CN103342576A - Preparation method of nanocomposite Al2O3 ceramic filter element - Google Patents
Preparation method of nanocomposite Al2O3 ceramic filter element Download PDFInfo
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- CN103342576A CN103342576A CN2013102578134A CN201310257813A CN103342576A CN 103342576 A CN103342576 A CN 103342576A CN 2013102578134 A CN2013102578134 A CN 2013102578134A CN 201310257813 A CN201310257813 A CN 201310257813A CN 103342576 A CN103342576 A CN 103342576A
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Abstract
The invention discloses a preparation method of a nanocomposite Al2O3 ceramic filter element with high strength. The preparation method is characterized by comprising the following steps of: firstly, preparing an Al2O3 porous matrix with macroscopic straight pores; and secondly, preparing a porous nannocomposite coating on the walls of the macroscopic straight pores of the Al2O3 porous matrix, wherein the second step comprises the following concrete steps of: (1) dissolving aluminum isopropoxide into distilled water with the temperature of 70-90 DEG C, stirring the solution, and adding nitric acid to control the pH value, wherein the aluminum isopropoxide is hydrolyzed to form a sol; (2) carrying out ultrasonic treatment at the temperature of 40 DEG C under one atmospheric pressure, and ageing the sol; (3) completely immersing the sintered Al2O3 porous matrix with the macroscopic straight pores into the aged sol, impregnating, lifting, and then carrying out freeze drying so that the sol becomes a gel; (4) carrying out thermal treatment on the gel at the temperature of 500-600 DEG C, and then, cooling along with a furnace; and (5) finally, sintering the gel at the temperature of 900-1100 DEG C to obtain the nanocomposite Al2O3 ceramic filter element.
Description
Technical field
The present invention relates to a kind of food, medical industry of can be used for as the Al of filter core or strainer tube
2O
3Ceramic products preparation method.
Background technology
Al
2O
3Advantages such as that ceramic element (strainer tube) has is high temperature resistant, wear-resistant, corrosion-resistant, low cost have broad application prospects in fields such as oil, chemical industry, environmental protection, food, pharmacy.But filter for many fine chemistry industries, require filtering accuracy to reach nanometer scale, and have higher Gas permeability.
Adopt general traditional porous ceramics technology of preparing, aperture size is difficult to reach high precision and filters in micron level.If adopt homogeneous nanoporous Al
2O
3Pottery, filtering accuracy, maximum aperture size are limited in nanometer scale, and (30～60nm) is not inaccessible, but the strainer tube Gas permeability obviously is difficult to reach.General Al
2O
3Porous matrix adopts larger particles Al
2O
3(granularity is at 30～50 μ m) powder carries out sintering.But Al on the present market
2O
3The particle size distribution of powder is wideer, and out-of-shape causes porous Al
2O
3The gas cell distribution of pottery is inhomogeneous, and Gas permeability is little, and ceramics strength descends.
Summary of the invention
For solving Al
2O
3Contradiction between ceramic element (strainer tube) filtering accuracy and the ventilation property the invention provides a kind of filtering accuracy nanometer scale, the high strength Al that Gas permeability is higher
2O
3The preparation method of ceramic element.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of nanometer complex phase Al
2O
3The preparation method of ceramic element is characterized in that, comprises the steps:
The first step, spherical Al
2O
3The powder preparation contains the Al of macroscopical straight hole
2O
3Porous matrix;
Second step is at Al
2O
3Preparation nanoporous complex phase coating on the porous matrix macroscopic view straight hole hole wall, wherein, second step comprised following concrete steps:
(1) aluminum isopropylate is dissolved in 70～90 ℃ of distilled water, stirs and add nitric acid and control pH=1～3, aluminum isopropylate generation hydrolysis forms colloidal sol, adds 80～90vt% nanometer ZrO in the colloidal sol for preparing
2Powder stirs de-bubble, obtains composite mortar;
(2) at 40 ℃, ultrasonic under 1 barometric point, ageing;
(3) will sinter and contain macroscopical straight hole Al
2O
3Porous matrix is immersed in the good colloidal sol of ageing fully, floods, lifts, then lyophilize;
(4) at 500 ℃～600 ℃ gel is heat-treated, then furnace cooling;
(5) carry out sintering at 900～1100 ℃ at last, obtain nanometer complex phase Al
2O
3Ceramic element.
In the above-mentioned technology, gel heat-treated adopt the staged heating mode for described 500 ℃～600 ℃.Described dipping time is 5～15min.Described pull rate is 2～6cm/min.Described lyophilize is to freeze at-40 ℃ of fast deeps, and insulation 2h slowly is warming up to-20 ℃, and heating mode is infrared heating, and temperature rise rate is 1 ℃/min, in-20 ℃ of insulation 24h, vacuum-drying.
