CN105753459A - Preparation method and products of organic metal complex and aluminum oxide compound - Google Patents

Preparation method and products of organic metal complex and aluminum oxide compound Download PDF

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CN105753459A
CN105753459A CN201610129144.6A CN201610129144A CN105753459A CN 105753459 A CN105753459 A CN 105753459A CN 201610129144 A CN201610129144 A CN 201610129144A CN 105753459 A CN105753459 A CN 105753459A
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aluminium
hydroxyquinoline
oxide
organometallic complex
sintering
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CN105753459B (en
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陈琦
王玉来
刘彩玫
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YANGZHOU ZHONGTIANLI NEW MATERIAL Co Ltd
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YANGZHOU ZHONGTIANLI NEW MATERIAL Co Ltd
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Abstract

The invention provides organic metal complex.The organic metal complex is prepared by mixing bis(2-methyl-8-oxyquinoline-N1, O8)-(1, 1'-biphenyl-4-hydroxyl)aluminum and 8-oxychinolin aluminum, wherein the weight ratio of the bis(2-methyl-8-oxyquinoline-N1, O8)-(1, 1'-biphenyl-4-hydroxyl)aluminum and 8-oxychinolin aluminum to the 8-oxychinolin aluminum is 2-5:5-8.Atmosphere generated during high-temperature decomposition can have embedding and co-growth of certain degree, so that the growth orientation of crystals can be changed, the atomic structure on the surface of microcosmic particles can be improved, and functional material crystal structure design is achieved.When aluminum oxide compound obtained from the organic metal complex is prepared into a coating membrane, the coating membrane is outstanding in water absorption performance, and the self-discharge performance, voltage drop performance and normal-temperature circulation performance of the coating membrane are evidently better than those of a common aluminum oxide coating membrane.The preparation method of the organic metal complex is simple, practical, evident in effect, and capable of satisfying the requirements of large-scale industrial production.

