CN102912174A - Lead and graphene composite material - Google Patents
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Abstract
The invention discloses a lead and graphene composite material which is obtained by coating lead particles on the surface of the graphene by adopting the electrochemical deposition method. The weight of the graphenein the lead and graphene composite material accounts for 10-90%, each graphene sheet contains 1-50 carbon atom layers, and the size of the lead particles is 100nm to 10m. The lead and the graphene are combined effectively, and the lead and the grapheme can be more uniformly mixed with the negative electrode active material such as the lead powder of the lead-acid battery. The lead and graphene composite material disclosed by the invention can be directly used as the negative electrode of the lead-acid battery or the additive of the negative electrode of the lead-carbon super battery so that the charge acceptance capacity of the battery can be impropved and the HRPSoC cycle life can be prolonged.
Description
Technical field
The present invention relates to plumbous carbon composite and preparation method thereof, especially plumbous and graphene composite material and preparation method thereof, this matrix material can directly as the negative pole of lead acid cell, also can be used as the cathode additive agent of plumbous charcoal superbattery.
Background technology
Secondary power supply in emerging power and the application of energy storage field mainly contains the superbattery that traditional lead acid batteries, lithium ion battery, nickel metal hydride battery, flow battery, sodium-sulfur cell, ultracapacitor and a new generation adopt plumbous charcoal technology.Compared to other secondary power supplies, lead-acid cell has good security and cheap price, occupies critical role always.The plumbous charcoal superbattery of development in recent years, combine the characteristics of traditional lead acid batteries and ultracapacitor, by in the negative pole of lead acid cell, adding the Carbon Materials of a certain amount of high-specific surface area, utilize the high capacitance characteristic of Carbon Materials and good conductive characteristic, the instantaneous large-current that passes through in the buffering negative plate, the sulphating that suppresses the negative plate surface, improve utilization ratio and the charge acceptance of plumbous active substance, on the basis of low price, safety, significantly improved the cycle life under battery partial state of charge high current charge-discharge (HRPSoC) operating mode.
Carbonaceous additive in the plumbous charcoal superbattery mainly contains gac, graphite, carbon black etc.The specific surface area of gac is large, and the electric capacity activity is high, but electroconductibility is relatively poor, and foreign matter content is high, and overpotential of hydrogen evolution is low; The electroconductibility of graphite is better, but almost without capacitance characteristic, can't cushion the instantaneous large-current that passes through in the negative plate; The excellent electric conductivity of carbon black, but the electric capacity activity is low, easily reunites, and suction seriously is difficult to realize closing cream when content surpasses 1%.Graphene is a kind of special carbon material, is with sp by carbon atom
2The hexangle type that hybridized orbital forms is the flat film of honeycomb lattice.Because the feature of monoatomic layer crystalline structure, Graphene has special power electro-optic-thermal characteristic, and its electronic mobility surpasses 15000cm under the normal temperature
2/ Vs, and resistivity only approximately 10
-6Ω cm, lower than copper or silver, be the present in the world material of resistivity minimum.Graphene only has the accurate two-dimensional material of a carbon atom as thickness, also have very high specific surface area and high electric capacity activity.Therefore, with the cathode additive agent of Graphene as plumbous charcoal superbattery, can improve the specific conductivity of negative pole, the buffering instantaneous large-current, suppress the sulphating on negative plate surface, improved the cycle life under battery partial state of charge high current charge-discharge (HRPSoC) operating mode.
In the present plumbous charcoal superbattery manufacturing processed, the addition manner of Carbon Materials mainly is to carry out mechanically mixing with lead powder.Because Carbon Materials density is far smaller than the density of lead powder, therefore be difficult to realize both even mixing, and the mode by mechanically mixing, effective contact interface of plumbous active substance and carbon material is less, can not give full play to the electricity of carbon and lead and the electric capacity advantage.The present invention adopts the method for electrochemical deposition to coat plumbous particle on the Graphene surface, make this matrix material have simultaneously the high power characteristic of carbon material and the high capacity characteristics of plumbous active substance concurrently, this lead graphene composite material directly is used as the negative pole of lead acid cell, or as the cathode additive agent of plumbous charcoal superbattery, can significantly improve charge acceptance and the HRPSoC cycle life of battery.
Summary of the invention
One object of the present invention is for difficult, few with the effective contact interface of the plumbous active substance problem of Carbon Materials Uniform Dispersion in the plumbous charcoal superbattery negative pole, a kind of plumbous graphene composite material is provided, consistency plumbous and Graphene is good in this matrix material, also can realize mixing more uniformly with lead powder, can be directly as the negative pole of lead acid cell, or as the cathode additive agent of plumbous charcoal superbattery.
