CN101638734A - Method for preparing foamed metal nickel - Google Patents
Method for preparing foamed metal nickel Download PDFInfo
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- CN101638734A CN101638734A CN200910018024A CN200910018024A CN101638734A CN 101638734 A CN101638734 A CN 101638734A CN 200910018024 A CN200910018024 A CN 200910018024A CN 200910018024 A CN200910018024 A CN 200910018024A CN 101638734 A CN101638734 A CN 101638734A
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- nickel
- foamed metal
- metal nickel
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Abstract
The invention discloses a method for preparing metal nickel, in particular to a method for preparing foamed metal nickel. In the method, polyether polyurethane is used as a matrix to prepare the foamed metal nickel through the processes of conductive treatment, electrodeposition nickel plating and heat treatment under the protection of hydrogen. Compared with the original technology, the technology of the invention reduces the vacuum degree by one order of magnitude, shortens the vacuumizing time by half, saves the electricity by over 50% and realizes continuous sputtering.
Description
(1) technical field
The present invention relates to a kind of preparation method of metallic nickel, particularly a kind of preparation method of foamed metal nickel.
(2) background technology
The preparation method of existing foamed metal nickel mainly comprises the substrate alligatoring, makes the processes such as negative electrode, nickel plating, aftertreatment of using of electroplating.With the immediate technology one of the present invention be the patent application of EUROPEAN PATENT OFFICE disclosed " Method for the production of a metal foam and a metalfoam obtained ", application number 93200510.1, open day on September 1st, 93, publication number EP0558142; The 2nd, domestic disclosed " a kind of preparation method of spongy foam nickel ", the patent No.: ZL95102640.2.
The former to Polyurethane, polyester, polystyrene, polypropylene and so on organic foam matrix plating conducting metal (copper or nickel) conduction processing, is made into metal foam through electroplating with the cathode sputtering method again.This preparation method's shortcoming is: (1) because during conductionization processing, and the temperature height easily makes foam substrate be out of shape even burn, and has perhaps stopped up the foam hole, makes the interior sputter of hole less than conducting metal, influences the quality of foamed metal; (2) if with copper to the processing of matrix conduction, the purity of nickel foam is affected; (3) owing to be subjected to the high restriction of cathode sputtering method temperature can not obtain the big area finished product, adding does not have aftertreatment, and has poor toughness thereby be not easy to keeping, transportation and use.
The latter's deficiency is: (1) owing to must carry out roughening treatment to substrate, thereby produce a large amount of waste water, contaminate environment; (2) chip production, yield rate is low; (3) vacuum tightness is too high, and the pumpdown time is long, the energy consumption height, and production efficiency is low-cost high.
(3) summary of the invention
The present invention provides a kind of preparation method who improves yield rate and the indeformable foamed metal nickel of matrix in order to remedy the deficiencies in the prior art.
The present invention is achieved through the following technical solutions:
A kind of preparation method of foamed metal nickel, with the polyethers polyurethane as matrix, heat treatment process under conductionization processing, electrodeposit nickel plating and atmosphere of hydrogen protection, prepare foamed metal nickel, it is characterized in that: described matrix conductionization processing adopts the method for magnetic control vacuum sputtering to carry out, and is in the anodic coating equipment at housing, fill with argon gas atmosphere, with the pure nickel is the negative electrode target, and control sputter energy is 5～15kw, with the continuous sputter of the speed of per minute 0.5m～8m; Sputter is guaranteed the minimum vacuum tightness for (0.5～4.0) * 10
-2Pa, vacuum tightness is (1～5) * 10 when charging into the argon gas sputter
-1Pa; After the sputter, deposition one deck nickel in matrix surface and space, the work in-process of formation foamed metal nickel; Described heat treatment process is to reduce sintering under the hydrogen shield atmosphere between 400～1300 ℃, removes body material, forms the high purity foamed metal nickel.
The present invention compares than prior art, has saved matrix roughening treatment step, has reduced production cost, has avoided the environmental pollution that causes because of roughening treatment, and simultaneously, electrodeposit nickel plating and heat treatment process have realized serialization production.
Matrix can be polyester type or polyether-type sponge, also can be man-made fiber such as nylon, polypropylene or exempts from Web materials of textured fiber textiles etc.
Heat treatment process is removed the sponge skeleton that still remains in foamed metal nickel inside after the galvanic deposit by naked light incendiary method, thermolysis process is divided into electric heating process, combustion of hydrogen method.Through residue, the carbon deposit of the further high temperature oxidation process of foamed metal nickel that pyrolysis processing is crossed to remove sponge, under atmosphere of hydrogen, reduce sintering then, improve its crystalline network, finally obtain well behaved foamed metal nickel.
Electrodeposit nickel plating of the present invention is to adopt electrodeposition apparatus to carry out serialization production in nickeliferous ionic electroplate liquid.
