CN110554078A - Method for detecting LATP (LATP) of solid electrolyte lithium titanium aluminum phosphate - Google Patents
Method for detecting LATP (LATP) of solid electrolyte lithium titanium aluminum phosphate Download PDFInfo
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- CN110554078A CN110554078A CN201910924235.2A CN201910924235A CN110554078A CN 110554078 A CN110554078 A CN 110554078A CN 201910924235 A CN201910924235 A CN 201910924235A CN 110554078 A CN110554078 A CN 110554078A
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- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 96
- 229910000664 lithium aluminum titanium phosphates (LATP) Inorganic materials 0.000 title claims abstract description 68
- CVJYOKLQNGVTIS-UHFFFAOYSA-K aluminum;lithium;titanium(4+);phosphate Chemical compound [Li+].[Al+3].[Ti+4].[O-]P([O-])([O-])=O CVJYOKLQNGVTIS-UHFFFAOYSA-K 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title description 23
- 238000007599 discharging Methods 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 15
- -1 polytetrafluoroethylene Polymers 0.000 claims description 33
- 238000012360 testing method Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 13
- 229910052744 lithium Inorganic materials 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 9
- 239000002482 conductive additive Substances 0.000 claims description 9
- 239000011889 copper foil Substances 0.000 claims description 9
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000004743 Polypropylene Substances 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000004816 latex Substances 0.000 claims description 6
- 229920000126 latex Polymers 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 6
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 6
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000002174 Styrene-butadiene Substances 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000002134 carbon nanofiber Substances 0.000 claims description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 3
- 239000006245 Carbon black Super-P Substances 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 3
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 150000003973 alkyl amines Chemical class 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 229940077388 benzenesulfonate Drugs 0.000 claims description 3
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 claims description 3
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 3
- YWDYRRUFQXZJBG-UHFFFAOYSA-N butyl prop-2-enoate;2-methylprop-2-enoic acid Chemical compound CC(=C)C(O)=O.CCCCOC(=O)C=C YWDYRRUFQXZJBG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 230000001788 irregular Effects 0.000 claims description 3
- 239000011268 mixed slurry Substances 0.000 claims description 3
- 239000004745 nonwoven fabric Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 3
- 239000011118 polyvinyl acetate Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 229920005614 potassium polyacrylate Polymers 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 239000000661 sodium alginate Substances 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
- 229940005550 sodium alginate Drugs 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- 239000011115 styrene butadiene Substances 0.000 claims description 3
- 229920001909 styrene-acrylic polymer Polymers 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 238000001947 vapour-phase growth Methods 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 208000028659 discharge Diseases 0.000 abstract 6
- 238000000840 electrochemical analysis Methods 0.000 abstract 2
- 238000007405 data analysis Methods 0.000 abstract 1
- 238000011158 quantitative evaluation Methods 0.000 abstract 1
- 238000004364 calculation method Methods 0.000 description 9
- 238000004537 pulping Methods 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910010406 Li1.2Al0.2Ti1.8(PO4)3 Inorganic materials 0.000 description 2
- 229910009274 Li1.4Al0.4Ti1.6 (PO4)3 Inorganic materials 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 2
- 239000005486 organic electrolyte Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910009515 Li1.5Al0.5Ti1.5(PO4)3 Inorganic materials 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/4166—Systems measuring a particular property of an electrolyte
Abstract
The embodiment of the invention relates to a detection method of solid electrolyte lithium titanium aluminum phosphate (LATP), which comprises the quantitative evaluation of the purity of the LATP and the lithium ion transmission performance of the LATP, and specifically comprises the following steps: preparing a solid electrolyte LATP pole piece, assembling a half cell of the solid electrolyte LATP, and standing the half cell for 8-32 hours to perform electrochemical test, data analysis and quantitative arrangement. Wherein the electrochemical test adopts gradient multiplying power discharge treatment, and the discharge program is 20C discharge to 10mV-0.1V, 10C discharge to 10mV-0.1V and 5C discharge to 10 mV-0.1V; discharging at 2C to 10 mV-0.1V; discharging at 1C to 10 mV-0.1V; discharging at 0.1 deg.C to 10mV-0.1V, and discharging at 0.01 deg.C to 10 mV-0.1V. The purity is calculated by the measured specific discharge capacity, and the multiplying power performance is represented by the discharge capacity with high multiplying power.
