain nickel foam and make 30 on the battery of NI-G SC-1700mAh model.
Performance test
1, the physicochemical property of nickel foam test
(1) area density uniformity test: adopt the QNG-3 type mass thickness tester of nuclear energy institute of Tsing-Hua University to measure;
(2) hole density measurement: the quantity of observing the hole on nickel foam one inchage at microscope (XTL-2400 type, Shanghai plant and instrument factory) down;
(3) endwise tensile strength and transverse tensile strength: nickel foam is cut into 2 * 10 centimetres of sizes by vertical, horizontal, then by vertical, horizontal tensiometer (NK-50 pointer-type tensiometer, energy Instr Ltd. of Hangzhou section) draw, the power during fracture/2 obtain endwise tensile strength and transverse tensile strength;
(4) snappiness: doubling 180 degree are opened, and the cracking conduct is not once;
(5) content of nickel, iron, copper, manganese, sulphur and carbon: adopt Beijing Kechuang sea light GGX of Instr Ltd. type instrument aas determination.
2, the performance test of battery (pressing the IEC285:1993 standard)
Adopt above-mentioned physicochemical property testing method that embodiment 1-2 and Comparative Examples 1 resulting nickel foam are tested, resulting the results are shown in Table 1.
Table 1
| Performance | Embodiment 1 | Comparative Examples 1 | Embodiment 2 |
| Thickness (millimeter) | 1.9 | 1.9 | 1.9 |
| The area density homogeneity | 99.8％ | 90％ | 99.5％ |
| Hole density (quantity in hole on the inchage) | 110 | 110 | 110 |
| Endwise tensile strength (Newton/millimeter) | 2.1 | 2.0 | 2.0 |
| Transverse tensile strength (Newton/millimeter) | 1.8 | 1.8 | 1.8 |
| Snappiness (inferior) | 8 | 8 | 8 |
| Nickel (%) | 99.3 | 99.2 | 99.2 |
| Iron (ppm) | 38 | 30 | 30 |
| Copper (ppm) | 40 | 45 | 42 |
| Manganese (ppm) | 15 | 18 | 16 |
| Sulphur (ppm) | 30 | 25 | 25 |
| Carbon (ppm) | 100 | 110 | 120 |
Adopt above-mentioned battery performance test method, 30 batteries that respectively obtain in embodiment 1-2 and the Comparative Examples 1 are carried out performance test, the resulting table 2 that the results are shown in.
Table 2
| Performance | Embodiment 1 | Comparative Examples 1 | Embodiment 2 |
| Capacity (mAh) | 1700±20 | 1700±50 | 1700±25 |
| Internal resistance (m Ω) | 4.5±0.1 | 4.5±0.3 | 4.5±0.1 |
| The mean value of the capability retention (10C discharge) that the circulation of 30 batteries is 300 times | 90 | 88 | 91 |
As can be seen from Table 1, the area density homogeneity (99.8%) of resultant nickel foam is high more a lot of than the area density homogeneity (90%) of resultant nickel foam in the Comparative Examples 1 among the embodiment 1, and the content of other physicochemical property such as endwise tensile strength, transverse tensile strength, snappiness and nickel, iron, copper, manganese, sulphur and carbon is suitable substantially.
As can be seen from Table 2, the homogeneity of embodiment 1 resulting cell container and internal resistance is all than the height in the Comparative Examples 1, and capability retention is also higher.
Therefore the data in table 1 and the table 2 can illustrate, because the area density of the nickel foam that employing method provided by the invention obtains is more even, thereby the homogeneity of the capacity of the battery that is made by nickel foam of the present invention, internal resistance is all fine, and the qualification rate that makes battery is higher, and capability retention is higher.
Claims (12)
1, a kind of preparation method of foamed metal, this method comprise porous plastics matrix conductionization, are leading plated metal on the electrochemical porous plastics matrix, and plastic substrate then defoams; Comprise in the method for leading plated metal on the electrochemical porous plastics matrix, to lead electrochemical porous plastics matrix contacts with electroplate liquid as negative electrode, under galvanized condition, electroplate, described electroplate liquid is the aqueous solution of the salt of plated metal, it is characterized in that, in electroplating process, adopt insoluble anode, keeping the content of the salt of plated metal in the electroplate liquid is the 100-500 grams per liter, and the pH value is 2-5.
2, method according to claim 1, wherein, keeping the content of the salt of plated metal in the electroplate liquid is the 200-400 grams per liter, the pH value is 2.5-3.8.
3, method according to claim 1 and 2, wherein, by in electroplate liquid, adding the oxyhydroxide of plated metal and/or content and the pH value that oxide compound keeps the salt of plated metal in the electroplate liquid.
4, method according to claim 3, wherein, the oxyhydroxide of described metal and/or oxide compound are the oxyhydroxide and/or the oxide compound of nickel, copper, tin, palladium, gold or rhodium.
5, method according to claim 1, wherein, described insoluble anode is iridium titanium net, tantalum iridium titanium net, ruthenium-iridium-tantalum net, platinum or graphite.
6, method according to claim 1, wherein, described electroplate liquid also contains the pH value buffer reagent of 10-50 grams per liter.
7, method according to claim 6, wherein, described pH value buffer reagent is one or more in boric acid, thionamic acid, sulfuric acid and the hydrochloric acid.
8, method according to claim 1, wherein, the salt of described plated metal is the soluble salt of nickel, copper, tin, palladium, gold or rhodium.
9, according to claim 1 or 8 described methods, wherein, the salt of described plated metal is one or more in vitriol, carbonate, muriate and the organic acid salt.
10, method according to claim 1, wherein, described galvanized condition comprises that current density is 5-15A/dm
2, the temperature of electroplate liquid is 40-70 ℃, the galvanized time is 10-50 minute.
11, method according to claim 1 wherein, is led electrochemical method with the porous plastics matrix and is comprised the method that adopts coated with conductive glue, electroless plating or vacuum plating.
12, method according to claim 1, wherein, the process of the plastic substrate that defoams comprises, earlier the porous plastics behind the plated metal is burnt down at 300-700 ℃ in oxidizing atmosphere, reduces down at 500-1100 ℃ in hydrogen reducing atmosphere then.
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| CN108660489A (en) * | 2018-06-07 | 2018-10-16 | 常德力元新材料有限责任公司 | A kind of preparation method in aperture and the agonic three-dimensional porous metal material of physical property |
| 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 |
| CN111378998A (en) * | 2020-04-09 | 2020-07-07 | 烟台东方新程科技有限公司 | Foam metal processing technology |
| CN111378998B (en) * | 2020-04-09 | 2022-03-01 | 烟台东方新程科技有限公司 | Foam metal processing technology |
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