CN114031380A - Preparation method of alumina-zirconia ceramic sagger - Google Patents

Preparation method of alumina-zirconia ceramic sagger Download PDF

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CN114031380A
CN114031380A CN202111273606.9A CN202111273606A CN114031380A CN 114031380 A CN114031380 A CN 114031380A CN 202111273606 A CN202111273606 A CN 202111273606A CN 114031380 A CN114031380 A CN 114031380A
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alumina
equal
zirconia
sagger
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张拯
李延超
魏少西
雷复兴
马文鹏
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Luoyang Ceramtech Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/101—Refractories from grain sized mixtures
    • C04B35/106—Refractories from grain sized mixtures containing zirconium oxide or zircon (ZrSiO4)
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111—Fine ceramics
    • C04B35/117—Composites
    • C04B35/119—Composites with zirconium oxide
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/77—Density
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

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  • Ceramic Engineering (AREA)
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  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Composite Materials (AREA)

Abstract

A preparation method of an alumina-zirconia ceramic sagger relates to the field of high-temperature ceramics, and Al is added according to the mass percentage2O355-65% of alumina and ZrO in an amount of not less than 98.5wt%2+Y2O315-25% by weight of stabilized zirconia of not less than 99.5% by weight, ZrO2More than or equal to 99.5wt% of monoclinic zirconia 10-15% and additives 10-15% are added into a ball mill or a stirring mill according to the proportion, then an aqueous solution with the total amount of raw materials of 35-50% is added, mixed milling is carried out for 4-6 hours, slurry is prepared, a spray granulator is used for preparing granules, the granules are filled into a rubber mould, the mould is placed into an isostatic press for compression molding, and a molded blank is sintered at 1450-1550 ℃; the bulk density of the compact ceramic sagger manufactured by the invention is 4.3-4.5 g/cm3The apparent porosity is less than or equal to 0.1 percent, and the normal-temperature flexural strength is more than or equal to 400 mpa; the sagger is corrosion-resistant, impermeable, non-stick and non-slag-falling in the high-temperature use process, and can be used for calcining any lithium battery anode with super-strong corrosivityA material.

