CN1770509A - Method for making nickel foam - Google Patents
Method for making nickel foam Download PDFInfo
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- CN1770509A CN1770509A CNA200410052119XA CN200410052119A CN1770509A CN 1770509 A CN1770509 A CN 1770509A CN A200410052119X A CNA200410052119X A CN A200410052119XA CN 200410052119 A CN200410052119 A CN 200410052119A CN 1770509 A CN1770509 A CN 1770509A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
This invention relates to foam nickel process method, which comprises the steps of polyurethane sponge conductivity and electrical depositing and sintering and is characterized by the following: the said steps directly deacidize deposited polyurethane sponge for sintering, wherein, the decidizing gas is aminolysis gas with temperature of 400 to 1000 degrees and time about thirty to sixty minutes with analysis gas consumption of 0.4 to 0.8 L/g. This invention method is of high product rate and low consumption and good nickel mechanism property.
Description
Technical field
The present invention relates to the manufacture method of battery electrode material, particularly relate to the manufacture method of the foam nickel material that a kind of battery electrode uses.
Background technology
Nickel foam is a kind of material that is used to make battery electrode, and the production technology of regular-type foam nickel material is: earlier with the polyurethane sponge conductionization, carry out electro-deposition again, carry out sintering at last.In the above-mentioned steps, the conductionization processing generally comprises chemical plating, coated with conductive glue, three kinds of modes of vacuum plating; Electro-deposition can be sulfate or sulfamate nickel plating; Existing sintering process is to pass through air burn off polyurethane sponge earlier, what two steps of reduction sintering were finished under hydrogen reducing atmosphere then, wherein, air burn off polyurethane sponge is to carry out oxidation and decarbonization to handle under 300～700 ℃ of temperature; It is to reduce 30-60 minute under 800～1000 ℃ of hydrogen reducing atmosphere conditions that reduction is handled, and reducing atmosphere is a decomposed ammonia, and decomposing the tolerance consumption is 0.8-1.2L/g (every gram nickel need consume 0.8-1.2 and rise decomposed ammonia).In the existing sintering process, when removing the Polyurethane sponge, generally, nickel foam is also by complete oxidation, and nickel foam becomes fragile after oxidation, will ftracture by the external force effect; If the inequality of being heated, nickel foam can be out of shape arch upward, cracking and rate of finished products are low easily; Separate the too high or overlong time of temperature if burn, then can occur causing oxide skin to thicken, and producing inner grain boundary oxidation,, still can make porous metals have leakiness to connect, cause mechanical strength to reduce even reduce processing than severe oxidation.Owing to adopt oxidation technology, cause equipment investment and power consumption to increase, and temperature required height during reduction, hydrogen usage is big, the energy consumption height.
Summary of the invention
The present invention is intended to address the above problem, the sintering process in producing with effective improvement foam nickel material, and the manufacture method of a kind of rate of finished products height, energy consumption is low, the nickel foam mechanical performance is good nickel foam is provided.
For achieving the above object, the invention provides a kind of manufacture method of improved nickel foam, the step of this method comprises polyurethane sponge conductionization, electro-deposition and sintering, it is characterized in that described sintering step is with the direct pyrolysis sintering in reducing atmosphere of the foam polyurethane after the electro-deposition, wherein, reducing atmosphere is a decomposed ammonia, reduction temperature is 400～1000 ℃, and the recovery time is 30～60 minutes, and dividing the consumption of venting one's spleen is 0.4～0.8L/g.(every gram nickel need consume 0.4-0.8 and rise decomposed ammonia)
Described decomposed ammonia is the mist of nitrogen and hydrogen, and the volume ratio of nitrogen and hydrogen is 1: 3.
The reaction mechanism of method of the present invention is, the nickel foam that contains polyamine fat sponge after the electro-deposition is pyrolysis sintering in hydrogen reducing atmosphere directly, and carbon wherein and hydrogen effect generate CH
4, C
2H
6Deng hydrocarbon gas, above-mentioned gasification can be with the cleaner removal of the graphite C in the porous body.