Description

A kind of organometallic complex and the preparation method of alumina compound and product
Technical field
The present invention relates to dynamic lithium battery and manufacture field, especially a kind of organometallic complex and oxidation The preparation method of aluminium compound and product.
Background technology
Along with an urgent demand of new energy technology development, lithium-ion-power cell is high by specific energy density, The characteristic such as memory-less effect and relative environmental protection become new energy technology first selection, but common lithium Ion battery there is also certain potential safety hazard, is mainly manifested in thermal failure, external impacts and When falling, there is on fire or blast due to reasons such as barrier film breakages in battery.In recent years, the whole world is right Safety improvement means in lithium battery, especially dynamic lithium battery are mainly by pottery, are also with regard to alfa The methods such as phase alumina coating improve barrier film material deformation effect in the case of external force and thermal shock, to reach Purpose to safety improvement.
Common alumina material mainly has following several respects defect for power lithium battery:
1. grain structure is mainly random form is main, formed 2-4 micron thickness coating after, particle it Between there is obvious spatial joint clearance, it is impossible to preferably stop Li dendrite metal deposit growth because Reduce the effect improving lithium battery self discharge of ceramic-coated separator.
2., due to lithium battery diaphragm coating needs very thin thickness, typically within 5 micron thickness, therefore want Ask the primary granule particle diameter of aluminum oxide coating layer typically between 100-400nm.The negative issue thus brought is Submicron material has stronger water imbibition, and moisture can occur with the lithium salts in electrolyte after bringing lithium battery into Chemical reaction, the ionic conduction ability destroying lithium salts has formed HF, causes battery to produce more serious knot Structure destroys.
3. power lithium battery needs to ensure the durability of more than 10 years, therefore it is required that ceramic particle and bonding Must keep good and lasting cohesive between agent, current common alumina surface active site is relatively low, Typically significantly lost efficacy in 400-500 rear appearance of circulation, it is impossible to meet the primary demand of power lithium battery.
Therefore meet lithium battery, alfa phase alumina material that especially dynamic lithium battery security performance needs and Its preparation the most just becomes technological difficulties in the industry.
Summary of the invention
The technical problem to be solved is to provide a kind of organometallic complex.
Another technical problem to be solved by this invention is to provide applies above-mentioned organometallic complex to prepare The method of alumina compound.
Another technical problem to be solved by this invention is the product providing above-mentioned preparation method to be obtained Alumina compound.
For solving above-mentioned technical problem, the technical scheme is that
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline The mixture weight ratio of aluminium is 2-5:5-8.
Preferably, above-mentioned organometallic complex, described double (2-methyl-8-hydroxyquinoline-N1, O8)- (1,1'-biphenyl-4-hydroxyl) aluminium is 2:8 with the mixture weight ratio of 8-hydroxyquinoline aluminium.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with 8-hydroxyquinoline aluminium mixes, and to obtain final product.
The application in terms of preparing alumina compound of the above-mentioned organometallic complex, can change the life of crystal Long orientation.
According to defect (hole) mechanism of the crystal structure that practice draws, above-mentioned organic by adding in crystal Metal complex, the atmosphere that its pyrolysis process produces can occur a certain degree of in hexagonal Embed and symbiosis is long, thus change the orientation of growth of crystal, and improve the atomic structure on microscopic particles surface Composition, thus reach the purpose of functional material crystal structure design.
Preferably, the method that above-mentioned organometallic complex prepares alumina compound, concrete steps are applied For:
(1) by high-purity aluminium hydroxide micro powder by dry powder blender, with inorganic oxide additive and upper State organometallic complex be blended prepare aluminium hydroxide compound, described inorganic oxide additive for oxidation Barium, magnesia, yittrium oxide, chromium oxide, iron oxide, cesium oxide, titanium oxide, manganese oxide, silica With the one in calcium oxide or any combination, described aluminium hydroxide micro powder and inorganic oxide additive and have The consumption number of machine metal complex is aluminium hydroxide micro powder 920-970 part, inorganic oxide additive 30-60 Part, organometallic complex 10-30 part；
(2) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push-plate type and burns Knot kiln, carries out high temperature sintering, wherein, sintering temperature 1100-1300 DEG C, and single group crucible material is at sintering oven The middle time of staying is 4-8 hour, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing concentration Hot-air for 10-25% (volume ratio) carbon dioxide.
Preferably, the preparation method of above-mentioned alumina compound, in described step (1), dry powder blender is double spiral shells Rotation conical mixer.
Preferably, the preparation method of above-mentioned alumina compound, in described step (1), inorganic oxide adds Add the grain diameter of agent to be chosen at 0.8-4.0 micron grain size scope there is preferable sintering effect.
Preferably, the preparation method of above-mentioned alumina compound, in described step (1), inorganic oxide adds Add before agent uses and carry out Chemical Pretreatment, concretely comprise the following steps and inorganic oxide additive is placed on solidification bed In reactor, being passed through the steam that inorganic acid mixes with air, wherein inorganic acid is nitric acid, hydrochloric acid or sulfuric acid, The content of inorganic acid is 2.0-6.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 2.0-10.0kg/m2 Left and right, the process time in steam is 30-80min, and steam temperature is 20-50 DEG C.
