CN103647054B - A kind of nickel radical battery positive pole and preparation method thereof and the nickel radical battery using this positive pole - Google Patents
A kind of nickel radical battery positive pole and preparation method thereof and the nickel radical battery using this positive pole Download PDFInfo
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- CN103647054B CN103647054B CN201310565818.3A CN201310565818A CN103647054B CN 103647054 B CN103647054 B CN 103647054B CN 201310565818 A CN201310565818 A CN 201310565818A CN 103647054 B CN103647054 B CN 103647054B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/24—Electrodes for alkaline accumulators
- H01M4/32—Nickel oxide or hydroxide electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/24—Electrodes for alkaline accumulators
- H01M4/26—Processes of manufacture
- H01M4/28—Precipitating active material on the carrier
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of nickel radical battery positive pole and preparation method thereof and the nickel radical battery using this positive pole.Drip irrigation device of the present invention is: a kind of nickel radical battery positive pole, comprise positive electrode active materials, described positive electrode active materials contains nickel hydroxide and soluble calcium salt calcium metaborate or line borate, and wherein the content of soluble calcium salt calcium metaborate or line borate is the 0.01%-5% of weight of nickel hydroxide.The invention also discloses the preparation method of this nickel radical battery positive pole and use the Ni-based secondary cell of the alkalescence of this nickel radical battery positive pole.In soluble calcium salt of the present invention calcium ion be uniformly distributed the combination property effectively can improving nickel radical battery with the introducing of useful anion, comprise and reduce nickel radical battery internal resistance, improve high-temperature behavior and improve cycle performance.
Description
Technical field
The invention belongs to nickel radical battery technical field, be specifically related to a kind of nickel radical battery positive pole and preparation method thereof and the nickel radical battery using this positive pole.
Background technology
The Ni-based secondary cell of existing alkalescence comprises ickel-cadmium cell, Ni-H cell, zinc-nickel cell and Hawkins cell etc., has different performance and application approach, is widely used in daily life and industrial production, be in different developing stage separately.The cadmium that ickel-cadmium cell is poisonous because negative pole contains, can cause the environmental problem of heavy metal pollution, progressively be replaced at present by Ni-H cell, start to withdraw from the market.Ni-H cell negative pole is active material with hydrogen bearing alloy, has higher capacity and excellent electrical property, and environmental protection, be widely used the fields such as civilian and electric automobile, be with fastest developing speed at present, purposes is the widest, the Ni-based secondary cell that technique is the most ripe.In the last few years, along with the progress of zinc load technology and the improvement of its performance, the development visual field of people that had the zinc-nickel cell of last 100 years history to enter into again, receives more concern, is in the vigorous growth phase at present.Hawkins cell, owing to having best cost performance, along with people obtain constantly progress for the research of iron negative pole, in the last few years, also more and more received the concern of people, was still in the research and development phase at present.The common feature of the Ni-based secondary cell of alkalescence is exactly that they all adopt nickel hydroxide active material as positive pole, and method prepared by positive pole is all similar; In addition, Ni-based secondary cell is all positive limiting quantity, and that is the discharge performance of positive pole determines the capacity of nickel radical battery, therefore, is all same being suitable for for the improvement opportunity of nickel hydroxide positive plate for different nickel radical batteries.
In recent years, the improvement of Ni-based secondary cell high-temperature behavior receives the concern of people.Research finds, the principal element of restriction nickel radical battery high-temperature behavior is that under hot environment, the reduction of positive pole oxygen evolution potential causes.Therefore, the main path improving nickel radical battery high-temperature behavior is exactly improve the oxygen evolution potential of positive pole, improves nickel positive pole charge efficiency under the high temperature conditions.Prior art is improved by doping in nickel hydroxide active material, the high-temperature behavior of mode to nickel radical battery positive pole that be coated and use additive.Wherein, the doping of rare earth element and modification etc. that is coated, cobalt compound is comprised.These methods can improve the oxygen evolution potential of nickel radical battery positive pole to a certain extent, improve high temperature compression part.But rare earth element cost is high, method for coating complex process, the high expensive of preparation.Therefore, these methods can increase the cost of nickel radical battery to a certain extent significantly.In the last few years, cheap calcium salt, owing to having the effect of same raising nickel radical battery positive pole high temperature compression part, received the concern of people.