For this reason, the present invention is by the following technical solutions: it is for being electrochemically-deposited in plumbous particle in the formed matrix material in graphene platelet surface, the weight percentage of Graphene is 10%-90% in the plumbous graphene composite material, each graphene film comprises 1-50 carbon atomic layer, and the particle diameter of plumbous particle is 100nm-10m.
Another object of the present invention is to provide a kind of preparation method of plumbous graphene composite material.
For achieving the above object, the technical solution used in the present invention is as follows, and it may further comprise the steps:
(1), take pure stereotype as anode, have the conducting base of graphene film to be negative electrode take load, the plumbous particle of Constant Electric Current electroless plating on graphene film;
(2), the graphene film of deposit lead particle is washed, dry under 40-80 ° of C vacuum environment, film is scraped from the conducting base surface, its grinding is broken, obtain described plumbous graphene composite material.
On the basis of adopting technique scheme, the present invention also can adopt following further technical scheme:
Also have following steps described step (1) is front:
(1-1), with the oxidized graphite flake ultra-sonic dispersion in the magnesium nitrate aqueous isopropanol, form positively charged graphite oxide film sol;
(1-2), take the graphite oxide film sol as ionogen, constant voltage electrophoretic deposition oxidized graphite flake film on conducting base obtains graphene film by reduction again.
In the graphite oxide film sol of step (1), the weight ratio of graphite oxide and magnesium nitrate is 50:1-200:1.
The voltage of the constant voltage electrophoretic deposition of step (2) is 20-180V, and depositing time is 10s-10min.
The approach that the oxidized graphite flake film of step (2) is reduced into graphene film is to reduce 1-4h in the 60-90 ° of saturated hydrazine hydrate atmosphere of C, or in argon gas atmosphere, calcines 1-4h under 500 ° of C.
The conducting base of step (2) can be stereotype, titanium plate or platinum plate or other inactive, conductive material.
The plumbous plating bath of step (3) can be one or more the mixing plating bath in fluoroboric acid plating bath, silicofluoric acid plating bath, Seignette salt plating bath and the trolamine plating bath.
Step (3) is 0.1-4A/dm in the current density of graphene film surface electrical deposit lead particle
2, electrodeposition time is 1min-2h.
Compared with prior art, plumbous graphene composite material of the present invention is at the plumbous particle of Graphene surface deposition, lattice imperfection on the Graphene plane can play firmly to the plumbous particle of galvanic deposit " pinning " effect, realize the good combination of plumbous particle and Graphene, greatly increase contact interface plumbous and carbon.The surface coats plumbous Graphene and has larger proportion, is more easily to obtain to disperse uniformly when the negative electrode active material such as lead powder mixes.The preparation method of plumbous graphene composite material provided by the invention, can be by changing the concentration of graphite oxide film sol, the voltage of electrophoretic deposition and depositing time, the conditions such as the solution composition of galvanic deposit lead, deposition current, depositing time, realize the adjustment of plumbous in the matrix material and Graphene part by weight, and the adjustment of plumbous particle size.Plumbous graphene composite material of the present invention both can have been brought into play the capacity characteristic of plumbous active substance, can bring into play again the power characteristic of grapheme material, be made into plumbous charcoal superbattery negative pole, after tested, the power density of this lead charcoal superbattery obviously improves, carry out the high current charge-discharge circulation under partial state of charge, the cycle life of battery significantly improves.
Description of drawings
Fig. 1 is the preparation flow schematic diagram of plumbous graphene composite material.Wherein: 1. conducting base; 2. oxidized graphite flake; 3. graphene film; 4. plumbous; 5. plumbous graphene composite material.
Fig. 2 is the stereoscan photograph of plumbous graphene composite material.
Fig. 3 is the large current cycle life curve figure of plumbous graphene composite material.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1: with reference to Fig. 1,2,3
(1), with the oxidized graphite flake ultra-sonic dispersion in the magnesium nitrate aqueous isopropanol, the weight ratio of oxidized graphite flake and magnesium nitrate is 100:1, prepares positively charged graphite oxide film sol.
(2), take the graphite oxide film sol of step (1) as ionogen, electrophoretic deposition oxidized graphite flake film on pure stereotype, deposition voltage is made as 100V, behind the deposition 5min, the stereotype that is loaded with oxidized graphite flake is taken out dry 4h under the vacuum environment of 50 ° of C.
