CN105753459B - The preparation method and product of a kind of organometallic complex and alumina compound - Google Patents

The preparation method and product of a kind of organometallic complex and alumina compound Download PDF

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CN105753459B
CN105753459B CN201610129144.6A CN201610129144A CN105753459B CN 105753459 B CN105753459 B CN 105753459B CN 201610129144 A CN201610129144 A CN 201610129144A CN 105753459 B CN105753459 B CN 105753459B
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aluminium
organometallic complex
oxide
inorganic oxide
hydroxyquinoline
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CN105753459A (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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Abstract

The present invention provides a kind of organometallic complexs, are 25 by weight by bis- (2 methyl 8 oxyquinoline N1, O8) (1,1' biphenyl, 4 hydroxyl) aluminium and 8 hydroxyquinoline aluminums：58 mixtures form, a degree of insertion can occur in hexagonal in the atmosphere that pyrolysis process generates and symbiosis is long, to change the orientation of growth of crystal, and improve the atomic structure composition on microscopic particles surface, to achieve the purpose that functional material crystal structure designs, after coating is made in the alumina compound obtained by the organometallic complex, diaphragm water absorbing properties protrude, in terms of self discharge, it is substantially better than common aluminum oxide coating layer diaphragm in terms of voltage drop and normal-temperature circulating performance, preparation method is simple and practical, significant effect, it is suitble to the needs of scale industrial production.

Description

The preparation method and product of a kind of organometallic complex and alumina compound
Technical field
The present invention relates to dynamic lithium battery manufacturing field, especially a kind of organometallic complex and alumina compound Preparation method and product.
Background technology
With an urgent demand that new energy technology develops, lithium-ion-power cell is high by specific energy density, memoryless effect Answer and the characteristics such as relatively environment-friendly become the first choice of new energy technology, but common lithium-ion-power cell there is also Some potential safety problems, is mainly manifested in thermal failure, external impacts and when falling, and battery is due to originals such as diaphragm breakages Because on fire or explosion occurs.In recent years, the whole world is mainly logical for the safety improvement means of lithium battery, especially dynamic lithium battery Ceramics are crossed, and diaphragm is improved with regard to the methods of alfa phase aluminas coating and is imitated in external force and the material deformation of thermal shock Fruit, to achieve the purpose that safety improvement.
Common alumina material mainly has following several respects defect for power lithium battery：
1. grain structure is mainly based on random form, exist after forming the coating of 2-4 micron thickness, between particle apparent Spatial joint clearance, the growth of Li dendrite metal deposit cannot be preferably prevented, because reducing changing for ceramic-coated separator The effect of kind lithium battery self discharge.
2. due to lithium battery diaphragm coating needs very thin thickness, generally within 5 micron thickness, therefore it is required that aluminium oxide applies The primary granule particle diameter of layer is generally between 100-400nm.Thus the negative issue brought is submicron material with stronger Water imbibition, moisture can chemically react after bringing lithium battery into the lithium salts in electrolyte, destroy the ionic conductivity of lithium salts HF has been formed, has caused battery to generate more serious structure and destroys.
3. power lithium battery needs to ensure 10 years or more durabilities, therefore it is required that must between ceramic particle and adhesive Good and lasting adhesiveness must be kept, current common aluminium oxide surface-active point is relatively low, generally after cycle 400-500 times There is apparent failure, the primary demand of power lithium battery cannot be met.
Therefore meet the alfa phase aluminas material and its preparation that lithium battery, especially dynamic lithium battery security performance need Also just become technological difficulties in the industry.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of organometallic complex.
Another technical problem to be solved by this invention is to provide prepares aluminium oxide using above-mentioned organometallic complex The method of compound.
Another technical problem to be solved by this invention is to provide the product that above-mentioned preparation method is obtained --- oxidation Aluminium compound.
In order to solve the above technical problems, the technical scheme is that：
A kind of organometallic complex, by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) composition, bis- (2- first Base -8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 2-5：5-8.
Preferably, above-mentioned organometallic complex, bis- (the 2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- Biphenyl -4- hydroxyls) the mixture weight ratio of aluminium and 8-hydroxyquinoline aluminium is 2:8.
The preparation method of above-mentioned organometallic complex, is as follows：
(1) bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8- hydroxyls are weighed by prescription amount Base quinoline aluminum is raw material；
(2) by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium weighed and 8- hydroxyls Quinoline aluminum be uniformly mixed to get.
The orientation of growth of crystal can be changed in application of the above-mentioned organometallic complex in terms of preparing alumina compound.