Such as, in CN101357781A, disclose a kind of spherical nickel hydroxide for high-temperature nickel batteries, by the coated slightly solubility chloric metal-salt of nickel hydroxide surface, such as calcirm-fluoride; A kind of spherical nickel hydroxide for high-temperature nickel batteries is disclosed in CN101357780A, by the coated insoluble phosphate of nickel hydroxide surface, such as calcium phosphate; A kind of spherical nickel hydroxide for high-temperature nickel batteries is disclosed, by modifying calcium carbonate at nickel hydroxide surface in CN102760874A.Meanwhile, document also has use slightly solubility calcium salt calcium hydroxide, calcium carbonate or calcirm-fluoride directly to join the report used in nickel radical battery positive pole as anode additive.These methods all achieve certain effect for the improvement of nickel radical battery high-temperature behavior, but the procedure of coated slightly solubility calcium salt is complicated, and condition is harsh, and cost is higher.Therefore, the method that suitability for industrialized production adopts slightly solubility calcium salt (such as calcium hydroxide, calcium carbonate or calcirm-fluoride etc.) to adulterate usually is produced.But; because calcium salt is all non-conducting material; a small amount of slightly solubility calcium salt particle is difficult to mix with a large amount of micron-sized nickel hydroxide particle; the method can cause calcium ion skewness in positive pole; intercept the conductive network of nickel radical battery; cause nickel radical battery internal resistance to raise, cycle life is deteriorated.Therefore, although adopt the method cost of doping slightly solubility calcium salt lower relative to cladding process, the homogeneity that calcium ion distributes in nickel radical battery positive pole is poor, needs further to be improved.
Summary of the invention
The present invention solves the deficiencies in the prior art to provide a kind of nickel radical battery positive pole adopting soluble calcium salt to modify and preparation method thereof, solve calcium salt cladded type nickel hydroxide complicated process of preparation in prior art, the uneven technical problem causing nickel radical battery internal resistance higher of slightly solubility calcium salt additive dispersion, in addition, present invention also offers the Ni-based secondary cell of alkalescence adopting this nickel radical battery positive pole to prepare.
Technical scheme of the present invention is: a kind of nickel radical battery positive pole, comprise positive electrode active materials, it is characterized in that: described positive electrode active materials contains nickel hydroxide and soluble calcium salt calcium metaborate or line borate, and wherein the content of soluble calcium salt calcium metaborate or line borate is the 0.01%-5% of weight of nickel hydroxide.
A preparation method for nickel radical battery positive pole, is characterized in that comprising the following steps: the conductive agent of the nickel hydroxide of 100 weight portions and 0.5-10 weight portion mixes and obtains semifinal blend by (1), (2) soluble calcium salt of the hydrophilic agglomerant of 0.5-5 weight portion and 0.01-5 weight portion is mixed, be dissolved in the deionized water of 10-30 weight portion, (3) semifinal blend that step (1) is obtained is joined in the solution of step (2) gained, under the condition stirred, add the hydrophobic binder of 0.1-2 weight portion, through fully stirring the slurry preparing good fluidity, (4) slurry prepared by step (3) is coated on plus plate current-collecting body through pasting or slurry technique, through drying, compacting, be cut into the nickel radical battery positive pole of required size, wherein the conductive agent described in step (1) is cobalt protoxide or T255 nickel powder or the mixture of the two, hydrophilic agglomerant described in step (2) is sodium carboxymethylcellulose (CMC) or hydroxypropyl methylcellulose (HPMC), described soluble calcium salt is calcium metaborate or line borate, hydrophobic binder described in step (3) is polytetrafluoroethylene (PTFE) emulsion, plus plate current-collecting body described in step (4) is Foamed Nickel, fiber nickel or punched nickel-plated steel band.
As preferably, the preferred calcium metaborate further of the soluble calcium salt selected by the present invention, research finds, metaboric acid root is useful for the raising of the improvement of nickel radical battery cathode performance, particularly oxygen evolution potential.
As preferably, the hydrophobic binder selected by the present invention is CMC or HPMC, in view of HPMC and the good compatibility of calcium metaborate, and preferred HPMC further.
