CN108649148A - A kind of preparation method of lean property aluminium titanate composite material saggar - Google Patents
A kind of preparation method of lean property aluminium titanate composite material saggar Download PDFInfo
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- CN108649148A CN108649148A CN201810638918.7A CN201810638918A CN108649148A CN 108649148 A CN108649148 A CN 108649148A CN 201810638918 A CN201810638918 A CN 201810638918A CN 108649148 A CN108649148 A CN 108649148A
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- composite material
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- titanate composite
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- aluminium titanate
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- 239000004411 aluminium Substances 0.000 title claims abstract description 94
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 94
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 80
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 68
- 238000005453 pelletization Methods 0.000 claims abstract description 30
- 238000000748 compression moulding Methods 0.000 claims abstract description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical group [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 42
- 229910052744 lithium Inorganic materials 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000003825 pressing Methods 0.000 claims description 18
- 229910052878 cordierite Inorganic materials 0.000 claims description 11
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 11
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 10
- KAKVFSYQVNHFBS-UHFFFAOYSA-N (5-hydroxycyclopenten-1-yl)-phenylmethanone Chemical compound OC1CCC=C1C(=O)C1=CC=CC=C1 KAKVFSYQVNHFBS-UHFFFAOYSA-N 0.000 claims description 9
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 239000003595 mist Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 5
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 5
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 5
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000010433 feldspar Substances 0.000 claims 1
- 239000000463 material Substances 0.000 description 43
- 238000009472 formulation Methods 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 229910052661 anorthite Inorganic materials 0.000 description 12
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000000654 additive Substances 0.000 description 11
- 230000000996 additive effect Effects 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 239000003513 alkali Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 230000035939 shock Effects 0.000 description 7
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 6
- NWXHSRDXUJENGJ-UHFFFAOYSA-N calcium;magnesium;dioxido(oxo)silane Chemical compound [Mg+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O NWXHSRDXUJENGJ-UHFFFAOYSA-N 0.000 description 6
- 229910052637 diopside Inorganic materials 0.000 description 6
- 239000010405 anode material Substances 0.000 description 4
- -1 for example Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000004408 titanium dioxide Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- HCFOYBNXMYSROO-UHFFFAOYSA-N [K].C(C=CC1=CC=CC=C1)(=O)O Chemical compound [K].C(C=CC1=CC=CC=C1)(=O)O HCFOYBNXMYSROO-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/10—Primary casings; Jackets or wrappings
- H01M50/116—Primary casings; Jackets or wrappings characterised by the material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of preparation methods of lean property aluminium titanate composite material saggar, include the following steps:(1)Lean property aluminium titanate composite material powder is granulated, pelletizing is obtained;(2)By gained pelletizing compression moulding, idiosome is obtained;(3)Gained idiosome is sintered, saggar is obtained.
Description
Technical field
The present invention relates to a kind of lean property aluminium titanate composite material saggar, especially lithium battery with extra-strong corrosion resistant are special
The manufacturing method of saggar and application.
Background technology
With deepening continuously for lithium battery applications, usage amount increases year by year, and China is as lithium battery big producer, in the world
Key player is play in lithium battery production.Lithium battery type is various, and because of positive electrode difference, lithium ion battery is broadly divided into:
LiFePO4 (LFP), lithium nickelate (LNO), LiMn2O4 (LMO), cobalt acid lithium (LCO) and nickel cobalt mangaic acid ternary lithium (NCM), nickel
Cobalt aluminic acid ternary lithium (NCA), negative material mainly use graphitic carbon material.Wherein nickel cobalt mangaic acid ternary lithium (NCM), nickel cobalt aluminic acid
The features such as ternary lithium (NCA) is high, cycle-index is long with energy density, becomes the developing direction of the following lithium battery.Lithium battery to
Life is while offer convenience, production process can not avoid there are problems of energy consumption, wherein being mainly reflected under high temperature solid
Phase reaction is sintered, and in addition to the consumption of electricity in whole process, the main consumable material of another part is exactly kiln and kiln furnitures, wherein again
It is consumed using the saggar being in direct contact with lithium battery raw material as serious.The most of Anode of lithium cell material are currently on the market
Cordierite-mullite, mullite corundum sagger, such saggar have coefficient of expansion low-heat pinking good, and cost of material is low and is easy to get
The advantages that, other than ternary lithium battery, it is used as common Anode of lithium cell material sintering, service life is about 20 times or so, but
If being used as the container of ternary anode material of lithium battery reaction-sintered, service life is about 10 times, mainly scraps reason and is:
Ternary lithium battery raw material and refractory material reaction, produce a kind of erosion layer of glass phase substance, corrode the big thermal shock of the layer coefficient of expansion
Property difference it is easy to crack, and there are larger differences with the coefficient of expansion of original saggar ligand, it is easy to which the cracking pollution lithium battery that falls off is former
Material.It is all nickeliferous in ternary Anode of lithium cell material, it is needed using the saggar scrapped as trade waste as chemical treatments,
Not only processing cost is high, and easily causes the generation of secondary pollution.The service life of ternary lithium battery saggar is improved,
Through developing faced one of main pressure as current ternary lithium battery.The average index of domestic and international saggar consumption be it is per ton just
200-300 kilograms of pole material consumption causes prodigious pressure to environment, researches and develops the special casket of a suitable lithium battery sintering
Alms bowl is imperative.