Contribution of the present invention is, it efficiently solves easy to crack that the nickel foam that exists in the prior art exists in sintering process, and distortion is arched upward, and rate of finished products is low, energy consumption height, shortcomings such as nickel foam mechanical performance instability.Separate step (being oxidation step) owing to removed the air burning in the conventional method, and directly carry out the pyrolysis sintering in reducing atmosphere, thereby obtained significant effect, method of the present invention compared with prior art has following distinguishing feature:
One, nickel foam does not have cracking phenomena, the rate of finished products height.
Two, because no air oxidation step, thereby energy consumption and equipment investment cost are low.
Three, because no air oxidation step, thereby nickel foam mechanical performance and chemical property is good and stable performance.
Four, the nickel foam cost of manufacture is low.
Five, product strength behind the sintering, pliability are good, and carbon, oxygen content are low, and color and luster evenly, metallic luster is silvery white in color.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of the nickel foam of existing sintering technology making
Fig. 2 is the scanning electron microscope diagram of the nickel foam of method making of the present invention.
Embodiment
The manufacture method of nickel foam of the present invention is the sintering step in foam nickel material manufacturing process, and the air burning of removing in the conventional method is separated step (being oxidation step), and directly carries out the pyrolysis sintering in reducing atmosphere.The step of method of the present invention is: polyamine fat sponge conductionization-electro-deposition-sintering.Wherein, common process is adopted in polyamine fat sponge conductionization and electro-deposition, and conductionization can be chemical plating, coated with conductive glue, magnetron sputtering; Electro-deposition can be that sulfate system also can be the sulfamic acid salt system.The process conditions of sintering step are as follows: 400～1000 ℃ of temperature, and 30～60 minutes recovery times, reducing atmosphere is a decomposed ammonia, decomposing the tolerance consumption is 0.4～0.8L/g.(every gram nickel need consume 0.4-0.8 and rise decomposed ammonia)
Product strength behind the sintering, pliability are good, and carbon, oxygen content are low, and color and luster evenly, metal is silvery white in color.
The present invention may be better understood by following embodiment.
Embodiment 1
Get continuous polyurethane sponge (aperture 110PPI, thickness 1.9mm, width 1000mm) two volumes, each 150m conduction is designated I, II respectively.Conductionization employing coated with conductive adhesive process, I, II two twist in gluing under the identical conditions, the solid content 7～10% (weight) of glue, pH value 10～11,10～30 ℃ of temperature, viscosity 5～20mPas; Under identical conditions, adopt the electronickelling of sulfate nickel plating system then, nickel-plated quality 430 ± 25g/m2.I is carried out sintering by art methods, i.e. oxidation 8 minutes under 650 temperature conditions, tolerance 1L/g is decomposed in reduction 40 minutes under 900 ℃, 930 ℃, 900 ℃ temperature hydrogen reducing atmospheres then, promptly makes nickel foam I after the cooling.Again II is carried out sintering by sintering manufacture craft of the present invention, promptly directly reduced 40 minutes under 650 ℃, 850 ℃, 650 ℃ temperature hydrogen reducing atmospheres, decomposition tolerance is 0.6L/g, promptly makes nickel foam II after the cooling.
Performance test comparative example 1
Nickel foam I, II ftracture bad as table 1 in sintering process among the embodiment 1:
Table 1
| Cracking place number | Area of cracks (m 2) | (gross area is pressed 150m to fraction defective 2Meter) | |
| Nickel foam I | 8 | 3 | 2％ |
| Nickel foam II | 0 | 0 | 0 |
As shown in Table 1, the nickel foam of method sintering of the present invention does not have cracking phenomena, and fraction defective is 0, has improved the rate of finished products of nickel foam significantly.