The concrete steps of the described the first step are:
(1) powder of solid particles, fluidizer, solidifying agent, organic solvent are mixed, ball milling obtains mixed slurry after the mechanical stirring; Wherein, powder of solid particles 70～60wt%, fluidizer 30～40wt%, solidifying agent are the 3wt%～7wt% of fluidizer; Powder of solid particles comprises the spherical micron Al of 98wt%～99.1wt%
2O
3, 0.5wt%～1.0wt% TiO
2And 0.4wt%～1.0wt%MgO;
(2) the part organic solvent in the air-dry removal slip makes organic solvent quality percentage composition be lower than 5%, again 40～60 ℃ of following slakings, obtains mud shape raw material;
(3) mud shape raw material is packed into the inner chamber of extrusion molding mould, preform blank is extruded in pressurization;
(4) with preform blank 600～900 ℃ of pyrolysis, 1400～1600 ℃ of sintering under air atmosphere at last obtain to contain the Al of macroscopical straight hole
2O
3Porous matrix.
Wherein.Described fluidizer is resol or from Resins, epoxy.Described solidifying agent is oxalic acid or citric acid.Described organic solvent is ethanol.
The present invention is high-strength, nanometer complex phase Al
2O
3Ceramic filter tube (filter core) adopts spherical Al
2O
3(narrow particle size distribution, 20～50 μ m) powder carries out sintering as the raw materials for sintering of porous matrix under interpolation sintering aid and pore-forming material situation, the Gas permeability of porous ceramics and intensity are all increased.Al
2O
3After porous filtering pipe matrix reaches functional requirement, at matrix Al
2O
3Macroscopic view straight hole pipe adopts sol-gel (Sol-gel) legal system to be equipped with the porous complex phase (Al of 30～50nm
2O
3-ZrO
2) coating.Thereby obtain the filtering accuracy nanometer scale, high-strength, nanometer complex phase Al that Gas permeability is higher
2O
3Ceramic filter tube (filter core).High temperature resistant, corrosion-resistant, anti-oxidant, good permeability and filtering accuracy advantages of higher in filtering, food, chemical industry are arranged.
Description of drawings
Fig. 1 is nanometer complex phase Al of the present invention
2O
3Ceramic element (strainer tube) sectional view.
Among the figure: the porous matrix that 1, contains macroscopical straight hole; 2, nanometer complex phase Al
2O
3-ZrO
2Coating; 3, extrusion moulding macroscopic view straight hole.
Embodiment
Referring to Fig. 1, the present invention is high-strength, nanometer complex phase Al
2O
3Ceramic element (strainer tube) comprises micron-size spherical aluminum oxide (Al
2O
3) powder extrusion moulding sintering gained contain macroscopical straight hole porous matrix 1, the nanometer complex phase (Al of macroscopical straight hole hole wall
2O
3-ZrO
2) coating 2.Filter core (strainer tube) will directly contact with filtered liquid, requires whole filter core to have characteristics such as high temperature resistant, corrosion-resistant, anti-thermal shock, good permeability so.
Micron order Al
2O
3It is relatively large that matrix burns till the aperture of porous material size, and good permeability is as propping material.In order to improve filtering accuracy, adhere to the nano complex phase ceramics coating at the straight hole hole wall, filter thereby carry out high precision, make filtering accuracy reach nanometer scale.
The present invention is high-strength, nanometer complex phase Al
2O
3Ceramic element comprises the work of two aspects: on the one hand for containing the Al of macroscopical straight hole
2O
3The porous matrix preparation is nanoporous complex phase Al on macroscopical straight hole hole wall on the other hand
2O
3-ZrO
2The preparation of coating below gives division:
The present invention is high-strength, nanometer complex phase Al
2O
3Contain macroscopical straight hole Al in the ceramic element (strainer tube)
2O
3The matrix preparation method is maturation process, mainly comprises feedstock production, extrusion moulding, drying, pyrolysis and firing process.
This preparation method is main raw material with powder of solid particles with the macromolecular material with plastification, further after the subsequent disposal, prepares the tubulose preform blank in extrusion molding mould, last pyrolysis, sintering.Specific embodiment is formed as shown in table 1.
Table 1 contains macroscopical straight hole porous matrix prescription
Powder of solid particles is spherical micron Al
2O
3Powder, TiO
2Powder and MgO mixed powder.Spherical Al
2O
3Powder purity is more than 99.6%, size-grade distribution 20～50 μ m, TiO
2, MgO powder degree is at several micron.Fluidizer is resol or from Resins, epoxy; Solidifying agent is oxalic acid or citric acid.