The alumina compound obtained by above-mentioned preparation method, for laminated structure, radius-thickness ratio is at 8-30:1.
Described radius-thickness ratio uses crystal optics method to be measured, and the method is with spindle stage and polarized light microscopy Mirror measures radius-thickness ratio: be first bonded on the needle point of spindle stage by sheet-like particle powder, then by rotary needle Platform is fixed on petrographic microscope objective table；Subsequently rotate needle handle to be set level by particle, first measure horizontal Particle diameter under state；Finally rotate needle handle 90 degree, measure grain thickness.Thus obtain particle diameter and thickness, Finally calculate radius-thickness ratio.
The invention has the beneficial effects as follows:
Above-mentioned organometallic complex, the atmosphere produced in pyrolysis process can be sent out in hexagonal Raw a certain degree of embedding and symbiosis are long, thus change the orientation of growth of crystal, and improve microscopic particles table The atomic structure composition in face, thus reach the purpose of functional material crystal structure design, organic by this After the alumina compound that metal complex is obtained makes coating, barrier film water absorbing properties highlights, and is certainly putting Electricity aspect, voltage drop and normal-temperature circulating performance aspect are substantially better than common aluminum oxide coating layer barrier film, its system Preparation Method is simple and practical, and effect is notable, is suitable for the needs that large-scale industrial produces.
Accompanying drawing explanation
Fig. 1 is the alumina powder pattern SEM contrast after shaping；
Fig. 2 is the coated separator made by alumina compound of the present invention, and common commercialization pottery The water imbibition contrast of barrier film (common aluminum oxide coating layer), wherein, A is alumina composite of the present invention Thing coating, B is commercial alumina coating；
Fig. 3 is the capacity attenuation test comparison figure after alumina compound prepares battery；
Fig. 4 is the self discharge test comparison figure after alumina compound prepares battery.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline The mixture weight ratio of aluminium is 2:8.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with 8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 2
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline The mixture weight ratio of aluminium is 5:5.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with 8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 3
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline The mixture weight ratio of aluminium is 2:5.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with 8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 4
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline The mixture weight ratio of aluminium is 5:8.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with 8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 5
A kind of organometallic complex, by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) Aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) Composition, described double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline The mixture weight ratio of aluminium is 3:7.
The preparation method of above-mentioned organometallic complex, specifically comprises the following steps that
(1) double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium is weighed by prescription amount It is raw material with 8-hydroxyquinoline aluminium；
(2) by double (2-methyl-8-hydroxyquinoline-N1, O8)-(1,1'-biphenyl-4-hydroxyl) aluminium of weighing with 8-hydroxyquinoline aluminium mixes, and to obtain final product.
Embodiment 6
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the magnesia of 4:4:1:1, calcium oxide, yittrium oxide, cesium oxide, logical Crossing machinery powder mixing apparatus to carry out being simply mixed uniformly, wherein, the grain diameter of each inorganic oxide exists In the range of 1-3 micron grain size；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide Powder is placed in fixed bedreactor, is passed through the steam that nitric acid mixes with air, wherein the containing of nitric acid Amount is 3.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 3.0-4.0kg/m2, in steam The process time is 60min, between steam temperature about 40 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 950 is taken by weight Organometallic complex described in part, the inorganic oxide mixture 35 parts of step (2) gained, embodiment 1 15 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1200 DEG C, and single group crucible material is at sintering In kiln, the time of staying is 6 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense Degree is the hot-air of 20% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack, Make finished product.
Utilizing laser fineness gage to detect finished product, result is as it is shown in figure 1, in bimodal distribution.
Embodiment 7
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the barium monoxide of 5:3:2, chromium oxide, iron oxide, by machinery powder Mixing apparatus carries out being simply mixed uniformly, and wherein, the grain diameter of each inorganic oxide is at 0.8-4.0 micron In particle size range；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide Powder is placed in fixed bedreactor, is passed through the steam that hydrochloric acid mixes with air, wherein the containing of hydrochloric acid Amount is 6.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 2.0-5.0kg/m2, in steam The process time is 30min, between steam temperature about 50 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 920 is taken by weight Organometallic complex described in part, the inorganic oxide mixture 60 parts of step (2) gained, embodiment 1 30 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1100 DEG C, and single group crucible material is at sintering In kiln, the time of staying is 8 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense Degree is the hot-air of 10% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack, Make finished product.