By the analysis of lithium battery material material, it is found that lithium battery needs coefficient of expansion low-heat pinking good and resistance to saggar
Alkali, the lithium in common lithium battery are introduced in the form of lithium carbonate, alkalinity is smaller, but lithium is introduced as hydrogen in ternary lithium battery
Lithia, alkalinity is very big, and the ceramic materials such as mullite are typically all acidproof not alkaline-resisting, and especially under high temperature, alkali is to such material
Erosion it is very big.In terms of alkali resistance, there is a kind of ceramic material that there is very excellent performance, that is, aluminium titanates.Aluminium titanates
Mainly using ionic bond and covalent bond as associative key, from microstructure and state, there are crystal phase and stomata in inside, this is just
Determine aluminium titanates have the low thermal coefficient not available for metal material and high molecular material, anti-slag, it is alkaline-resisting, anti-corrosion, to more
Kind metal and glass have nonwettable advantage, therefore in the conditions harsh environment such as wear-resistant, high temperature resistant, alkali resistant, anticorrosive
Under have a wide range of applications, it is that the coefficient of expansion is minimum in known ceramic material especially to require the occasion of highly heatproof and shockproof, aluminium titanates
's.The disadvantages such as aluminium titanates also has 1100 DEG C or so easily to decompose simultaneously, and mechanical strength is low, so being difficult to obtain under pure aluminium titanates room temperature
, mechanical strength is very low, lacks practical utility value, stablizes and the aluminium titanates with good mechanical strength is generally with composite material
Form exist, aluminium titanate composite material not only has an above-mentioned advantage of aluminium titanates, while the shortcomings that evaded itself very well, this
Class aluminium titanate composite material is undoubtedly a kind of raw material being highly suitable for lithium battery industry saggar.But aluminium titanates composite wood
Material belongs to non-plastic raw material, does not have plasticity.
Invention content
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of saggar made of lean property aluminium titanate composite material
Preparation method.
A kind of preparation method of lean property aluminium titanate composite material saggar is provided herein, is included the following steps:
(1) lean property aluminium titanate composite material powder is granulated, obtains pelletizing;
(2) by gained pelletizing compression moulding, idiosome is obtained;
(3) gained idiosome is sintered, obtains saggar.
According to the invention, it is first granulated re-compacted molding, lean property aluminium titanate composite material can be made special requirement size
Saggar.
The lean property aluminium titanate composite material can be selected from aluminium titanates anorthite cordierite composite material.
Preferably, step (1) includes:
By lean property aluminium titanate composite material powder and relative to the powder weight 2~10% poly-vinyl alcohol solution, 40%~
100% water, 0.1%~0.5% sodium tripolyphosphate and 0.01%~0.1% n-octyl alcohol mixing and ball milling, obtain slurry;
And
By gained slurry mist projection granulating, pelletizing is obtained.
According to the invention, can obtain high solids content, stably dispersing lean property aluminium titanate composite material powdery pulp, into
And it can obtain suitable for dry-pressing formed pelletizing.
Preferably, the grain size of the lean property aluminium titanate composite material powder is 325 mesh or more.
Preferably, the moisture of gained pelletizing controls between 0.1%~1%, grain size is between 10~200um, preferably
Between 50~150um.
Preferably, in step (2), pressing pressure is 8~20MPa.