According to defect (hole) mechanism for the crystal structure that practice obtains, by the way that above-mentioned organometallic ligand is added in crystal Object is closed, the atmosphere that pyrolysis process generates a degree of insertion can occur in hexagonal and symbiosis is long, to Change the orientation of growth of crystal, and improve the atomic structure composition on microscopic particles surface, to reach functional material crystal knot The purpose of structure design.
Preferably, the method for preparing alumina compound using above-mentioned organometallic complex, the specific steps are：
(1) by high-purity aluminium hydroxide micro powder by dry powder blender, with inorganic oxide additive and above-mentioned organic gold Metal complex blending prepares aluminium hydroxide mixture, and the inorganic oxide additive is barium monoxide, magnesia, yttrium oxide, oxygen Change chromium, iron oxide, cesium oxide, titanium oxide, manganese oxide, silica and one kind in calcium oxide or arbitrary combination, the hydroxide Aluminium micro mist is 920-970 parts of aluminium hydroxide micro powder, nothing with the dosage number of inorganic oxide additive and organometallic complex 30-60 parts of machine oxide addition, 10-30 parts of organometallic complex；
(2) the aluminium hydroxide mixture mixed is placed in alumina ceramic crucible, into push-plate type sintering oven, is carried out High temperature sintering, wherein 1100-1300 DEG C of sintering temperature, single group crucible material residence time in sintering oven is 4-8 hours, is burnt Knot process carries out under closed environment, and sintering atmosphere is the hot-air containing a concentration of 10-25% (volume ratio) carbon dioxide.
Preferably, the preparation method of above-mentioned alumina compound, dry powder blender is double helix taper in the step (1) Batch mixer.
Preferably, the preparation method of above-mentioned alumina compound, the particle of inorganic oxide additive in the step (1) Grain size, which is chosen at 0.8-4.0 micron grain size ranges, has preferable sintering effect.
Preferably, the preparation method of above-mentioned alumina compound, in the step (1) before inorganic oxide additive use Carry out chemical pretreatment, the specific steps are inorganic oxide additive is placed in fixed bedreactor, be passed through inorganic acid with The steam of air mixing, wherein inorganic acid are nitric acid, hydrochloric acid or sulfuric acid, and the content of inorganic acid is 2.0-6.0% (wt), cures bed The inorganic oxide placement amount on surface is in 2.0-10.0kg/m2Left and right, the processing time in steam are 30-80min, steam temperature Degree is 20-50 DEG C.
The alumina compound obtained by above-mentioned preparation method is laminated structure, and radius-thickness ratio is in 8-30:1.
The radius-thickness ratio is measured using crystal optics method, and this method is to use spindle stage and determination of polarized light microscopy diameter Thickness rate：Sheet-like particle powder is sticked on the needle point of spindle stage first, spindle stage, which is then fixed on petrographic microscope, carries On object platform；Subsequently particle is laid flat by rotation needle handle, first measures the grain size under horizontality；Finally in 90 degree of needle handle of rotation, survey Measure grain thickness.Thus grain size and thickness are obtained, radius-thickness ratio is finally calculated.
The beneficial effects of the invention are as follows：
In the atmosphere that pyrolysis process generates certain journey can occur in hexagonal for above-mentioned organometallic complex The insertion and symbiosis of degree are long, to change the orientation of growth of crystal, and improve the atomic structure composition on microscopic particles surface, to Achieve the purpose that functional material crystal structure designs, the alumina compound obtained by the organometallic complex is made After coating, diaphragm water absorbing properties protrude, and common oxygen is substantially better than in terms of the self discharge, in terms of voltage drop and normal-temperature circulating performance Change aluminized coating diaphragm, preparation method is simple and practical, significant effect, is suitble to the needs of scale industrial production.
Description of the drawings
Fig. 1 is alumina powder pattern SEM comparisons after molding；
Fig. 2 is that coated separator made by alumina compound of the present invention and common commercial ceramic diaphragm are (common Aluminum oxide coating layer) water imbibition comparison, wherein A be alumina compound coating of the present invention, B be commercial alumina coating；
Fig. 3 is that alumina compound prepares the capacity attenuation test comparison figure after battery；
Fig. 4 is that alumina compound prepares the self discharge test comparison figure after battery.
Specific implementation mode
Technical solution of the present invention is further described with reference to specific embodiment.
Embodiment 1
A kind of organometallic complex, by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) composition, bis- (2- first Base -8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 2:8.
The preparation method of above-mentioned organometallic complex, is as follows：
(1) bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8- hydroxyls are weighed by prescription amount Base quinoline aluminum is raw material；
(2) by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium weighed and 8- hydroxyls Quinoline aluminum be uniformly mixed to get.