Performance test comparative example 2
Nickel foam I among the embodiment, II are done physics (machinery), chemical property test, its result such as table 2:
Table 2
| Performance | I | II |
| Thickness (mm) | 1.9 | 1.9 |
| Surface density (g/m2) | 430±25 | 430±25 |
| Aperture (PPI) | 110 | 110 |
| Outward appearance | Silvery white, color and luster is even | Silvery white, color and luster is even |
| Endwise tensile strength (N/mm) | 2.3 | 2.8 |
| Transverse tensile strength (N/mm) | 1.9 | 2.3 |
| Horizontal pliability (inferior) | 9 | 10 |
| Nickel (%) | 99.3 | 99.5 |
| Sulphur (ppm) | 30 | 34 |
| Carbon (ppm) | 110 | 110 |
| Oxygen (ppm) | 450 | 50 |
Pliability test in the last table is to be stainless steel bar coiling nickel foam one circle of 10mm with diameter, does not ftracture to once, opens and reels, and repeats above-mentioned action, the number of times of being reeled till ftractureing.Following pliability is tested all method herewith.
As shown in Table 2, the nickel foam that adopts method of the present invention to make, its mechanical performance (tensile strength, pliability) obviously are better than the nickel foam that prior art is made; The relatively middle carbon of chemical property, both no significant differences of sulfur content, but its oxygen content of nickel foam that adopts method of the present invention to make is starkly lower than the nickel foam that prior art is made.
Performance test comparative example 3
Nickel foam I, II in the foregoing description are scanned with scanning electron microscopy, obtain SEM figure as shown in Figure 1, 2.Its scanning electron microscopy adopts the JSM-5610LV type scanning electron microscopy of Jeol Ltd..
By last figure as seen, the nickel foam of prior art made has identical surface configuration and internal organizational structure with the nickel foam of method made of the present invention.
Performance test comparative example 4
Nickel foam I, II required energy consumption such as table 3 in sintering process among the embodiment:
Table 3
| Air burn separate temperature (℃) | Air burn and to separate the time (minute) | Reduction temperature (℃) | Recovery time (minute) | Decomposed ammonia amount (L/g) | |
| Nickel foam I | 650 | 8 | 900、930、 900 | 40 | 1 |
| Nickel foam II | No air burns to be separated | 0 | 650、850、 650 | 40 | 0.6 |
By in the table 3 as can be known, adopt method of the present invention, its energy consumption, reduction tolerance are starkly lower than the method for prior art.Method of the present invention has obviously reduced cost, and does not have oxidation step, has therefore reduced equipment cost.
Embodiment 2
The decomposition tolerance that only changes in the sintering technology of the present invention is 0.8L/g, and all the other steps and process conditions are with embodiment 1.
Performance test comparative example 5
Nickel foam I, II ftracture bad as table 4 in sintering process among the embodiment 2:
Table 4
| Nickel foam I | Cracking place several 9 | Area of cracks (m 2) 3.2 | (gross area is pressed 150m to fraction defective 2Meter) 2.13% |
| Nickel foam II | 0 | 0 | 0 |
As shown in Table 4, the nickel foam of method sintering of the present invention does not have cracking phenomena, and fraction defective is 0, has improved the rate of finished products of nickel foam significantly.
Performance test comparative example 6
Nickel foam I among the embodiment, II are done physics (machinery), chemical property test, its result such as table 5:
Table 5
| Performance | I | II |
| Thickness (mm) | 1.9 | 1.9 |
| Surface density (g/m2) | 430±25 | 430±25 |
| Aperture (PPI) | 110 | 110 |
| Outward appearance | Silvery white, color and luster is even | Silvery white, color and luster is even |
| Endwise tensile strength (N/mm) | 2.3 | 2.7 |
| Transverse tensile strength (N/mm) | 1.9 | 2.3 |
| Horizontal pliability (inferior) | 9 | 11 |
| Nickel (%) | 99.3 | 99.5 |
| Sulphur (ppm) | 30 | 28 |
| Carbon (ppm) | 110 | 107 |
| Oxygen (ppm) | 450 | 46 |
As shown in Table 5, the nickel foam that adopts method of the present invention to make, its mechanical performance (tensile strength, pliability) obviously are better than the nickel foam that prior art is made; The relatively middle carbon of chemical property, both no significant differences of sulfur content, but its oxygen content of nickel foam that adopts method of the present invention to make is starkly lower than the nickel foam that prior art is made.
