CN104671780A - Preparation method of pink zirconia ceramic - Google Patents
Preparation method of pink zirconia ceramic Download PDFInfo
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- CN104671780A CN104671780A CN201410856827.2A CN201410856827A CN104671780A CN 104671780 A CN104671780 A CN 104671780A CN 201410856827 A CN201410856827 A CN 201410856827A CN 104671780 A CN104671780 A CN 104671780A
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Abstract
The invention relates to a preparation method of pink zirconia ceramic. The preparation method comprises the following steps: with zirconia powder as a raw material of a ceramic matrix, adding erbium oxide powder to the zirconia powder to be used as a colorant and adding a binder to form a mixed material; preparing a ceramic body by using the mixed material; and carrying out multi-stage sintering treatment on the ceramic body to obtain a pink zirconia ceramic product, wherein the multi-stage sintering treatment at least comprises the following stages: firstly sintering for 7-9h at the temperature of room temperature to 600 DEG C, then sintering for 4-8h at the temperature of 600 DEG C-1200 DEG C, and then sintering for 6-8h at the temperature of 1200 DEG C-1500 DEG C. By utilizing the preparation method of the pink zirconia ceramic, zirconia can be stably colored to pink by pigment on premise of ensuring complete compactness of sintering of zirconia, and low manufacturing cost is maintained simultaneously.
Description
Technical field
The present invention relates to a kind of preparation method of pink zirconia ceramics.
Background technology
Zirconia ceramics is a kind of very important structural ceramic material, it has very excellent mechanical property, and have the flexural strength up to 1000MPa, fracture toughness property is up to 10MPam1/2, there is the good reputation of Ceramo-steel, therefore all in an increasingly wide range of applications in industrial machinery and daily life.
Beautiful outward appearance is often needed, such as color, gloss etc. as civilian zirconia ceramics product; But the powder sintered ceramic product out of pure zirconia is white, single this color is difficult to meet people's demand growing to zirconia ceramics ornament, therefore the zirconia ceramics product of exploitation different colours is imperative.
But because the zirconia material sintering temperature as structural ceramics is general all higher than 1400 DEG C, and generally as all non-constant of additive colorant high-temperature stability changing zirconium white color, only just can stablize painted at about 1300 DEG C, thus cause the colored zirconia ceramics product that sinters out very crisp, the whiteware product that intensity sinters out far away from pure zirconia.
In order to can make the general colorant of interpolation Zirconium oxide powder can at the temperature of about 1300 DEG C densified sintering product, also someone adopts hot pressed sintering to prepare colored zirconia ceramics product.But take this method very high to the performance requriements of sintering oven to prepare colored zirconia ceramics, and hot pressed sintering process and equipment complexity, production control requires very tight, moulding stock requires high, energy consumption is large, production efficiency is low, causes production cost sharply to rise, and is not suitable for the civilian china ornament market of relative low price in this way.
Summary of the invention
Main purpose of the present invention is for the deficiencies in the prior art, a kind of preparation method of pink zirconia ceramics is provided, under the complete fully dense prerequisite of guarantee Zirconium oxide sintering, make colorant at high temperature be coloured to pink to Zirconia-stabilized, keep lower cost of manufacture simultaneously.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for pink zirconia ceramics, comprises the following steps:
A. in the Zirconium oxide powder as ceramic matrix raw material, add Erbium trioxide powder as tinting material, and add binding agent, form compound;
B. described compound is used to make ceramic body;
C. multistage segmentation sintering processes is carried out to described ceramic body, obtain pink zirconia ceramics product; Wherein said multistage segmentation sintering processes at least comprised with the next stage: first at the temperature of room temperature-600 DEG C, sinter 7-9h, next at the temperature of 600 DEG C-1200 DEG C, sinter 4-8h, then at the temperature of 1200 DEG C-1500 DEG C, sinter 6-8h.
In step c, 8h is sintered at the temperature of room temperature-600 DEG C, 6h is sintered at the temperature of 600 DEG C-1200 DEG C, at the temperature of 1200 DEG C-1500 DEG C, be further divided into following two stages sinters: be greater than 1200 DEG C be less than the temperature of upper limit high temperature threshold value under sinter 3h, then at the temperature of described upper limit high temperature threshold value, 4h is sintered, wherein said upper limit high temperature threshold value value in 1450-1500 DEG C.
Described upper limit high temperature threshold value is 1465-1475 DEG C, is more preferably 1470 DEG C.
Described Zirconium oxide powder is the stable tetragonal zirconium dioxide powder containing yttrium oxide, and median size is 0.5 μm.
Erbium trioxide as tinting material is median size to be 50nm purity be 99.5% ultrafine powder, its weight is the 1-10% of Zirconium oxide powder.
Described binding agent is polyvinyl alcohol.