Embodiment 2
A kind of organometallic complex, by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) composition, bis- (2- first Base -8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 5：5.
The preparation method of above-mentioned organometallic complex, is as follows：
(1) bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8- hydroxyls are weighed by prescription amount Base quinoline aluminum is raw material；
(2) by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium weighed and 8- hydroxyls Quinoline aluminum be uniformly mixed to get.
Embodiment 3
A kind of organometallic complex, by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) composition, bis- (2- first Base -8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 2：5.
The preparation method of above-mentioned organometallic complex, is as follows：
(1) bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8- hydroxyls are weighed by prescription amount Base quinoline aluminum is raw material；
(2) by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium weighed and 8- hydroxyls Quinoline aluminum be uniformly mixed to get.
Embodiment 4
A kind of organometallic complex, by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) composition, bis- (2- first Base -8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 5：8.
The preparation method of above-mentioned organometallic complex, is as follows：
(1) bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8- hydroxyls are weighed by prescription amount Base quinoline aluminum is raw material；
(2) by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium weighed and 8- hydroxyls Quinoline aluminum be uniformly mixed to get.
Embodiment 5
A kind of organometallic complex, by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium (CAS146162-54-1, molecular formula C32H25AlN2O3) and 8-hydroxyquinoline aluminium (C27H18AlN3O3) composition, bis- (2- first Base -8-hydroxyquinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 3：7.
The preparation method of above-mentioned organometallic complex, is as follows：
(1) bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8- hydroxyls are weighed by prescription amount Base quinoline aluminum is raw material；
(2) by bis- (2- methyl -8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium weighed and 8- hydroxyls Quinoline aluminum be uniformly mixed to get.
Embodiment 6
A kind of alumina compound, preparation method are as follows：
(1) it is 4 to choose molar ratio：4：1：1 magnesia, calcium oxide, yttrium oxide, cesium oxide, are mixed by mechanical powder Equipment be simply mixed uniformly, wherein the grain diameter of each inorganic oxide is within the scope of 1-3 micron grain sizes；
(2) chemical pretreatment is carried out to mixed powder：Above-mentioned mixed inorganic oxide mixture powder is put It sets in fixed bedreactor, is passed through the steam that nitric acid is mixed with air, the wherein content of nitric acid is 3.0% (wt), cures bed The inorganic oxide placement amount on surface is in 3.0-4.0kg/m2, the processing time in steam is 60min, about 40 DEG C of steam temperature Between；
(3) taking high-purity hydrogen alumina powder in parts by weight, (commercially available, purity is more than 99.9%) 950 parts, step (2) institute 35 parts of inorganic oxide mixture, 15 parts of organometallic complex described in embodiment 1, dry powder blender is used after mixture (double helix conical mixer) mechanical mixture is uniform；
(4) uniformly mixed aluminium hydroxide mixture is placed in alumina ceramic crucible, into push-plate type sintering oven, Carry out high temperature sintering, wherein about 1200 DEG C of sintering temperature, single group crucible material residence time in sintering oven is 6 hours, sintering Process carries out under closed environment, and sintering atmosphere is the hot-air containing a concentration of 20% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than -40 DEG C), solid abrasive is carried out using nanon ball-mill, obtained by step (4) Powder is ground 4-6 hours, is ground to D50<Within 1.2um, discharging packs, finished product is made.
Finished product is detected using laser fineness gage, the results are shown in Figure 1, is in bimodal distribution.
Embodiment 7
A kind of alumina compound, preparation method are as follows：
(1) it is 5 to choose molar ratio：3：2 barium monoxide, chromium oxide, iron oxide pass through mechanical powder mixing apparatus and carry out letter It is single to be uniformly mixed, wherein the grain diameter of each inorganic oxide is within the scope of 0.8-4.0 micron grain sizes；
(2) chemical pretreatment is carried out to mixed powder：Above-mentioned mixed inorganic oxide mixture powder is put It sets in fixed bedreactor, is passed through the steam that hydrochloric acid is mixed with air, the wherein content of hydrochloric acid is 6.0% (wt), cures bed The inorganic oxide placement amount on surface is in 2.0-5.0kg/m2, the processing time in steam is 30min, about 50 DEG C of steam temperature Between；
(3) taking high-purity hydrogen alumina powder in parts by weight, (commercially available, purity is more than 99.9%) 920 parts, step (2) institute 60 parts of inorganic oxide mixture, 30 parts of organometallic complex described in embodiment 1, dry powder blender is used after mixture (double helix conical mixer) mechanical mixture is uniform；
(4) uniformly mixed aluminium hydroxide mixture is placed in alumina ceramic crucible, into push-plate type sintering oven, Carry out high temperature sintering, wherein about 1100 DEG C of sintering temperature, single group crucible material residence time in sintering oven is 8 hours, sintering Process carries out under closed environment, and sintering atmosphere is the hot-air containing a concentration of 10% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than -40 DEG C), solid abrasive is carried out using nanon ball-mill, obtained by step (4) Powder is ground 4-6 hours, is ground to D50<Within 1.2um, discharging packs, finished product is made.
