CN109704742A - A kind of corrosion-resistant cracking resistance special ceramic material, preparation method and applications - Google Patents
A kind of corrosion-resistant cracking resistance special ceramic material, preparation method and applications Download PDFInfo
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Abstract
The present invention provides a kind of corrosion-resistant cracking resistance special ceramic materials, preparation method and applications, by adjusting the raw material components and its content of special ceramic material basis material, and add the three-dimensional net structure alumina aerogels micro mist of certain partial size, it is scattered in it in body basis material and serves as microskeleton structure, enhance basal body binding force, and the stomata generated in sintering procedure is reduced, the stress variation in process of expansion and contraction is buffered, thermal shock resistance is improved；Furthermore, the special ceramic material can also enhance and the vitreous adhesion strength of Aluminosilicates, make special ceramic material basis material be not easy to peel off and then influence the quality of lithium ion anode material, while the further erosion of lithium ion during sintering can also be inhibited, its corrosion resistance is remarkably reinforced.Be applied to prepare saggar during, be recycled that number is high, and lithium ion depth of erosion is shallow, can reduce consumables cost.
Description
Technical field
The present invention relates to a kind of special ceramic materials, preparation method and applications, and in particular to one kind have highly corrosion resistant,
The good anode material of lithium battery of cracking resistance, which is fired, uses special ceramic material, preparation method and applications.
Background technique
In recent years, with the continuous renewal of science and technology and the continuous promotion of performance of lithium ion battery, lithium ion battery
There is extensive development prospect in fields such as mobile phone, laptop, new-energy automobile, energy storage.Especially nearest various countries are declared
Cloth suspends sale of conventional fuel oil car timetable, and China will suspend sale of fuel vehicle in 2025, it is intended to carry out energy-saving and environment-friendly new energy energetically
Source automobile, and the most important component of new-energy automobile is exactly rechargeable battery.Lithium ion battery is mainly by positive electrode, cathode material
Material, electrolyte and diaphragm are constituted.It wherein, include LiFePO4, cobalt acid lithium, nickel cobalt manganese, nickel cobalt aluminium ternary system in positive electrode
Positive electrode etc.；Negative electrode material includes the materials such as graphite, lithium titanate.The performance of positive and negative pole material determines the basic nature of battery
Energy, especially energy density etc..The production process of positive electrode can be briefly described are as follows: by the precursor of positive electrode, i.e. metal oxygen
Change cobalt or hydroxide, such as cobalt oxide, cobaltosic oxide, cobalt hydroxide, hydroxide nickel cobalt manganese, hydroxide nickel cobalt, hydroxide
Nickel cobalt aluminium, nickel hydroxide manganese etc., after being mixed according to a certain percentage with lithium source (such as lithium carbonate, lithium hydroxide etc.), according to one
Fixed amount is packed into a ceramic saggar, is then sintered for a long time in 800~1100 DEG C of high temperature.
During firing anode material of lithium battery oxidate for lithium, in order to guarantee to contain sufficient amount in final oxide
Lithium, mostly participate in pyroreaction using excessive lithium source, alkaline oxidate for lithium has very high activity at high temperature, can be with saggar
In material reaction, the liquid phase of similar glassy state, the continuous erosion under the variation of viscosity of these liquid phase ingredients are generated under high temperature
The solid phase surface of saggar, and the stomata on saggar surface can provide channel also for these erosions, with the accumulation of time, similar glass
The alkali metal oxide of glass state is constantly permeated toward saggar depths, this channel is deeper and deeper, corrodes the impurity of generation increasingly
It is more, the eutectics mine phases such as eucryptite, lithium metasilicate, lithium aluminosilicate are generated, along with saggar passing in and out in kiln, impurity mine phase
The coefficient of expansion have a larger difference with saggar, phenomena such as peeling, cracking of the hot and cold alternation to cause saggar surface, to influence
The service life of saggar.
