KR101652397B1 - zirconia-alumina composite and method for manufacturing the same - Google Patents
zirconia-alumina composite and method for manufacturing the same Download PDFInfo
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- KR101652397B1 KR101652397B1 KR1020150049149A KR20150049149A KR101652397B1 KR 101652397 B1 KR101652397 B1 KR 101652397B1 KR 1020150049149 A KR1020150049149 A KR 1020150049149A KR 20150049149 A KR20150049149 A KR 20150049149A KR 101652397 B1 KR101652397 B1 KR 101652397B1
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- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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Abstract
Description
The present invention relates to a zirconia-alumina composite molded article and a manufacturing method thereof, and more particularly, to a zirconia-alumina composite molded article having increased mechanical strength and a manufacturing method thereof.
A molded body in which a ceramic powder, a metal powder, and a mixed powder thereof are formed in a plate shape can be used as a sputtering target material or an abrasion resistant material after being molded and subjected to plastic working. The sputtering target material can be used as a material for forming a thin film by a sputtering method and is used in the manufacture of LCD (liquid crystal display), EL (electroluminescence), and semiconductor.
For example, products such as ceramic board, ring, and disc used in semiconductor equipment mainly use alumina (Al 2 O 3 ). However, alumina often breaks down due to strength problems during use.
In order to overcome these problems, it is necessary to try various studies to increase the mechanical properties (strength, fracture toughness) while taking advantage of alumina.
The present invention provides a method of manufacturing a large zirconia-alumina composite article that can increase mechanical properties through a cold hydrostatic pressing process.
In addition, the present invention provides a method of manufacturing a zirconia-alumina composite molded article in which deformation of a molded body can be minimized at the time of processing or after processing.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory and are not intended to limit the invention to the precise form disclosed. There will be.
According to an aspect of the present invention, A mixing step of mixing the alumina powder and the partially stabilized zirconia powder; A filling step of filling the mixed powder into a mold; Molding the mold into a pressure vessel for cold isostatic pressing and pressurizing the outside of the mold at a set pressure to form a zirconia-alumina composite molded article; A demolding step of separating the molded zirconia-alumina composite article from the mold; And a sintering step of sintering the deformed disk at a set temperature.
In one embodiment, in the mixing step, 70 to 95 wt% of the alumina powder and 5 to 30 wt% of the zirconia powder may be mixed with respect to 100 wt% of the mixed powder.
In one embodiment, in the mixing step, the particle size of the alumina powder is 0.4 to 0.8 mu m, and the particle size of the zirconia powder is 0.5 to 2.0 mu m.
In one embodiment, in the forming step, the mold having been assembled and filled is vertically injected into the pressure vessel, and the pressure medium is applied to the mold at a pressure of 1000 to 1500 bar to burn the zirconia-alumina composite body.
In one embodiment, it may further comprise a vacuum step of forming the interior of the mold into a vacuum state after the filling step.
In one embodiment, in the vacuum step, the air in the mold can be sucked from the vacuum port formed at one side of the mold.
In one embodiment, in the sintering step, the sintering process may be performed at 1500 to 1650 ° C after calcination at 950 to 1100 ° C.
In one embodiment, the method may further include a surface treatment step for imparting a roughness of 0.28 to 0.40 and a flatness of 0.015 to 0.035 to the molded body after the demoulding step.
In one embodiment, it may further include a shape processing step of processing the size, shape, and thickness of the molded body after the demoulding step to a set value.
In one embodiment, the sintering step may further include a precision machining step of finely machining the size, shape and thickness of the formed body so as to correspond to the set values.
Further, another embodiment of the present invention provides a zirconia-alumina composite molded article produced by the above-described production method.
According to an embodiment of the present invention, While maintaining the benefits of an alumina mechanical properties (strength, fracture toughness) are dispersed in a second phase of the partially stabilized zirconia (ZrO 2) dispersed in the alumina ceramic base in order to increase the mechanical properties that zirconia increased-clay composite (ZTA: Zirconia Toughened Alumina).