Description
Technical Field
the invention relates to the technical field of lithium battery materials, in particular to a method for detecting the purity and rate capability of solid electrolyte lithium titanium aluminum phosphate (LATP).
Background
The lithium ion battery has the characteristics of high output voltage, high energy density, long cycle life, good safety performance, no memory effect and the like, and is successfully applied to the field of mobile power sources as a main energy storage device. In order to further meet the requirements of power grid energy storage, electric vehicles and consumer electronic products on energy storage devices, electrode materials and lithium battery systems with longer cycle life, better safety and higher energy density become research hotspots.
The lithium ion battery mainly comprises four major parts, namely a positive electrode, a negative electrode, a diaphragm and an electrolyte. In the working process of the lithium ion battery, lithium ions shuttle in the positive electrode and the negative electrode through the electrolyte. However, in the current commercial lithium battery, the electrolyte contains combustible liquid organic electrolyte, and when the liquid lithium battery is subjected to severe impact or the temperature of the battery is too high, the electrolyte is extremely easy to burn, so that the battery is ignited and more serious safety accidents are caused. Therefore, the solid electrolyte is adopted to replace the existing liquid organic electrolyte, and the method becomes a means for effectively improving the safety performance of the lithium battery.
For this reason, solid electrolyte technology has been proposed in the art, but there is currently no method for accurately measuring the purity and rate capability of a solid electrolyte.
disclosure of Invention
The invention aims to provide a detection method of solid electrolyte Lithium Aluminum Titanium Phosphate (LATP), which can accurately measure the purity and the rate performance of the LATP by reasonably setting the homogenate proportion of the solid electrolyte and the surface quality of a pole piece, assembling the coated LATP pole piece of the solid electrolyte, a diaphragm and metal lithium of a button cell and according to a gradient rate discharge test mode. The method is simple to operate and high in measurement precision, and provides a reliable method for purity determination and rate performance characterization of the solid electrolyte LATP.
In order to achieve the above object, the present invention provides a method for detecting LATP, which is a solid electrolyte, of lithium titanium aluminum phosphate, comprising:
Preparing a solid electrolyte LATP pole piece by using 1-99.99 wt% of solid electrolyte LATP powder material to be tested, 0.01-10 wt% of binder, 0-10 wt% of conductive additive, 0-2 wt% of dispersant and 0-2 wt% of assistant to form mixed slurry, wherein the surface mass of the solid electrolyte LATP pole piece is 0.01g/cm 2 -40g/cm 2;
Assembling the solid electrolyte LATP pole piece, a diaphragm and metal lithium into a button type half cell;
standing the button half cell for 8-32 hours;
Performing gradient multiplying power discharge on the button type half cell, wherein the discharging multiplying power comprises a set of set discharging multiplying power values, and the discharging cutoff voltage is selected within a set threshold range;
and testing the actual discharge specific capacity of the button type half battery, determining the purity of the solid electrolyte LATP according to the ratio of the actual discharge specific capacity to the theoretical specific capacity, and measuring the rate performance of the solid electrolyte LATP according to the ratio of the discharge specific capacity under the highest rate in the set discharge rate to the actual discharge specific capacity.
