CN111640906B - Positive electrode of high-specific-energy quick-activation seawater battery and preparation method - Google Patents
Positive electrode of high-specific-energy quick-activation seawater battery and preparation method Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a positive electrode of a high-specific energy quick-activated seawater battery and a preparation method thereof, belonging to the field of battery technology engineering application, wherein the positive electrode consists of lead chloride, a binder and a conductive agent, and the preparation method comprises the following steps: 1) ball milling; 2) and flour; 3) tabletting; 4) surfing the Internet; 5) and (5) drying. And (4) finely pressing the positive plate to a proper process size according to batteries of different models. The invention has the beneficial effects that: the preparation method is simple and easy to operate, effectively improves the discharge capacity of the seawater battery, greatly shortens the activation time of the seawater battery, and can be quickly activated when the seawater battery works at high and low temperatures.
Description
Technical Field
The invention relates to the field of battery technology engineering application, in particular to a preparation method of a high-specific-energy quick-activation seawater battery.
Background
The seawater battery is developed by Beel laboratory design of America and general electric company during the second world war, and has the most prominent characteristic that the seawater battery does not need to carry electrolyte and can use natural seawater to form electrolyte when needed. The seawater cell has many different types for different purposes, such as a power cell for high-power underwater equipment, a long-period and low-power battery for underwater detection instruments, a power cell for underwater navigation bodies, a semi-fuel seawater cell and the like. With the requirement of vigorously developing deep and far seas in China, it is one of the future development directions to develop a magnesium seawater battery technology which can be loaded and is durable in marine environment to meet the requirements of unmanned underwater traffic and detection tools, such as UUV (unmanned underwater vehicle), DSRV (deep sea rescue vehicle), marine underwater instrument power supply and the like, and the magnesium seawater battery technology can be particularly used for an autonomous small-sized detection navigation body to collect marine sea conditions and surrounding dynamic information such as seawater flow velocity, seabed topography and sea area information and monitor the changeable marine nature and surrounding environment in China, thereby realizing investigation and information collection work. Various life-saving equipment, sonobuoys and the like in China gradually turn from imports to independent research and development, and matched seawater batteries also gradually need to be researched and developed independently. The magnesium seawater battery which is environment-friendly, low in price and excellent in performance can provide better energy for equipment such as a sonobuoy, aviation lifesaving, submarine communication, an autonomous underwater vehicle and the like, has a wide application prospect in the aspect of military and civil integration, and has important significance for maintaining sea defense construction and promoting marine industry development.
Magnesium-lead chloride is one of the most widely applied systems of seawater batteries, and the current magnesium-lead chloride seawater batteries have relatively low specific energy, discharge rate and activation performance and are difficult to meet market requirements. The new achievements of the material technology development are fully utilized, the anode formula is modified, and the manufacturing process is improved, so that the effects of improving the specific energy of the magnesium-lead chloride seawater battery, improving the activation voltage and shortening the activation time are achieved.
Disclosure of Invention
Based on the defects of the prior art, the technical problem to be solved by the invention is to provide the preparation method of the high-specific-energy quick-activation seawater battery, the positive electrode formula of the preparation method is successfully applied with a new material, the specific energy, the activation characteristic and the temperature adaptability of the battery are greatly improved, and a new idea of improving and researching the battery performance is expanded. The invention improves the preparation process of the positive pole piece, improves the manufacturing efficiency of the positive pole, and has simple preparation method and easy operation.
In order to solve the technical problems, the invention provides a preparation method of a high-specific-energy quick-activation seawater battery anode, which comprises the following steps:
1) carrying out ball milling and refining on the lead chloride powder to obtain lead chloride fine powder; lead chloride powder is ground by ball milling, active sites of chemical reaction are fully exposed, and the specific surface area participating in the reaction is increased;
2) adding a conductive agent into the refined lead chloride fine powder obtained in the step 1), continuously ball-milling, and uniformly mixing; lead chloride and conductive agent are fully ball-milled to form a conductive coating network structure, so that the transmission capability of the battery is improved;
3) adding the binder into the uniform powder obtained in the step 2), and fully stirring;
4) putting the anode powder uniformly mixed in the step 3) into a mould, and pressing into an anode powder cake;
5) wrapping the anode powder cake prepared in the step 4) with a cut current collecting net, putting the anode powder cake into a net clamping mold, and pressing the anode powder cake into an anode plate; the positive plate is finely pressed to a proper process size according to batteries of different models;
6) drying the positive plate prepared in the step 5) at the temperature of 50-180 ℃ to obtain the positive electrode of the high-specific-energy quick-activation seawater battery.