In addition, the ZTA granule powder is filled in the rubber mold and the CIP process is carried out to produce a uniform molded article. The molded article can be processed in various forms such as a panel, a disc, a ring, Size can be produced.
It should be understood that the effects of the present invention are not limited to the above effects and include all effects that can be deduced from the detailed description of the present invention or the configuration of the invention described in the claims.
1 is a flow chart showing a method of manufacturing a zirconia-alumina composite molded article according to the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described with reference to the accompanying drawings. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.
Throughout the specification, when a part is referred to as being "connected" to another part, it includes not only "directly connected" but also "indirectly connected" . Also, when an element is referred to as "comprising ", it means that it can include other elements, not excluding other elements unless specifically stated otherwise.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart illustrating a method of manufacturing a zirconia-alumina composite article.
1, a method of manufacturing a zirconia-alumina composite molded article according to an embodiment includes a mixing step S10, a filling step S20, a vacuum step S30, a molding step S40, a demolding step S50, A surface treatment step S60, a shape machining step S70, a sintering step S80 and a precision machining step S90.
In the mixing step (S10), alumina powder and zirconia powder are uniformly mixed and dispersed, and mixed powder of granules is formed. At this time, 70 to 95 wt% of alumina powder and 5 to 30 wt% of zirconia powder may be mixed with 100 wt% of mixed powder. If the zirconia powder is less than 5 wt%, it may not meet the purpose of increasing the mechanical strength. If the zirconia powder is more than 30 wt%, the content of the impurities may increase, which may make the production of dense molded articles difficult.
It is preferable that the alumina powder having a particle size of 0.40 to 0.80 μm and the zirconia powder having a particle size of 0.5 to 2.0 μm are uniformly distributed in the mixed powder. If the particle size is out of the above-described range, it affects the moldability and the strength of the formed body after the cold isostatic pressing step, and the sintering strength and the sintered density of the final sintered body are affected by this phenomenon. Therefore, if the particle distribution is uneven, the molding density is lowered and the physical properties of the sintered body are affected. If the particle distribution is only in a specific range, the filling rate is poor and the voids are increased.
On the other hand, zirconia exists in three crystal phases, monoclinic, tetragonal and cubic depending on the temperature.
These three different crystalline phases are mutually transformed when an external force is applied to the surface of the zirconia, and in this process, volume changes occur at the site receiving the external force. In other words, when stress is applied, the fracture energy causes a transformation of the T-M, thereby expanding the volume at that site and preventing further progression of the fracture.
The molten zirconia forms a cubic crystal phase at 2680 ° C upon cooling and a martensite transformation at a temperature of 2370 ° C and a monoclinic system at 950 ° C at a temperature of 2370 ° C. When the monoclinic system at room temperature is heated, the phase is transformed again to the tetragonal system at 1150 ° C. The difference between the transition temperatures at cooling and the transition temperatures at elevated temperatures is due to the supercooling required for nucleation when phase transitions occur.
In this way, zirconia is present as a stable tetragonal crystal phase at high temperature. When zirconia is slowly cooled to room temperature, it shows a volume increase of 3 ~ 5% and a shear strain of about 8% So that the zirconia is broken. Therefore, partially stabilized zirconia in which a metal oxide (stabilizer) such as Y 2 O 3 , CeO 2 , MgO, CaO or the like is partially added to stabilize the phase transition at room temperature is preferably used. Especially, among the stabilized metal oxides, zirconia using Y 2 O 3 is better than the other mechanical properties. Since the tetragonal crystal phase can be obtained at room temperature by the stabilizer, the phase transition occurs due to the high stress disturbance around the cracks during the growth of the crack due to the external stress, and the strength and toughness can be improved by increasing the volume.
The filling step S20 is a step of filling the inside of the mold with zirconia-alumina mixed powder as a starting material.
The mold for cold isostatic pressing has a shape corresponding to the length, diameter, and thickness of the zirconia-alumina composite molded article to be produced, for example, a cylinder or a polygonal column. It is sufficient to cope with the pressure applied to the molded body during the cold pressing process And can be made of rubber or latex material having elasticity and tensile strength.