Preferably, the solid electrolyte LATP powder material is Li 1+x A x B 2-x (PO4) 3, wherein x is between 0.01 and 0.5, A is one or more of Al, Y, Ga, Cr, In, Fe, Se or La, and B is one or more of Ti, Ge, Ta, Zr, Sn, Fe, V, hafnium, Hf and derivatives thereof;
the binder is one or a mixture of polyvinylidene fluoride, styrene-butadiene latex, styrene-acrylic latex, polyvinyl alcohol, ethylene-vinyl acetate, sodium alginate, polyacrylamide, polymethyl methacrylate-butyl acrylate, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyacrylamide, polyethylene oxide and polytetrafluoroethylene;
The conductive additive is one or a mixture of carbon black, conductive graphite, carbon fiber, carbon nano tube, acetylene black, Keqin carbon, graphene, metal silver, metal gold, vapor-phase growth carbon fiber VGCF, conductive graphite KS-6 and carbon black SUPER-P;
The dispersing agent is one or more of sodium polyacrylate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium hexametaphosphate, polyacrylic acid, hexadecyl trimethyl ammonium bromide, polyethylene glycol, potassium polyacrylate, octyl phenol polyoxyethylene or sulfonate fluorine dispersing agent;
The auxiliary agent is one or a combination of more of polydimethylsiloxane, silicone oil, polyethers, sodium polyacrylate, polyvinyl alcohol, alkyl polyoxyethylene ether sodium carboxylate, polyoxyethylene alkylphenol ether, sodium alkyl benzene sulfonate, alkylphenol polyoxyethylene, polyoxyethylene alkylamine and polyoxyethylene amide.
Preferably, the diaphragm includes: polypropylene PP membrane, polyethylene PE membrane, non-woven fabrics diaphragm, fibre diaphragm, ceramic diaphragm, solid electrolyte diaphragm one or more complex film.
Preferably, the discharge multiplying power is 20C, 10C, 5C, 2C, 1C, 0.1C and 0.01C, and the discharge cutoff voltage is 10 mV-0.1V; the step of performing gradient multiplying power discharge on the button half cell specifically comprises the following steps:
Sequentially discharging to 10mV-0.1V at 20C discharge rate, to 10mV-0.1V at 10C discharge rate, to 10mV-0.1V at 5C discharge rate, to 10mV-0.1V at 2C discharge rate, to 10mV-0.1V at 1C discharge rate, to 10mV-0.1V at 0.1C discharge rate, and to 10mV-0.1V at 0.01C discharge rate.
preferably, at the 10C, 5C, 2C, 1C, 0.1C, 0.01C, the discharge cutoff voltage is between 10mV and 50 mV.
Preferably, at 10C, 5C, 2C, 1C, 0.1C, 0.01C, the discharge cutoff voltage is 20mV to 50 mV.
Preferably, the solid electrolyte LATP powder material is spherical, ellipsoidal or irregular polygonal particles.
Preferably, the carrier of the solid electrolyte LATP pole piece is a copper foil with the shape of a circle, a square or a rectangle of 2-50um, and the area is between 0.5cm 2 and 10cm 2.
Further preferably, the carrier of the solid electrolyte LATP pole piece is 3-45um copper foil, and the surface quality is 0.1g/cm 2 -40g/cm 2.
Further preferably, the carrier of the solid electrolyte LATP pole piece is a copper foil with the thickness of 5-40um, and the surface quality is 1g/cm 2 -40g/cm 2.
According to the detection method of the solid electrolyte LATP provided by the embodiment of the invention, the purity and the rate performance of the solid electrolyte LATP can be accurately measured according to a gradient rate discharge test mode by reasonably setting the homogenate proportion of the solid electrolyte and the surface quality of the pole piece, assembling the coated solid electrolyte LATP pole piece, the diaphragm and the metal lithium into the button cell. The method is simple to operate and high in measurement precision, and provides a reliable method for purity determination and rate performance characterization of the solid electrolyte LATP.
Drawings
fig. 1 is a flow chart of a method for detecting LATP in a solid electrolyte provided in an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a button half cell according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of test results provided in example 2 of the present invention;
Fig. 4 is a schematic diagram of a test result provided in embodiment 10 of the present invention.