Preferably, in step (1), by weight ratio 1:2~1:The lean property metatitanic acid of grain size between 0.1mm~1mm between 1
Aluminium composite material aggregate and lean property aluminium titanate composite material powder, and with relative to the aggregate and the powder mixed weight
0.5~1% carboxymethyl cellulose, 1%~2% potassium laurate solution, 3~10% water are granulated.
According to the invention, the pelletizing dry-pressing formed suitable for half can be obtained.
Preferably, step (1) includes:
The lean property aluminium titanate composite material powder and the carboxymethyl cellulose are mixed, mixed powder is obtained;
The potassium laurate solution and the water are mixed, mixing liquid is obtained;And
The lean property aluminium titanates composite aggregate is put into disintegrating apparatus and is crushed, it is described mixed that part is added in crushing process
Liquid is closed, in aggregate after uniform moisture, the mixed powder is added, and be homogeneously added into remaining mixing liquid, until crushing
At shape of sand, granulation terminates powder in equipment.
Preferably, the disintegrating apparatus is edge runner.
Preferably, in step (2), pressing pressure is 8~20MPa.
According to the present invention it is possible to which it is multiple to obtain the aluminium titanates that expansion rate is low, thermal shock resistance is good, alkali resistance is strong by simple method
Condensation material saggar.
Specific implementation mode
It is further illustrated the present invention below in conjunction with following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.In this specification, unless otherwise indicated, all percentage is weight percentage.
It is disclosed a kind of preparation method of aluminium titanate composite material saggar.
In the disclosure, " aluminium titanate composite material saggar " refers to the saggar made of aluminium titanate composite material." saggar " is
Refer to the container of firing." aluminium titanate composite material " refers to the material that aluminium titanates is combined with other components, including has been synthesized
Aluminium titanate composite material and calcining when synthesize aluminium titanate composite material formulation material (raw material) etc..In the disclosure, to metatitanic acid
Aluminium composite material is not particularly limited, but is primarily directed to lean property aluminium titanate composite material.So-called lean property refers to being mixed with water
Afterwards without viscosity, the raw material obtained after the ceramic powder or calcining after all calcinings belongs to poor material.As lean property aluminium titanates
The specific example of composite material, for example, aluminium titanates anorthite cordierite composite material and aluminium titanates anorthite cordierite it is compound
The formulation material of material.
Aluminium titanates anorthite cordierite composite material contains aluminium titanates, anorthite CaOAl2O3·2SiO2And cordierite
Mg2Al4Si5O18Compound phase.In one preferred embodiment, in aluminium titanates anorthite cordierite composite material, by mass, titanium
The content of sour aluminium is 60~80%, anorthite CaOAl2O3·2SiO2Content be 10~20%, cordierite Mg2Al4Si5O18
Content be 10~20%.
In one example, the formulation material of aluminium titanates anorthite cordierite composite material includes alumina powder, titanium dioxide
Powder, diopside powder, these belong to poor material.In one preferred embodiment, the weight percent of each raw material is:Aluminium oxide
Powder 40~55%, titanium dioxide powder 25~35%, diopside powder 15~35%.
In addition, the saggar in the disclosure is preferably lithium battery saggar, specifically, being anode material of lithium battery sintering
Saggar, preferably ternary anode material of lithium battery sintering saggar.Ternary anode material of lithium battery is, for example, nickel cobalt mangaic acid ternary
Lithium (NCM), nickel cobalt aluminic acid ternary lithium (NCA) etc..
The production technology of aluminium titanate composite material saggar may include molding, dry, sintering etc..
In one embodiment, production molding is carried out using dry-pressing form.Hereinafter, the forming step is described in detail.
First, by aluminium titanate composite material powder together with additive ball milling, obtain slurry.Here, " aluminium titanates composite wood
Feed powder body " can be the aluminium titanate composite material powder synthesized, can also be the formula for synthesizing aluminium titanate composite material
Feed powder body.
The grain size of aluminium titanate composite material powder can be 325 mesh or more, can obtain finer and close idiosome in this way, reduce gas
The porosity, acceleration of sintering.It is highly preferred that the grain size of aluminium titanate composite material powder is 800~1250 mesh.
Additive may include the poly-vinyl alcohol solution as binder, the water as decentralized medium (preferably pure water), make
For water-reducing agent sodium tripolyphosphate and and as antifoaming agent n-octyl alcohol.