Embodiment 8
A kind of alumina compound, preparation method are as follows：
(1) it is 4 to choose molar ratio：2：1 magnesia, titanium oxide, silica pass through mechanical powder mixing apparatus and carry out letter It is single to be uniformly mixed, wherein the grain diameter of each inorganic oxide is within the scope of 2-4 micron grain sizes；
(2) chemical pretreatment is carried out to mixed powder：Above-mentioned mixed inorganic oxide mixture powder is put It sets in fixed bedreactor, is passed through the steam that sulfuric acid is mixed with air, the wherein content of sulfuric acid is 2.0% (wt), cures bed The inorganic oxide placement amount on surface is in 7.0-10.0kg/m2, the processing time in steam is 80min, steam temperature about 20 Between DEG C；
(3) taking high-purity hydrogen alumina powder in parts by weight, (commercially available, purity is more than 99.9%) 970 parts, step (2) institute 30 parts of inorganic oxide mixture, 10 parts of organometallic complex described in embodiment 1, dry powder blender is used after mixture (double helix conical mixer) mechanical mixture is uniform；
(4) uniformly mixed aluminium hydroxide mixture is placed in alumina ceramic crucible, into push-plate type sintering oven, Carry out high temperature sintering, wherein about 1300 DEG C of sintering temperature, single group crucible material residence time in sintering oven is 4 hours, sintering Process carries out under closed environment, and sintering atmosphere is the hot-air containing a concentration of 25% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than -40 DEG C), solid abrasive is carried out using nanon ball-mill, obtained by step (4) Powder is ground 4-6 hours, is ground to D50<Within 1.2um, discharging packs, finished product is made.
Embodiment 9
A kind of alumina compound, preparation method are as follows：
(1) it is 7 to choose molar ratio:3 magnesia, manganese oxide by mechanical powder mixing apparatus be simply mixed It is even, wherein the grain diameter of each inorganic oxide is within the scope of 2-3 micron grain sizes；
(2) chemical pretreatment is carried out to mixed powder：Above-mentioned mixed inorganic oxide mixture powder is put It sets in fixed bedreactor, is passed through the steam that nitric acid is mixed with air, the wherein content of nitric acid is 4.0% (wt), cures bed The inorganic oxide placement amount on surface is in 4.0-7.0kg/m2, the processing time in steam is 70min, about 35 DEG C of steam temperature Between；
(3) taking high-purity hydrogen alumina powder in parts by weight, (commercially available, purity is more than 99.9%) 940 parts, step (2) institute 45 parts of inorganic oxide mixture, 20 parts of organometallic complex described in embodiment 1, dry powder blender is used after mixture (double helix conical mixer) mechanical mixture is uniform；
(4) uniformly mixed aluminium hydroxide mixture is placed in alumina ceramic crucible, into push-plate type sintering oven, Carry out high temperature sintering, wherein about 1200 DEG C of sintering temperature, single group crucible material residence time in sintering oven is 6 hours, sintering Process carries out under closed environment, and sintering atmosphere is the hot-air containing a concentration of 15% (volume ratio) carbon dioxide；
(5) in drying room (dew point is less than -40 DEG C), solid abrasive is carried out using nanon ball-mill, obtained by step (4) Powder is ground 4-6 hours, is ground to D50<Within 1.2um, discharging packs, finished product is made.
Below in conjunction with specific test example, the present invention is described in detail.
Aluminum oxide coating layer prepares power lithium battery application test
Select embodiment 6 described in alumina compound, water, polyacrylate (adhesive), polycarboxylic acids (dispersant) and Analyze pure propyl alcohol (wetting agent), the alumina compound, water, polyacrylate, polycarboxylic acids and the weight ratio for analyzing pure propyl alcohol It is 40:50:4:1:0.5, by way of high speed dispersion, be made the aluminium oxide glue of 50% solid content, viscosity in 50-80CP, By way of micro- gravure coater one side coating, is applied twice in Asahi Chemical Industry's PE12um matrix surfaces, form each 4um's in two sides Aluminum oxide coating layer, diaphragm overall thickness 20um；
Choose just extremely ternary material, cathode is the 30AH standard lithium batteries of modified graphite, using above-mentioned coated separator and The double-surface ceramics diaphragm (12um matrixes, each 4um coatings in two sides) of common commercial carries out contrast test.