Detailed Description
the technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
The embodiment of the invention provides a detection method of a solid electrolyte LATP, which is used for detecting the purity and lithium ion transmission performance of the solid electrolyte LATP, namely the rate performance can be quantitatively evaluated.
Fig. 1 is a flow chart of a method for detecting a solid electrolyte LATP according to an embodiment of the present invention, which is mainly implemented by the following steps according to fig. 1.
step 110, forming mixed slurry by using 1-99.99 wt% of solid electrolyte LATP powder material to be tested, 0.01-10 wt% of binder, 0-10 wt% of conductive additive, 0-2 wt% of dispersant and 0-2 wt% of auxiliary agent to prepare a solid electrolyte LATP pole piece;
The solid electrolyte LATP powder material is Li 1+x A x B 2-x (PO4) 3, wherein x is 0.01-0.5, A is one or more of Al, Y, Ga, Cr, In, Fe, Se or La, B is one or more of Ti, Ge, Ta, Zr, Sn, Fe, V, hafnium element Hf and derivative materials thereof, and the form of the solid electrolyte LATP powder material is spherical, ellipsoidal or irregular polygonal particles.
The binder is one or a mixture of polyvinylidene fluoride, styrene-butadiene latex, styrene-acrylic latex, polyvinyl alcohol, ethylene-vinyl acetate, sodium alginate, polyacrylamide, polymethyl methacrylate-butyl acrylate, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyacrylamide, polyethylene oxide and polytetrafluoroethylene;
The conductive additive is one or a mixture of carbon black, conductive graphite, carbon fiber, carbon nano tube, acetylene black, Keqin carbon, graphene, metal silver, metal gold, vapor-grown carbon fiber VGCF, conductive graphite KS-6 and carbon black SUPER-P;
The dispersing agent is one or more of sodium polyacrylate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium hexametaphosphate, polyacrylic acid, cetyl trimethyl ammonium bromide, polyethylene glycol, potassium polyacrylate, octyl phenol polyoxyethylene or sulfonate fluorine dispersing agent;
The auxiliary agent is one or a combination of more of polydimethylsiloxane, silicone oil, polyethers, sodium polyacrylate, polyvinyl alcohol, alkyl polyoxyethylene ether sodium carboxylate, polyoxyethylene alkylphenol ether, sodium alkyl benzene sulfonate, alkylphenol polyoxyethylene, polyoxyethylene alkylamine or polyoxyethylene amide.
The carrier for preparing the solid electrolyte LATP pole piece is a round, square or rectangular copper foil with the thickness of 2-50um, the area is between 0.5cm 2 -10cm 2, and the surface quality is between 0.01g/cm 2 -40g/cm 2;
Preferably, the carrier of the solid electrolyte LATP pole piece is a copper foil with the thickness of 3-45um, and the surface quality is 0.1g/cm 2 -40g/cm 2.
Further preferably, the carrier of the solid electrolyte LATP pole piece is a copper foil with the thickness of 5-40um, and the surface quality is between 1g/cm 2 and 40g/cm 2.
Step 120, assembling the solid electrolyte LATP pole piece, a diaphragm and metal lithium into a button type half cell;
Specifically, assembling a solid electrolyte LATP pole piece as a positive pole; the assembled button cell structure is shown in fig. 2.
The separator used comprises: polypropylene PP membrane, polyethylene PE membrane, non-woven fabrics diaphragm, fibre diaphragm, ceramic diaphragm, solid electrolyte diaphragm one or more complex film.
step 130, standing the button type half cell for 8-32 hours;
Preferably, the standing time is 8-24 hours; more preferably 8-16 hours.