The mold may be provided with an inlet for filling the mixed powder at one side thereof or for taking out the formed molded body, and at least one or more vacuum ports may be formed in a part of the mold. The vacuum port is connected to the vacuum pump through a vacuum hose to form a vacuum state in the mold before the cold isostatic pressing process to achieve a denser filling state.
The vacuum step S30 is a step of forming the inside of the mold into a vacuum state. That is, when filling of the mixed powder is completed, the inlet of the mold is closed to make the inside closed, the hose is connected to the vacuum port provided in the mold, and the air in the mold is sucked by using a vacuum pump.
The forming step S40 is a step of putting the mold into the pressure vessel for cold isostatic pressing and then performing the cold isostatic pressing step.
Cold isostatic pressing applies the Pascal principle that the pressure applied to a portion of the fluid stopping in a closed container acts perpendicularly to all parts of the fluid.
That is, the filled mold is vertically injected into the pressure vessel in a state of being fixed by using a supporting stand or the like.
Thereafter, when power is applied to the pressure vessel, the pressure medium presses the mold, thereby applying the set pressure to the zirconia-alumina mixed powder filled in the mold. As the pressure medium, liquid such as water, glycerin, and oil may be used.
For example, a mold is placed in a pressure vessel for cold isostatic pressing to uniformly provide pressure. At this time, it is preferable to slowly apply atmospheric pressure and pressure for 10 to 60 minutes at a pressure of 1000 to 1500 bar so as not to subject the organization chart to sudden impact and deformation, and the firing is completed while adjusting the pressure according to the thickness of the mold, Thereby producing a molded article in the form of a disk.
At this time, the pressure can be adjusted according to the use and the specification of the formed body to be manufactured. However, if the pressure is less than 1000 bar, deformation, cracking and breakage occur regardless of the additional pressing time. If the pressure is more than 1500 bar, the molding density is high, But the product may be destroyed during the debinding process in the course of the calcination process, which is the sintering process. Further, if the pressing time is less than 10 minutes in the pressure condition, sufficient firing result and organization chart can not be obtained, and if the pressing time exceeds 60 minutes, brittle and non-uniform organization can be obtained.
In the demolding step (S50), the mold is separated from the cold isostatic pressing apparatus and the fired zirconia-alumina composite molded article is taken out of the mold.
After the firing of the zirconia-alumina composite molded body is completed by applying pressure for a sufficient time, the fired molded body is separated from the mold.
The surface treatment step S60 is a step of imparting the illuminance and the flatness to the formed body after the de-molding step. For example, in one embodiment, the roughness of 0.28 to 0.40 and the flatness of 0.015 to 0.035 are given by polishing using a surface grinder at a rotational speed of the formed body of 240 to 360 rpm.
The shaping step S70 is a step of shaping the formed body, which has been formed into a predetermined shape after the de-molding step, into a predetermined size and shape, and then cutting the shaped body so as to be close to the set thickness.
Sintering step S80 is a step of sintering the demolded formed body at a set temperature. In the sintering step, the calcining step is firstly performed at 950 to 1100 ° C to remove impurities contained in the formed body, and the sintered body is formed by secondary sintering at 1500 to 1650 ° C.
The precision machining step (S90) is a step of finely machining the formed body primarily processed in the shape machining step to a size, thickness and shape corresponding to the values set after the sintering step.
Example
1. Mixed powders for ZTA moldings
Granule powders were prepared by granular alumina powders and partially stabilized zirconia powders as raw materials. The samples were named ZTA-10 and ZTA-20 according to PSZ content. ZTA-10 means a sample mixed with 90 wt% of Al 2 O 3 and 10 wt% of ZrO 2 .
2. Filling of mixed powder
ZTA-10 and ZTA-20 were used to prepare specimens, and 215 kg of granular powder was filled with a 20 mm rubber mold. At this time, the ZTA granule powder was slowly charged into the rubber mold so as to be filled to the highest density, and filled with a vibrator.
3. Molding
The rubber mold was subjected to CIP molding after sealing the inlet to prevent water from entering the mold during CIP molding. The maximum molding pressure at this time was 1300 bar. The size of the molded body after demolding was φ473 * 290mm for ZTA-10 and φ475 * 295mm for ZTA-20. .
