CN113206258A - Primary lithium battery and preparation method thereof - Google Patents
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- CN113206258A CN113206258A CN202110441903.3A CN202110441903A CN113206258A CN 113206258 A CN113206258 A CN 113206258A CN 202110441903 A CN202110441903 A CN 202110441903A CN 113206258 A CN113206258 A CN 113206258A
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/80—Porous plates, e.g. sintered carriers
- H01M4/806—Nonwoven fibrous fabric containing only fibres
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- H01M4/06—Electrodes for primary cells
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/06—Electrodes for primary cells
- H01M4/08—Processes of manufacture
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M6/00—Primary cells; Manufacture thereof
- H01M6/14—Cells with non-aqueous electrolyte
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
A primary lithium battery and a method for preparing the same are disclosed. The negative electrode of the primary lithium battery is composed of a stretch-resistant ultrathin lithium foil, and the stretch-resistant ultrathin lithium foil comprises: the conductive porous tensile-resistant layer is formed by bonding inorganic fiber materials; a discontinuous lithium metal material disposed in the pores of the porous tensile layer, wherein the discontinuous lithium metal material is dispersed as a discrete lithium metal material in the pores of the porous tensile layer; and an optional surface protective layer on the porous stretch resistant layer. The primary lithium battery overcomes the problems that the tensile strength of the traditional lithium belt cathode is low, the specific energy is reduced by using a thick lithium belt, and the lithium resource is wasted.
Description
Technical Field
The invention relates to the technical field of energy storage, in particular to a primary lithium battery and a preparation method thereof.
Background
The primary lithium battery has the advantages of high specific energy, high voltage, small self-discharge and wide working temperature range, and is widely applied to the fields of cameras, intelligent instruments, water meters, electricity meters, gas meters, oil exploration, medical instruments, anti-theft alarm and the like. The lithium metal has small atomic mass and most negative electrochemical potential, and has high specific energy with positive electrode materials such as thionyl chloride and manganese dioxide and batteries consisting of non-aqueous electrolytes. At present, most of the negative electrodes of primary lithium batteries are thick metal lithium tapes, the thickness of the lithium tapes is more than or equal to 1mm, but the thickness of the actually used metal lithium is not so thick, and partial metal lithium remains and does not participate in the reaction, so that the waste of metal lithium resources is caused. The metal lithium strip is soft and has low tensile strength (about 1.156MPa), and when the metal lithium strip with the thickness less than or equal to 0.1mm is used as the negative electrode of the primary battery, metal foils such as copper foil, stainless steel foil and the like are required to be used as supporting base materials of the metal lithium strip, so that the metal lithium strip can be wound and unwound better for use. However, metal foils are generally heavy, which reduces the specific energy of the battery.
Disclosure of Invention
The invention mainly aims to provide a primary lithium battery and a preparation method thereof, which can solve the problem of low tensile strength of a pure lithium belt used in the primary lithium battery.
The invention adopts the following technical scheme:
in some embodiments, a lithium primary battery is provided having a negative electrode comprised of a stretch-resistant ultra-thin lithium foil, the stretch-resistant ultra-thin lithium foil comprising: an electrically conductive porous tensile layer formed by bonding inorganic fiber materials, the porous tensile layer having a pore size of 1 nm to 200 μm and a porosity of 10% to 85%; a discontinuous lithium metal material disposed in the pores of the porous tensile layer, wherein the discontinuous lithium metal material is dispersed as discrete lithium metal within the pores of the porous tensile layer; and optionally a surface protective layer on the porous stretch resistant layer.
In some embodiments, there is provided a method of making a primary lithium battery as described above, the method comprising: punching the coiled stretch-resistant ultrathin lithium foil into a sheet (a circular sheet or a rectangular sheet) with a certain size through a die cutting machine to be used as a negative plate; and the negative plate, the electrolyte, the diaphragm and the positive electrode form a primary lithium battery, or the negative plate, the solid electrolyte and the positive electrode form the primary lithium battery.
The present invention may have at least one of the following advantageous effects:
(1) the negative electrode body of the primary lithium battery has small density and light weight, and the high energy density of the battery is realized.
