CN101993239A - Method for preparing fine-grain high-strength high-purity alumina ceramics - Google Patents
Method for preparing fine-grain high-strength high-purity alumina ceramics Download PDFInfo
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Abstract
The invention discloses a method for preparing fine-grain high-strength high-purity alumina ceramics, which comprises the following steps of: firstly, adding high-purity alumina ceramic balls and domestic commercial high-purity alumina powder into a sand mill according to the mass ratio of 10:1; using deionized water as grinding media; adding a proper amount of organic dispersing agents DOLAPIX CE 64, inorganic dispersing agents (NH4)2SO4 and sintering addition agents MgO for wet process grinding for 2 to 4 hours; then, drying obtained pulp materials for 20 to 30 hours at 80 to 100 DEG C; sieving the materials by a nylon sieve of 200 meshes; placing the sieved materials in a muffle furnace to be calcined for 1 to 3 hours at 550 to 650 DEG C; obtaining alumina ceramic biscuits through cold isostatic pressing treatment after dry pressing molding; and finally, placing the biscuits into the muffle furnace for pressureless sintering for 1 to 3 hours at 1450 to 1600 DEG C. The method has simple preparation process, low raw material cost and low temperature sintering, reduces the energy consumption and is applicable to large-scale production.
Description
Technical field
The present invention relates to a kind of method for preparing the high-strength high-purity alumina ceramic of thin crystalline substance, specifically, relating to the homemade commercialization high-purity alpha-alumina of a kind of employing powder is raw material and low temperature pressureless sintering technology, the method of the thin brilliant high-strength high-purity alumina ceramic of preparation belongs to the alumina ceramic material preparing technical field.
Background technology
The exploitation of alumina-ceramic has surpassed over half a century, because of it has excellent mechanical property, electrical property, chemical stability, and raw material sources are extensive, low cost of manufacture, be the base mateiral of making high strength, wear-resistant, high temperature resistant contour performance ceramic component, be widely used in fields such as machinery, communication, semi-conductor, medicine, food, oil, chemical industry and aerospace.
Alumina-ceramic can be divided into common alumina-ceramic and high-purity alpha-alumina pottery.Common alumina-ceramic is based on 95 alumina ceramics and 99 alumina ceramics, and prepared sparking plug, valve tube, mill Jie and sealing member etc. have obtained to use widely in industries such as automobile, communication, machinery and chemical industry.Yet the sintering temperature of this class material is greater than 1650 ℃, and the crystal grain of material is thick, and the about 260～380MPa of bending strength causes a large amount of energy consumptions and stove consumption simultaneously.High-purity alumina ceramic can be divided into high-strength aluminum oxide of thin crystalline substance and transparent alumina.The former is mainly used in semiconductor machining industry such as abrasive sheet, guide rail etc.; The latter then is mainly used in the electric light source industry, as the electric arc tube of high-pressure mercury lamp and ceramic gold-halogen lamp.
At present, the raw material of preparation high-purity alumina ceramic mainly relies on companies such as French BAIKOWSKI, SUMITOMO CHEMICAL chemical industry and big bright chemistry in the world wide.Their powder median size is little, even particle size distribution, and foreign matter content is extremely low, is suitable for preparing close grain or transparent alumina ceramics.In the thin brilliant high-strength high-purity alumina ceramic process of preparation, very strict to the requirement of material powder, must be there not to be high purity submicron or the nanometer alpha-Al that reunites
2O
3Powder is a raw material.In fact at present the high-strength high-purity alumina ceramic of thin crystalline substance of report has almost completely adopted the low high sintering active alpha-Al of reunion of TM-DAR type of Japanese Taimei Chemicals Co., Ltd. production
2O
3Powder is a raw material.Simultaneously in order to realize low-temperature sintering, control grain growth, obtain the high-performance alumina-ceramic, nearly all be to adopt special sintering technologies such as hot pressing, hot isostatic pressing or discharge plasma sintering, propose to adopt vacuum heating-press sintering technology as Chinese patent CN1304903A, the alumina-ceramic bending strength that obtains at 1500～1650 ℃ of following sintering reaches 610～660MPa.A.Krell then adopts heat and other static pressuring processes to prepare relative density to be higher than 99.95% sub-micron crystal alumina ceramic, and bending strength reaches 709 ± 49MPa.Zhao's Zhe (Chinese patent CN101306943A) and high Lian people such as (Chinese patent CN101624290A) adopt the discharge plasma sintering process to prepare high performance alumina transparent ceramic.Compare with non-pressure sintering technology, the agglomerating plant that above arts demand is special is invested big cost height, is not suitable for large-scale industrial production.