Matrix carries out electroforming in special galvanic deposit mode on specific equipment after the conductionization processing, form the foamed metal nickel of different thickness, and the galvanic deposit mode is the zonal mode of working continuously of serialization.The electrodeposition apparatus that is adopted in this production is a specific equipment, has been declared patent, and its patent No. is ZL2008202244848.
Galvanic deposit tank liquor of the present invention mainly adopts sulfamate type or sulfate type, and its processing parameter is as follows:
(1) sulfamate type:
Nickel sulfamic acid (Ni (NH
2SO
3)
24H
2O) 250～600g/L
Nickelous chloride (NiCl
26H
2O) 5～20g/L
Sodium Fluoride (NaF) 1～5g/L
Boric acid (H
3BO
3) 20～50g/L
PH value 3～3.5
40～50 ℃ of temperature
(2) sulfate type:
Single nickel salt (NiSO
47H
2O) 180～300g/L
Nickelous chloride (NiCl
26H
2O) 20～50g/L
Boric acid (H
3BO
3) 30～45g/L
PH value 4.0～4.5
40～55 ℃ of temperature
The present invention aims to provide a kind of production technique of preparing the continous way foamed metal nickel, and the coating of continous way foamed metal nickel is fine and close evenly firmly.The material that the present invention makes can effectively improve the filling consistence to electrode for secondary battery active substance, catalystic material, thereby can improve cell container consistence and catalytic efficiency, in addition, can also be as noise reduction, filtration, antibiotic and mechanical damping material use.
Technology of the present invention is compared with original technology, and vacuum tightness has reduced an order of magnitude, and the pumpdown time has shortened half, and conservation of power can reach more than 50%; Owing to realized continuous sputter, it is too much thoroughly to have overcome in the prior art sputter, and matrix surface is stuck with paste dead easily, and when nickel plating, matrix inside will plate less than nickel, or sputter is very few, the nickel firm inadequately phenomenon of growing.
(4) description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Fig. 1 is matrix conductionization processing synoptic diagram of the present invention;
Fig. 2 is an electrodeposition apparatus synoptic diagram of the present invention;
Fig. 3 is a process flow sheet of the present invention;
Fig. 4 is the process flow sheet of galvanic deposit of the present invention;
Fig. 5 is a process of thermal treatment schema of the present invention.
1 matrix, 2 negative electrode targets, 3 axis of traction, 4 transition axises, 5 unwinding devices, 6 wrap-ups, 7 housings, preliminary draft treatment unit before 8 platings, 9 anode compacting apparatus.
(5) embodiment
The preparation method of this embodiment as shown in Figure 3.
(1) matrix conductionization processing
The conduction treatment process process of matrix 1 as shown in Figure 1.
Utilize the method for magnetic control vacuum sputtering to carry out, matrix 1 is connected with wrap-up 6 with unwinding device 5 respectively with transition axis 4 by axis of traction 3, with the pure nickel is negative electrode target 2, at housing 7 is in the anodic coating equipment, fill with argon gas atmosphere, control sputter energy is 5 ~ 15kw, with the continuous sputter of operation of per minute 0.5m～8m speed; Sputter is guaranteed the minimum vacuum tightness for (0.5～4.0) * 10
-2Pa, vacuum tightness is in (1～5.0) * 10 when charging into the argon gas sputter
-1Pa; After the sputter, deposition one deck nickel makes matrix 1 have electroconductibility in matrix 1 top layer and hole.
(2) galvanic deposit
Electrodeposition apparatus as shown in Figure 2.
Conductionization back matrix 1 carries out preliminary draft through the preliminary draft treatment unit 8 of gambling earlier, on the anode compacting apparatus, carry out electroforming then in special galvanic deposit mode, form the foamed metal nickel of different thickness, the galvanic deposit mode is the zonal mode of working continuously of serialization.
Technical process as shown in Figure 4.
1. power supply: adopt the HF switch electroplating power supply.
2. area density controller: with area density controller on-line Control area density homogeneity.
3. electroplate liquid: electroplate liquid mainly is made up of single nickel salt, nickelous chloride, boric acid etc., adds auxiliary material to strengthen the smooth finish of product, improves hardness.
4. the automatic closely knit device of anode: the process for producing of foamed metal nickel adopts unique automatic anode compacting apparatus 9, has both reduced labour intensity, has improved working efficiency, has solved the problem of area density lack of homogeneity again.
5. galvanic deposit: in electrodeposition process, adopt unique electrodeposition apparatus (seeing accompanying drawing 2), make foamed metal nickel be able to continuous automatic production, finish the work in-process of foamed metal nickel again through clean, air-dry etc.
(3) pyrolysis, redox
This technological process is removed the sponge skeleton that still remains in foamed metal nickel inside by naked light incendiary method, thermolysis process is divided into electric heating process, combustion of hydrogen method.Through residue, the carbon deposit of the further high temperature oxidation process of foamed metal nickel that pyrolysis processing is crossed to remove sponge, under atmosphere of hydrogen, reduce sintering then, improve its crystalline network, finally obtain well behaved foamed metal nickel.Its technical process as shown in Figure 5.