Application No. is the Chinese invention patents of CN201410174356.7 to disclose a kind of preparation of alkali-resistant property saggar
Method, comprising: 1) be substrate material filling sintering synthesis aluminum-spinel by anhydrous magnesium chloride and Alpha's aluminium oxide, by synthesis
The aluminum-spinel is mixed with sodium rice gamma aluminium oxide, obtains fine grained；2) by coarse granule and the fine grained according to 6:4 ratio
Example carries out grain mixture ratio mixing, coarse granule 60%, fine grained 40%, wherein the coarse granule includes electrofused mullite and electric smelting
The mixture of fused alumina zirconia；3) above-mentioned raw materials mixed are put into after squeezing out air in film band and are tightened, cohered in waterless resin
Agent acts on lower compression moulding；4) it after the blank after compression moulding being conserved preset time, carries out loading of kiln and is fired into finished product, the hair
The bright corrosion that highly basic is effective against by addition magnesium aluminate spinel.
Application No. is the Chinese invention patents of CN200910146662.9 to disclose a kind of saggar, is for manufacturing lithium ion
The saggar of the positive active material of battery contains 30 mass of mass %~70 % of spinelle, 15 matter of mass %~70 of cordierite
The % and 0 mass % of mass %~35 of mullite is measured, the original of positive active material when facilitating for firing is investigated to spinelle
The corrosion resistance of the diffusion of material.It is understood that when the containing ratio of spinelle is less than 30 mass %, for positive active material
Raw material diffusion corrosion resistance reduce.On the other hand it is believed that when the containing ratio of spinelle is more than 70 mass %, saggar
Coefficient of thermal expansion increase, be easy to happen crackle, the saggar be coefficient of thermal expansion be not higher than containing 90% or more magnesia or point it is brilliant
The composition of the saggar of stone, therefore the generation for the crackle being able to suppress in cooling process when manufacturing positive active material.
By above-mentioned record it is found that the aforementioned prior art improves saggar corrosion resistance, the design to prolong the service life is logical
It crosses control to prepare component and the content of saggar raw material to realize, however only has saggar by the component and content of saggar raw material
Standby corrosion resisting property is very limited, and is highly prone to raw material supply caused by regional difference and limits.Therefore, develop it is a kind of from
The method that saggar corrosion resistance and cracking resistance can be improved in institutional framework, and then prolonged its service life seems especially heavy
It wants.
Summary of the invention
It is in view of the shortcomings of the prior art and insufficient, the primary purpose of the present invention is that providing a kind of corrosion-resistant cracking resistance Special clay
Ceramic material, the ceramic material can be used in saggar, and are able to use the raw material being commonly easy to get and extend making for special ceramic material
Use the service life.
The specific technical solution of the present invention is as follows:
A kind of corrosion-resistant cracking resistance special ceramic material, the special ceramic material is mainly by the raw material system of following parts by weight
At: 10-20 parts of kaolin, 8-18 parts of alumina aerogels micro mists, 20-40 parts of roller stick powder, 25-35 parts of cordierite, 8-
12 parts of mullites, 2-5 parts of yellow starch gum, 4-8 parts of water.
Further, it is preferable to which the special ceramic material is mainly prepared by the raw material of following parts by weight: 15 parts of height
Ridge soil, 12 parts of alumina aerogels micro mists, 30 parts of roller stick powder, 30 parts of cordierite, 10 parts of mullites, 3 parts of yellow starch gum, 6
The water of part.
Further, preferred 50-120 μm of the partial size of the alumina aerogels micro mist, more preferable 80 μm.
Another object of the present invention, which also resides in, provides a kind of preparation method of corrosion-resistant cracking resistance special ceramic material.
A kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) weigh raw material for standby by following parts by weight: 10-20 parts of kaolin, 8-18 parts of alumina aerogels micro mists,
20-40 parts of roller stick powder, 25-35 parts of cordierite, 8-12 parts of mullites, 2-5 parts of yellow starch gum, 4-8 parts of water；
(2) above-mentioned raw materials are added in edge runner and mix 20-40min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) dry after standing the green body of step (4), then it is fired.