4. Surface treatment and shape machining
ZTA-10 and ZTA-20 molded by CIP were surface treated and shaped using a lathe. The reason for processing the CIP shaped body is to prevent the occurrence of cracks during sintering by imparting flatness to the compacted body and to process the size of the sintered body obtained after sintering to approach the final size, I want to save money. Green processing was carried out while changing the rotational speed of the main shaft to 240 to 360 rpm in order to establish optimum working conditions so as to prevent cracks and chips occurring during machining.
5. ZTA specimen sintering
The sintering process is one of the processes most influencing the physical properties such as density and strength in the production of ceramics. A ZTA shaped body processed into a disk shape was sintered. The sintering process was carried out in two stages, and the first stage was calcined at 1050 ° C in a calcination process and subjected to a degreasing process. The second sintering process was sintered at 1650 ° C for ZTA-10 and sintered at 1630 ° C for ZTA-20.
6. Processing of sintered body
The ZTA sintered body was processed by using a planar grinder to make the flatness and the thickness of the sintered body target. First, roughing was performed to a thickness of 9 mm using a diamond wheel (510 × 50 × 5 mm, 200 mesh). At this time, the processing conditions were set to 50 탆 at one infeed. In addition, a second diamond wheel (510 × 50 × 5 mm, 400 mesh) was used to finish the workpiece to a thickness of 9 mm. At this time, the amount of infiltration once was 5 to 10 탆.
7. Characteristics of ZTA sintered body
1) Illuminance and flatness
To measure the roughness of the finished ZTA sintered body, the center line surface roughness (Ra) was measured using a Mitutoyo roughness tester, and the measurement was expressed as a mean value measured by dividing the sintered body into nine equal parts. The average roughness values were 0.35 μm for ZTA-10 and 0.31 μm for ZTA-20.
The flatness of the ZTA sintered body was measured using a contact type three-dimensional measuring machine, and the average value was measured by measuring 9 parts of the sintered body. As a result, the average flatness was 0.02 mm and excellent flatness was exhibited.
2) Outer diameter and thickness
The outer diameter of the finished ZTA sintered body was measured in a noncontact manner using a three-dimensional measuring machine. As a result, the outer diameter of the ZTA-10 was 329.0 mm and the outer diameter of ZTA-20 was 327.0 mm.
The thickness of the ZTA sintered body was measured using a Mitutoyo Micrometer. As a result, the thicknesses of both ZTA-10 and ZTA-20 were measured to be 9.07 mm.
3) Measurement of density, bending strength, fracture toughness and thermal expansion coefficient
Density, bending strength, fracture toughness and thermal expansion coefficient were measured in order to confirm the physical and thermal properties of the finished ZTA sintered body.
end. Density
The specific gravity was measured by the apparent specific gravity measurement method of KS L 3114 (appearance, porosity, absorption rate and specific gravity of refractory bricks). The size of the specimen was measured as 10 × 10 × 10 mm and the average value was taken as 4.08 for ZTA-10 and 4.20 for ZTA-20.
I. Bending Strength
The bending strength was measured by the three-point bending strength test method of KS L 1591 (test method of bending strength at room temperature of fine ceramics monolithic ceramics). The specimens were chamfered with 3 × 4 × 35 mm, 10 chamfered, and polished on both sides. The average value was taken as 459 MPa for ZTA-10 and 657 MPa for ZTA-20.
All. Fracture Toughness
Fracture toughness was measured by the Indentation Fracture Method of KS L 1600 (Fracture Toughness Test Method for High Performance Ceramics). The size of the specimen was 20 × 20 × 5 mm and the surface to be measured was measured by mirror polishing. The value is 5.0 for ZTA-10
la. Coefficient of Thermal Expansion
The thermal expansion coefficient was measured in a temperature range of 25 to 600 ° C using a dilatometer based on KS L 1590 (Test method of thermal expansion coefficient of enamel, glaze and ceramics: thermal expansion method). ? 6 × 25 mm. The value of ZTA-10 was 6.83 × 10 -6 / K at 100 ° C., 7.56 × 10 -6 / K at 600 ° C., 6.34 × 10 -6 / K at 100 ° C. and 7.34 × 10 -6 / × 10 -6 / K.