(2) The tensile layer formed by bonding the conductive inorganic fiber material not only plays a role in supporting the lithium metal layer and improving the tensile strength of the lithium metal layer, but also has conductivity and can play a role in collecting a current.
(3) Thin metal lithium can be used, and metal lithium resources are saved. .
(4) The stretch-resistant ultrathin lithium foil can be coiled and uncoiled for use, and is favorable for industrial continuous production.
Drawings
Fig. 1 is a physical diagram of a stretch-resistant ultra-thin lithium foil product obtained according to example 1 of the present invention.
Detailed Description
In one aspect of the present invention, there is provided a primary lithium battery having a negative electrode formed of a stretch-resistant ultra-thin lithium foil, the stretch-resistant ultra-thin lithium foil comprising:
an electrically conductive porous tensile layer formed from an inorganic fibrous material, wherein the porous tensile layer has a pore size of from 1 nanometer to 200 microns and a porosity of from 10% to 85%;
a discontinuous lithium metal material disposed in the pores of the porous tensile layer, wherein the discontinuous lithium metal material is dispersed as discrete lithium metal within the pores of the porous tensile layer; and
optionally a surface protective layer on the porous stretch resistant layer.
The lithium metal material comprises pure lithium metal or lithium alloy, the lithium alloy is an alloy of lithium metal and one or more of Ag, Al, Au, Ba, Be, Bi, C, Ca, Cd, Co, Cr, Cs, Fe, Ga, Ge, Hf, Hg, In, Ir, K, Mg, Mn, Mo, N, Na, Nb, Ni, Pt, Pu, Rb, Rh, S, Se, Si, Sn, Sr, Ta, Te, Ti, TIY, V, Zn, Zr, Pb, Pd, Sb and Cu, and the content of the lithium metal is 1-99.9%.
Preferably, the porous stretch resistant layer has a pore size of from 5nm to 100 microns, more preferably from 10 nm to 50 microns.
Preferably, the porosity of the porous tensile layer is from 15% to 80%, more preferably from 25% to 70%.
In some embodiments, the porous stretch resistant layer is formed by bonding inorganic fiber materials with a binder.
In some embodiments, the inorganic fiber material includes at least one selected from the group consisting of carbon nanotubes, carbon fibers, metal fibers, semiconductor fibers, and inorganic oxide fibers. For example, the metal fibers may comprise Ni, Pt, Au, Al or stainless steel fibers, the semiconductor fibers may comprise InP, Si or GaN fibers, and the inorganic oxide fibers may comprise SiO2Or TiO2A fiber.
In some embodiments, the inorganic fiber material is an inorganic fiber material modified by vapor deposition, magnetron sputtering, electroplating, atomic doping, atomic etching, or a combination thereof. For example, the surface treatment may include surface graphitization, amination, acid etching, coating polyethylene oxide, or deposition of nano-alumina, and the atomic doping may include nano-silver particle doping, graphene doping, or conductive graphite doping.
In some embodiments, the inorganic fiber material has a diameter of 1 nanometer to 30 micrometers, preferably 5 nanometers to 10 micrometers.
In some embodiments, the inorganic fiber material has a length of 10 nanometers or more, preferably 50nm or more.
In some embodiments, the average thickness of the stretch resistant ultra-thin lithium foil is from 0.1 microns to 200 microns, preferably from 1 micron to 50 microns, more preferably from 5 microns to 20 microns.
In some embodiments, the surface roughness of the stretch resistant ultra-thin lithium foil is 5 microns or less.
In some embodiments, the tensile modulus of the ultra-thin lithium foil is in the range of 1MPa to 300MPa, preferably in the range of 10MPa to 300MPa, and more preferably in the range of 100MPa to 300 MPa.
In some embodiments, the surface protection layer has a thickness of 5nm to 100 microns, more preferably 10 nm to 50 microns.
In some embodiments, the material of the surface protective layer includes at least one selected from an organic polymer and an inorganic compound. For example, the organic polymer may include polyethylene oxide, oleic acid, or PVDF, and the inorganic compound may include lithium phosphate, lithium carbide, lithium fluoride, an oxide solid electrolyte, or glass ceramic.