The concentration of poly-vinyl alcohol solution can be 5~15%, such as 10%.The additive amount of poly-vinyl alcohol solution can be powder weight
2~10%, more preferably the 5~10% of amount.It is possible thereby to the mechanical strength of compacting idiosome is improved, while effectively control was burnt into
Organic matter loss on ignition in journey.
The additive amount of water can be the 40%~100% of powder weight, more preferably 50~60%.It is possible thereby to both ensure that
The mobility of slurry, and obtain the preferable pelletizing of compactness.
The additive amount of sodium tripolyphosphate can be the 0.1%~0.5% of powder weight, more preferably 0.1~0.2%.Thus
The slurry that can obtain higher solids content can obtain the slurry of good fluidity in the case where 50% pure water is added.
The additive amount of n-octyl alcohol can be the 0.01%~0.1% of powder weight, more preferably 0.02%.It is possible thereby to ball milling
Pulp surface non-foam is finished, foam is not generated during batch turning.
Ball-milling Time can be 30~60 minutes, such as 30 minutes or so.
The slurry of acquisition is granulated, mist projection granulating is carried out preferably by ceramic Spray granulation equipment, obtains pelletizing.
The moisture of pelletizing is can be controlled between 0.1%~1%, and more preferably 0.5~1%.As a result, in pressing process, pressure is the same
In the case of, the better idiosome of intensity can be obtained.The size tunable system of pelletizing between 10~200um, more preferable 50~
Between 150um.It is possible thereby to increase the mobility of pelletizing, be conducive to the discharge of internal gas in pressing process, reduce internal
Defect.
By pelletizing compression moulding, saggar idiosome is obtained.Pressing pressure can be 8~20MPa.In one example, it will be granulated
Powder is added in the sagger special mold of great tonnage press, and using the pressure of great tonnage press, pelletizing, which is pressed into, to be had
The saggar idiosome of certain mechanical strength.
Using dry pressuring forming process, product densification can be made and surface is smooth.
In one embodiment, production molding is carried out using half-dried swaging formula.Hereinafter, the forming step is described in detail.
First, aluminium titanate composite material aggregate and aluminium titanate composite material powder are granulated together with additive.Here,
" aluminium titanate composite material aggregate " can be the aluminium titanate composite material aggregate synthesized, can also be multiple for synthesizing aluminium titanates
The formulation material aggregate of condensation material." aluminium titanate composite material powder " can be the aluminium titanate composite material powder synthesized, also may be used
To be the formulation material powder for synthesizing aluminium titanate composite material.
Aluminium titanate composite material aggregate refers to the particulate material that grain size is more than 0.1mm, can be crushed, sieving of milling obtains.Metatitanic acid
The grain size of aluminium composite ceramics aggregate is preferably between 0.1mm~1mm.
The grain size of aluminium titanate composite material powder can be between 325~800 mesh.
Aluminium titanate composite material aggregate and aluminium titanate composite material powder are granulated together, can be produced to avoid with mist projection granulating
Raw high energy consumption issues.
Aluminium titanate composite material aggregate and aluminium titanate composite material powder weight ratio can be 1:2~1:It, in this way can be between 1
Obtain the pelletizing of more preferable particle size.
Additive may include the carboxymethyl cellulose (CMC) as binder, the potassium laurate as forming lubricant, with
And the water (preferably pure water) as decentralized medium.
The additive amount of carboxymethyl cellulose can be that aluminium titanates composite ceramics aggregate and alumina titanate ceramics composite material powder are mixed
Close the 0.5~1% of weight (hereinafter referred to as mixed weight).It is possible thereby to solve that poor material is inviscid in pressing process to ask
Topic, by high pressure, will be bonded together between powder and powder, obtain the idiosome for meeting intensity requirement.
Potassium laurate can add in form of an aqueous solutions, and concentration can be 30~40%, for example, 30%.Potassium laurate water
The additive amount of solution can be the 1%~2% of mixed weight.It is possible thereby to increase the lubricity of poor material, improve the flowing of pug
Property, allow pelletizing to be conducive to compression moulding.
The additive amount of water can be the 4~12% of mixed weight.Pug material is adjusted to suitable compacting saggar.
In one example, aluminium titanate composite material powder and carboxymethyl cellulose (CMC) are sufficiently mixed, mixed
Close powder.Potassium laurate solution and water are uniformly mixed, mixing liquid is obtained.
It is preferably edge runner to be granulated device used, aggregate and powder can be allowed to be formed with bone by rolling repeatedly in this way
Material is core, and surrounding wraps up the little particle of powder, is commonly called as being granulated.