The above-mentioned moulds are all customized.
As a preferred aspect of the above technical solution, the method for preparing a high specific energy rapid activation seawater battery positive electrode provided by the present invention further comprises a part or all of the following technical features:
as an improvement of the technical scheme, the mass percent of the lead chloride is 80-90%, the mass percent of the polytetrafluoroethylene is 2.5-10%, and the mass percent of the conductive agent is 1-12%.
As an improvement of the technical scheme, the conductive agent is one or a mixture of several of metal conductive powder, carbon black, graphite, graphene and carbon nanotubes.
As an improvement of the technical scheme, the binder is one of high molecular polyethylene, polytetrafluoroethylene, polyvinylidene fluoride, CMC (sodium carboxymethylcellulose) and microcrystalline cellulose.
As an improvement of the technical scheme, the current collecting net is one of a copper net, a silver-plated copper net and a stainless steel net.
As an improvement of the above technical scheme, in the step 1), the mass ratio of the lead chloride powder to the ball milling beads is 1: 0.5-1: 3; in the step 6), the drying temperature is 50-180 ℃.
The battery anode consists of 80-90% by mass of lead chloride, 2.5-10% by mass of polytetrafluoroethylene and 1-12% by mass of a conductive agent.
As a preferred aspect of the above technical solution, the positive electrode of the high specific energy rapid activation seawater battery provided by the present invention further comprises part or all of the following technical features:
as an improvement of the technical scheme, the conductive agent is one or a mixture of several of metal conductive powder, carbon black, graphite, graphene and carbon nanotubes.
As an improvement of the technical scheme, the binder is one of high molecular polyethylene, polytetrafluoroethylene, polyvinylidene fluoride, CMC (sodium carboxymethylcellulose) and microcrystalline cellulose.
As an improvement of the technical scheme, the positive electrode of the battery is prepared by any one of the methods.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: the seawater battery prepared by the positive pole piece has the advantages of greatly improved specific energy, quick activation time, high activation voltage and good temperature adaptability, expands a new idea of battery performance improvement research, and has the effects of improving the specific energy of the magnesium-lead chloride seawater battery, improving the activation voltage and shortening the activation time.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the contents of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.
FIG. 1(a) is a 600mA normal temperature constant current discharge curve of a seawater battery pack according to an embodiment of the present invention;
FIG. 1(b) is a 600mA low temperature low salt discharge curve for a seawater battery pack in accordance with an embodiment of the present invention;
fig. 1(c) is a 600mA high temperature high salt discharge curve of a seawater battery pack according to an embodiment of the present invention.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention.
The anode formula material provided by the invention contains 80-90% of lead chloride, 2.5-10% of binder and 1-12% of conductive agent.
The preparation of the positive pole piece adopts the following five steps: 1) ball milling; 2) and flour; 3) tabletting; 4) surfing the Internet; 5) and drying, the specific energy of the seawater battery prepared by the positive plate is improved, the activation speed is high, and the temperature adaptability is strong.
Examples of the invention and comparative examples are presented below:
the first embodiment is as follows: putting lead chloride into a ball milling tank, and controlling the ball-material ratio to be 0.6: 1-2: ball milling for 2h and sieving between 1. 30.67g of ground lead chloride was taken and mixed in a 1: 4, adding the carbon nano tube and the silver-plated copper powder, uniformly ball-milling, adding the adhesive polytetrafluoroethylene, and uniformly stirring. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with good specific energy and activation performance described in the patent. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The battery is discharged at normal temperature, the activation time is less than 5s (the minimum acquisition precision of the equipment is 5s, the actual battery is activated instantly), the activation voltage reaches 1.25V, and the 500mA discharge capacity is 4.7 Ah.
Example two: putting lead chloride into a ball milling tank, and controlling the ball-material ratio to be 0.6: 1-2: ball milling for 2h and sieving between 1. 30.67g of ground lead chloride was taken and mixed in a 1: 3, adding the carbon nano tube and the silver-plated copper powder, uniformly ball-milling, adding the adhesive polytetrafluoroethylene, and uniformly stirring. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with good specific energy and activation performance described in the patent. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The battery is discharged at normal temperature, the activation time is less than 5s, the activation voltage reaches 1.37V, and the 500mA discharge capacity is 5.0 Ah.