The stretch-resistant ultra-thin lithium foil as described above may be prepared by a method comprising the steps of:
step 1: mixing an inorganic fiber material, a binder, a pore former and an optional inorganic filler to prepare a slurry, and coating and high-temperature carbonizing the slurry to form a porous tensile layer, wherein the porous tensile layer has a pore size of 1 nanometer to 200 micrometers and a porosity of 10% to 85%;
step 2: attaching lithium metal to the pores of the porous tensile layer to form discontinuous lithium metal, the discontinuous lithium metal being dispersed as discrete lithium metal within the pores of the porous tensile layer; and
and step 3: optionally, a surface protective layer is applied over the porous stretch resistant layer.
In some embodiments, the pore former comprises at least one of ammonium bicarbonate, naphthalene, polystyrene, and ammonium carbonate.
In some embodiments, the pore former has a size of 10 nanometers to 10 micrometers, more preferably 20 nanometers to 5 micrometers.
In some embodiments, the binder comprises at least one of polymethylmethacrylate, polytetrafluoroethylene, styrene-butadiene rubber, polyvinylidene fluoride, polyepoxy, polystyrene, carboxymethylcellulose, polyvinylpyrrolidone, polyvinyl alcohol, sucrose, polyphenylene sulfide, and polyphenylene oxide resin.
In some embodiments, the inorganic filler comprises at least one of conductive graphite, carbon black, ketjen black, graphene, metal nanoparticles, and metal oxides.
In some embodiments, the temperature of the high temperature carbonization treatment is 300-3000 ℃, preferably 400-2000 ℃.
In some embodiments, the method further comprises the step of modifying the inorganic fiber material by vapor deposition, magnetron sputtering, electroplating, atomic doping, atomic etching, or combinations thereof prior to step 1.
In some embodiments, attaching metallic lithium to the porosity of the porous tensile layer includes attaching metallic lithium to the porosity of the porous tensile layer by melt impregnation or melt infiltration.
In some embodiments, the positive active material of the primary lithium battery includes manganese dioxide, oxysulfinylchloride, iron disulfide, carbon fluoride, sulfur dioxide, sulfuryl chloride, and the like.
The matching electrolytes can be selected as follows: thionyl chloride (electrolyte: LiAlCl)4、SOCl2) (ii) a Sulfuryl chloride (electrolyte: LiAlCl)4、SO2Cl2) (ii) a Sulfur dioxide (electrolyte: lithium bromide, acetonitrile);
for other positive electrode materials (manganese dioxide, carbon fluoride, iron disulfide), the electrolyte can be selected to be a combination of lithium salt and solvent; wherein the lithium salt comprises: LiPF6(lithium hexafluorophosphate), LiClO4(lithium perchlorate), LiAlCl4(lithium homoaluminate), LiBr (lithium bromide), LiI (lithium iodide), LiTFSI (lithium bis (trifluoromethylsulfonyl) imide or lithium bis (trifluoromethylsulfonate) imide); the solvent may include: acetonitrile, methyl formate, propylene carbonate, gamma-butyrolactone, dimethyl sulfoxide, dimethyl sulfite, 1, 2-dimethylethane and tetrahydrofuran.
For primary lithium batteries, the electrolyte may also be selected from solid state electrolytes, such as: LiPON, oxide solid electrolytes (lithium phosphorus oxynitride), sulfide solid electrolytes (lithium sulfur phosphorus compounds), (anti-) perovskites, garnet structures (lithium lanthanum zirconium oxide) and/or polymer solid electrolytes (polyethylene oxide, polyvinylidene fluoride, polyacrylates, polyvinyl carbonates, polymethacrylic acid, polyacrylonitrile).
In some embodiments, the separator may be polypropylene/polyethylene (PP/PE), a ceramic-or polymer-coated separator may be used, separator thickness: 10-40 microns.