Description

Preparation method of alumina-zirconia ceramic sagger
Technical Field
The invention relates to the field of high-temperature ceramics, in particular to a preparation method of an alumina-zirconia ceramic sagger.
Background
The ceramic sagger is a key high-temperature container for calcining the anode material in the lithium battery industry, and the requirement on the ceramic sagger is higher and higher along with the development of the lithium battery. The development trend of the lithium battery industry is represented by (1) high-end quality requirements: firstly, the positive electrode material develops towards high nickel lithium salt, and the sagger is required to have higher erosion resistance; secondly, the purity of the material is improved, and the sagger is required not to pollute the material, stick the material and peel off and drop slag; thirdly, the uniformity of the material calcination temperature is improved, and the wall thickness of the sagger is required to be as thin as possible; (2) the automatic operation requirements are as follows: the mechanical arm is used for clamping and grabbing the saggar, so that the requirements on the strength, the overall dimension and the weight of the wall of the saggar are more strict; (3) the energy consumption requirement is as follows: the sagger is required to be thin-walled and light in weight so as to reduce the heat storage capacity of the sagger; (4) the raw material saving requirement is as follows: the high density of the saggar is required to minimize the penetration of the positive electrode material into the saggar. However, at present, saggars and crucibles are formed by a mechanical pressing method in China, so that the quality of the saggars and the crucibles is very poor; the main performance is as follows: (1) the volume density uniformity is very poor, so that the internal structure is locally loose, and the strength, the high temperature resistance, the erosion resistance and the service life of the composite material greatly fluctuate; (2) the sagger has large wall thickness, heavy weight, large heat storage capacity and large energy consumption; (3) the surface is rough, the material is easy to stick, the slag is easy to peel off, and the cleanliness of the lithium battery raw material is directly polluted. Therefore, the performance of the ceramic sagger produced in China at present cannot meet the requirement of high-end lithium battery materials.
Disclosure of Invention
In order to overcome the defects in the background art, the invention discloses a preparation method of an alumina-zirconia ceramic sagger.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of an alumina-zirconia ceramic sagger comprises the following specific operation steps:
(1) and the raw material ratio is as follows:
according to mass percent, Al2O355-65% of alumina and ZrO in an amount of not less than 98.5wt%2+Y2O315-25% by weight of stabilized zirconia of not less than 99.5% by weight, ZrO2More than or equal to 99.5wt% of monoclinic zirconia 10-15 wt%, and additive 10-15 wt%％；
(2) And preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to a ratio, adding an aqueous solution accounting for 35-50% of the total amount of the raw materials, and carrying out mixed milling for 4-6 hours to prepare slurry;
wherein the aqueous solution contains a bonding agent, and the addition amount of the bonding agent is 0.1-0.4% of the amount of the aqueous solution;
(3) and spray granulation:
preparing the prepared slurry into granulating materials through a spray granulator, wherein the granulating materials are spherical particles;
(4) and isostatic pressing:
putting the granulated material into a rubber mold, and then putting the mold into an isostatic press for pressure forming, wherein the forming pressure is 120-180 mpa;
(5) and firing:
and (3) firing the formed blank at 1450-1550 ℃, wherein the heat preservation time is 4-6 hours.
In the preparation method of the alumina-zirconia ceramic sagger, in the step (1), the alumina crystal phase composition is more than or equal to 90 percent, and the granularity D is90Less than or equal to 3 mu m; the stable zirconia crystal phase has a tetragonal phase more than or equal to 80 percent and a particle size D90Less than or equal to 3 mu m; the monoclinic zirconia crystal phase comprises a monoclinic phase of more than or equal to 90 percent and a granularity D90≤3μm。
In the preparation method of the alumina-zirconia ceramic sagger, the additive in the step (1) adopts any one of calcium silicate, magnesium silicate, lithium metasilicate or yttrium titanate synthesized by high-temperature calcination of high-purity raw materials; the calcium silicate is prepared by mixing and calcining high-purity quartz powder and calcium carbonate powder; the magnesium silicate is prepared by mixing and calcining high-purity quartz powder and magnesium carbonate powder; the lithium metasilicate is prepared by mixing and calcining high-purity quartz powder and lithium hydroxide powder; the yttrium titanate is prepared by mixing high-purity titanium dioxide powder and yttrium oxide powder and then calcining.