Performance test comparative example 7
Nickel foam I, II required energy consumption such as table 6 in sintering process among the embodiment:
Table 6
| Air burn separate temperature (℃) | Air burn and to separate the time (minute) | Reduction temperature (℃) | Recovery time (minute) | Decomposed ammonia amount (L/g) | |
| Nickel foam I | 650 | 8 | 900、930、 900 | 40 | 1 |
| Nickel foam II | No air burns to be separated | 0 | 650、850、 650 | 40 | 0.8 |
By in the table 6 as can be known, adopt method of the present invention, its energy consumption, reduction tolerance are starkly lower than the method for prior art.Method of the present invention has obviously reduced cost, and does not have oxidation step, has therefore reduced equipment cost.
Embodiment 3
The decomposition tolerance that only changes in the sintering technology of the present invention is 0.9L/g, and all the other steps and process conditions are with embodiment 1.
Performance test comparative example 8
Nickel foam I, II ftracture bad as table 7 in sintering process among the embodiment 3:
Table 7
| Cracking place number | Area of cracks (m 2) | (gross area is pressed 150m to fraction defective 2Meter) | |
| Nickel foam I | 9 | 2.5 | 1.67％ |
| Nickel foam II | 0 | 0 | 0 |
As shown in Table 7, the nickel foam of method sintering of the present invention does not have cracking phenomena, and fraction defective is 0, has improved the rate of finished products of nickel foam significantly.
Performance test comparative example 9
Nickel foam I among the embodiment, II are done physics (machinery), chemical property test, its result such as table 8:
Table 8
| Performance | I | II |
| Thickness (mm) | 1.9 | 1.9 |
| Surface density (g/m2) | 430±25 | 430±25 |
| Aperture (PPI) | 110 | 110 |
| Outward appearance | Silvery white, color and luster is even | Silvery white, color and luster is even |
| Endwise tensile strength (N/mm) | 2.3 | 2.8 |
| Transverse tensile strength (N/mm) | 1.9 | 2.3 |
| Horizontal pliability (inferior) | 9 | 10 |
| Nickel (%) | 99.3 | 99.4 |
| Sulphur (ppm) | 30 | 28 |
| Carbon (ppm) | 110 | 108 |
| Oxygen (ppm) | 450 | 49 |
As shown in Table 8, the nickel foam that adopts method of the present invention to make is decomposed tolerance its mechanical performance (tensile strength, pliability) when 0.9L/g and obviously is better than the nickel foam that prior art is made; The relatively middle carbon of chemical property, both no significant differences of sulfur content, but its oxygen content of nickel foam that adopts method of the present invention to make is starkly lower than the nickel foam that prior art is made.But compare the performance no significant difference with embodiment of the invention two-phase, when decomposing tolerance the nickel foam performance is not had obvious improvement, when 0.8L/g, be advisable so decompose the tolerance upper limit above 0.8L/g.