(3), with the stereotype that is loaded with oxidized graphite flake reductase 12 h in 60 ° of saturated hydrazine hydrate atmosphere of C of step (2), obtain graphene film, each graphene film comprises 10-20 carbon atomic layer;
(4), plating bath adopts the fluoroboric acid plating bath, plating bath is as the plumbous plating bath of preparation of raw material take 200g/L lead fluoborate, 220g/L fluoroboric acid, 40g/L boric acid, 0.5g/L peptone, take pure stereotype as anode, load take step (3) has the stereotype of graphene film as negative electrode, deposit lead particle on graphene film, current density is made as 1A/dm
2, depositing time is made as 30min;
(5), step (4) Graphene/plumbous laminated film is washed, dry 8h under 60 ° of C vacuum environments scrapes film from the conducting base surface, suitably grinds, and obtains plumbous graphene composite material.
(6), by energy spectrum analysis, adopt in the plumbous graphene composite material of this embodiment preparation, weight percent plumbous and Graphene is respectively 82% and 18%.Fig. 2 is the stereoscan photograph of this lead graphene composite material, and as we know from the figure, plumbous particle is grown directly upon the graphene platelet surface, and the size of plumbous particle is about 300nm, and plumbous contact area with Graphene is large and combination is good.
(7), should the lead graphene composite material add respectively water and acid forms creme, evenly be coated on the stereotype grid, as negative pole, as positive pole, be assembled into a slice negative plate and two 2V simulated batteries that positive plate consists of with the stereotype that is coated with plumbic oxide.After battery is discharged to 50% charging state with 0.1C, under the 2C multiplying power, carry out charge and discharge cycles, charging 90s, pressure limiting 2.35V, discharge 60s is considered as battery failure when final discharging voltage is lower than 1.7V.From the cyclic curve of Fig. 3 as can be known, adopt the battery of plumbous Graphene negative pole after circulation 10,000 times, the sparking voltage of battery still maintains 1.8V stably, and the battery that adopts plumbous negative pole is after circulation more than 5000 times, and the sparking voltage of battery lost efficacy with regard to being down to below the 1.7V.As seen, can significantly improve the HRPSoC cycle life of battery take plumbous graphene composite material as negative pole.
Embodiment 2: with reference to Fig. 1
(1), with the oxidized graphite flake ultra-sonic dispersion in the magnesium nitrate aqueous isopropanol, the weight ratio of oxidized graphite flake and magnesium nitrate is 50:1, prepares positively charged graphite oxide film sol.
(2), take the graphite oxide film sol of step (1) as ionogen, electrophoretic deposition oxidized graphite flake film on pure titanium plate, deposition voltage is made as 120V, behind the deposition 10min, the stereotype that is loaded with oxidized graphite flake is taken out dry 4h under the vacuum environment of 50 ° of C.
(3), the titanium plate that is loaded with oxidized graphite flake of step (2) is placed argon gas atmosphere, calcine 2h under 500 ° of C, obtain graphene film, each graphene film comprises 10-20 carbon atomic layer;
(4), plating bath adopts the fluoroboric acid plating bath, plating bath is as the plumbous plating bath of preparation of raw material take 200g/L lead fluoborate, 220g/L fluoroboric acid, 40g/L boric acid, 0.5g/L peptone, take pure stereotype as anode, load take step (3) has the stereotype of graphene film as negative electrode, deposit lead particle on graphene film, adopt two sections Constant Electric Current deposition process, be respectively 3A/dm
2Deposition 20s, 1A/dm
2Deposition 5min;
(5), step (4) Graphene/plumbous laminated film is washed, dry 8h under 60 ° of C vacuum environments scrapes film from the conducting base surface, suitably grinds, and obtains plumbous graphene composite material.
(6), by energy spectrum analysis, adopt in the plumbous graphene composite material of this embodiment preparation, weight percent plumbous and Graphene is respectively 59% and 41%.
Embodiment 3: with reference to Fig. 1
(1), with the oxidized graphite flake ultra-sonic dispersion in the magnesium nitrate aqueous isopropanol, the weight ratio of graphite oxide and magnesium nitrate is 150:1, prepares positively charged graphite oxide film sol.
(2), take the graphite oxide film sol of step (1) as ionogen, electrophoretic deposition oxidized graphite flake film on pure stereotype, deposition voltage is made as 80V, behind the deposition 10min, the stereotype that is loaded with oxidized graphite flake is taken out dry 4h under the vacuum environment of 50 ° of C.
