CN103382112A - Preparation method of dark-blue zirconia ceramic - Google Patents
Preparation method of dark-blue zirconia ceramic Download PDFInfo
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- CN103382112A CN103382112A CN2013102709130A CN201310270913A CN103382112A CN 103382112 A CN103382112 A CN 103382112A CN 2013102709130 A CN2013102709130 A CN 2013102709130A CN 201310270913 A CN201310270913 A CN 201310270913A CN 103382112 A CN103382112 A CN 103382112A
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Abstract
The invention provides a preparation method of dark-blue zirconia ceramic. The method comprises following steps: step one, taking zirconia powder as the base material, adding at least one component from following components: cobalt ferrite, cobalt oxide and cobalt aluminate in the zirconia powder as the coloring agent, and adding polyvinyl alcohol water solution in the zirconia powder as the binder; step two, putting the mixture of the ceramic raw materials prepared in the step one into a ball-grinding bottle to grind until the mixture is homogenously mixed, pouring out the suspending liquid in the ball-grinding bottle, drying the suspending liquid to remove the water, and obtaining ceramic powder; step three, pressing the ceramic powder obtained in the step two into required ceramic bodies through the dry pressing technology or the isostatic pressing technology; step four, putting the ceramic bodies obtained in the step three into a high-temperature sintering furnace after slow glue discharging to sinter into products. The preparation method produces a dark-blue zirconia ceramic, and the ceramic contains a coloring material. The coloring material can stably exist at the temperature of 1500 DEG C, furthermore, the coloring material not only can guarantee that zirconia is sintered into a completely compact state, but also makes the zirconia ceramic have a dark-blue appearance.
Description
Technical field
The invention belongs to the oxide ceramics technical field, relate to a kind of preparation method of pottery, especially in regard to a kind of preparation method of mazarine zirconia ceramics.
Background technology
Molar fraction is that 3% the partially stabilized tetragonal zircite ceramic of yttrium oxide (3Y-TZP) is a kind of very important structural ceramic material, it has very excellent mechanical property, has the flexural strength up to 1000MPa, fracture toughness property is up to 10MPa m1/2, therefore the good reputation that Ceramo-steel is arranged has more and more important application in industrial machinery and daily life.Often need good outward appearance as civilian zirconia ceramics product, such as color, gloss etc., but the zirconium white product of natural sintering is ivory white, single this color is difficult to satisfy people's demand growing to the zirconium white ornament, therefore the zirconium white product of exploitation different colours is imperative.But due to as the zirconia material sintering temperature of structural ceramics all higher than 1400 ℃, and as the additive colorant high-temperature stability that changes the zirconium white color non-constant all, generally only can stablize below 1300 ℃ painted, in order to make zirconium white densified sintering product at the temperature below 1300 ℃, someone adopts hot pressed sintering to prepare colored zirconia, but the zirconium white of preparation is very high to the sintering oven requirement like this, and production cost sharply rises, and is not suitable for the civilian ornament market of relative low price.
Summary of the invention
The purpose of this invention is to provide and a kind ofly have the colorant that can exist at 1500 ℃ of high temperatures, and this colorant is guaranteeing to play the preparation method who zirconium white is coloured to navy blue mazarine zirconia ceramics under the complete fully dense prerequisite of Zirconium oxide sintering.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of preparation method of mazarine zirconia ceramics, it comprises the steps:
Step 1, use Zirconium oxide powder to be matrix material, add one or more raw materials in cobalt ferrite, cobalt oxide, Leyden blue as tinting material, add polyvinyl alcohol water solution as binding agent;
Step 2, with the mixture of the ceramic raw material in step 1 put into the ball milling bottle be milled to mix after, pour out the suspension liquid in the ball milling bottle, liquid moisture is removed in oven dry, obtains ceramic powder;
Step 3, by dry-pressing or isostatic pressing process, the ceramic powder that obtains in step 2 is pressed into required ceramic body;
Step 4, sinter through putting into high temperature sintering furnace after slow binder removal the ceramic body that obtains in step 3 into goods.
As the preparation method's of a kind of mazarine zirconia ceramics of the present invention preferred version, wherein said zirconium white is that molar fraction is 3% stabilized with yttrium oxide tetragonal zircite, and its median size is 0.5 μ m.
Preferred version as the preparation method of a kind of mazarine zirconia ceramics of the present invention, wherein said cobalt ferrite, cobalt oxide, Leyden blue are nanoscale powder, purity is 99.5%, and median size is 50nm, and its add-on as tinting material accounts for the 1-10% of zirconic weight percent
As the preparation method's of a kind of mazarine zirconia ceramics of the present invention preferred version, the add-on of wherein said binding agent accounts for the 1-5% of the weight percent of whole ceramic powder.