Embodiment 8
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the magnesia of 4:2:1, titanium oxide, silica, by machinery powder Mixing apparatus carries out being simply mixed uniformly, and wherein, the grain diameter of each inorganic oxide is at 2-4 micron grain size In the range of；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide Powder is placed in fixed bedreactor, is passed through the steam that sulfuric acid mixes with air, wherein the containing of sulfuric acid Amount is 2.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 7.0-10.0kg/m2, in steam The process time is 80min, between steam temperature about 20 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 970 is taken by weight Organometallic complex described in part, the inorganic oxide mixture 30 parts of step (2) gained, embodiment 1 10 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1300 DEG C, and single group crucible material is at sintering In kiln, the time of staying is 4 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense Degree is the hot-air of 25% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack, Make finished product.
Embodiment 9
A kind of alumina compound, preparation method is as follows:
(1) choosing mol ratio is the magnesia of 7:3, manganese oxide, is carried out by machinery powder mixing apparatus Being simply mixed uniformly, wherein, the grain diameter of each inorganic oxide is in the range of 2-3 micron grain size；
(2) mixed powder is carried out Chemical Pretreatment: mixed by above-mentioned mixed inorganic oxide Powder is placed in fixed bedreactor, is passed through the steam that nitric acid mixes with air, wherein the containing of nitric acid Amount is 4.0% (wt), and the inorganic oxide placement amount on solidification bed surface is at 4.0-7.0kg/m2, in steam The process time is 70min, between steam temperature about 35 DEG C；
(3) high-purity hydrogen alumina powder (commercially available, purity is more than 99.9%) 940 is taken by weight Organometallic complex described in part, the inorganic oxide mixture 45 parts of step (2) gained, embodiment 1 20 parts, after mixture, use dry powder blender (double helix conical mixer) mechanical mixture uniform；
(4) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push pedal Formula sintering oven, carries out high temperature sintering, wherein, sintering temperature about 1200 DEG C, and single group crucible material is at sintering In kiln, the time of staying is 6 hours, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing dense Degree is the hot-air of 15% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than-40 DEG C), nanon ball-mill is used to carry out solid abrasive, will Step (4) gained powder grind 4-6 hour, be ground to D50 < within 1.2um, discharging, pack, Make finished product.
Below in conjunction with concrete test example, the present invention is described in detail.
Aluminum oxide coating layer prepares power lithium battery application test
Select alumina compound, water, polyacrylate (adhesive), polycarboxylic acids described in embodiment 6 (dispersant) and analyze pure propyl alcohol (wetting agent), described alumina compound, water, polyacrylic acid The weight ratio of the pure propyl alcohol of ester, polycarboxylic acids and analysis is 40:50:4:1:0.5, by the way of high speed dispersion, and system Becoming the aluminum oxide glue of 50% solid content, viscosity is at 50-80CP, by the coating of micro-gravure coater one side Mode, applies twice at Asahi Chemical Industry's PE12um matrix surface, forms the aluminum oxide coating layer of each 4um in two sides, Barrier film gross thickness 20um；
Choosing the most extremely ternary material, negative pole is the 30AH standard lithium battery of modified graphite, uses above-mentioned The double-surface ceramics barrier film (12um matrix, two sides each 4um coating) of coated separator and common commercial is carried out Contrast test.
Test shows:
As in figure 2 it is shown, alumina composite material prepared by the present invention, after making coating, hence it is evident that micro- See and be different from commercially available common alumina material (double-surface ceramics barrier film), after measured, averagely in architectural feature Radius-thickness ratio is 16:1, and common commercial alumina is irregularly shaped, and radius-thickness ratio is between 1:1-2.4:1.
And as can be seen from Table 1, coated separator water imbibition is substantially better than common aluminum oxide coating layer； It addition, at ternary material (nickel cobalt manganese molar ratio 5:2:3) as positive pole, modifying natural graphite material Battery evaluation is carried out as (energy density is 480wh/L) in the 30Ah square aluminum housing battery of negative pole. such as figure Shown in 3 and Fig. 4, after making dynamic lithium battery, in terms of self discharge, use barrier film of the present invention every In regulation ageing time, (7 days) voltage reduces to 6.02 millivolts to film battery, and control cell is at 9.32 millivolts, Keeping battery voltage performance made by this patent is substantially better than common aluminum oxide coating layer barrier film；Final battery is normal Temperature cycle performance is also significantly better than the battery of common aluminum oxide coating layer barrier film, made by barrier film of the present invention Circulating battery 600 times, capability retention about 87%, control cell capacity then less than 80%, And rapid corruptions occurs.
Table 1 moisture entrapment content balance
Described test specimen refers to alumina composite material of the present invention；Reference sample refers to commercially available common Alumina material.
Above-mentioned with reference to embodiment to this for the alumina compound applying dynamic lithium battery and preparation method thereof The detailed description carried out, is illustrative rather than determinate, if can according to restriction scope list Dry embodiment, therefore changing and modifications under without departing from present general inventive concept, should belong to the present invention's Within protection domain.