In sum, in view of the price advantage of homemade high-purity alpha-alumina powder, it is carried out modification handle, develop a kind of low temperature and do not have sintering under the press strip spare, the preparation method who takes into account mechanical property and high-compactness alumina-ceramic will have very important significance.
Summary of the invention
The present invention is directed to above-mentioned existing in prior technology defective and problem, it is raw material, low temperature pressureless sintering technology that the homemade commercialization high-purity alpha-alumina of a kind of employing powder is provided, the method for the thin brilliant high-strength high-purity alumina ceramic of preparation.
The method of the thin brilliant high-strength high-purity alumina ceramic of preparation provided by the invention comprises following concrete steps:
A) high-purity alpha-alumina Ceramic Balls and homemade commercialization high-purity alpha-alumina powder being added in the sand mill by 10: 1 mass ratioes, is grinding medium with the deionized water, adds an amount of organic dispersing agent DOLAPIX CE64, inorganic dispersant (NH4)
2SO
4And sintering aid MgO, carried out wet grinding 2～4 hours;
B) slurry that obtains is following dry 20～30 hours at 80～100 ℃;
C) cross 200 order nylon mesh, insert then in the retort furnace and calcined 1～3 hour down in 550～650 ℃;
D) dry-pressing formed after the isostatic cool pressing processing obtains the alumina-ceramic biscuit;
E) above-mentioned alumina-ceramic biscuit is inserted in the retort furnace, under 1450～1600 ℃, carried out pressureless sintering 1～3 hour.
Described high-purity alpha-alumina Ceramic Balls is meant alumina content greater than 99.9%, and diameter is the alumina-ceramic ball of 3mm.
Described homemade commercialization high-purity alpha-alumina powder is meant that principal crystalline phase is the α phase, and purity is greater than 99.99%, and powder granularity skewness, meta particle diameter D50 are the alumina powder jointed of 7～8 μ m.
Deionized water in the step a) and alumina powder jointed mass ratio be preferably 1: 1～and 3: 1.
The volumetric usage of organic dispersing agent DOLAPIX CE 64 in the step a) is preferably 0.01～0.5% of grinding medium deionized water volume.
Inorganic dispersant in the step a) (NH4)
2SO
4The quality consumption be preferably 0.01～2% of alumina powder jointed quality.
The quality consumption of sintering aid MgO in the step a) is preferably 0.01～0.1% of alumina powder jointed quality.
The pressure that isostatic cool pressing in the step d) is handled is preferably 200MPa.
Pressureless sintering condition optimization in the step e) is for carrying out pressureless sintering 2 hours under 1500 ℃.
Compared with prior art, the present invention has following beneficial effect:
1) handles by grinding modification, reduced alumina powder jointed reunion degree and granularity, and make powder have the homogeneous particle diameter distribution, thereby improved the sintering activity of powder, help reducing sintering temperature homemade high-purity alpha-alumina powder.
2) because the active raising of powder sintering, just can obtain relative density at 1500 ℃ of following sintering of lesser temps and be higher than 98% high-purity alumina ceramic, and have the advantage that crystal grain is tiny, intensity is high, this suitability for industrialized production to high-purity alumina ceramic has great importance.
Description of drawings
Fig. 1 is the grain size distribution curve figure of the used homemade high-purity alpha-alumina powder of the present invention.
Fig. 2 is the grain size distribution curve figure of the used homemade high-purity alpha-alumina powder of the present invention through the powder after the wet grinding art breading of the present invention.
Fig. 3 is the scanning electron photomicrograph of the used homemade high-purity alpha-alumina powder of the present invention.
Fig. 4 is the scanning electron photomicrograph of the used homemade high-purity alpha-alumina powder of the present invention through the powder after the wet grinding art breading of the present invention.
Fig. 5 is the section microstructure photograph of embodiment 1 prepared alumina-ceramic sample.
Fig. 6 is the section microstructure photograph of embodiment 2 prepared alumina-ceramic samples.
Fig. 7 is the section microstructure photograph of embodiment 3 prepared alumina-ceramic samples.
Fig. 8 is the section microstructure photograph of embodiment 4 prepared alumina-ceramic samples.
Specific implementation method
The present invention is described in further detail and completely below in conjunction with embodiment, but limit the present invention by no means, and the present invention is not the content that only is confined to embodiment yet.