The weight of polyvinyl alcohol is the 1-5% of Zirconium oxide powder.
Step b comprises: put into by described compound after ball grinder is milled to and mixes, pour out the suspension liquid in ball grinder, dry removing liquid moisture, mill after sieving and obtain ceramic powder; By compression moulding technique, described ceramic powder is pressed into described ceramic body.
Described compression moulding technique comprises dry-pressing and cold isostatic compaction technique.
Step b comprises the injection molding after banburying of the described compound of use and becomes ceramic body.
Compared with prior art, the present invention has at least following beneficial effect:
The present invention is to by ceramic matrix powder, tinting material, the ceramic body that binding agent is formed carries out multistage segmentation sintering processes, wherein at least pass through with the next stage: first at the temperature of room temperature-600 DEG C, sinter 7-9h, next at the temperature of 600 DEG C-1200 DEG C, 4-8h is sintered, then at the temperature of 1200 DEG C-1500 DEG C, 6-8h is sintered, research finds, sectional type sintering is carried out according to such temperature and time, both Erbium trioxide tinting material can be made to stablize on ceramic product painted, can reach again for enough sintering temperatures and time zirconia material simultaneously, make product compactness good, to performance undamaged, and manufacture craft cost of the present invention is lower, air sintering process with no pressure can be adopted to prepare pink zirconia ceramic product, mode than hot pressed sintering greatly reduces cost.Preparation technology of the present invention is simple and easy to use, is applicable to large batch of commercially producing.
Embodiment
Below embodiments of the present invention are elaborated.It is emphasized that following explanation is only exemplary, instead of in order to limit the scope of the invention and apply.
According to embodiments of the invention, the preparation method of pink zirconia ceramics comprises the following steps:
In the Zirconium oxide powder as ceramic matrix raw material, add Erbium trioxide powder as tinting material, and add binding agent, form compound.Compound is used to make ceramic body.Multistage segmentation sintering processes is carried out to obtain pink zirconia ceramics product to ceramic body, this multistage segmentation sintering processes at least comprised with the next stage: first at the temperature of room temperature-600 DEG C, sinter 7-9h, next at the temperature of 600 DEG C-1200 DEG C, sinter 4-8h, then at the temperature of 1200 DEG C-1500 DEG C, sinter 6-8h.Preferably, at the temperature of 1200 DEG C-1500 DEG C, be further divided into following two stages sinters: be greater than 1200 DEG C be less than the temperature of upper limit high temperature threshold value under sinter 3h, then at the temperature of upper limit high temperature threshold value, 4h is sintered, wherein upper limit high temperature threshold value value in 1450-1500 DEG C.In an advantageous embodiment, upper limit high temperature threshold value is 1465-1475 DEG C, most preferably is 1470 DEG C.
In comparatively specific embodiment, the preparation method of pink zirconia ceramics can comprise the following steps:
Step one, use Zirconium oxide powder are matrix material, add Erbium trioxide as tinting material, add polyvinyl alcohol water solution as binding agent.
Step 2, the mixture of the ceramic raw material in step one put into after ball grinder is milled to and mixes, pours out the suspension liquid in ball grinder, dry removing liquid moisture, mill after sieving and obtain ceramic powder.
Step 3, by dry-pressing and cold isostatic compaction technique, the ceramic powder obtained in step 2 is pressed into required ceramic body.
Step 4, the ceramic body obtained directly is put into high temperature sintering furnace make pink zirconia ceramics product by binder removal, sintering integrated technique in step 3, sintering control process is as follows: first at the temperature of room temperature-600 DEG C, sinter 7-9h, next at the temperature of 600 DEG C-1200 DEG C, sinter 4-8h, then at the temperature of 1200 DEG C-1500 DEG C, sinter 6-8h.Preferably, first at the temperature of room temperature-600 DEG C, sinter 8h, next at the temperature of 600 DEG C-1200 DEG C, sinter 6h, then at the temperature of 1200 DEG C-1470 DEG C, sinter 3h, finally at the temperature of 1470 DEG C, sinter 4h.Above-mentioned preferred binder removal, sintering integrated technique are divided into four sections of sintering curres, first paragraph by relatively low temperature pyrolysis to remove binding agent polyvinyl alcohol; Again according to second and third, four sections of temperature arranged and time of distributing sinters, make colorant coloring stabilized and sinter ceramic body into dense structure.In most preferred embodiment 1470 DEG C using as upper limit high temperature threshold value, but value also can obtain more satisfactory effect in 1450-1500 DEG C, is especially good with value in 1450-1500 DEG C.
In a preferred embodiment, described Zirconium oxide powder is the stable tetragonal zirconium dioxide powder containing yttrium oxide, and its median size is 0.5 μm.