A kind of nickel radical battery, comprises battery container, and seal electrode group in the cell housing and electrolyte, described electrode group comprises positive pole, and negative pole and barrier film, is characterized in that, described positive pole adopts nickel radical battery positive pole provided by the present invention.In view of nickel radical battery positive pole production method and formulation differences less, it is applicable all equally that nickel radical battery positive pole prepared by this invention comprises ickel-cadmium cell, Ni-H cell, zinc-nickel cell and Hawkins cell etc. for the Ni-based secondary cell of alkalescence, and this is conventionally known to one of skill in the art.
In the preparation method of nickel radical battery positive pole of the present invention, by with slurry process in add soluble calcium salt, make calcium ion to be blended in anode sizing agent easily equably, through slurry or pasting, dry, compacting, cut and make pole plate.Due to the superior dispersibility of soluble calcium salt, make the distribution of calcium ion in final pole plate very even, to much less than slightly solubility calcium salt of the harmful effect of positive pole conductivity.After being assembled into alkaline secondary cell, add alkali lye, at this moment the calcium ion meeting in positive plate and the hydroxide ion in alkali lye form calcium hydroxide, be distributed in active material surface with dividing equally, thus make the equally distributed calcium ion previously added change equally distributed calcium hydroxide (exist due to carbonate may be had in alkali lye, therefore also can form fraction calcium carbonate) into.This invention is for the selection of soluble calcium salt, carry out based on useful anion, research finds, it is useful that the introducing of the anion such as metaboric acid root and borate improves for the electrical property of nickel radical battery positive pole, and other soluble calcium salt, as calcium nitrate or calcium chloride etc. all can introduce the anion causing nickel radical battery penalty, such as nitrate anion can have a strong impact on the self-discharge performance of nickel radical battery.In a word, the preparation method of nickel radical battery positive pole provided by the invention is obvious to cathode performance improvement effect, and step is simple, is easy to realize.
The beneficial effect that the present invention is compared with the prior art is: preparation method's step of the present invention is simple, easy to implement, being evenly distributed of calcium ion effectively can improve the combination property of nickel radical battery with the introducing of useful anion, comprise and reduce nickel radical battery internal resistance, improve high-temperature behavior and improve cycle performance.This method solve the difficulties in dispersion using slightly solubility calcium salt to cause in current alkaline Ni-based anode of secondary battery preparation, nickel radical battery internal resistance is high, the problems such as cycle performance difference and the high cost using the coated nickel hydroxide of slightly solubility calcium salt to face, complex process, the problems such as condition is harsh.
Accompanying drawing explanation
Fig. 1 is that the EDX calcium ion profiles versus of nickel radical battery positive pole prepared by the nickel radical battery positive pole prepared of the embodiment of the present invention 1 and embodiment 6 schemes.
Embodiment
The embodiment of form by the following examples, is described in further details foregoing of the present invention, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment.All technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
The preparation of positive pole: ball-shape nickel hydroxide 100g, cobalt protoxide 5g and T255 nickel powder 5g mix by (1), make active material compound; (2) join in the deionized water of 20g after 1.0g calcium metaborate and 2.5g hydroxypropyl methylcellulose being mixed, stir and form the uniform aqueous solution; (3) active material compound obtained for step (1) is joined in the aqueous solution of step (2), and add 1.0g ptfe emulsion and mix and make slurry; (4) by slurry, dry, cut, clear powder, the operations such as welding electrode ear are prepared into the positive pole finished product that length and width are of a size of 90mm × 42mm.
The preparation of negative pole: used by hydrogen-bearing alloy powder the roll-in of Ni-MH battery dry method negative pole technique online to negative pole matrix copper, at its surface infiltration one deck ptfe emulsion, after drying and roll-in, cuts into the negative pole finished product made and be of a size of 125mm × 42mm.
Battery assembles: by above-mentioned nickel positive pole, storage hydrogen negative pole therebetween is across the barrier film of PP material sulfonation process, being coiled into multi-turn type core with winder winding enters in AA shaped steel shell, implantation quality concentration be 30% KOH and mass concentration be 2% LiOH electrolyte, the Ni-H cell of AA1700 is made in finally sealing.