Step 140, performing gradient multiplying power discharge on the button type half cell, wherein the discharging multiplying power is 20C, 10C, 5C, 2C, 1C, 0.1C and 0.01C, and the discharging is cut to the voltage of 10 mV-0.1V;
Specifically, the discharge rate includes a set of set discharge rate values, and the discharge cutoff voltage is selected within a set threshold range. In the specific embodiment of the invention, the button type half cell is tested by adopting the discharge multiplying power of 20C, 10C, 5C, 2C, 1C, 0.1C and 0.01C and the discharge cutoff voltage of 10 mV-0.1V. Specifically, the discharge is performed in the following sequence: discharge to 10mV-0.1V at 20C discharge rate, discharge to 10mV-0.1V at 10C discharge rate, discharge to 10mV-0.1V at 5C discharge rate, discharge to 10mV-0.1V at 2C discharge rate, discharge to 10mV-0.1V at 1C discharge rate, discharge to 10mV-0.1V at 0.1C discharge rate, and discharge to 10mV-0.1V at 0.01C discharge rate.
In a preferred embodiment, the discharge is cut to a voltage of 10mV to 50mV, more preferably 20mV to 50mV, at 10C, 5C, 2C, 1C, 0.1C, 0.01C.
and 150, testing the actual discharge specific capacity of the button type half battery, determining the purity of the solid electrolyte LATP according to the ratio of the actual discharge specific capacity to the theoretical specific capacity, and measuring the multiplying power performance of the solid electrolyte LATP according to the ratio of the discharge specific capacity to the actual discharge specific capacity at 20C.
specifically, the method adopts the ratio of the discharge specific capacity at the highest rate in the set discharge rates to the actual discharge specific capacity to measure the rate performance of the solid electrolyte LATP. In this embodiment, the highest magnification is 20C. The discharge capacity can be read through a storage battery pack charge-discharge capacity testing device and the like, and the purity and the rate capability of the solid electrolyte LATP can be calculated.
The purity calculation method of the solid electrolyte LATP comprises the following steps: purity-actual specific discharge capacity/theoretical specific capacity; the rate capability of the solid electrolyte LATP can be characterized by the ratio of the specific discharge capacity at 20C to the actual specific capacity.
According to the detection method of the solid electrolyte LATP provided by the embodiment of the invention, the purity and the rate performance of the solid electrolyte LATP can be accurately measured according to a gradient rate discharge test mode by reasonably setting the homogenate proportion of the solid electrolyte and the surface quality of the pole piece, assembling the coated solid electrolyte LATP pole piece, the diaphragm and the metal lithium into the button cell. The method is simple to operate and high in measurement precision, and provides a reliable method for purity determination and rate performance characterization of the solid electrolyte LATP.
the following is a further detailed description of the present invention with reference to several specific examples.
Example 1
the solid electrolyte material of the embodiment 1 is Li 1.2 Al 0.2 Ti 1.8 (PO 4) 3, the components of the pulping material are 80% of solid electrolyte powder, 10% of binder Styrene Butadiene Rubber (SBR) and 10% of conductive additive conductive carbon black (SP), the button cell assembly adopts a metal lithium sheet with a negative electrode sheet of 14mm, a circular sheet with a diaphragm of PP with a diaphragm of 16mm, a solid electrolyte LATP sheet with a diameter of 12mm and an electrolyte of 1 mol of LiPF 6 (EC/DMC 1: 1). The test steps are static for 24 hours, 20C rate discharge to 50mV, 10C rate discharge to 50mV, 5C rate discharge to 50mV, 2C discharge to 50mV, 1C discharge to 50mV, 0.1C discharge to 50mV and 0.01C discharge to 50mV, and the test results are shown in Table 1, wherein the specific first cycle discharge capacity is 748.5mAh/g, 20C discharge to 46.1mAh/g, the calculated purity of the solid electrolyte is 85.29%, and the discharge capacity is 16.6C discharge rate.
