CN105712745A - Colored ceramic and preparation method thereof - Google Patents
Colored ceramic and preparation method thereof Download PDFInfo
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- CN105712745A CN105712745A CN201410720796.8A CN201410720796A CN105712745A CN 105712745 A CN105712745 A CN 105712745A CN 201410720796 A CN201410720796 A CN 201410720796A CN 105712745 A CN105712745 A CN 105712745A
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Abstract
The present invention discloses a colored ceramic preparation method, and the colored ceramic preparation method is characterized by comprising contacting a ceramic with a colored metal melt and / or a colored metal steam, wherein the contact temperature is higher than colored metal melting point temperature. The present invention also provides a colored ceramic prepared by the method, and the colored ceramic exhibits bright and uniform color.
Description
Technical field
The present invention relates to a kind of colored ceramic and preparation method thereof, particularly a kind of dark-grey pottery to black and preparation method thereof.
Background technology
Generally, colorant or coloring agent are joined in ceramic body or glaze by being prepared by of common colored ceramic, and are burnt till by high temperature and obtain.Especially for zirconia ceramics and aluminium oxide ceramics, its sintering temperature is higher, is typically in 1550-1650 DEG C.At this temperature, most colorant or coloring agent can decompose, volatilize.Therefore, the simple method adding colorant or coloring agent is adopted, it is difficult to prepare the colored ceramic of uniform in color.
Summary of the invention
It is an object of the invention to the defect of the painted difficulty overcoming the preparation process of existing colored ceramic to exist, it is provided that a kind of color method is simple and the preparation method of the colored ceramic of uniform in color and prepared colored ceramic thereof.
Present inventors discovered unexpectedly that, during the temperature heated to fusing point by coloring metal, the metal and/or the vaporish metal that produce liquid penetrate in pottery, can change original ceramic structure, the lattice making pottery is distorted, so that pottery presents color bright, uniform.And present inventor have further discovered that the pottery that the present invention is especially suitable for preparation Dark grey to black colour system.Based on above-mentioned opinion, the present inventor completes the present invention.
For this, the preparation method that the present invention provides a kind of colored ceramic, wherein, the method includes contacting pottery with the melt of coloring metal and/or the steam of coloring metal, and the temperature of described contact is more than the melting temperature of described coloring metal.
Present invention also offers the colored ceramic prepared and obtain by said method.
By the preparation method adopting the colored ceramic of the present invention, directly the pottery after sintering can be contacted with the melt of coloring metal and/or the steam of coloring metal, and by the temperature of control contact more than the melting temperature of described coloring metal, then can complete to pottery painted, from without adding a colorant to also unsintered pottery, thereby is achieved that color method is simple, the colored ceramic of uniform coloring.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention.
The preparation method that the present invention provides a kind of colored ceramic, wherein, the method includes: being contacted with the melt of coloring metal and/or the steam of coloring metal by pottery, the temperature of described contact is more than the melting temperature of described coloring metal.
According to the present invention, described pottery is the pottery after sinter molding, and the kind of pottery is not particularly limited by the present invention, it is possible to for commercially available product, it is also possible to the preparation method being the pottery conventional by this area is prepared.Owing to the preparation method of the colored ceramic of the present invention is comparatively applicable to the painted of zirconia ceramics and/or aluminium oxide ceramics, it is particularly suitable for the painted of zirconia ceramics, therefore, the pottery of the present invention is preferably zirconia ceramics and/or aluminium oxide ceramics, it is particularly preferred to for zirconia ceramics.For this, the preparation method that the present invention will provide zirconia ceramics and aluminium oxide ceramics especially, wherein, the preparation method of the zirconia ceramics of the present invention preferably includes following steps:
(1) claiming a certain amount of white oxide zirconium pelletizing to fill to mould, pressurize about 10-45s under absolute pressure 6-15MPa, mould unloading takes out ceramic body；
(2) being sintered by the ceramic body of step (1) gained, the condition of this sintering processes includes: is incubated 0.5-2h at 550-700 DEG C, then is incubated 0.5-2h at 1100-1300 DEG C, then is incubated 1-3h at 1400-1500 DEG C.