Example three: putting lead chloride into a ball milling tank, and controlling the ball-material ratio to be 0.6: 1-2: ball milling for 2h and sieving between 1. 33.47g of ground lead chloride is taken, 0.9g of carbon nano tube is added, the ball milling is uniform, and then the adhesive polytetrafluoroethylene is added and the stirring is uniform. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with good specific energy and activation performance described in the patent. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The battery is discharged at normal temperature, the activation time is less than 5s, the activation voltage reaches 1.37V, and the 500mA discharge capacity is 5.8 Ah.
Example four: putting lead chloride into a ball milling tank, and controlling the ball-material ratio to be 0.6: 1-2: ball milling for 2h and sieving between 1. 33.47g of ground lead chloride is taken, 0.9g of carbon nano tube is added, the ball milling is uniform, and then the adhesive polytetrafluoroethylene is added and the stirring is uniform. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with good specific energy and activation performance described in the patent. The pole piece and the magnesium plate are respectively used as the anode and the cathode of the seawater battery to form the seawater battery with a 13-string structure, and the anode and cathode leads are welded to test the normal-temperature, low-temperature and high-temperature performance of the battery pack. The test results are shown in attached Table 1 and attached FIG. 1.
Comparative example one: the lead chloride is smashed by a conventional method (aiming at the agglomeration part), 30.67g of lead chloride is taken, 3.7g of silver-plated copper powder is added, the mixture is uniformly mixed, then the adhesive polytetrafluoroethylene is added, and the mixture is uniformly stirred. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) placing the positive plate at 70 ℃ and baking for 21h to obtain the positive plate. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The formula battery discharges at normal temperature, the activation time is 5 s-10 s, the activation voltage is 1.05V, and the 500mA discharge capacity is 2.6 Ah.
Comparative example two: the lead chloride is smashed by a conventional method (aiming at the agglomeration part), 33.47g of lead chloride is taken, 0.9g of carbon nano tube is added, the mixture is uniformly mixed, then the adhesive polytetrafluoroethylene is added, and the mixture is uniformly stirred. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with a good state. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The battery is discharged at normal temperature, the activation time is less than 5s, the activation voltage reaches 1.10V, and the 500mA discharge capacity is 3.2 Ah.
Comparative example three: putting lead chloride into a ball milling tank, and controlling the ball-material ratio to be 0.6: 1-2: ball milling for 2h and sieving between 1. 33.47g of lead chloride is taken, 0.9g of carbon nano tube is added, the mixture is uniformly mixed, then the adhesive polytetrafluoroethylene is added, and the mixture is uniformly stirred. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with a good state. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The battery is discharged at normal temperature, the activation time is less than 5s, the activation voltage reaches 1.10V, and the 500mA discharge capacity is 3.7 Ah.
Comparative example four: the lead chloride is smashed by a conventional method (aiming at the agglomeration part), 33.47g of lead chloride is taken, 0.9g of carbon nano tube is added, the ball milling is uniform, then the adhesive polytetrafluoroethylene is added, and the stirring is uniform. And (3) filling the mixed anode powder into a mold, adjusting the parameters of a press, pressing and molding the anode powder cake, wrapping the anode powder cake with a copper mesh, putting the anode powder cake into a customized mold, adjusting the parameters of the press, and pressing and molding the anode sheet. And (3) drying the positive plate for 21h at 70 ℃ to obtain the positive plate with a good state. The pole piece and the magnesium plate form a seawater battery, and positive and negative leads are welded for battery testing. The battery is discharged at normal temperature, the activation time is less than 5s, the activation voltage reaches 1.10V, and the 500mA discharge capacity is 3.8 Ah.
Comparative example five: the industrial indexes of the seawater battery of the model are that the normal temperature activation time is less than 30s, the low temperature activation time is less than 180s, the monomer activation voltage is more than 0.77V, and the 500mA discharge capacity is 4.00 Ah.
The positive plate prepared by the high-specific-energy quick-activation seawater battery positive electrode formula is used for manufacturing the battery, the normal-temperature activation performance of the obtained seawater battery is doubled, the low-temperature activation performance is far superior to the industrial level, the high-low-temperature adaptability is high, the activation voltage is high, and the discharge capacity is obviously improved. The preparation process method of the high-specific-energy quick-activation seawater battery anode is simple and easy to operate, has high efficiency, and can be popularized to batteries of other types and even batteries of other systems of the same system.