8000g high-purity alpha-alumina Ceramic Balls and the homemade commercialization high-purity alpha-alumina of 800g powder are added in the sand mill, add the 1600g deionized water again as grinding medium, and add 1.6ml organic dispersing agent DOLAPIX CE 64[and provide by Si Mahuagong company limited], 4g inorganic dispersant (NH
4)
2SO
4, 0.4g sintering aid MgO, carried out wet grinding 3 hours; Slurry after grinding is inserted in 90 ℃ of baking ovens dry 24 hours; Cross 200 order nylon mesh, insert then in the retort furnace in 600 ℃ of calcinings 2 hours; Adopt dry-pressing formed and obtain the alumina-ceramic biscuit after the 200MPa isostatic cool pressing is handled; The alumina-ceramic biscuit is inserted in the retort furnace, under 1450 ℃, carried out pressureless sintering 2 hours, promptly make the alumina-ceramic sample.
Used high-purity alpha-alumina Ceramic Balls is meant alumina content greater than 99.9%, and diameter is the alumina-ceramic ball of 3mm.
Used homemade commercialization high-purity alpha-alumina powder is meant that principal crystalline phase is the α phase, and purity is greater than 99.99%, and powder granularity skewness, meta particle diameter D50 are the alumina powder jointed of 7～8 μ m.
The present invention has carried out analyzing relatively to the micro impurity element of used homemade commercialization high-purity alpha-alumina powder in the powder before and after wet grinding is handled, and the results are shown in Table shown in 1.
The micro impurity element content of table 1 in alumina powder jointed before and after wet grinding is handled
By table 1 result as seen: the used homemade commercialization high-purity alpha-alumina powder of the present invention is after wet grinding art breading of the present invention, big change does not take place in the content of the micro impurity element in alumina powder jointed, and wet grinding technology of the present invention can not cause secondary pollution to alumina powder jointed.
The Mastersizer 2000 type laser particle analyzers that the present invention also adopts Malvern company to produce characterize in the size distribution of handling the powder of front and back through wet grinding used homemade commercialization high-purity alpha-alumina powder, the results are shown in illustrated in figures 1 and 2.As seen from Figure 1: the particle size distribution range of used homemade commercialization high-purity alpha-alumina powder is quite wide, between submicron to tens micron; As seen from Figure 2: used homemade commercialization high-purity alpha-alumina powder is through after the wet grinding art breading of the present invention, and alumina powder jointed size distribution is significantly improved, and distribution range is at 0.1～1 μ m.
The present invention also adopts scanning electronic microscope (SEM) that the pattern and the size of the powder of used homemade commercialization high-purity alpha-alumina powder before and after handling through wet grinding are observed, and the results are shown in Figure 3 and shown in Figure 4.As seen from Figure 3: the particle diameter of used homemade commercialization high-purity alpha-alumina powder is very thick, is made up of the small-particle of many reunions; As seen from Figure 4: used homemade commercialization high-purity alpha-alumina powder is through after the wet grinding art breading of the present invention, and alumina powder jointed pattern is spherical, and particle diameter is very even, is about 0.2～0.3 μ m, has good dispersiveness.
The present invention has also carried out following performance test to the prepared alumina-ceramic sample of present embodiment:
1) relative density: Archimedes's drainage, test result is shown in Table 2.
2) bending strength: ceramics sample is processed into 36 * 4 * 3mm strip, and the test surfaces twin polishing is measured (5 strips of every batch sample test are averaged) with three-point bending method, span 30mm, and pressure head speed 0.5mm/min, test result is shown in Table 2.
3) Vickers' hardness: after the ceramics sample surface finish become minute surface, on AKASHI (AVK-A) microhardness instrument, test.Each data point is tested five points at least, gets its mean value, and load is 49N in the experiment, and test result is shown in Table 2.
The present invention also adopts scanning electronic microscope (SEM) that the cross-section morphology of the prepared alumina-ceramic sample of present embodiment strip is observed, and the results are shown in shown in Figure 5.As seen from Figure 5: the prepared alumina-ceramic of present embodiment has the grain-size high conformity, and grain size is about 2 μ m.
Embodiment 2
The difference of present embodiment and embodiment 1 only is: the alumina-ceramic biscuit is inserted in the retort furnace, carried out pressureless sintering 2 hours under 1500 ℃, make the alumina-ceramic sample.
All the other contents are all with identical described in the embodiment 1.
The present invention also tests relative density, bending strength and the Vickers' hardness of the prepared alumina-ceramic sample of present embodiment by the testing method described in the embodiment 1, and test result is shown in Table 2.