Further, the time of the aging processing is 10 hours or more.
Further, the technological parameter of the isothermal static pressure are as follows: in 1000-1200 DEG C of processing 30-50min.
Further, the time that the green body is stood is 10 hours or more.
Further, the temperature of the drying is 300-500 DEG C, and the time is 10 hours or more.
Further, the temperature of the firing is 1340-1380 DEG C, and the time is 6-7 hours.
Further, the method also includes special ceramic material carry out flash polishing, blow off the step of.
A kind of foregoing application of the corrosion-resistant cracking resistance special ceramic material in saggar.
After roller stick powder use herein is the aluminium oxide ceramics roller stick recovery and rinsing that will be discarded, the roller stick that crushes
Waste material powder, wherein the content (mass ratio) of aluminium oxide is 60% or so.
Alumina aerogels use herein have the characteristics that high-specific surface area, high porosity, low-density, containing big
The micropore of amount and mesoporous, thermal conductivity is low, is a kind of ideal heat-barrier material.The application selection has the aluminium oxide of specified particle size
Aeroge is that the bulk alumina aerogels grinding being prepared by supercritical drying sieves to obtain, broken tiny oxidation
Aluminium aeroge micro mist rough surface, is dispersed in special ceramic material raw material, after aging compression moulding, binder with
Its binding ability, plays the role of microskeleton in green body.Due to oxidation aeroge micro mist duct by entanglement without chapter
3 D pore canal composition, other raw materials cannot be introduced into internal gutter in mixed process, first in sintering procedure, the gas of generation
It is easy to escape from aeroge duct, big stomata will not be generated, and then be not easy to crack.Secondly, in special cermacis material
Expect recycling process, constantly heating, cooling can generate the expansion and contraction of special ceramic material, should can be by three-dimensional space
Netted aerogel structure buffering is fallen, and also very little, progress can obtain preferable thermal shock resistance to itself thermal expansion coefficient.
When carrying out anode material for lithium-ion batteries sintering, alkaline oxidate for lithium can be with the acid oxygen in special ceramic material
Compound generates LiAlO if certain chemical reaction occurs for silica, amphoteric oxide aluminum oxide2、Li4SiO4、
LiAlSiO4Etc. glassy substances.By low heat conductivity possessed by alumina aerogels and the had hair of micropore, meso-hole structure
The skin glass metallic substance that tubule effect can hinder the glassy substances of production further internally to corrode, and be formed is molten
Melt and be embedded into well in the coarse alumina aerogels surface layer on special ceramic material surface layer under state, it is strong to enhance its bonding
Degree, it is not easily to fall off, this contain lithium alumino-silicate substance in turn and can inhibit lithium ion to special ceramic material basis material into
One step corrodes, and then the corrosion resistance of special ceramic material can be improved.
Have in the application for the partial size of alumina aerogels micro mist and particularly limits preferred 50-120 μm, more preferable 80 μ
m；Its partial size is excessive, and crackle is easy to appear in program was recycled, and the service life is shorter, and partial size is too small, is unable to fully utilize it
The barrier action of three-dimensional network space structure, and then corrosion resistance and thermal shock resistance can not be improved.
Compared with prior art, the invention has the following advantages:
The present invention and adds certain partial size by adjusting the raw material components and its content of special ceramic material basis material
Three-dimensional net structure alumina aerogels micro mist is scattered in it in basis material and serves as microskeleton structure, and enhancing matrix combines
Power, and the stomata generated in sintering procedure is reduced, the stress variation in process of expansion and contraction is buffered, thermal shock resistance is improved；
In addition, the special ceramic material can also enhance with the vitreous adhesion strength of Aluminosilicates, make special ceramic material matrix material
Material is not easy to peel off and then influence the quality of lithium ion anode material, while lithium ion during sintering can also be inhibited further to invade
Erosion, is remarkably reinforced its corrosion resistance.During being applied to saggar, number height, lithium ion depth of erosion is recycled
Shallowly, consumables cost brought by replacement saggar can be reduced.