In a preferred embodiment, described colorant Erbium trioxide is ultrafine powder, and purity is 99.5%, and median size is 50nm, and its add-on as tinting material is the 1-10% of Zirconium oxide powder weight.
In a preferred embodiment, the add-on of described binding agent polyvinyl alcohol accounts for the weight percent of whole Zirconium oxide powder is 1-5%.
Further combined with specific examples, the present invention is made an explanation below:
Example:
Taking 20 grams of polyvinyl alcohol is dissolved in 1000 grams of water, pour in 5L ball grinder after abundant dissolving, add 1000 grams of stable tetragonal zircite powder (purity be 99%, median size be 0.5 μm) containing yttrium oxide and 50 grams of Erbium trioxides, after ball milling 24h, suspension liquid is poured out, after drying removing moisture, ceramic powder is milled and after mistake 500 eye mesh screens, is prepared into through dry-pressing and isostatic cool pressing the zirconium white cake that diameter is 28 millimeters, thickness is 8 millimeters.Put into high temperature sintering furnace binder removal again, sinter pink zirconia ceramic product into.
Binder removal, sintering integrated technique segmentation can be expressed as:
Experiment test is carried out to the zirconia ceramic product fired, wherein, adopt 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.Before detection, the polishing of sample diamond wheel and centrifugal finishing machine are polished to roughness Ra less than 0.1, and the pink zirconia ceramics after polishing demonstrates extraordinary gloss.Analytical results shows, and the pink zirconia ceramics product sintered density that present method obtains reaches 6.02g/cm
3, micro-vickers hardness Hv0.5 is 1500MPa, and three-point bending strength is 600MPa.This mechanical experimental results shows, and after adding Erbium trioxide colorant, zirconic physical strength does not obviously decline, and shows that the pink zirconia ceramics material made with present invention process still can maintain the mechanical property of its excellence.Colorimetric detection result shows, and after adding 5% tinting material, zirconium white presents pink, demonstrates good gloss after polishing.Further experiment test display, change the amount of tinting material, can change the depth of pink zirconia ceramics color, this shows, according to manufacture craft of the present invention, is that tinting material can be stablized and diversely colored zirconium oxide material with Erbium trioxide.
Above content combines concrete/preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; its embodiment that can also describe these makes some substituting or modification, and these substitute or variant all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. a preparation method for pink zirconia ceramics, is characterized in that, comprises the following steps:
A. in the Zirconium oxide powder as ceramic matrix raw material, add Erbium trioxide powder as tinting material, and add binding agent, form compound;
B. described compound is used to make ceramic body;
C. multistage segmentation sintering processes is carried out to described ceramic body, obtain pink zirconia ceramics product; Wherein said multistage segmentation sintering processes at least comprised with the next stage: first at the temperature of room temperature-600 DEG C, sinter 7-9h, next at the temperature of 600 DEG C-1200 DEG C, sinter 4-8h, then at the temperature of 1200 DEG C-1500 DEG C, sinter 6-8h.
2. the preparation method of pink zirconia ceramics as claimed in claim 1, it is characterized in that, in step c, 8h is sintered at the temperature of room temperature-600 DEG C, 6h is sintered at the temperature of 600 DEG C-1200 DEG C, at the temperature of 1200 DEG C-1500 DEG C, be further divided into following two stages sinters: be greater than 1200 DEG C be less than the temperature of upper limit high temperature threshold value under sinter 3h, then at the temperature of described upper limit high temperature threshold value, sinter 4h, wherein said upper limit high temperature threshold value value in 1450-1500 DEG C.
3. the preparation method of pink zirconia ceramics as claimed in claim 2, is characterized in that, described upper limit high temperature threshold value is 1465-1475 DEG C, is more preferably 1470 DEG C.
4. the preparation method of the pink zirconia ceramics as described in any one of claim 1-3, is characterized in that, described Zirconium oxide powder is the stable tetragonal zirconium dioxide powder containing yttrium oxide, and median size is 0.5 μm.
5. the preparation method of the pink zirconia ceramics as described in any one of claim 1-4, is characterized in that, the Erbium trioxide as tinting material is median size to be 50nm purity be 99.5% ultrafine powder, its weight is the 1-10% of Zirconium oxide powder.
6. the preparation method of the pink zirconia ceramics as described in any one of claim 1-4, is characterized in that, described binding agent is polyvinyl alcohol.
7. the preparation method of pink zirconia ceramics as claimed in claim 6, is characterized in that, the weight of described polyvinyl alcohol is the 1-5% of Zirconium oxide powder.
8. the preparation method of the pink zirconia ceramics as described in any one of claim 1-4, it is characterized in that, step b comprises: put into by described compound after ball grinder is milled to and mixes, pour out the suspension liquid in ball grinder, dry removing liquid moisture, mill after sieving and obtain ceramic powder; By compression moulding technique, described ceramic powder is pressed into described ceramic body.