The cross-section morphology of the prepared alumina-ceramic sample of present embodiment strip is seen shown in Figure 6, as seen from Figure 6: the prepared alumina-ceramic of present embodiment is with respect to embodiment 1 prepared alumina-ceramic, density increases, but grain-size slightly grows up, about 3 μ m.
Embodiment 3
The difference of present embodiment and embodiment 1 only is: the alumina-ceramic biscuit is inserted in the retort furnace, carried out pressureless sintering 2 hours under 1550 ℃, make the alumina-ceramic sample.
All the other contents are all with identical described in the embodiment 1.
The present invention also tests relative density, bending strength and the Vickers' hardness of the prepared alumina-ceramic sample of present embodiment by the testing method described in the embodiment 1, and test result is shown in Table 2.
The cross-section morphology of the prepared alumina-ceramic sample of present embodiment strip is seen shown in Figure 7, as seen from Figure 7: the prepared alumina-ceramic of present embodiment is with respect to embodiment 1 prepared alumina-ceramic, density significantly improves, but grain-size obviously grows up, and reaches about 5 μ m.
Embodiment 4
The difference of present embodiment and embodiment 1 only is: the alumina-ceramic biscuit is inserted in the retort furnace, carried out pressureless sintering 2 hours under 1600 ℃, make the alumina-ceramic sample.
All the other contents are all with identical described in the embodiment 1.
The present invention also tests relative density, bending strength and the Vickers' hardness of the prepared alumina-ceramic sample of present embodiment by the testing method described in the embodiment 1, and test result is shown in Table 2.
The cross-section morphology of the prepared alumina-ceramic sample of present embodiment strip is seen shown in Figure 8, as seen from Figure 8: the prepared alumina-ceramic of present embodiment is with respect to embodiment 1 prepared alumina-ceramic, density significantly improves, but grain-size obviously grows up, and reaches about 5～10 μ m.
The The performance test results of table 2 embodiment 1～4 prepared alumina-ceramic sample
By table 2 as seen: adopt preparation method of the present invention, prepared alumina ceramic material just can be reached 1500 ℃ relative density be higher than 98%, bending strength reaches 480～603MPa, Vickers' hardness reaches 16.1～18.5GPa, grain-size has the high-strength characteristic of thin crystalline substance at 2～3 μ m.
Claims (9)
1. a method for preparing the high-strength high-purity alumina ceramic of thin crystalline substance is characterized in that, comprises following concrete steps:
A) high-purity alpha-alumina Ceramic Balls and homemade commercialization high-purity alpha-alumina powder being added in the sand mill by 10: 1 mass ratioes, is grinding medium with the deionized water, adds an amount of organic dispersing agent DOLAPIX CE64, inorganic dispersant (NH4)
2SO
4And sintering aid MgO, carried out wet grinding 2～4 hours;
B) slurry that obtains is following dry 20～30 hours at 80～100 ℃;
C) cross 200 order nylon mesh, insert then in the retort furnace and calcined 1～3 hour down in 550～650 ℃;
D) dry-pressing formed after the isostatic cool pressing processing obtains the alumina-ceramic biscuit;
E) above-mentioned alumina-ceramic biscuit is inserted in the retort furnace, under 1450～1600 ℃, carried out pressureless sintering 1～3 hour.
2. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1, it is characterized in that: described high-purity alpha-alumina Ceramic Balls is meant alumina content greater than 99.9%, diameter is the alumina-ceramic ball of 3mm.
3. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1, it is characterized in that: described homemade commercialization high-purity alpha-alumina powder is meant that principal crystalline phase is the α phase, purity is greater than 99.99%, powder granularity skewness, meta particle diameter D50 are the alumina powder jointed of 7～8 μ m.
4. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1, it is characterized in that: deionized water in the step a) and alumina powder jointed mass ratio are 1: 1～3: 1.
5. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1, it is characterized in that: the volumetric usage of the organic dispersing agent DOLAPIX CE 64 in the step a) is 0.01～0.5% of a grinding medium deionized water volume.
6. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1 is characterized in that: the inorganic dispersant in the step a) (NH4)
2SO
4The quality consumption be 0.01～2% of alumina powder jointed quality.
7. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1, it is characterized in that: the quality consumption of the sintering aid MgO in the step a) is 0.01～0.1% of an alumina powder jointed quality.
8. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1 is characterized in that: the pressure that the isostatic cool pressing in the step d) is handled is 200MPa.
9. the method for the thin brilliant high-strength high-purity alumina ceramic of preparation according to claim 1 is characterized in that: the pressureless sintering condition in the step e) is for carrying out pressureless sintering 2 hours under 1500 ℃.
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