In order to develop ZTA sintered bodies as described above, ZTA-10 and ZTA-20 granular powders were selected as raw materials, CIP molding was performed with a disk, and sintered bodies obtained by processing and sintering were subjected to physical properties measurement and comparative examples Table 1 summarizes.
(ZTA-10)
(ZTA-20)
(Al 2 O 3)
As shown in Table 1, the zirconia-alumina composite molded article shows improved mechanical properties such as density, strength, fracture toughness and the like compared with the case where alumina is used alone.
It will be understood by those skilled in the art that the foregoing description of the present invention is for illustrative purposes only and that those of ordinary skill in the art can readily understand that various changes and modifications may be made without departing from the spirit or essential characteristics of the present invention. will be. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive. For example, each component described as a single entity may be distributed and implemented, and components described as being distributed may also be implemented in a combined form.
The scope of the present invention is defined by the appended claims, and all changes or modifications derived from the meaning and scope of the claims and their equivalents should be construed as being included within the scope of the present invention.
Claims (11)
A filling step of filling the mixed powder into a mold;
Molding the mold into a pressure vessel for cold isostatic pressing and pressurizing the outside of the mold at a set pressure to form a zirconia-alumina composite molded article;
A demolding step of separating the molded zirconia-alumina composite article from the mold; And
A sintering step of sintering the deformed disk at a set temperature;
/ RTI >
In the molding step, a mold having been assembled and filled is vertically injected into a pressure vessel, and a pressure medium is applied to the mold at a pressure of 1000 to 1500 bar for 10 to 60 minutes to burn the zirconia-alumina composite molded body, , The molding density, and the porosity,
In the sintering step, a calcining process is performed at 950 to 1100 ° C to remove impurities contained in the formed body, and then the sintering process is performed at 1500 to 1650 ° C,
The partially stabilized zirconia contains yttria (Y 2 O 3 ), forms a tetragonal crystal phase at room temperature,
In the mixing step, 70 to 95 wt% of alumina powder and 5 to 30 wt% of zirconia powder are mixed with 100 wt% of mixed powder,
In the mixing step, the average particle size of the alumina powder is 04 to 0.8 mu m, the average particle size of the zirconia powder is 0.5 to 2.0 mu m,
Further comprising a vacuum step of forming the inside of the mold into a vacuum state after the filling step,
In the vacuum step, air in the mold is sucked from a vacuum port formed at one side of the mold,
And a surface treatment step of imparting a roughness of 0.28 to 0.40 and a smoothness of 0.015 to 0.035 to the formed body after the demolding step.
Further comprising a shape processing step of processing the size, shape and thickness of the formed body close to the set values after the demolding step.
Further comprising a precision machining step of finely machining the size, shape and thickness of the formed body after the sintering step so as to correspond to the set numerical values.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101924502B1 (en) * | 2017-06-13 | 2018-12-04 | (주)씨이케이 | Manufacturing method of porous ceramic using a hip |
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| KR100983875B1 (en) * | 2009-11-18 | 2010-09-27 | 천효민 | Zirconia-alumina ceramic compositions for artificial joint and method thereof |
| KR20120110129A (en) | 2009-12-28 | 2012-10-09 | 파나소닉 주식회사 | Method for producing zirconia-alumina composite ceramic material, zirconia-alumina composite granulated powder, and zirconia beads |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100983875B1 (en) * | 2009-11-18 | 2010-09-27 | 천효민 | Zirconia-alumina ceramic compositions for artificial joint and method thereof |
| KR20120110129A (en) | 2009-12-28 | 2012-10-09 | 파나소닉 주식회사 | Method for producing zirconia-alumina composite ceramic material, zirconia-alumina composite granulated powder, and zirconia beads |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101924502B1 (en) * | 2017-06-13 | 2018-12-04 | (주)씨이케이 | Manufacturing method of porous ceramic using a hip |
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