As the preparation method's of a kind of mazarine zirconia ceramics of the present invention preferred version, the temperature of wherein said high temperature sintering is 1400-1550 ℃.
As the preparation method's of a kind of mazarine zirconia ceramics of the present invention preferred version, described sintering temperature is controlled as follows:
Temperature | Room temperature-1200 ℃ | 1200-1400℃ | 1400-1550℃ |
Time | 7-10h | 3-5h | 4-6h |
。
As the preparation method's of a kind of mazarine zirconia ceramics of the present invention preferred version, described sintering temperature is controlled as follows:
。
Compared with prior art, the present invention has following at least beneficial effect:
One, raw material sources are wide, and matrix material adopts the commercial oxidation zirconium powder of selling on the market, and tinting material adopts homemade nanometer cobalt salt, need not to worry the source problem that comes of raw material.
Two, cost is lower, adopts non-pressure sintering technology to prepare the mazarine zircite product, has reduced greatly cost than the mode of hot pressed sintering.
Three, performance undamaged, tinting material at high temperature still can stable existence, makes zirconic sintering can reach temperature required, has guaranteed the original mechanical property of zirconium white.
Four, make simply, be fit to large batch of commercially producing.
Description of drawings
Fig. 1 is blue characterization spectrogram in embodiment two.
Embodiment
The preparation method of a kind of mazarine zirconia ceramics of the present invention, it comprises the steps: one, uses Zirconium oxide powder to be matrix material, add one or more raw materials in cobalt ferrite, cobalt oxide, Leyden blue as tinting material, add polyvinyl alcohol water solution as binding agent; Two, the mixture of above-mentioned ceramic raw material is put into the ball milling bottle be milled to mix after, pour out the suspension liquid in the ball milling bottle, liquid moisture is removed in oven dry, obtains ceramic powder; Three, by dry-pressing or isostatic pressing process, ceramic powder is pressed into required ceramic body; Four, sinter ceramic body into goods through putting into high temperature sintering furnace after slow binder removal.Below in conjunction with specific embodiment, the present invention is made detailed explanation:
Embodiment one:
taking 30 gram polyvinyl butyral acetals is dissolved in 5000 gram raw spirits, fully pour in 5L ball milling bottle after dissolving, adding 1000 gram molar fractions is that (purity is 99% to 3% yttria-stabilized zirconia powder, median size is 0.5 μ m), take 20 gram Leyden blues and 10 gram cobalt oxides add in the ball milling bottle simultaneously, Leyden blue and cobalt oxide are analytical pure, take 10 gram polymines as dispersion agent, after ball milling 24h, suspension liquid is poured out, after alcohol is removed in oven dry, after grinding ceramic powder broken and crossing 500 eye mesh screens, the standby one-tenth of isostatic pressing diameter is 20 millimeters, length is the zirconium white rod of 100 millimeters.Through after slow binder removal, put into high temperature sintering furnace and sinter goods into.During sintering, heating curve is:
The zircite product of firing adopts the Archimedes' principle detection density, adopt the Vickers' hardness of microhardness instrument test material, adopt the flexural strength of three point bending test machine testing material, adopt shade Eye computer-aided colorimeter to detect zirconic color, adopt the CIE-1976-LAB colorimeter system.Before detection, to roughness Ra below 0.1, the zirconium white after polishing demonstrates extraordinary gloss to sample with diamond polishing.
Analytical results shows, the mazarine zirconium white product sintered density that this method is done reaches 6.02g/cm3, micro-vickers hardness Hv0.5 is 1500MPa, three-point bending strength is 600MPa, this mechanical experimental results shows, after adding blue colorant cobalt salt, zirconic mechanical strong team does not obviously descend, and surperficial this zirconia material is still kept its excellent mechanical property.The demonstration of colorimetric detection result, after adding the 5wt% tinting material, zirconium white presents mazarine (L=9 ± 0.5, a=22 ± 3, b=-75 ± 3), demonstrates good gloss through after polishing.Further experiment shows, changes the amount of tinting material, can change the depth of blue oxide zirconium color, and this shows, take nanocrystal cobalt aluminate and cobalt oxide as the composite coloration agent, can at high temperature stablize the colored zirconium oxide material.