By the prescription in the table 1 desired raw material is mixed, add organic solvent ethanol (mass concentration 〉=99%), making the massfraction of solute is 60wt%, and ball milling obtains mixed slurry after the mechanical stirring.Part organic solvent in the air-dry removal slip makes organic solvent quality percentage composition be lower than 5%, and recurring 30min obtains mud shape raw material.With pack into the inner chamber of extrusion molding mould of mud shape raw material, preform blank is extruded in pressurization.
With preform blank pyrolysis (0.5 ℃/min of heat-up rate, insulation 1.5h), sintering (5 ℃ of temperature rise rates/min), obtain to contain the Al of macroscopical straight hole under air atmosphere at last
2O
3Porous matrix.6 specific embodiment corresponding technological parameters are as shown in table 2 in the preparation matrix process.
Table 2 matrix preparation technology parameter
| Embodiment | Curing temperature (℃) | Pyrolysis temperature (℃) | Sintering temperature (℃) | The sintered heat insulating time (h) |
| 1 | 40 | 600 | 1400 | 1 |
| 2 | 50 | 650 | 1500 | 1.5 |
| 3 | 60 | 700 | 1400 | 2 |
| 4 | 40 | 750 | 1600 | 1 |
| 5 | 60 | 800 | 1500 | 1.5 |
| 6 | 50 | 600 | 1400 | 2 |
The prepared porous matrix performance of different embodiment is difference to some extent, and table 3 is the test result of embodiment 2.
The The performance test results of table 3 embodiment 2 matrixes
| Performance index | Design requirements | The preparation material property |
| Bending strength (MPa) | >40 | 40～50 |
| Void content (%) | >30 | 30～35 |
Compare with other 5 groups of embodiment test results, gained matrix strength, void content are all higher under embodiment 2 prescription and technology.Therefore, adopt embodiment 2 sintering results as following Prepared by Sol Gel Method coating of material.
The present invention is at Al
2O
3The coating that has prepared four embodiment under the matrix condition of porous matrix embodiment 2 preparations, concrete processing parameter is as shown in table 4.
Press table 4 processing parameter, aluminum isopropylate is dissolved in the distilled water, the mol ratio of aluminum isopropylate and deionized water is 1:80, stirs and adds nitric acid in thermostatically heating magnetic stirring apparatus high speed and control pH value, and aluminum isopropylate generation hydrolysis forms colloidal sol.In above-mentioned colloidal sol, add nanometer ZrO
2Powder stirs 30min, and de-bubble obtains composite mortar.
Colloidal sol is in ageing process, and colloidal particle is assembled the formation network structure gradually.The ageing condition, at 40 ℃, ageing under 1 normal atmosphere, ultrasonic (table 4).With porous Al
2O
3Matrix is immersed in the good colloidal sol of ageing, floods, lifts matrix (table 4).Freeze at-40 ℃ of fast deeps, insulation 2h slowly is warming up to-20 ℃, and heating mode is infrared heating, and temperature rise rate is 1 ℃/min, in-20 ℃ of insulation 24h, vacuum-drying.
Gel thermal treatment under table 4 maturing temperature adopts the staged heating mode to discharge macromole and solvent in the gel, and temperature rise rate is at 1～2 ℃/min, last furnace cooling.The nano-scale particle pore of growing up stops up when avoiding sintering temperature too high, sintering under table 4 sintering temperature at last, insulation 1h.
The processing parameter that table 4 coating preparation of the present invention relates to
Claims (9)
1. nanometer complex phase Al
2O
3The preparation method of ceramic element is characterized in that, comprises the steps:
The first step, spherical Al
2O
3The powder preparation contains the Al of macroscopical straight hole
2O
3Porous matrix;
Second step is at Al
2O
3Preparation nanoporous complex phase coating on the porous matrix macroscopic view straight hole hole wall, wherein, second step comprised following concrete steps:
(1) aluminum isopropylate is dissolved in 70～90 ℃ of distilled water, stirs and add nitric acid and control pH=1～3, aluminum isopropylate generation hydrolysis forms colloidal sol, adds 80～90vt% nanometer ZrO in the colloidal sol for preparing
2Powder stirs de-bubble, obtains composite mortar;
(2) at 40 ℃, ultrasonic under 1 barometric point, ageing;
(3) will sinter and contain macroscopical straight hole Al
2O
3Porous matrix is immersed in the good colloidal sol of ageing fully, floods, lifts, then lyophilize;
(4) at 500 ℃～600 ℃ gel is heat-treated, then furnace cooling;
(5) carry out sintering at 900～1100 ℃ at last, obtain nanometer complex phase Al
2O
3Ceramic element.
2. nanometer complex phase Al as claimed in claim 1
2O
3The preparation method of ceramic element is characterized in that, gel heat-treated adopts the staged heating mode for described 500 ℃～600 ℃.