Aluminium titanates composite ceramics aggregate is put into edge runner, starts edge runner, in right amount addition part mixing liquid, in aggregate
After moisture is substantially uniform, mixed powder part is added, residual mixed liquor body is slowly homogeneously added into, until the powder in edge runner
At shape of sand, granulation terminates.
The moisture of the pelletizing of gained can be 3~10%, and grain size can be 0.2~3mm.
By pelletizing compression moulding, saggar idiosome is obtained.Pressing pressure can be 8~20MPa.In one example, it will be granulated
Powder is added in the sagger special mold of great tonnage press, and using the pressure of great tonnage press, pelletizing, which is pressed into, to be had
The saggar idiosome of certain mechanical strength.
Using half dry pressuring forming process, advantage is that its is simple for process, production cost is low.
Obtained saggar idiosome can be dried, and sintering obtains saggar.Sintering temperature can be according to aluminium titanate composite material not
It is same and different, it may generally be 1450~1550 DEG C.
In the disclosure, aluminium titanate composite material saggar expansion rate obtained is low, thermal shock resistance is good, alkali resistance is strong.For example, it is anti-
Thermal shock resistance is 650~800 DEG C and does not crack three times that coefficient of thermal expansion is 0.5~1.2 × 10E-6 DEG C, is particularly suitable as lithium battery
Sagger special.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1 is dry-pressing formed
In the present embodiment, aluminium titanate composite material is the formulation material of aluminium titanates anorthite diopside, including 50%
Alumina powder, 35% titanium dioxide powder, 15% diopside powder.
1, ball milling:Aluminium titanate composite material formulation material powders more than 1250 mesh adds powder weight 10% a concentration of 10%
PVA solution, add 50% pure water of powder weight, add 0.2% sodium tripolyphosphate as water-reducing agent, add 0.01% n-octyl alcohol conduct
Ball mill ball milling, about ball milling 30 minutes or so is added in antifoaming agent together, obtains high solids content, the aluminium titanates for being uniformly dispersed, stablizing
The powdery pulp of composite-material formula material.
2, it is granulated:The powdery pulp for the aluminium titanate composite material formulation material that ball milling is obtained utilizes ceramic Spray granulation equipment
Mist projection granulating is carried out, powder moisture is controlled in 0.5-1%, and pelletizing grain size is in 50-150um.
3, dry-pressing:Aluminium titanate composite material pelletizing is quantitatively adding in the sagger special mold of great tonnage press,
Using the pressure (15MPa) of great tonnage press, pelletizing is pressed into the saggar idiosome with certain mechanical strength.
4, dry, sintering:By saggar idiosome dry 4 hours at 120 DEG C, then 1550 DEG C of sintered heat insulatings 6 hours, obtain casket
Alms bowl.
Embodiment 2 half is dry-pressing formed
In the present embodiment, aluminium titanate composite material is the formulation material of aluminium titanates anorthite diopside, including 50%
Alumina powder, 35% titanium dioxide powder, 15% diopside powder.
1, the preparation of material:The formulation material aggregate of 0.1-0.7mm grain sizes and the formulation material powder weight of 325-800 mesh grain sizes
Than 40:60, the carboxymethyl cellulose (CMC) of formulation material aggregate and formulation material powder mixed weight 1% is used as binder, mixing
Pure water of the potassium laurate of the concentration 30% of weight 2% as forming lubricant and mixed weight 6%.
2, it is granulated:Preparation is in advance to be sufficiently mixed formulation material powder and carboxymethyl cellulose (CMC), by the moon
Cinnamic acid potassium solution and pure water are uniformly mixed, and granulation is granulated using edge runner, and formulation material aggregate is first put into edge runner, is started
Edge runner, is added partially liq in right amount, and after moisture is substantially uniform in formulation material aggregate, powder section is added, slowly equably plus
Enter remaining liq, until the powder in edge runner is at shape of sand, granulation terminates.Powder moisture is 5%, and pelletizing grain size is 0.5-
Between 2mm.
3, half dry-pressing:The pelletizing that formulation material aggregate and formulation material powder form is quantitatively adding mounted in great tonnage press
In sagger special mold, using the pressure (18MPa) of great tonnage press, pelletizing is pressed into the casket with certain mechanical strength
Alms bowl idiosome.