(3), with the stereotype that is loaded with oxidized graphite flake reductase 12 h in 60 ° of saturated hydrazine hydrate atmosphere of C of step (2), obtain graphene film, each graphene film comprises 10-20 carbon atomic layer;
(4), plating bath adopts the fluoroboric acid plating bath, plating bath is as the plumbous plating bath of preparation of raw material take 15g/L plumbous oxide, 120g/L Seignette salt, 40g/L disodium ethylene diamine tetraacetate, take pure stereotype as anode, load take step (3) has the stereotype of graphene film as negative electrode, deposit lead particle on graphene film, current density is made as 1.2A/dm
2, depositing time is made as 1min;
(5), step (4) Graphene/plumbous laminated film is washed, dry 8h under 60 ° of C vacuum environments scrapes film from the conducting base surface, suitably grinds, and obtains plumbous graphene composite material.
(6), by energy spectrum analysis, adopt in the plumbous graphene composite material of this embodiment preparation, weight percent plumbous and Graphene is respectively 27% and 73%.
(7), should the lead graphene composite material join in the conventional cathode lead plaster with 10% weight percent, the assembling of battery and life test are identical with method among the embodiment 1.The lead carbon battery that negative pole is added with plumbous graphene composite material carries out the HRPSoC circulation, and cycle life reaches 14000-16000 time, is more than the twice in conventional batteries life-span.As seen, take plumbous graphene composite material as cathode additive agent, can significantly improve the HRPSoC cycle life of battery.
Adopt plumbous graphene composite material of the present invention directly to be used as the negative pole of lead acid cell, or as the additive of negative pole, after being assembled into valve control type sealed cell, charge acceptance improves 1-2 doubly, HRPSoC cycle life improves 2-3 doubly, is a kind of desirable lead carbon battery negative material and lead carbon battery cathode additive agent material.
Claims (10)
1. plumbous graphene composite material, it is characterized in that it is that plumbous particle is electrochemically-deposited in the formed matrix material in graphene platelet surface, the weight percentage of Graphene is 10%-90% in the plumbous graphene composite material, each graphene film comprises 1-50 carbon atomic layer, and the particle diameter of plumbous particle is 100nm-10m.
2. the preparation method of plumbous graphene composite material described in the claim 1 is characterized in that it may further comprise the steps:
(1), take pure stereotype as anode, have the conducting base of graphene film to be negative electrode take load, the plumbous particle of Constant Electric Current electroless plating on graphene film;
(2), the graphene film of deposit lead particle is washed, dry under 40-80 ° of C vacuum environment, film is scraped from the conducting base surface, its grinding is broken, obtain described plumbous graphene composite material.
3. method claimed in claim 2 is characterized in that also having following steps described step (1) is front:
(1-1), with the oxidized graphite flake ultra-sonic dispersion in the magnesium nitrate aqueous isopropanol, form positively charged graphite oxide film sol;
(1-2), take the graphite oxide film sol as ionogen, constant voltage electrophoretic deposition oxidized graphite flake film on conducting base obtains graphene film by reduction again.
4. in accordance with the method for claim 3, it is characterized in that: in the graphite oxide film sol of step (1-1), the weight ratio of oxidized graphite flake and magnesium nitrate is 50:1-200:1.
5. in accordance with the method for claim 3, it is characterized in that: the voltage of the constant voltage electrophoretic deposition of step (1-2) is 20-180V, and depositing time is 10s-30min.
6. in accordance with the method for claim 2, it is characterized in that: the approach that the oxidized graphite flake film of step (1-2) is reduced into graphene film is to reduce 1-4h in the 60-90 ° of saturated hydrazine hydrate atmosphere of C, or in argon gas atmosphere, 500 ℃ of lower calcining 1-4h.
7. it is characterized in that in accordance with the method for claim 2: the conducting base of step (1) is inactive, conductive material.
8. it is characterized in that in accordance with the method for claim 2: the conducting base of step (1) can be stereotype, titanium plate, platinum plate.
9. it is characterized in that in accordance with the method for claim 2: the plumbous plating bath of step (1) is one or more the mixing plating bath in fluoroboric acid plating bath, silicofluoric acid plating bath, Seignette salt plating bath and the trolamine plating bath.
10. it is characterized in that in accordance with the method for claim 2: step (1) is 0.1-4A/dm in the current density of graphene film surface electrical deposit lead particle
2, electrodeposition time is 1min-2h.