Embodiment two:
taking 35 gram polyvinyl butyral acetals is dissolved in 5500 gram raw spirits, fully pour in 5L ball milling bottle after dissolving, adding 1100 gram molar fractions is that (purity is 99% to 4% yttria-stabilized zirconia powder, median size is 0.8 μ m), take 22 gram Leyden blues and 12 gram cobalt oxides add in the ball milling bottle simultaneously, Leyden blue and cobalt oxide are analytical pure, take 11 gram polymines as dispersion agent, after ball milling 24h, suspension liquid is poured out, after alcohol is removed in oven dry, after grinding ceramic powder broken and crossing 500 eye mesh screens, the standby one-tenth of isostatic pressing diameter is 20 millimeters, length is the zirconium white rod of 100 millimeters.Through after slow binder removal, put into high temperature sintering furnace and sinter goods into.During sintering, heating curve is:
The zircite product of firing adopts the Archimedes' principle detection density, adopt the Vickers' hardness of microhardness instrument test material, adopt the flexural strength of three point bending test machine testing material, adopt shade Eye computer-aided colorimeter to detect zirconic color, adopt the CIE-1976-LAB colorimeter system.Before detection, to roughness Ra below 0.1, the zirconium white after polishing demonstrates extraordinary gloss to sample with diamond polishing.
Analytical results shows, more than the mazarine zirconium white product sintered density that this method is done reaches 6.01g/cm3, micro-vickers hardness Hv0.5 is 1600MPa, three-point bending strength is 650MPa, this mechanical experimental results shows, after adding blue colorant cobalt salt, zirconic physical strength does not obviously descend, and surperficial this zirconia material is still kept its excellent mechanical property.The demonstration of colorimetric detection result, after adding the 5wt% tinting material, zirconium white presents mazarine (L=9 ± 0.5, a=22 ± 3, b=-75 ± 3), demonstrates good gloss through after polishing, and this indigo plant characterization spectrum is as shown in Figure 1.Because of the patent document requirement, represent blueness with black.
Further experiment shows, changes the amount of tinting material, can change the depth of blue oxide zirconium color, and this shows, take nanocrystal cobalt aluminate and cobalt oxide as the composite coloration agent, can at high temperature stablize the colored zirconium oxide material.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (8)
1. the preparation method of a mazarine zirconia ceramics, it is characterized in that: described method comprises the steps:
Step 1, use Zirconium oxide powder to be matrix material, add one or more raw materials in cobalt ferrite, cobalt oxide, Leyden blue as tinting material, add binding agent;
Step 2, with the mixture of the ceramic raw material in step 1 be milled to mix after, moisture is removed in oven dry, obtains ceramic powder;
Step 3, by dry-pressing or isostatic pressing process, the ceramic powder that obtains in step 2 is pressed into required ceramic body;
Step 4, the ceramic body that obtains in step 3 is become goods through high temperature sintering after binder removal.
2. the preparation method of a kind of mazarine zirconia ceramics according to claim 1, it is characterized in that: described binding agent is polyvinyl alcohol water solution.
3. the preparation method of a kind of mazarine zirconia ceramics according to claim 1, it is characterized in that: described zirconium white is that molar fraction is 3%~4% stabilized with yttrium oxide tetragonal zircite, and its median size is 0.5 μ m~0.8 μ m.
4. the preparation method of a kind of mazarine zirconia ceramics according to claim 1, it is characterized in that: described cobalt ferrite, cobalt oxide, Leyden blue are nanoscale powder, purity is 99.5%, and median size is 50nm, accounts for the 1-10% of zirconic weight percent as the add-on of tinting material.
5. the preparation method of a kind of mazarine zirconia ceramics according to claim 1, it is characterized in that: the add-on of described binding agent accounts for the 1-5% of the weight percent of whole ceramic powder.
6. the preparation method of a kind of mazarine zirconia ceramics according to claim 1, it is characterized in that: the temperature of described high temperature sintering is 1400 ° of C-1550 ° of C.
7. the preparation method of a kind of mazarine zirconia ceramics according to claim 1 is characterized in that: described sintering temperature is controlled as follows:
。
8. the preparation method of a kind of mazarine zirconia ceramics according to claim 1 is characterized in that: described sintering temperature is controlled as follows:
。
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JP2016216289A (en) * | 2015-05-19 | 2016-12-22 | 東ソー株式会社 | Blue zirconia sintered body |
CN106810245A (en) * | 2015-11-30 | 2017-06-09 | 比亚迪股份有限公司 | Zirconium base composite ceramic material(Pink colour)And preparation method thereof with shell or ornament |
CN106810243A (en) * | 2015-11-30 | 2017-06-09 | 比亚迪股份有限公司 | Zirconium base composite ceramic material(Black)And preparation method thereof with shell or ornament |
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