In the preparation method of the alumina-zirconia ceramic sagger, the binding agent in the step (2) is any one of polyvinyl alcohol, gum arabic or pyrrolidone.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. the preparation method of the alumina-zirconia ceramic sagger adopts high-purity raw materials to synthesize calcium silicate, magnesium silicate, lithium metasilicate and yttrium titanate by high-temperature calcination, and the additive can be partially decomposed at high temperature to form SiO2、MgO、CaO、Li2O、Y2O3、TiO2Etc. which not only have good combustion-supporting effect on the product, but also can react with Al2O3Reacting to form small amounts of compounds having low coefficients of thermal expansion, e.g. aluminum titanate (Al)2O3·TiO2) Eucryptite (LiAlSiO)4) Etc. in which SiO is free2Can be reacted with Al2O3The reaction produces mullite (Al) with low thermal expansion coefficient2O3·SiO2) (ii) a Thus free SiO in the product2The content is very low, the corrosion resistance is not greatly influenced, and the thermal shock stability of the product is favorably improved.
2. According to the preparation method of the alumina-zirconia ceramic sagger, the granulating material is spherical particles, so that the fluidity is very good, and the uniformity of the density of a formed blank body is facilitated; the density consistency of the formed blank body can be ensured by adopting isostatic pressing, so that various properties of the product also have good consistency; and the wall thickness of the sagger product is easy to control, and the sagger product with any wall thickness can be formed.
3. The invention relates to a preparation method of an alumina-zirconia ceramic sagger, which comprises the following raw material requirements: a. the strong base corrosion resistance is good: the aluminum oxide and the zirconium oxide belong to neutral materials, and particularly, the zirconium oxide is non-wetting and non-bonding to an alkaline melt and has super-strong corrosion resistance; b. the requirement of chemical purity is as follows: impurities in the material (e.g. SiO)2、Fe2O3、Na2O、K2O, etc.) may reduce its corrosion resistance; c. the crystal phase composition requires that: the alumina is mainly high-temperature alpha phase, and the tetragonal phase and the monoclinic phase of the zirconia generate martensite phase transformation at high temperature, so that the toughening effect is generated on the alumina to form zirconia toughened alumina ceramic (ZTA); d. the granularity requirement is as follows: requires the powder to be at high temperatureAnd a certain amount of shrinkage is generated in the sintering process, so that the product is densified to form dense ceramic with the porosity of almost 0, and the product has excellent properties of permeation resistance and corrosion resistance.
4. According to the preparation method of the alumina-zirconia ceramic sagger, the volume density of the compact ceramic sagger prepared by the invention is 4.3-4.5 g/cm3The apparent porosity is less than or equal to 0.1 percent, and the normal-temperature flexural strength is more than or equal to 400 mpa; the sagger is corrosion resistant, impermeable, non-stick and non-slag-falling in the high-temperature use process, and can be used for calcining any lithium battery anode material with super-strong corrosivity.
Detailed Description
The present invention will be explained in detail by the following examples, which are disclosed for the purpose of protecting all technical improvements within the scope of the present invention.
The preparation method of the alumina-zirconia ceramic sagger comprises the following specific operation steps:
(1) and the raw material ratio is as follows:
according to mass percent, Al2O355-65% of alumina and ZrO in an amount of not less than 98.5wt%2+Y2O315-25% by weight of stabilized zirconia of not less than 99.5% by weight, ZrO2More than or equal to 99.5wt% of monoclinic zirconia 10-15% and additive 10-15%;
the alumina crystal phase composition is alpha more than or equal to 90 percent, and the granularity D90Less than or equal to 3 mu m; the stable zirconia crystal phase has a tetragonal phase more than or equal to 80 percent and a particle size D90Less than or equal to 3 mu m; the monoclinic zirconia crystal phase comprises a monoclinic phase of more than or equal to 90 percent and a granularity D90≤3μm；
The additive is any one of calcium silicate, magnesium silicate, lithium metasilicate or yttrium titanate synthesized by high-purity raw materials through high-temperature calcination; the additive is any one of calcium silicate, magnesium silicate, lithium metasilicate or yttrium titanate synthesized by high-purity raw materials through high-temperature calcination; the calcium silicate is prepared by mixing and calcining high-purity quartz powder and calcium carbonate powder; the magnesium silicate is prepared by mixing and calcining high-purity quartz powder and magnesium carbonate powder; the lithium metasilicate is prepared by mixing and calcining high-purity quartz powder and lithium hydroxide powder; the yttrium titanate is formed by mixing and calcining high-purity titanium dioxide powder and yttrium oxide powder;
(2) and preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to a ratio, adding an aqueous solution accounting for 35-50% of the total amount of the raw materials, and carrying out mixed milling for 4-6 hours to prepare slurry; wherein the aqueous solution contains a bonding agent, and the addition amount of the bonding agent is 0.1-0.4% of the amount of the aqueous solution; the binder is any one of polyvinyl alcohol, gum arabic or pyrrolidone;
(3) and spray granulation:
preparing the prepared slurry into granulating materials through a spray granulator, wherein the granulating materials are spherical particles;
(4) and isostatic pressing:
putting the granulated material into a rubber mold, and then putting the mold into an isostatic press for pressure forming, wherein the forming pressure is 120-180 mpa;
(5) and firing:
and (3) firing the formed blank at 1450-1550 ℃, wherein the heat preservation time is 4-6 hours.
Example 1
The preparation method of the alumina-zirconia ceramic sagger comprises the following specific operation steps:
the main raw materials and requirements (see table below):
Figure BDA0003328656420000051
Figure BDA0003328656420000061
(1) the mixture ratio (mass percent):
55% of alumina, 20% of stabilized zirconia, 15% of monoclinic zirconia and 10% of calcium silicate;
(2) and preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to a ratio, adding 40% of water solution containing a binding agent, and carrying out mixed milling for 4 hours to prepare slurry; the binding agent is polyvinyl alcohol, and the addition amount of the binding agent is 0.4%;
(3) and spray granulation:
and (4) preparing the prepared slurry into granules by a spray granulator.
(4) And isostatic pressing:
and (3) filling the granulated material into a rubber mold, and putting the rubber mold into an isostatic press for pressure forming, wherein the forming pressure is 120 mpa.
(5) And firing:
and sintering the formed blank at 1550 ℃ for 4 hours.
Example 2
The preparation method of the alumina-zirconia composite ceramic sagger is characterized by comprising the following steps:
the main raw materials and requirements (see table below):
Figure BDA0003328656420000062
Figure BDA0003328656420000071
(1) the mixture ratio (mass percent):
65% of alumina, 15% of stabilized zirconia, 10% of monoclinic zirconia and 10% of added magnesium silicate;
(2) and preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to a ratio, adding 50% of aqueous solution containing a binding agent, and carrying out mixed milling for 5 hours to prepare slurry; the binding agent is pyrrolidone, and the addition amount of the binding agent is 0.1%;
(3) and spray granulation: preparing the prepared slurry into granules by a spray granulator;
(4) and isostatic pressing: and (3) filling the granulated material into a rubber mold, and putting the rubber mold into an isostatic press for pressure forming, wherein the forming pressure is 140 mpa.
(5) And firing: and sintering the formed blank at 1520 ℃ for 5 hours.
Example 3
The preparation method of the alumina-zirconia composite ceramic sagger is characterized by comprising the following steps:
the main raw materials and requirements (see table below):
name of raw materials Chemical composition in wt% Crystal phase composition% Particle size, μm
Alumina oxide Al2O3≥98.5 α≥90 D90≤3
Stabilized zirconia ZrO2+Y2O3≥99.5 Tetragonal phase is greater than or equal to 80 D90≤3
Monoclinic zirconia ZrO2≥99.5 Monoclinic phase is more than or equal to 90 D90≤2
(1) The mixture ratio (mass percent):
58% of alumina, 18% of stabilized zirconia, 12% of monoclinic zirconia and 12% of lithium metasilicate;
(2) and preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to a ratio, adding 35% of water solution containing a binding agent, and carrying out mixed milling for 5 hours to prepare slurry; the binder is gum arabic, and the addition amount of the binder is 0.2%.
(3) And spray granulation: preparing the prepared slurry into granules by a spray granulator;
(4) and isostatic pressing: putting the granulated material into a rubber mold, and putting the rubber mold into an isostatic press for pressure forming, wherein the forming pressure is 160 mpa;
(5) and firing: the formed green body is sintered at 1480 ℃ and the heat preservation time is 4 hours.
Example 4
The preparation method of the alumina-zirconia composite ceramic sagger is characterized by comprising the following steps:
the main raw materials and requirements (see table below):
name of raw materials Chemical composition in wt% Crystal phase composition% Particle size, μm
Alumina oxide Al2O3≥98.5 α≥90 D90≤3
Stabilized zirconia ZrO2+Y2O3≥99.5 Tetragonal phase is greater than or equal to 80 D90≤3
Monoclinic zirconia ZrO2≥99.5 Monoclinic phase is more than or equal to 90 D90≤2
(1) The mixture ratio (mass percent):
56% of aluminum oxide, 16% of stabilized zirconia, 13% of monoclinic zirconia and 15% of yttrium titanate;
(2) and preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to the proportion, adding 55 percent of water solution containing a binding agent, and carrying out mixed milling for 6 hours to prepare slurry; the binding agent is polyvinyl alcohol, and the addition amount of the binding agent is 0.3%.
(3) And spray granulation: preparing the prepared slurry into granules by a spray granulator;
(4) and isostatic pressing: putting the granulated material into a rubber mold, and putting the rubber mold into an isostatic press for pressure forming, wherein the forming pressure is 180 mpa;
(5) and firing: the formed green body is sintered at 1450 ℃ and the heat preservation time is 6 hours.
Examples 1 to 4 firing the resulting sintered pellets to give bulk densities of 4.3 to 4.5g/cm3The apparent porosity is less than or equal to 0.1 percent, and the normal-temperature rupture strength is more than or equal to 400 mpa.
The present invention is not described in detail in the prior art.
The embodiments selected for the purpose of disclosing the invention, are presently considered to be suitable, it being understood, however, that the invention is intended to cover all variations and modifications of the embodiments which fall within the spirit and scope of the invention.