Test shows：
As shown in Fig. 2, alumina composite material prepared by the present invention, after coating is made, hence it is evident that in microstructure characteristic On be different from commercially available common alumina material (double-surface ceramics diaphragm), after measured, average aspect ratio 16:1, and it is common commercially available Aluminium oxide is in irregular shape, and radius-thickness ratio is 1:1-2.4:Between 1.
And as can be seen from Table 1, common aluminum oxide coating layer is substantially better than in coated separator water imbibition；In addition, three First material (nickel cobalt manganese molar ratio 5：2：3) as anode, 30Ah rectangular aluminum hull electricity of the modifying natural graphite material as cathode (energy density 480wh/L) progress battery evaluation is as shown in Figure 3 and Figure 4 in pond, after dynamic lithium battery is made, in self discharge Aspect, using the diaphragm cell of diaphragm of the present invention, (7 days) voltage is reduced to 6.02 millivolts in regulation ageing time, and compares For battery at 9.32 millivolts, the keeping battery voltage performance made by this patent is substantially better than common aluminum oxide coating layer diaphragm；Final electricity Pond normal-temperature circulating performance is also significantly better than the battery of common aluminum oxide coating layer diaphragm, and the battery made by diaphragm of the present invention follows Ring 600 times, capacity retention ratio is 87% or so, and control cell capacity is then less than 80%, and rapid corruptions occurs.
1 residual moisture content balance of table
The test specimen refers to alumina composite material of the present invention；Reference sample refers to commercially available common oxidation aluminium Material.
What the above-mentioned alumina compound and preparation method thereof for being used to apply dynamic lithium battery to this with reference to embodiment carried out Detailed description is illustrative without being restrictive, and can enumerate several embodiments according to limited range, therefore not The change and modification being detached under present general inventive concept, should belong within protection scope of the present invention.

Claims (4)

1. a kind of method that organometallic complex prepares alumina compound, the organometallic complex is by bis- (2- methyl- 8-hydroxyquinoline-N1, O8)-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium composition, bis- (2- methyl -8- hydroxyls Quinoline-N1, O8) the mixture weight ratio of-(1,1'- biphenyl -4- hydroxyls) aluminium and 8-hydroxyquinoline aluminium is 2-5：5-8, feature exist In：The specific steps are：
(1) by high-purity aluminium hydroxide micro powder by dry powder blender, with inorganic oxide additive and above-mentioned organometallic ligand Close object blending and prepare aluminium hydroxide mixture, the inorganic oxide additive be barium monoxide, magnesia, yttrium oxide, chromium oxide, One kind in iron oxide, cesium oxide, titanium oxide, manganese oxide, silica and calcium oxide or arbitrary combination, the aluminium hydroxide micro powder It is 920-970 parts of aluminium hydroxide micro powder, inorganic oxide with the dosage number of inorganic oxide additive and organometallic complex 30-60 parts of object additive, 10-30 parts of organometallic complex；
(2) the aluminium hydroxide mixture mixed is placed in alumina ceramic crucible, into push-plate type sintering oven, carries out high temperature Sintering, wherein 1100-1300 DEG C of sintering temperature, single group crucible material residence time in sintering oven is 4-8 hours, sintered Journey carries out under closed environment, and sintering atmosphere is to contain the hot-air that concentration volume ratio is 10-25% carbon dioxide.
2. the method that organometallic complex according to claim 1 prepares alumina compound, it is characterised in that：It is described The grain diameter of inorganic oxide additive is chosen at 0.8-4.0 micron grain size ranges in step (1), and there is preferable sintering to imitate Fruit.
3. the method that organometallic complex according to claim 1 prepares alumina compound, it is characterised in that：It is described Inorganic oxide additive uses preceding carry out chemical pretreatment in step (1), and the specific steps are put inorganic oxide additive It sets in fixed bedreactor, is passed through the steam that inorganic acid is mixed with air, wherein inorganic acid is nitric acid, hydrochloric acid or sulfuric acid, nothing The content of machine acid is weight ratio 2.0-6.0%, and the inorganic oxide placement amount on solidification bed surface is in 2.0-10.0kg/m2, steaming Processing time in gas is 30-80min, and steam temperature is 20-50 DEG C.
4. the alumina compound obtained by one of claim 1-3 the methods, it is characterised in that：In the form of sheets, radius-thickness ratio exists 8-30:Between 1.
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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
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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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