| Solid electrolyte material | Li1.2Al0.2Ti1.8(PO4)3 |
| Theoretical specific capacity | 877.6mAh/g |
| First cycle actual specific discharge capacity | 748.5mAh/g |
| 20C (50mV) discharge capacity | 46.1mAh/g |
| Purity of | 85.29％ |
| Rate capability | 6.16％ |
TABLE 1
Example 2
The solid electrolyte material of this example 2 was Li 1.4 Al 0.4 Ti 1.6 (PO 4) 3, the slurry material was 80% solid electrolyte powder, 10% binder SBR, and 10% conductive additive SP, the button cell assembly used a 14mm metal lithium sheet as the negative electrode sheet, a 16mm PP circular sheet as the separator, a 14mm solid electrolyte LATP sheet as the positive electrode, and 1 mole of LiPF 6 (EC/DMC 1:1) as the electrolyte, and the test procedure was 8 hours at rest, 5C rate discharge was 50mV, 2C discharge was 50mV, 1C discharge was 50mV, 0.1C discharge was 50mV, and 0.01C discharge was 50mV, and the test results are shown in table 2, with the test curve shown in fig. 3, first cycle discharge capacity was 699.6mAh/g, 5C discharge capacity was 27.5 h/g, and the solid electrolyte purity was 89.02% and 5C rate discharge performance was 3.93%.
| Solid electrolyte material | Li1.4Al0.4Ti1.6(PO4)3 |
| Theoretical specific capacity | 785.8mAh/g |
| first cycle actual specific discharge capacity | 699.6mAh/g |
| 5C (50mV) discharge capacity | 27.5mAh/g |
| Purity of | 89.02％ |
| rate capability | 3.93％ |
TABLE 2
Example 3
the solid electrolyte material of this example 3 was Li 1.5 Al 0.5 Ti 1.5 (PO 4) 3, the slurrying component was 80% of solid electrolyte powder, 8% of binder SBR, 12% of conductive additive SP, and the button cell was assembled as in example 2. the test procedure was that it was left to stand for 8 hours, 20C rate discharge was performed to 20mV, 10C rate discharge was performed to 20mV, 5C rate discharge was performed to 20mV, 2C discharge was performed to 20mV, 1C discharge was performed to 20mV, 0.1C discharge was performed to 20mV, and the test results are shown in table 3, in which the first cycle discharge capacity was 646.0mAh/g, 20C discharge capacity was 90.9mAh/g, and the purity of the solid electrolyte was 87.37%, and the 20C rate discharge performance was 14.07%.
TABLE 3
Example 4
The solid electrolyte material and pulping process of this example 4 was carried out as in example 1 and the button cell was assembled as in example 2. The testing steps are as follows: standing for 8 hours; 5C rate discharge to 50 mV; 2C to 50 mV; 1C to 50 mV; 0.1C to 50mV, 0.01C to 50 mV; the test result is as follows: the first week discharge capacity is 749.9mAh/g, the 5C discharge capacity is 81.74mAh/g, and the purity of the solid electrolyte is 85.45 percent and the 5C rate discharge performance is 10.49 percent through calculation.
example 5
The solid electrolyte material and pulping process of this example 5 was carried out as in example 1 and the button cell was assembled as in example 2. The testing steps are as follows: standing for 8 hours; 20mV discharge at 20C rate, 20mV discharge at 10C rate, and 20mV discharge at 5C rate; 2C to 20 mV; 1C to 20 mV; 0.1C to 20mV, 0.01C to 20 mV; the test result is as follows: the first week discharge capacity is 758.6mAh/g, the 20C discharge capacity is 55.9mAh/g, and the purity of the solid electrolyte is 86.44% and the 20C rate discharge performance is 7.37% by calculation.
Example 6
The solid electrolyte material and pulping method of example 6 was performed as in example 2, and the button cell was assembled as in example 2. The testing steps are as follows: standing for 8 hours; discharging at 20C rate to 50 mV; 10C to 50 mV; 5C rate discharge to 50 mV; 2C to 50 mV; 1C to 50 mV; 0.1C to 50mV, 0.01C to 50 mV; the test result is as follows: the first week discharge capacity is 707.8mAh/g, the 20C discharge capacity is 20.3mAh/g, and the purity of the solid electrolyte is 90.17 percent and the 20C multiplying power discharge performance is 2.87 percent through calculation.