Claims (4)
1. the preparation method of a foamed metal nickel, with the polyethers polyurethane as matrix, heat treatment process under conductionization processing, electrodeposit nickel plating and atmosphere of hydrogen protection, prepare foamed metal nickel, it is characterized in that: described matrix conductionization processing adopts the method for magnetic control vacuum sputtering to carry out, and is in the anodic coating equipment at housing, fill with argon gas atmosphere, with the pure nickel is the negative electrode target, and control sputter energy is 5～15kw, with the continuous sputter of the speed of per minute 0.5m～8m; Sputter is guaranteed the minimum vacuum tightness for (0.5～4.0) * 10
-2Pa, vacuum tightness is (1～5) * 10 when charging into the argon gas sputter
-1Pa; After the sputter, deposition one deck nickel in matrix surface and space, the work in-process of formation foamed metal nickel; Described heat treatment process is to reduce sintering under the hydrogen shield atmosphere between 400～1300 ℃, removes body material, forms the high purity foamed metal nickel.
2. the preparation method of foamed metal nickel according to claim 1 is characterized in that: described electrodeposit nickel plating is to adopt electrodeposition apparatus to carry out serialization production in nickeliferous ionic electroplate liquid.
3. the preparation method of foamed metal nickel according to claim 1 and 2, it is characterized in that: described galvanic deposit tank liquor is the sulfamate type, and its processing parameter is as follows:
Nickel sulfamic acid (Ni (NH
2SO
3)
24H
2O) 250～600g/L
Nickelous chloride (NiCl
26H
2O) 5～20g/L
Sodium Fluoride (NaF) 1～5g/L
Boric acid (H
3BO
3) 20～50g/L
PH value 3～3.5
40～50 ℃ of temperature
4. the preparation method of foamed metal nickel according to claim 1 and 2, it is characterized in that: described galvanic deposit tank liquor is a sulfate type, and its processing parameter is as follows:
Single nickel salt (NiSO
47H
2O) 180～300g/L
Nickelous chloride (NiCl
26H
2O) 20～50g/L
Boric acid (H
3BO
3) 30～45g/L
PH value 4.0～4.5
40～55 ℃ of temperature
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910018024A CN101638734A (en) | 2009-08-18 | 2009-08-18 | Method for preparing foamed metal nickel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910018024A CN101638734A (en) | 2009-08-18 | 2009-08-18 | Method for preparing foamed metal nickel |
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| Publication Number | Publication Date |
|---|---|
| CN101638734A true CN101638734A (en) | 2010-02-03 |
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ID=41613913
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492966A (en) * | 2011-12-22 | 2012-06-13 | 菏泽天宇科技开发有限责任公司 | Foam nickel with ultra-low surface density and high aperture ratio and manufacturing method thereof |
| CN102691078A (en) * | 2012-02-20 | 2012-09-26 | 南京航空航天大学 | Foam metal, quick preparation method thereof, and device used in method |
| CN103789798A (en) * | 2014-01-08 | 2014-05-14 | 菏泽天宇科技开发有限责任公司 | Nickel foam production process |
| CN104577135A (en) * | 2015-01-04 | 2015-04-29 | 哈尔滨工业大学 | Preparation method of three-dimensional silver mesh |
| CN106252095A (en) * | 2016-08-25 | 2016-12-21 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of sponge-type nickel lanthanum alloy carrying transition metal oxide electrode material |
| CN111575755A (en) * | 2020-04-18 | 2020-08-25 | 无锡荣峻环保科技有限公司 | Preparation method of foam copper alloy with strong antibacterial effect |
-
2009
- 2009-08-18 CN CN200910018024A patent/CN101638734A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492966A (en) * | 2011-12-22 | 2012-06-13 | 菏泽天宇科技开发有限责任公司 | Foam nickel with ultra-low surface density and high aperture ratio and manufacturing method thereof |
| CN102691078A (en) * | 2012-02-20 | 2012-09-26 | 南京航空航天大学 | Foam metal, quick preparation method thereof, and device used in method |
| CN103789798A (en) * | 2014-01-08 | 2014-05-14 | 菏泽天宇科技开发有限责任公司 | Nickel foam production process |
| CN104577135A (en) * | 2015-01-04 | 2015-04-29 | 哈尔滨工业大学 | Preparation method of three-dimensional silver mesh |
| CN106252095A (en) * | 2016-08-25 | 2016-12-21 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of sponge-type nickel lanthanum alloy carrying transition metal oxide electrode material |
| CN106252095B (en) * | 2016-08-25 | 2018-03-02 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of sponge-type nickel lanthanum alloy carrying transition metal oxide electrode material |
| CN111575755A (en) * | 2020-04-18 | 2020-08-25 | 无锡荣峻环保科技有限公司 | Preparation method of foam copper alloy with strong antibacterial effect |
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Application publication date: 20100203 |