Claims (7)

1. an organometallic complex, it is characterised in that: by double (2-methyl-8-hydroxyquinoline-N1, O8)- (1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline aluminium composition, described double (2-methyl-8-hydroxyquinolines -N1, O8) the mixture weight ratio of-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline aluminium is 2-5:5-8.
Organometallic complex the most according to claim 1, it is characterised in that: described double (2- Methyl-8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'-biphenyl-4-hydroxyl) aluminium and 8-hydroxyquinoline aluminium For 2:8.
3. the application in terms of preparing alumina compound of the organometallic complex described in claim 1, The orientation of growth of crystal can be changed.
4., by the application of organometallic complex described in claim 3, prepare the side of alumina compound Method, it is characterised in that: concretely comprise the following steps:
(1) by high-purity aluminium hydroxide micro powder by dry powder blender, with inorganic oxide additive and upper State organometallic complex be blended prepare aluminium hydroxide compound, described inorganic oxide additive for oxidation Barium, magnesia, yittrium oxide, chromium oxide, iron oxide, cesium oxide, titanium oxide, manganese oxide, silica With the one in calcium oxide or any combination, described aluminium hydroxide micro powder and inorganic oxide additive and have The consumption number of machine metal complex is aluminium hydroxide micro powder 920-970 part, inorganic oxide additive 30-60 Part, organometallic complex 10-30 part；
(2) the aluminium hydroxide compound mixed is placed in alumina ceramic crucible, enters push-plate type and burns Knot kiln, carries out high temperature sintering, wherein, sintering temperature 1100-1300 DEG C, and single group crucible material is at sintering oven The middle time of staying is 4-8 hour, and sintering process is carried out in the environment of airtight, and sintering atmosphere is containing concentration Hot-air for 10-25% (v/v) carbon dioxide.
The preparation method of alumina compound the most according to claim 4, it is characterised in that: described In step (1), the grain diameter of inorganic oxide additive is chosen at 0.8-4.0 micron grain size scope and has relatively Good sintering effect.
The preparation method of alumina compound the most according to claim 4, it is characterised in that: described In step (1), inorganic oxide additive carries out Chemical Pretreatment before using, and concretely comprises the following steps inorganic oxygen Compound additive is placed in fixed bedreactor, is passed through the steam that inorganic acid mixes, Qi Zhongwu with air Machine acid is nitric acid, hydrochloric acid or sulfuric acid, and the content of inorganic acid is 2.0-6.0% (wt), solidifies the inorganic of bed surface Oxide placement amount is at 2.0-10.0kg/m2Left and right, the process time in steam is 30-80min, steam temperature Degree is for 20-50 DEG C.
7. the alumina compound obtained by the described preparation method of one of claim 4-6, it is characterised in that: In the form of sheets, radius-thickness ratio is between 8-30:1.
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CN110379984A (en) * 2018-04-13 2019-10-25 通用汽车环球科技运作有限责任公司 Partition for lithium metal base battery group
CN111192992A (en) * 2020-01-20 2020-05-22 武汉中兴创新材料技术有限公司 Preparation method and device of ultrathin coating diaphragm
CN115445304A (en) * 2022-07-29 2022-12-09 扬州中天利新材料股份有限公司 High-purity magnesium oxide production is with electric pressure release all-in-one of straining

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EP1621519A1 (en) * 2004-07-28 2006-02-01 SOLVAY (Société Anonyme) Alkaline - earth metal carbonate core coated with at least one Group IV transition metal compound
CN101694866A (en) * 2009-09-22 2010-04-14 昆山维信诺显示技术有限公司 Organic electroluminescence device
CN104064677A (en) * 2013-03-21 2014-09-24 海洋王照明科技股份有限公司 Organic electroluminescent device and preparation method thereof

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EP1621519A1 (en) * 2004-07-28 2006-02-01 SOLVAY (Société Anonyme) Alkaline - earth metal carbonate core coated with at least one Group IV transition metal compound
CN101694866A (en) * 2009-09-22 2010-04-14 昆山维信诺显示技术有限公司 Organic electroluminescence device
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* Cited by examiner, † Cited by third party
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CN110379984A (en) * 2018-04-13 2019-10-25 通用汽车环球科技运作有限责任公司 Partition for lithium metal base battery group
CN111192992A (en) * 2020-01-20 2020-05-22 武汉中兴创新材料技术有限公司 Preparation method and device of ultrathin coating diaphragm
CN115445304A (en) * 2022-07-29 2022-12-09 扬州中天利新材料股份有限公司 High-purity magnesium oxide production is with electric pressure release all-in-one of straining

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