Specific embodiment
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, below to of the invention further detailed
Explanation.But following embodiments is only simple example of the invention, does not represent or limit the scope of the present invention, this
Invention protection scope is subject to claims.
Embodiment 1: a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) raw material for standby is weighed by following parts by weight: 10 parts of kaolin, 8 parts of alumina aerogels micro mists, 20 parts of roller
Stick powder, 25 parts of cordierite, 8 parts of mullites, 2 parts of yellow starch gum, 4 parts of water；The partial size of aeroge micro mist is 50 μm；
(2) above-mentioned raw materials are added in edge runner and mix 20min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing 10h；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) will step (4) green body stand 10h after be dried, dry temperature is 300 DEG C, and the dry time is
Then 10h is fired 5h at 1340 DEG C.With grinding stone polishing quadrangle, base peak, flash after firing, then blows off, obtain special cermacis
Finished material.
Embodiment 2: a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) raw material for standby is weighed by following parts by weight: 15 parts of kaolin, 12 parts of alumina aerogels micro mists, 30 parts
Roller stick powder, 30 parts of cordierite, 10 parts of mullites, 3 parts of yellow starch gum, 6 parts of water；The partial size of aeroge micro mist is 80 μm；
(2) above-mentioned raw materials are added in edge runner and mix 30min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing 12h；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) will step (4) green body stand 12h after be dried, dry temperature is 400 DEG C, and the dry time is
Then 11h is fired 6h at 1360 DEG C.With grinding stone polishing quadrangle, base peak, flash after firing, then blows off, obtain special cermacis
Finished material.
Embodiment 3: a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) raw material for standby is weighed by following parts by weight: 20 parts of kaolin, 18 parts of alumina aerogels micro mists, 40 parts
Roller stick powder, 35 parts of cordierite, 12 parts of mullites, 5 parts of yellow starch gum, 8 parts of water；The partial size of aeroge micro mist is 120 μm；
(2) above-mentioned raw materials are added in edge runner and mix 40min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing 14h；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) will step (4) green body stand 14h after be dried, dry temperature is 500 DEG C, and the dry time is
Then 12h is fired 7h at 1380 DEG C.With grinding stone polishing quadrangle, base peak, flash after firing, then blows off, obtain special cermacis
Finished material.
Embodiment 4: a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) weigh raw material for standby by following parts by weight: 15 parts of kaolin, 12 parts of alumina powders, 30 parts of roller stick powder,
30 parts of cordierite, 10 parts of mullites, 3 parts of yellow starch gum, 6 parts of water；The average grain diameter of alumina powder is 80 μm；
(2) above-mentioned raw materials are added in edge runner and mix 30min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing 12h；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) will step (4) green body stand 12h after be dried, dry temperature is 400 DEG C, and the dry time is
Then 11h is fired 6h at 1360 DEG C.With grinding stone polishing quadrangle, base peak, flash after firing, then blows off, obtain special cermacis
Finished material.
Embodiment 5: a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) raw material for standby is weighed by following parts by weight: 15 parts of kaolin, 12 parts of alumina aerogels micro mists, 30 parts
Cordierite, 10 parts of mullites, 3 parts of yellow starch gum, 6 parts of water；The partial size of aeroge micro mist is 80 μm；
(2) above-mentioned raw materials are added in edge runner and mix 30min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing 12h；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) will step (4) green body stand 12h after be dried, dry temperature is 400 DEG C, and the dry time is
Then 11h is fired 6h at 1360 DEG C.With grinding stone polishing quadrangle, base peak, flash after firing, then blows off, obtain special cermacis
Finished material.