Example 7
The solid electrolyte material and pulping process of this example 7 was carried out as in example 2 and button cell batteries were assembled as in example 2. The testing steps are as follows: standing for 8 hours; 20mV discharge at 20C rate, 20mV discharge at 10C rate, and 20mV discharge at 5C rate; 2C to 20 mV; 1C to 20 mV; 0.1C to 20mV, 0.01C to 20 mV; the test result is as follows: the first week discharge capacity is 712.9mAh/g, the 20C discharge capacity is 28.9mAh/g, and the purity of the solid electrolyte is 90.72 percent and the 20C multiplying power discharge performance is 4.05 percent through calculation.
example 8
The solid electrolyte material and pulping process of this example 8 was carried out as in example 3 and the button cell was assembled as in example 1. The testing steps are as follows: standing for 8 hours; 5C rate discharge to 20 mV; 2C to 20 mV; 1C to 20 mV; 0.1C to 20mV, 0.01C to 20 mV; the test result is as follows: the first week discharge capacity is 641.6mAh/g, the 5C discharge capacity is 107.3mAh/g, and the purity of the solid electrolyte is 86.77 percent and the 5C rate discharge performance is 16.73 percent through calculation.
example 9
the solid electrolyte material and pulping process of this example 9 was carried out as in example 3 and the button cell was assembled as in example 1. The testing steps are as follows: standing for 24 hours; discharging at 20C rate to 10mV, discharging at 10C rate to 10mV, and discharging at 5C rate to 10 mV; 2C to 10 mV; 1C to 10 mV; 0.1C to 10mV, 0.01C to 10 mV; the test result is as follows: the first week discharge capacity is 661.5mAh/g, the 20C discharge capacity is 103.5mAh/g, and the purity of the solid electrolyte is 89.47% and the 20C rate discharge performance is 15.64% by calculation.
Example 10
The solid electrolyte material and the pulping method of this example 10 were carried out as in example 1, and the button cell was assembled as in example 1. The testing steps are as follows: standing for 32 hours; 1C to 20 mV; 0.5C to 20 mV; 0.2C to 20 mV; 0.1C to 20 mV; 0.05C to 20 mV; the test result is as follows: the first week discharge capacity is 747.2mAh/g, the 1C discharge capacity is 117.1mAh/g, and the purity of the solid electrolyte is 85.14 percent and the 1C multiplying power discharge performance is 15.67 percent through calculation.
according to the data of the fourth table, the fifth table and the sixth table, the purity obtained by calculation is relatively close by adopting different test programs, the comparison of the fourth table and the fifth table shows that the multiplying power performance index can only qualitatively explain the multiplying power performance of the material, and the quality of the multiplying power performance of different materials cannot influence the judgment of the quality of the multiplying power performance of different materials due to the difference of the test programs.
TABLE 4
TABLE 5
TABLE 6
the above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present invention and are not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A detection method of solid electrolyte lithium titanium aluminum phosphate (LATP), which is characterized by comprising the following steps:
Preparing a solid electrolyte LATP pole piece by using 1-99.99 wt% of solid electrolyte LATP powder material to be tested, 0.01-10 wt% of binder, 0-10 wt% of conductive additive, 0-2 wt% of dispersant and 0-2 wt% of assistant to form mixed slurry, wherein the surface mass of the solid electrolyte LATP pole piece is 0.01g/cm 2 -40g/cm 2;
assembling the solid electrolyte LATP pole piece, a diaphragm and metal lithium into a button type half cell;
Standing the button half cell for 8-32 hours;
performing gradient multiplying power discharge on the button type half cell, wherein the discharging multiplying power comprises a set of set discharging multiplying power values, and the discharging cutoff voltage is selected within a set threshold range;
and testing the actual discharge specific capacity of the button type half battery, determining the purity of the solid electrolyte LATP according to the ratio of the actual discharge specific capacity to the theoretical specific capacity, and measuring the rate performance of the solid electrolyte LATP according to the ratio of the discharge specific capacity under the highest rate in the set discharge rate to the actual discharge specific capacity.