Performance test comparative example 10
Nickel foam I, II required energy consumption such as table 9 in sintering process among the embodiment:
Table 9
| Air burn separate temperature (℃) | Air burn and to separate the time (minute) | Reduction temperature (℃) | Recovery time (minute) | Decomposed ammonia amount (L/g) | |
| Nickel foam I | 650 | 8 | 900、930、 900 | 40 | 1 |
| Nickel foam II | No air burns to be separated | 0 | 650、850、 650 | 40 | 0.9 |
By in the table 9 as can be known, adopt method of the present invention, its energy consumption, reduction tolerance are starkly lower than the method for prior art.Method of the present invention has obviously reduced cost, and does not have oxidation step, has therefore reduced equipment cost.But compare with embodiment two, divide the consumption of venting one's spleen many, cost is advisable at 0.8L/g so decompose the tolerance upper limit than embodiment two height.
Embodiment 4
The decomposition tolerance that only changes in the sintering technology of the present invention is 0.4L/g, and all the other steps and process conditions are with embodiment 1.
Performance test comparative example 11
Nickel foam I, II ftracture bad as table 10 in sintering process among the embodiment 2:
Table 10
| Cracking place number | Area of cracks (m 2) | (gross area is pressed 150m to fraction defective 2Meter) | |
| Nickel foam I | 9 | 3.1 | 2.06％ |
| Nickel foam II | 0 | 0 | 0 |
As shown in Table 10, the nickel foam of method sintering of the present invention does not have cracking phenomena, and fraction defective is 0, has improved the rate of finished products of nickel foam significantly.
Performance test comparative example 12
Nickel foam I among the embodiment, II are done physics (machinery), chemical property test, its result such as table 11:
Table 11
| Performance | I | II |
| Thickness (mm) | 1.9 | 1.9 |
| Surface density (g/m2) | 430±25 | 430±25 |
| Aperture (PPI) | 110 | 110 |
| Outward appearance | Silvery white, color and luster is even | Silvery white, color and luster is even |
| Endwise tensile strength (N/mm) | 2.3 | 2.6 |
| Transverse tensile strength (N/mm) | 1.9 | 2.2 |
| Horizontal pliability (inferior) | 9 | 10 |
| Nickel (%) | 99.3 | 99.3 |
| Sulphur (ppm) | 30 | 28 |
| Carbon (ppm) | 110 | 112 |
| Oxygen (ppm) | 450 | 60 |
As shown in Table 11, the nickel foam that adopts method of the present invention to make, its mechanical performance (tensile strength, pliability) obviously are better than the nickel foam that prior art is made; The relatively middle carbon of chemical property, both no significant differences of sulfur content, but its oxygen content of nickel foam that adopts method of the present invention to make is starkly lower than the nickel foam that prior art is made.
Performance test comparative example 13
Nickel foam I, II required energy consumption such as table 12 in sintering process among the embodiment:
Table 12
| Air burn separate temperature (℃) | Air burn and to separate the time (minute) | Reduction temperature (℃) | Recovery time (minute) | Decomposed ammonia amount (L/g) | |
| Nickel foam I | 650 | 8 | 900、930、 900 | 40 | 1 |
| Nickel foam II | No air burns to be separated | 0 | 650、850、 650 | 40 | 0.4 |
By in the table 12 as can be known, adopt method of the present invention, its energy consumption, reduction tolerance are starkly lower than the method for prior art.Method of the present invention has obviously reduced cost, and does not have oxidation step, has therefore reduced equipment cost.
Embodiment 5
The decomposition tolerance that only changes in the sintering technology of the present invention is 0.3L/g, and all the other steps and process conditions are with embodiment 1.
Performance test comparative example 14
Nickel foam I, II ftracture bad as table 13 in sintering process among the embodiment 2:
Table 13
| Nickel foam I | Cracking place several 9 | Area of cracks (m 2) 2.7 | (gross area is pressed 150m to fraction defective 2Meter) 1.8% |
| Nickel foam II | 0 | 0 | 0 |
As shown in Table 13, the nickel foam of method sintering of the present invention does not have cracking phenomena, and fraction defective is 0, has improved the rate of finished products of nickel foam significantly.