3. nanometer complex phase Al as claimed in claim 1
2O
3The preparation method of ceramic element is characterized in that, described dipping time is 5～15min.
4. nanometer complex phase Al as claimed in claim 1
2O
3The preparation method of ceramic element is characterized in that, described pull rate is 2～6cm/min.
5. nanometer complex phase Al as claimed in claim 1
2O
3The preparation method of ceramic element is characterized in that, described lyophilize is to freeze at-40 ℃ of fast deeps, and insulation 2h slowly is warming up to-20 ℃, and heating mode is infrared heating, and temperature rise rate is 1 ℃/min, in-20 ℃ of insulation 24h, vacuum-drying.
6. nanometer complex phase Al as claimed in claim 1
2O
3The preparation method of ceramic element is characterized in that, the concrete steps of the described the first step are:
(1) powder of solid particles, fluidizer, solidifying agent, organic solvent are mixed, ball milling obtains mixed slurry after the mechanical stirring; Wherein, powder of solid particles 70～60wt%, fluidizer 30～40wt%, solidifying agent are the 3wt%～7wt% of fluidizer; Powder of solid particles comprises the spherical micron Al of 98wt%～99.1wt%
2O
3, 0.5wt%～1.0wt% TiO
2And 0.4wt%～1.0wt%MgO;
(2) the part organic solvent in the air-dry removal slip makes organic solvent quality percentage composition be lower than 5%, again 40～60 ℃ of following slakings, obtains mud shape raw material;
(3) mud shape raw material is packed into the inner chamber of extrusion molding mould, preform blank is extruded in pressurization;
(4) with preform blank 600～900 ℃ of pyrolysis, 1400～1600 ℃ of sintering under air atmosphere at last obtain to contain the Al of macroscopical straight hole
2O
3Porous matrix.
7. nanometer complex phase Al as claimed in claim 6
2O
3The preparation method of ceramic element is characterized in that, described fluidizer is resol or from Resins, epoxy.
8. nanometer complex phase Al as claimed in claim 6
2O
3The preparation method of ceramic element is characterized in that, described solidifying agent is oxalic acid or citric acid.
9. nanometer complex phase Al as claimed in claim 6
2O
3The preparation method of ceramic element is characterized in that, described organic solvent is ethanol.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193310A (en) * | 2014-08-29 | 2014-12-10 | 潮州三环（集团）股份有限公司 | Ceramic material and preparation method thereof |
| CN104987047A (en) * | 2015-06-03 | 2015-10-21 | 浙江沁园水处理科技有限公司 | Nanometer ZrO2-loaded microcrystalline ball, and preparation method and application thereof |
| CN106830973A (en) * | 2017-02-09 | 2017-06-13 | 江苏省陶瓷研究所有限公司 | A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method |
| CN107281847A (en) * | 2016-04-05 | 2017-10-24 | 株式会社昌承 | Highly dense multiple hollow type ceramic filter |
| CN110204318A (en) * | 2019-05-17 | 2019-09-06 | 西安交通大学 | A kind of intensity enhancing method of the aluminum oxide porous material based on powder bed melting |
| CN111517766A (en) * | 2020-05-11 | 2020-08-11 | 镇江华鑫磨具有限公司 | Method for manufacturing porous ceramic filter plate |
| CN111592379A (en) * | 2020-06-15 | 2020-08-28 | 深圳市万泽中南研究院有限公司 | Preparation method of ceramic core coating based on dipping freeze drying technology |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193310A (en) * | 2014-08-29 | 2014-12-10 | 潮州三环（集团）股份有限公司 | Ceramic material and preparation method thereof |
| CN104987047A (en) * | 2015-06-03 | 2015-10-21 | 浙江沁园水处理科技有限公司 | Nanometer ZrO2-loaded microcrystalline ball, and preparation method and application thereof |
| CN107281847A (en) * | 2016-04-05 | 2017-10-24 | 株式会社昌承 | Highly dense multiple hollow type ceramic filter |
| CN106830973A (en) * | 2017-02-09 | 2017-06-13 | 江苏省陶瓷研究所有限公司 | A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method |
| CN110204318A (en) * | 2019-05-17 | 2019-09-06 | 西安交通大学 | A kind of intensity enhancing method of the aluminum oxide porous material based on powder bed melting |
| CN111517766A (en) * | 2020-05-11 | 2020-08-11 | 镇江华鑫磨具有限公司 | Method for manufacturing porous ceramic filter plate |
| CN111592379A (en) * | 2020-06-15 | 2020-08-28 | 深圳市万泽中南研究院有限公司 | Preparation method of ceramic core coating based on dipping freeze drying technology |
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Application publication date: 20131009 |