Embodiment 2
The making of positive pole: ball-shape nickel hydroxide 100g, cobalt protoxide 0.25g and T255 nickel powder 0.25g mix by (1), make active material compound; (2) 0.01g line borate and 0.5g sodium carboxymethylcellulose are mixed join in the deionized water of 10g, stir and form the uniform aqueous solution; (3) active material compound obtained for step (1) is joined in the aqueous solution of step (2), and add 0.1g ptfe emulsion and mix and make slurry; (4) by slurry, dry, cut, clear powder, the operations such as welding electrode ear are prepared into the positive pole finished product that length and width are of a size of 90mm × 42mm.
The preparation of negative pole: used by hydrogen-bearing alloy powder the roll-in of Ni-MH battery dry method negative pole technique online to negative pole matrix copper, at its surface infiltration one deck ptfe emulsion, after drying and roll-in, cuts into the negative pole finished product made and be of a size of 125mm × 42mm.
Battery assembles: by above-mentioned nickel positive pole, storage hydrogen negative pole therebetween is across the barrier film of PP material sulfonation process, being coiled into multi-turn type core with winder winding enters in AA shaped steel shell, implantation quality concentration be 30% KOH and mass concentration be 2% LiOH electrolyte, the Ni-H cell of AA1700 is made in finally sealing.
Embodiment 3
The making of positive pole: ball-shape nickel hydroxide 100 parts, cobalt protoxide 2g and T255 nickel powder 4g mix by (1), make active material compound; (2) 5g calcium metaborate and 5g hydroxypropyl methylcellulose are mixed join in the deionized water of 30g, stir and form the uniform aqueous solution; (3) active material compound obtained for step (1) is joined in the aqueous solution of step (2), and add 2g ptfe emulsion and mix and make slurry; (4) by slurry, dry, cut, clear powder, the operations such as welding electrode ear are prepared into the positive pole finished product that length and width are of a size of 90mm × 42mm.
The preparation of negative pole: used by hydrogen-bearing alloy powder the roll-in of Ni-MH battery dry method negative pole technique online to negative pole matrix copper, at its surface infiltration one deck ptfe emulsion, after drying and roll-in, cuts into the negative pole finished product made and be of a size of 125mm × 42mm.
Battery assembles: by above-mentioned nickel positive pole, storage hydrogen negative pole therebetween is across the barrier film of PP material sulfonation process, being coiled into multi-turn type core with winder winding enters in AA shaped steel shell, implantation quality concentration be 30% KOH and mass concentration be 2% LiOH electrolyte, the Ni-H cell of AA1700 is made in finally sealing.
Embodiment 4
The negative pole of control group 1 is prepared same as the previously described embodiments, and calcium metaborate or line borate are not added in the difference of the preparation of positive pole, and other formula is identical with preparation method, and the preparation method of Ni-H cell is also same as the previously described embodiments.
Embodiment 5
The negative pole preparation of control group 2 is identical with above-mentioned embodiment, calcium metaborate or line borate are not added in the difference of the preparation of positive pole, but adding the calcirm-fluoride of 1.0g, other formula is identical with preparation method, and the preparation method of Ni-H cell is also same as the previously described embodiments.
Embodiment 6
The negative pole preparation of control group 3 is identical with above-mentioned embodiment, calcium metaborate or line borate are not added in the difference of the preparation of positive pole, but adding the calcium hydroxide of 1.0g, other formula is identical with preparation method, and the preparation method of Ni-H cell is also same as the previously described embodiments.
The contrast that in positive pole prepared by the positive pole of embodiment 1 preparation and embodiment 6, calcium ion distributes:
In order to verify the distribution situation of calcium ion in positive pole, the carrying out of nickel radical battery positive pole prepared by nickel radical battery positive pole embodiment 1 prepared and embodiment 6 EDX calcium ion profiles versus, as shown in Figure 1, adopt positive pole calcium ion of the present invention to be evenly distributed in positive pole, and adopt the positive pole calcium ion skewness of slightly solubility calcium salt.Absolutely proved by contrast, adopt this simple method of soluble calcium salt can solve slightly solubility calcium salt problem pockety in positive pole easily.