Performance test comparative example 15
Nickel foam I among the embodiment, II are done physics (machinery), chemical property test, its result such as table 14:
Table 14
| Performance | I | II |
| Thickness (mm) | 1.9 | 1.9 |
| Surface density (g/m2) | 430±25 | 430±25 |
| Aperture (PPI) | 110 | 110 |
| Outward appearance | Silvery white, color and luster is even | Be black on a small quantity, the color and luster inequality |
| Endwise tensile strength (N/mm) | 2.3 | 2.5 |
| Transverse tensile strength (N/mm) | 1.9 | 2.0 |
| Horizontal pliability (inferior) | 9 | 7 |
| Nickel (%) | 99.3 | 98.6 |
| Sulphur (ppm) | 30 | 45 |
| Carbon (ppm) | 110 | 480 |
| Oxygen (ppm) | 450 | 260 |
As shown in Table 14, the nickel foam that adopts method of the present invention to make, when decomposition tolerance is 0.3L/g, carbon content, oxygen content in its appearance luster inequality, the chemical property are higher, pliability is relatively poor in the physical property, thus the nickel foam that adopts method of the present invention to make, when decomposing tolerance less than 0.4L/g, the performance of nickel foam does not reach the requirement of regular-type foam nickel, is advisable at 0.4L/g so decompose the tolerance lower limit.
The foregoing description and performance test comparative example result show, when method of the present invention is 0.4-0.8L/g in decomposition tolerance, have improved rate of finished products significantly, have eliminated the cracking phenomena in the sintering process; The physics of nickel foam, chemical property, particularly tensile strength and oxygen content are good.The present invention greatly reduces energy consumption, has also reduced equipment investment cost and nickel foam cost of manufacture.
Claims (2)
1, a kind of manufacture method of nickel foam, its step comprises polyurethane sponge conductionization, electro-deposition and sintering, it is characterized in that, described sintering step is with the direct pyrolysis sintering in reducing atmosphere of the foam polyurethane after the electro-deposition, wherein, reducing atmosphere is a decomposed ammonia, and reduction temperature is 400～1000 ℃, recovery time is 30～60 minutes, and dividing the consumption of venting one's spleen is 0.4～0.8L/g.
2, the method for claim 1 is characterized in that, described decomposed ammonia is the mist of nitrogen and hydrogen, and the volume ratio of nitrogen and hydrogen is 1: 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200410052119XA CN1770509A (en) | 2004-11-03 | 2004-11-03 | Method for making nickel foam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200410052119XA CN1770509A (en) | 2004-11-03 | 2004-11-03 | Method for making nickel foam |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1770509A true CN1770509A (en) | 2006-05-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200410052119XA Pending CN1770509A (en) | 2004-11-03 | 2004-11-03 | Method for making nickel foam |
Country Status (1)
| Country | Link |
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| CN (1) | CN1770509A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191395A (en) * | 2011-04-15 | 2011-09-21 | 兰州大学 | Preparation method of foamed nickel or foamed nickel-cobalt alloy |
| CN106076297A (en) * | 2016-06-24 | 2016-11-09 | 青岛贞正分析仪器有限公司 | Integral type stir bar sorptive extraction and preparation method thereof |
-
2004
- 2004-11-03 CN CNA200410052119XA patent/CN1770509A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191395A (en) * | 2011-04-15 | 2011-09-21 | 兰州大学 | Preparation method of foamed nickel or foamed nickel-cobalt alloy |
| CN102191395B (en) * | 2011-04-15 | 2013-07-24 | 兰州大学 | Preparation method of foamed nickel or foamed nickel-cobalt alloy |
| CN106076297A (en) * | 2016-06-24 | 2016-11-09 | 青岛贞正分析仪器有限公司 | Integral type stir bar sorptive extraction and preparation method thereof |
| CN106076297B (en) * | 2016-06-24 | 2018-09-18 | 青岛贞正分析仪器有限公司 | Integral type stir bar sorptive extraction and preparation method thereof |
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