2. The detection method according to claim 1,
the solid electrolyte LATP powder material is Li 1+x A x B 2-x (PO4) 3, wherein x is between 0.01 and 0.5, A is one or more of Al, Y, Ga, Cr, In, Fe, Se or La, and B is one or more of Ti, Ge, Ta, Zr, Sn, Fe, V, hafnium element Hf and derivative materials thereof;
The binder is one or a mixture of polyvinylidene fluoride, styrene-butadiene latex, styrene-acrylic latex, polyvinyl alcohol, ethylene-vinyl acetate, sodium alginate, polyacrylamide, polymethyl methacrylate-butyl acrylate, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, sodium carboxymethyl cellulose, polyacrylamide, polyethylene oxide and polytetrafluoroethylene;
the conductive additive is one or a mixture of carbon black, conductive graphite, carbon fiber, carbon nano tube, acetylene black, Keqin carbon, graphene, metal silver, metal gold, vapor-phase growth carbon fiber VGCF, conductive graphite KS-6 and carbon black SUPER-P;
The dispersing agent is one or more of sodium polyacrylate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium hexametaphosphate, polyacrylic acid, hexadecyl trimethyl ammonium bromide, polyethylene glycol, potassium polyacrylate, octyl phenol polyoxyethylene or sulfonate fluorine dispersing agent;
The auxiliary agent is one or a combination of more of polydimethylsiloxane, silicone oil, polyethers, sodium polyacrylate, polyvinyl alcohol, alkyl polyoxyethylene ether sodium carboxylate, polyoxyethylene alkylphenol ether, sodium alkyl benzene sulfonate, alkylphenol polyoxyethylene, polyoxyethylene alkylamine and polyoxyethylene amide.
3. The detection method according to claim 1, wherein the diaphragm comprises: polypropylene PP membrane, polyethylene PE membrane, non-woven fabrics diaphragm, fibre diaphragm, ceramic diaphragm, solid electrolyte diaphragm one or more complex film.
4. The detection method according to claim 1, wherein the discharge rate is 20C, 10C, 5C, 2C, 1C, 0.1C, 0.01C, and the discharge cutoff voltage is 10 mV-0.1V; the step of performing gradient multiplying power discharge on the button half cell specifically comprises the following steps:
Sequentially discharging to 10mV-0.1V at 20C discharge rate, to 10mV-0.1V at 10C discharge rate, to 10mV-0.1V at 5C discharge rate, to 10mV-0.1V at 2C discharge rate, to 10mV-0.1V at 1C discharge rate, to 10mV-0.1V at 0.1C discharge rate, and to 10mV-0.1V at 0.01C discharge rate.
5. The detection method according to claim 1 or 4, wherein the discharge cutoff voltage is 10mV to 50mV at 10C, 5C, 2C, 1C, 0.1C, 0.01C.
6. The detection method according to claim 1 or 4, wherein the discharge cutoff voltage is 20mV to 50mV at 10C, 5C, 2C, 1C, 0.1C, 0.01C.
7. the detection method according to claim 1, wherein the solid electrolyte LATP powder material is a spherical, ellipsoidal or irregular polygonal particle.
8. The detection method as claimed in claim 1, wherein the carrier of said solid electrolyte LATP sheet is a copper foil of 2-50um in round, square or rectangular shape with an area of 0.5cm 2 -10cm 2.
9. The detection method as claimed in claim 8, wherein the carrier of said solid electrolyte LATP sheet is 3-45um copper foil with a surface mass between 0.1g/cm 2 -40g/cm 2.
10. The detection method as claimed in claim 9, wherein the carrier of said solid electrolyte LATP sheet is 5-40um copper foil with a surface mass between 1g/cm 2 -40g/cm 2.
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