9. the preparation method of the pink zirconia ceramics as described in any one of claim 1-4, is characterized in that, described compression moulding technique comprises dry-pressing and cold isostatic compaction technique.
10. the preparation method of the pink zirconia ceramics as described in any one of claim 1-4, is characterized in that, step b comprises the injection molding after banburying of the described compound of use and becomes ceramic body.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174916A (en) * | 2015-08-27 | 2015-12-23 | 哈尔滨工业大学 | Preparation method for nano-structure oxide ceramic material and application and detection method for trace substance amount by using the nano-structure oxide ceramic material |
| CN105827759A (en) * | 2016-05-06 | 2016-08-03 | 东莞劲胜精密组件股份有限公司 | Electronic product frame structure made of carbon fiber ceramic composite material and manufacturing method of the structure |
| CN106977197A (en) * | 2016-11-26 | 2017-07-25 | 佛山市尚好门窗有限责任公司 | Oxide yellow zirconia material |
| CN107500761A (en) * | 2017-09-29 | 2017-12-22 | 无锡特科精细陶瓷有限公司 | A kind of preparation method of dark-blue zirconia ceramic |
| CN108530061A (en) * | 2018-04-27 | 2018-09-14 | 深圳市丁鼎制造科技发展有限公司 | A kind of production method of emerald green zirconia ceramics |
| CN108689706A (en) * | 2018-08-10 | 2018-10-23 | 韶关市曲江区国睿高新材料有限公司 | A kind of preparation method of colored zirconia ceramics |
| CN109400150A (en) * | 2018-11-26 | 2019-03-01 | 江西赛瓷材料有限公司 | A kind of high-intensitive pink zirconia ceramics powder and its preparation method and application |
| CN111515378A (en) * | 2019-04-02 | 2020-08-11 | 深圳市泛海统联精密制造股份有限公司 | Process for directly forming colorful metal by MIM (metal injection molding) |
| CN115959903A (en) * | 2023-01-17 | 2023-04-14 | 领胜城科技（江苏）有限公司 | Colored zirconia ceramic product and preparation method and application thereof |
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| CN103382112A (en) * | 2013-06-28 | 2013-11-06 | 无锡特科精细陶瓷有限公司 | Preparation method of dark-blue zirconia ceramic |
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| CN103896626A (en) * | 2012-12-31 | 2014-07-02 | 秦皇岛爱迪特高技术陶瓷有限公司 | Dyeing technology for novel zirconia dental prosthesis |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174916A (en) * | 2015-08-27 | 2015-12-23 | 哈尔滨工业大学 | Preparation method for nano-structure oxide ceramic material and application and detection method for trace substance amount by using the nano-structure oxide ceramic material |
| CN105174916B (en) * | 2015-08-27 | 2017-06-16 | 哈尔滨工业大学 | Using micro-nano structure oxide ceramic material to the detection method of trace materials content |
| CN105827759A (en) * | 2016-05-06 | 2016-08-03 | 东莞劲胜精密组件股份有限公司 | Electronic product frame structure made of carbon fiber ceramic composite material and manufacturing method of the structure |
| CN106977197A (en) * | 2016-11-26 | 2017-07-25 | 佛山市尚好门窗有限责任公司 | Oxide yellow zirconia material |
| CN107500761A (en) * | 2017-09-29 | 2017-12-22 | 无锡特科精细陶瓷有限公司 | A kind of preparation method of dark-blue zirconia ceramic |
| CN108530061A (en) * | 2018-04-27 | 2018-09-14 | 深圳市丁鼎制造科技发展有限公司 | A kind of production method of emerald green zirconia ceramics |
| CN108689706A (en) * | 2018-08-10 | 2018-10-23 | 韶关市曲江区国睿高新材料有限公司 | A kind of preparation method of colored zirconia ceramics |
| CN109400150A (en) * | 2018-11-26 | 2019-03-01 | 江西赛瓷材料有限公司 | A kind of high-intensitive pink zirconia ceramics powder and its preparation method and application |
| CN109400150B (en) * | 2018-11-26 | 2021-11-02 | 江西赛瓷材料有限公司 | High-strength pink zirconia ceramic powder and preparation method and application thereof |
| CN111515378A (en) * | 2019-04-02 | 2020-08-11 | 深圳市泛海统联精密制造股份有限公司 | Process for directly forming colorful metal by MIM (metal injection molding) |
| CN115959903A (en) * | 2023-01-17 | 2023-04-14 | 领胜城科技（江苏）有限公司 | Colored zirconia ceramic product and preparation method and application thereof |
| CN115959903B (en) * | 2023-01-17 | 2024-02-20 | 领胜城科技（江苏）有限公司 | Colored zirconia ceramic product and preparation method and application thereof |
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