Claims (4)

1. A preparation method of an alumina-zirconia ceramic sagger is characterized by comprising the following steps: the specific operation steps are as follows:
(1) and the raw material ratio is as follows:
according to mass percent, Al2O355-65% of alumina and ZrO in an amount of not less than 98.5wt%2+Y2O315-25% by weight of stabilized zirconia of not less than 99.5% by weight, ZrO2More than or equal to 99.5wt% of monoclinic zirconia 10-15% and additive 10-15%;
(2) and preparing slurry:
adding the raw materials into a ball mill or a stirring mill according to a ratio, adding an aqueous solution accounting for 35-50% of the total amount of the raw materials, and carrying out mixed milling for 4-6 hours to prepare slurry;
wherein the aqueous solution contains a bonding agent, and the addition amount of the bonding agent is 0.1-0.4% of the amount of the aqueous solution;
(3) and spray granulation:
preparing the prepared slurry into granulating materials through a spray granulator, wherein the granulating materials are spherical particles;
(4) and isostatic pressing:
putting the granulated material into a rubber mold, and then putting the mold into an isostatic press for pressure forming, wherein the forming pressure is 120-180 mpa;
(5) and firing:
and (3) firing the formed blank at 1450-1550 ℃, wherein the heat preservation time is 4-6 hours.
2. The method of making an alumina-zirconia ceramic sagger as claimed in claim 1, wherein: in the step (1), the alumina crystal phase composition is more than or equal to 90 percent, and the granularity D90Less than or equal to 3 mu m; the stable zirconia crystal phase has a tetragonal phase more than or equal to 80 percent and a particle size D90Less than or equal to 3 mu m; the monoclinic zirconia crystal phase comprises a monoclinic phase of more than or equal to 90 percent and a granularity D90≤3μm。
3. The method of making an alumina-zirconia ceramic sagger as claimed in claim 1, wherein: in the step (1), the additive is any one of calcium silicate, magnesium silicate, lithium metasilicate or yttrium titanate synthesized by high-temperature calcination of a high-purity raw material; the calcium silicate is prepared by mixing and calcining high-purity quartz powder and calcium carbonate powder; the magnesium silicate is prepared by mixing and calcining high-purity quartz powder and magnesium carbonate powder; the lithium metasilicate is prepared by mixing and calcining high-purity quartz powder and lithium hydroxide powder; the yttrium titanate is prepared by mixing high-purity titanium dioxide powder and yttrium oxide powder and then calcining.
4. The method of making an alumina-zirconia ceramic sagger as claimed in claim 1, wherein: the binding agent in the step (2) is any one of polyvinyl alcohol, gum arabic and pyrrolidone.
CN202111273606.9A 2021-10-29 2021-10-29 Preparation method of alumina-zirconia ceramic sagger Pending CN114031380A (en)

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CN208419627U (en) * 2018-07-16 2019-01-22 江西微纳特电瓷有限公司 A kind of Special saggar for lithium battery cathode material
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102914165A (en) * 2012-10-22 2013-02-06 江苏三恒高技术窑具有限公司 High-stability long-service-life sagger for roasting lithium battery anode material and manufacturing method
CN208419627U (en) * 2018-07-16 2019-01-22 江西微纳特电瓷有限公司 A kind of Special saggar for lithium battery cathode material
CN112028650A (en) * 2020-09-03 2020-12-04 深圳市飞粤新材料科技有限公司 Sagger for lithium ion battery anode material

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Application publication date: 20220211