The battery that embodiment makes and the battery performance that control group makes contrast:
Battery high-temperature behavior is tested:
Ni-H cell prepared by the Ni-H cell prepare embodiment 1 and control group charges 1.2 hours with 1800mA respectively under 25 DEG C and 70 DEG C of conditions, battery shelves 20 minutes afterwards, then 0.2C is discharged to voltage is 1.0V, and measure the capacity of battery, test result is in table 1.
Table 1 battery high-temperature behavior is tested
Cycle performance of battery is tested:
The method of testing that Ni-H cell prepared by the Ni-H cell prepare embodiment 1 and control group carries out 1C charge-discharge test cycle life respectively under 25 DEG C and 70 DEG C of ambient temperatures carries out cycle life test, capacity attenuation stops test with 80% of initial capacity, and test result is in table 2.
Table 2 cycle performance of battery is tested
As can be seen from above test result, the Ni-H cell of the positive pole adopting the present invention to prepare can effectively improve battery high-temperature discharge capacity and cycle life.Compare with 6 with embodiment 5, Ni-H cell internal resistance prepared by embodiments of the invention 1 is obviously on the low side, this is mainly owing to the be uniformly distributed introducing with useful anion of calcium ion in positive pole inside, in addition, the obtained Ni-H cell of the embodiment of the present invention 2,3 and embodiment 5 are compared with 6 and are also had comparatively excellent high-temperature behavior and cycle performance.
Embodiment above describes general principle of the present invention, principal character and advantage.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (1)
1. a preparation method for nickel radical battery positive pole, is characterized in that comprising the following steps: the conductive agent of the nickel hydroxide of 100 weight portions and 0.5-10 weight portion mixes and obtains semifinal blend by (1); (2) the soluble calcium salt calcium metaborate of the hydrophilic agglomerant of 0.5-5 weight portion and 0.01-5 weight portion or line borate are mixed, be dissolved in the deionized water of 10-30 weight portion; (3) semifinal blend that step (1) is obtained is joined in the solution of step (2) gained, under the condition stirred, add the hydrophobic binder of 0.1-2 weight portion, through fully stirring the slurry preparing good fluidity; (4) slurry prepared by step (3) is coated on plus plate current-collecting body through pasting or slurry technique, through drying, compacting, be cut into the nickel radical battery positive pole of required size, conductive agent described in step (1) is cobalt protoxide or T255 nickel powder or the mixture of the two, hydrophilic agglomerant described in step (2) is sodium carboxymethylcellulose or hydroxypropyl methylcellulose, hydrophobic binder described in step (3) is ptfe emulsion, and the plus plate current-collecting body described in step (4) is Foamed Nickel, fiber nickel or punched nickel-plated steel band.
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| CN104157848B (en) * | 2014-08-26 | 2017-03-22 | 常德力元新材料有限责任公司 | Positive plate of nickel-hydrogen power battery, preparation method thereof and the nickel-hydrogen power battery |
| CN109546091B (en) * | 2018-11-07 | 2021-10-26 | 超威电源集团有限公司 | Preparation method of high-specific-energy zinc-nickel battery positive electrode |
| CN111463434B (en) * | 2020-03-18 | 2022-01-11 | 山东合泰新能源有限公司 | High specific energy zinc-nickel battery positive electrode |
| CN111463429B (en) * | 2020-03-18 | 2022-01-07 | 山东合泰新能源有限公司 | Preparation method of high specific energy zinc-nickel battery positive electrode slurry |
| CN112164799A (en) * | 2020-09-29 | 2021-01-01 | 浙江大学 | Boron crosslinked binder, electrode slice and preparation method |
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| Enhancement of the high-temperature of advanced nickel-metal hydride batteries with NaOH electrolyte containing NaBO2;Enbo Shangguan等;《International Journal of Hydrogen Energy》;20130709;第38卷;第10623页的结论部分 * |
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Effective date of registration: 20180816 Address after: 453000 chemical and physical power industry park, Makino District, Xinxiang, Henan Patentee after: Henan Heng Ming new energy Co., Ltd. Address before: 453007 46 East Jianhe Road, Xinxiang, Henan Patentee before: Henan Normal University |
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