The battery shape is selected from one of the following: button cell, cylindrical battery, laminate polymer battery.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The preparation method comprises the steps of adopting a carbon nano tube (model GT-300, Shandong Dachang, diameter: 12-15nm) as an inorganic fiber material, mixing the carbon nano tube, polymethyl methacrylate and ammonium bicarbonate powder as a pore forming agent to obtain carbon nano tube slurry, coating the slurry to prepare a stretch-proof layer film, and placing the film in a tubular furnace protected by nitrogen atmosphere to carry out high-temperature carbonization treatment for 8 hours to obtain the porous stretch-proof layer.
And (3) soaking the porous stretch-proofing layer in molten metal lithium liquid, taking out the porous stretch-proofing layer, rolling and leveling the porous stretch-proofing layer, and thus obtaining a stretch-proofing ultrathin lithium foil product with the thickness of 80 micrometers.
Fig. 1 shows a photograph of a stretch resistant ultra thin lithium foil product according to this example, where the bright spots indicate discontinuous lithium metal and the dark areas indicate the framework material of the porous stretch resistant layer. As can be seen in fig. 1, the discrete lithium metal is dispersed in the pores of the porous tensile layer in the form of discrete lithium metal.
Example 2:
the anti-stretching ultrathin lithium foil in example 1 was used as the negative electrode of a primary lithium battery; the positive active material is manganese dioxide material, and the mass ratio of manganese dioxide (national drug group chemical reagent limited) is as follows: acetylene black (alfa aesar): polytetrafluoroethylene (Shenzhen, Chinzhi Zhida science and technology Limited) was weighed at 90:5:5 and added to N-methylpyrrolidone (Shanghai Arlatin Biotechnology technology Limited) at a solid to liquid ratio of 200mg:1mL, and the slurry was mixed overnight (more than 12 hours). Coating the slurry on the surface of an aluminum foil through a coating machine, carrying out blade coating on two sides to obtain a coating thickness of 300 micrometers, and carrying out vacuum drying at 120 ℃ for 24 hours. And punching the coiled positive electrode and negative electrode into wafers serving as positive electrode and negative electrode pole pieces by mechanical equipment (with the help of unreeling equipment) in a drying workshop (at the dew point of-45 ℃). The cell adopts a CR2450 button cell, and the electrolyte is 1MLiClO4，PC(LiClO4Lithium perchlorate, PC propylene carbonate, Suzhou Qianshen chemical reagent, Inc.), the diaphragm is a PP/PE/PP three-layer composite membrane, the charging and discharging voltage interval is 3.5-2V, and the constant current charging and discharging current is 0.5 mA.
Comparative example 1:
a metal lithium tape with a thickness of 1500 μm was used as the negative electrode of the primary lithium battery, and the positive electrode material, separator, electrolyte and battery assembly were identical to those of example 2. When the metal lithium belt with the thickness of 1500 microns is used as the negative electrode, the 1500 micron thick lithium belt does not generate tensile deformation and is not pulled to break when the negative electrode sheet is punched by the aid of unreeling equipment.
Comparative example 2:
a lithium metal strip with a thickness of 80 microns was used as the negative electrode of the primary lithium cell, and the positive electrode material, separator, electrolyte and cell assembly were identical to those of example 2. When the metal lithium belt with the thickness of 80 microns is used as the negative electrode, when the negative electrode piece is punched by the unreeling device, the belt is easily broken when the 80 micron lithium belt is unreeled, and the lithium belt can not be used in batches.
Table 1 comparison of three negative electrodes
| Experimental number | Negative electrode | Tensile strength/MPa | Specific energy/(wh/kg) |
| Example 2 | Stretch-proof ultrathin lithium foil | 130 | 386 |
| Comparative example 1 | 1500 micron lithium belt | 22 | 374 |
| Comparative example 2 | 80 micron lithium belt | 2.9 (easy to break when unreeling) | 388 |
Claims (10)
1. A primary lithium battery, comprising: the negative pole of primary lithium cell comprises stretch-proofing ultra-thin lithium foil, stretch-proofing ultra-thin lithium foil includes:
an electrically conductive porous tensile layer formed by bonding inorganic fiber materials, the porous tensile layer having a pore size of 1 nm to 200 μm and a porosity of 10% to 85%;
a discontinuous lithium metal material disposed in the pores of the porous tensile layer, wherein the discontinuous lithium metal material is dispersed as discrete lithium metal within the pores of the porous tensile layer; and
optionally a surface protective layer on the porous stretch resistant layer.