4, dry, sintering:It is 4 hours dry at 120 DEG C after saggar idiosome is dried in the shade 2 days naturally, then 1550 DEG C of sintering 6
Hour, obtain saggar.
Performance test
The expansion rate that gained saggar is tested using MEASURING THE THERMAL EXPANSION COEFFICIENT instrument method, 650 DEG C are directly placed into using from room temperature
Or 30 minutes methods for further taking out natural cooling under room temperature environment are kept the temperature in 800 DEG C of electric furnace, the heat of test gained saggar
Pinking, using the alkali resistance for putting into nickelic ternary lithium battery production method test gained saggar.
With the saggar (embodiment 1) for the aluminium titanates anorthite cordierite composite material that mist projection granulating plus dry process obtain,
For the coefficient of expansion at 0.5 × 10E-6 DEG C or so, thermal shock resistance can accomplish that 800 DEG C are not cracked three times, and it is strongest to be used as current corrosivity
In nickelic ternary lithium battery saggar, access times about 40 times or so, performance is best currently on the market, including import saggar.
The saggar (embodiment 2) for the aluminium titanates anorthite cordierite composite material for adding half dry-pressing prilling to obtain is granulated with edge runner,
For the coefficient of expansion at 1.5 × 10E-6 DEG C or so, thermal shock resistance can accomplish that 600 DEG C are not cracked three times, and it is strongest to be used as current corrosivity
In nickelic ternary lithium battery saggar, access times about 25 times or so and existing market upper inlet saggar service life are substantially similar.
It is found that adding the saggar that dry process obtains using mist projection granulating, there is better compactness and consistency, can obtain
More low-expansion product is obtained, there is better thermal shock performance, simultaneously because compactness is good, the lower porosity is corrosion-resistant
Property is more preferable.It is granulated with edge runner plus the saggar technique of half dry-pressing prilling acquisition is simpler, production cost is lower.
Claims (10)
1. a kind of preparation method of lean property aluminium titanate composite material saggar, which is characterized in that include the following steps:
(1)Lean property aluminium titanate composite material powder is granulated, pelletizing is obtained;
(2)By gained pelletizing compression moulding, idiosome is obtained;
(3)Gained idiosome is sintered, saggar is obtained.
2. preparation method according to claim 1, which is characterized in that the lean property aluminium titanate composite material is aluminium titanates calcium
Feldspar cordierite composite material.
3. preparation method according to claim 1 or 2, which is characterized in that step(1)Including:
By lean property aluminium titanate composite material powder and relative to the powder weight 2~10% poly-vinyl alcohol solution, 40%~100%
Water, 0.1%~0.5% sodium tripolyphosphate and 0.01%~0.1% n-octyl alcohol mixing and ball milling, obtain slurry;And
By gained slurry mist projection granulating, pelletizing is obtained.
4. preparation method according to claim 3, which is characterized in that the grain size of the lean property aluminium titanate composite material powder
More than 325 mesh.
5. preparation method according to claim 3 or 4, which is characterized in that the control of the moisture of gained pelletizing 0.1%~
Between 1%, grain size is between 10~200um.
6. preparation method according to any one of claim 3 to 5, which is characterized in that step(2)In, pressing pressure 8
~20MPa.
7. preparation method according to claim 1 or 2, which is characterized in that step(1)In, by weight ratio 1:2~1:1
Between 0.1mm~1mm between grain size lean property aluminium titanate composite material aggregate and lean property aluminium titanate composite material powder, and
With the carboxymethyl cellulose relative to the aggregate and the powder mixed weight 0.5~1%, 1%~2% potassium laurate solution,
3~10% water is granulated.
8. preparation method according to claim 7, which is characterized in that step(1)Including:
The lean property aluminium titanate composite material powder and the carboxymethyl cellulose are mixed, mixed powder is obtained;
The potassium laurate solution and the water are mixed, mixing liquid is obtained;And
The lean property aluminium titanate composite material aggregate is put into progress rolling granulation in rolling machine equipment, is added during rolling
In aggregate after uniform moisture the mixed powder is added, and be homogeneously added into remaining mixed liquor in the part mixing liquid
Body, until the powder in disintegrating apparatus is at shape of sand, granulation terminates.
9. preparation method according to claim 7 or 8, which is characterized in that step(2)In, pressing pressure is 8~20MPa.
10. preparation method according to any one of claim 1 to 9, which is characterized in that the saggar is lithium battery casket
Alms bowl.
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