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Cited By (9)
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| CN103456931B (en) * | 2013-09-30 | 2015-07-01 | 合肥工业大学 | Lead-carbon battery negative electrode material preparation method based on high-intensity graphene oxide gel |
| CN104795572A (en) * | 2015-05-12 | 2015-07-22 | 昆明冶金研究院 | Method for preparing lead-graphene composite material |
| CN105140524A (en) * | 2015-08-28 | 2015-12-09 | 天能电池集团有限公司 | Lead storage battery grid containing lead-graphene composite material |
| CN106180678A (en) * | 2016-08-02 | 2016-12-07 | 东南大学 | A kind of method preparing lead atom chain |
| TWI583043B (en) * | 2014-03-31 | 2017-05-11 | 長興材料工業股份有限公司 | Electrolyte composition |
| CN110828790A (en) * | 2019-10-15 | 2020-02-21 | 桂林理工大学 | Preparation method and application of lead-coated sweet sorghum stalk-based carbon material |
| CN112864391A (en) * | 2021-01-27 | 2021-05-28 | 华侨大学 | Preparation method and application of lead/reduced graphene oxide nanocomposite |
| CN114905039A (en) * | 2021-02-07 | 2022-08-16 | 深圳市先进石墨烯科技有限公司 | Graphene/metal composite material and preparation method and application thereof |
| CN116031424A (en) * | 2023-03-24 | 2023-04-28 | 南方科技大学 | Flow battery composite electrode, preparation method thereof and flow battery |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103456931B (en) * | 2013-09-30 | 2015-07-01 | 合肥工业大学 | Lead-carbon battery negative electrode material preparation method based on high-intensity graphene oxide gel |
| TWI583043B (en) * | 2014-03-31 | 2017-05-11 | 長興材料工業股份有限公司 | Electrolyte composition |
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| CN105140524A (en) * | 2015-08-28 | 2015-12-09 | 天能电池集团有限公司 | Lead storage battery grid containing lead-graphene composite material |
| CN105140524B (en) * | 2015-08-28 | 2017-05-03 | 天能电池集团有限公司 | Lead storage battery grid containing lead-graphene composite material |
| CN106180678A (en) * | 2016-08-02 | 2016-12-07 | 东南大学 | A kind of method preparing lead atom chain |
| CN110828790A (en) * | 2019-10-15 | 2020-02-21 | 桂林理工大学 | Preparation method and application of lead-coated sweet sorghum stalk-based carbon material |
| CN112864391A (en) * | 2021-01-27 | 2021-05-28 | 华侨大学 | Preparation method and application of lead/reduced graphene oxide nanocomposite |
| CN112864391B (en) * | 2021-01-27 | 2022-05-03 | 华侨大学 | Preparation method and application of lead/reduced graphene oxide nanocomposite |
| CN114905039A (en) * | 2021-02-07 | 2022-08-16 | 深圳市先进石墨烯科技有限公司 | Graphene/metal composite material and preparation method and application thereof |
| CN114905039B (en) * | 2021-02-07 | 2024-01-19 | 深圳贝特瑞钠电新材料科技有限公司 | Graphene/metal composite material and preparation method and application thereof |
| CN116031424A (en) * | 2023-03-24 | 2023-04-28 | 南方科技大学 | Flow battery composite electrode, preparation method thereof and flow battery |
| CN116031424B (en) * | 2023-03-24 | 2023-06-23 | 南方科技大学 | Flow battery composite electrode, preparation method thereof and flow battery |
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Address after: 311305, No. 72, landscape Avenue, Qingshan Town, Ling'an Economic Development Zone, Zhejiang, Hangzhou Applicant after: Nandu Electric Power Co., Ltd., Zhejiang Applicant after: Hangzhou Narada Battery Co., Ltd Applicant after: Hangzhou Nandu Energy Technology Co., Ltd. Address before: 310013 No. 50 Bauhinia Road, Zhejiang, Hangzhou Applicant before: Nandu Electric Power Co., Ltd., Zhejiang Applicant before: Hangzhou Narada Battery Co., Ltd Applicant before: Hangzhou Nandu Energy Technology Co., Ltd. |
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| CB02 | Change of applicant information |
Address after: 311305 Ling'an Qingshan Lake Street landscape Avenue, No. 72, No. Applicant after: Nandu Electric Power Co., Ltd., Zhejiang Applicant after: Hangzhou Narada Battery Co., Ltd Applicant after: Hangzhou Nandu Energy Technology Co., Ltd. Address before: 311305, No. 72, landscape Avenue, Qingshan Town, Ling'an Economic Development Zone, Zhejiang, Hangzhou Applicant before: Nandu Electric Power Co., Ltd., Zhejiang Applicant before: Hangzhou Narada Battery Co., Ltd Applicant before: Hangzhou Nandu Energy Technology Co., Ltd. |
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| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130206 |