2. A primary lithium battery as claimed in claim 1, characterized in that:
the inorganic fiber material comprises at least one selected from carbon nanotubes, carbon fibers, metal fibers, semiconductor fibers, inorganic oxide fibers, wherein the inorganic fiber material is optionally modified by vapor deposition, magnetron sputtering, electroplating, atomic doping, atomic etching, or combinations thereof.
3. A primary lithium battery as claimed in claim 1, characterized in that: the average thickness of the tensile ultrathin lithium foil is 0.1-200 microns; the tensile strength of the tensile ultrathin lithium foil is in the range of 1MPa to 300 MPa.
4. A primary lithium battery as claimed in claim 1, characterized in that: the metal lithium material comprises pure metal lithium or a lithium alloy, the lithium alloy is an alloy of metal lithium and one or more of Ag, Al, Au, Ba, Be, Bi, C, Ca, Cd, Co, Cr, Cs, Fe, Ga, Ge, Hf, Hg, In, Ir, K, Mg, Mn, Mo, N, Na, Nb, Ni, Pt, Pu, Rb, Rh, S, Se, Si, Sn, Sr, Ta, Te, Ti, Y, V, Zn, Zr, Pb, Pd, Sb and Cu, and the content of the metal lithium is 1-99.9%.
5. A primary lithium battery as claimed in claim 1, characterized in that: the primary lithium battery includes a lithium-manganese dioxide battery, a lithium-thionyl chloride battery, a lithium-iron disulfide battery, a lithium-sulfur dioxide battery, or a lithium-carbon fluoride battery.
6. A primary lithium battery as claimed in claim 1, characterized in that: the shape of the primary lithium battery comprises a cylindrical battery, a soft package battery or a button battery.
7. A method of preparing a primary lithium battery according to any one of claims 1-6, characterized in that the method comprises:
punching the coiled stretch-resistant ultrathin lithium foil into pieces with certain sizes through a die cutting machine to serve as negative electrodes;
and the negative plate, the electrolyte, the diaphragm and the positive electrode form a primary lithium battery, or the negative plate, the solid electrolyte and the positive electrode form the primary lithium battery.
8. The method of claim 7, wherein the stretch resistant ultra thin lithium foil is prepared by:
step 1: mixing an inorganic fiber material, a binder, a pore former, and an optional inorganic filler to make a slurry, and coating and high temperature carbonizing the slurry to form a porous tensile layer having a pore size of 1 nanometer to 200 micrometers and a porosity of 10% to 85%, wherein the inorganic fiber material is optionally modified by vapor deposition, magnetron sputtering, electroplating, atomic doping, atomic etching, or a combination thereof;
step 2: attaching a metallic lithium material to the pores of the porous tensile layer to form a discontinuous metallic lithium material, the discontinuous metallic lithium material being dispersed as a discrete metallic lithium material within the pores of the porous tensile layer; and
and step 3: optionally, a surface protective layer is applied over the porous stretch resistant layer.
9. The method of claim 8, wherein the pore former comprises at least one of ammonium bicarbonate, naphthalene, polystyrene, and ammonium carbonate, and the pore former has a size of 10 nanometers to 10 micrometers;
the inorganic filler includes at least one of conductive graphite, carbon black, ketjen black, graphene, metal nanoparticles, and metal oxide;
the binder comprises at least one of polymethyl methacrylate, polytetrafluoroethylene, styrene butadiene rubber, polyvinylidene fluoride, polyepoxy resin, polystyrene, carboxymethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol, sucrose, polyphenylene sulfide and polyphenylene oxide resin.
10. The method of claim 8 wherein attaching metallic lithium material to the porosity of the porous tensile layer includes attaching metallic lithium or a lithium alloy to the porosity of the porous tensile layer by melt impregnation or melt infiltration.
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