TABLE 1 seawater Battery pack 600mA discharge
The raw materials listed in the invention, the upper and lower limits and interval values of the raw materials of the invention, and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can all realize the invention, and the examples are not listed.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (4)
1. A preparation method of a high-specific-energy quick-activation seawater battery anode is characterized by comprising the following steps:
1) carrying out ball milling and refining on the lead chloride powder to obtain lead chloride fine powder;
2) adding a conductive agent into the refined lead chloride fine powder obtained in the step 1), continuously ball-milling, uniformly mixing, fully ball-milling the lead chloride and the conductive agent to form a conductive coating network structure, wherein the mass ratio of the lead chloride powder to the ball milling beads is 1: 0.5-1: 3, ball milling time is 2 hours;
3) adding the binder into the uniform powder obtained in the step 2), and fully stirring;
4) putting the anode powder uniformly mixed in the step 3) into a mould, and pressing into an anode powder cake;
5) wrapping the anode powder cake prepared in the step 4) with a cut current collecting net, putting the anode powder cake into a net clamping mold, and pressing the anode powder cake into an anode plate;
6) drying the positive plate prepared in the step 5) at the temperature of 50-180 ℃ to obtain the positive electrode of the high-specific-energy quick-activation seawater battery, wherein the activation time is less than 5 s;
the mass percent of the lead chloride is 80-90%, the mass percent of the binder is 2.5-10%, and the mass percent of the conductive agent is 1-12%;
the conductive agent is one or a mixture of more of metal conductive powder, carbon black, graphite, graphene and carbon nanotubes;
the binder is one of high-molecular polyethylene, polytetrafluoroethylene, polyvinylidene fluoride, sodium carboxymethylcellulose and microcrystalline cellulose;
the current collecting net is one of a copper net, a silver-plated copper net and a stainless steel net.
2. The positive electrode of the high-specific energy quick-activation seawater battery is characterized in that: the preparation method of the battery positive electrode comprises the following steps of preparing the battery positive electrode by the preparation method of claim 1, wherein the battery positive electrode comprises 80-90% by mass of lead chloride, 2.5-10% by mass of a binder and 1-12% by mass of a conductive agent.
3. The high specific energy rapid activation anode of a seawater battery as claimed in claim 2, wherein: the conductive agent is one or a mixture of several of metal conductive powder, carbon black, graphite, graphene and carbon nanotubes.
4. The high specific energy rapid activation anode of a seawater battery as claimed in claim 2, wherein: the binder is one of high molecular polyethylene, polytetrafluoroethylene, polyvinylidene fluoride, sodium carboxymethylcellulose and microcrystalline cellulose.
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Citations (2)
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|---|---|---|---|---|
| US4021597A (en) * | 1976-01-28 | 1977-05-03 | Globe-Union Inc. | Sea water battery with a lead chloride cathode and method of making the same |
| CN108232194A (en) * | 2018-01-19 | 2018-06-29 | 中南大学 | A kind of seawater battery positive electrode and preparation method thereof and seawater battery |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1391300A (en) * | 2002-07-12 | 2003-01-15 | 华南理工大学 | Seawater battery |
| TWI617075B (en) * | 2016-04-18 | 2018-03-01 | 國立清華大學 | Sea water battery circulation system, sea water battery, cathode of sea water battery and fabrication method thereof |
| CN109244359B (en) * | 2018-11-06 | 2021-02-05 | 南京径祥新材料科技有限公司 | Forming process of cuprous chloride positive electrode piece of high-capacity magnesium seawater battery and obtained battery |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4021597A (en) * | 1976-01-28 | 1977-05-03 | Globe-Union Inc. | Sea water battery with a lead chloride cathode and method of making the same |
| CN108232194A (en) * | 2018-01-19 | 2018-06-29 | 中南大学 | A kind of seawater battery positive electrode and preparation method thereof and seawater battery |
Non-Patent Citations (3)
| Title |
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| "海水电池用粘结剂法制二氯化铅正极的研究";孙黎光等，;《船工科技》;19861231(第44期);第11-14页 * |
| "纳米氯化银的合成及其作为海水电池正极材料的性能研究";王益成，;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20190731(第07期);第37-41页 * |
| 孙黎光等，."海水电池用粘结剂法制二氯化铅正极的研究".《船工科技》.1986,(第44期),第11-14页. * |
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