Embodiment 6: a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, described method includes following steps:
(1) raw material for standby is weighed by following parts by weight: 15 parts of kaolin, 12 parts of alumina aerogels micro mists, 30 parts
Roller stick powder, 30 parts of cordierite, 10 parts of mullites, 3 parts of yellow starch gum, 6 parts of water；The partial size of aeroge micro mist is 200 μm；
(2) above-mentioned raw materials are added in edge runner and mix 30min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing 12h；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) will step (4) green body stand 12h after be dried, dry temperature is 400 DEG C, and the dry time is
Then 11h is fired 6h at 1360 DEG C.With grinding stone polishing quadrangle, base peak, flash after firing, then blows off, obtain special cermacis
Finished material.
The performance test of special ceramic material: Li is packed into the special ceramic material that above-described embodiment is prepared2CO3
And CoCO3, the sintering preparation cobalt acid lithium at 1000 DEG C, after keeping the temperature 20h, special ceramic material inner wall is rotten under observation different temperatures
The depth of erosion.And be recycled, until special ceramic material cracks or cannot use, record service life.It is related
Data are as shown in table 1.
The corrosion resistance and service life of 1 the application special ceramic material of table
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of corrosion-resistant cracking resistance special ceramic material, it is characterised in that the special ceramic material is mainly by following parts by weight
Raw material is made: 10-20 parts of kaolin, 8-18 parts of alumina aerogels micro mists, 20-40 parts of roller stick powder, 25-35 parts of violet are green
Stone, 8-12 part mullite, 2-5 parts of yellow starch gum, 4-8 parts of water.
2. a kind of corrosion-resistant cracking resistance special ceramic material according to claim 1, it is characterised in that the special cermacis material
Material is mainly prepared by the raw material of following parts by weight: 15 parts of kaolin, 12 parts of alumina aerogels micro mists, 30 parts of roller stick
Powder, 30 parts of cordierite, 10 parts of mullites, 3 parts of yellow starch gum, 6 parts of water.
3. a kind of corrosion-resistant cracking resistance special ceramic material according to claim 1, it is characterised in that the aluminium oxide airsetting
Preferred 50-120 μm of the partial size of glue micro mist.
4. a kind of corrosion-resistant cracking resistance special ceramic material according to claim 3, it is characterised in that the aluminium oxide airsetting
More preferable 80 μm of the partial size of glue micro mist.
5. a kind of preparation method of corrosion-resistant cracking resistance special ceramic material, it is characterised in that described method includes following steps:
(1) raw material for standby is weighed by following parts by weight: 10-20 parts of kaolin, 8-18 parts of alumina aerogels micro mists, 20-40
Roller stick powder, 25-35 parts of the cordierite, 8-12 parts of mullites, 2-5 parts of yellow starch gum, 4-8 parts of water of part；
(2) above-mentioned raw materials are added in edge runner and mix 20-40min, be then sieved, remove iron；
(3) mixed raw material that step (2) obtains is placed in sealing container and carries out aging processing；
(4) step (3) is placed in progress isothermal hydrostatic profile on pressure forming machine through the raw material of aging processing and obtains green body；
(5) dry after standing the green body of step (4), then it is fired.
6. a kind of preparation method of corrosion-resistant cracking resistance special ceramic material according to claim 5, it is characterised in that described
The time of aging processing is 10 hours or more.
7. a kind of preparation method of corrosion-resistant cracking resistance special ceramic material according to claim 5, it is characterised in that described
The time that green body is stood is 10 hours or more.
8. a kind of preparation method of corrosion-resistant cracking resistance special ceramic material according to claim 5, it is characterised in that described
Dry temperature is 300-500 DEG C, and the time is 10 hours or more.
9. a kind of preparation method of corrosion-resistant cracking resistance special ceramic material according to claim 5, it is characterised in that described
The temperature of firing is 1340-1380 DEG C, and the time is 6-7 hours.
10. a kind of application of corrosion-resistant cracking resistance special ceramic material according to any one of claims 1-4 in saggar.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851318A (en) * | 2021-01-19 | 2021-05-28 | 湖南省醴陵市兆荣瓷业有限公司 | Preparation method for improving thermal stability and strength of ceramic by permeating aerogel ultrafine powder |
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| CN109704742B (en) | 2021-11-05 |
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