The sintering of other kinds of pottery can be adjusted correspondingly in the condition of sintering processes, for instance for aluminium oxide ceramics, the condition of its sintering processes preferably includes: 0.5-2h under being incubated at 550-700 DEG C, then is incubated 1-3h at 1500-1600 DEG C.
As above, although the preparation method of the colored ceramic of the present invention is comparatively applicable to the painted of aluminium oxide ceramics and/or zirconia ceramics, but the present inventor deeply finds, the preparation method of the present invention is more favorable for the painted of zirconia ceramics, painted more bright, that be more uniformly distributed zirconia ceramics, particularly Dark grey or black zirconia ceramics can be accessed.
According to the present invention, in order to carry out painted to described pottery better, it is preferable that in situation, described pottery is laminated structure, and its thickness can be 0.1-2mm, it is preferred to 0.5-1.6mm.Skilled person would appreciate that, the pottery of laminated structure here both can refer to potsherd, can also be ceramic body (such as ceramic cup, ceramic bottle etc.), as long as this ceramic body has uniform thickness, particularly thickness in above-mentioned thickness range.
According to the present invention, described coloring metal is not particularly limited, the metal enabling to ceramic coloring that any this area is conventional can be adopted, but the present invention finds through repetitious test, described coloring metal preferably employs the metal that metal saturated vapor pressure is higher, particularly preferably, described coloring metal is one or more in metallic aluminium and alloy, magnesium metal and alloy, manganese metal and alloy thereof and metal zirconium and alloy thereof, more preferably metallic aluminium, magnesium metal, manganese metal and metal zirconium and one or more in alloy thereof.It addition, the pottery more black in order to obtain chroma color, it is particularly preferred to for zirconium-base alloy, for instance zirconium alloy, zirconium magnesium alloy, zirconium kirsite.Preferably employ the zirconium-base alloy that zr element content is more than 50 weight %.Particularly preferably adopting chemical formula is Zr65Al20Ni15Zirconium alloy.
According to the present invention, in order to be conducive to the fusing of described coloring metal and produce steam, the coloring metal adopted can be lamellar, block and Powdered, it is preferable that have the metal dust that granularity is less, such as the granularity of described coloring metal is 1-500 μm, it is preferred to 10-150 μm.
According to the present invention, although pottery is contacted with the melt of coloring metal and/or the steam of coloring metal, and described pottery is heated making described pottery can be painted to some extent at the temperature of the contact of the present invention, but so that the painted of described pottery is more uniformly distributed and becomes clear, under preferable case, relative to every mm2The surface area of described pottery, the consumption 0.1-1mg of described coloring metal.
According to the present invention, owing to the coloring process of the present invention both can utilize the melt of described coloring metal and contacting of described pottery, the steam of described coloring metal and contacting of described pottery can be utilized again, therefore, the position relationship of described coloring metal Yu described pottery is not particularly limited by the present invention, such as, before described contact, described coloring metal and described pottery are for being partially separated ground, being totally separated ground or be not positioned separately completely.That is, before described contact, can arbitrarily shelve in reaction vessel when described coloring metal and described pottery are joined in reaction vessel, such as can be laid on the surface of described pottery by described coloring metal part another part and then separate with pottery and shelve, or described coloring metal almost can be laid on the surface of described pottery completely, or by described coloring metal with described pottery is completely separable shelves.Additionally, be in that be partially separated and complete unseparated situation at described coloring metal and described pottery, it is possible to utilize the melt of coloring metal to contact with pottery under the Contact Temperature of the present invention, thus completing painted.Therefore, when above-mentioned position relationship is not specially required by the present invention, for convenient operation, those skilled in the art can preferably employ modes of emplacement that is that be partially separated or that be kept completely separate.And painted in order to be beneficial to, those skilled in the art can preferably employ again be partially separated and complete unseparated modes of emplacement.
According to the present invention, as long as although namely the temperature of described contact can realize the goal of the invention of the present invention more than the melting temperature of described coloring metal, but consider from for the restriction reducing cost and firing equipment, under preferable case, the temperature of described contact is in the temperature range between the melting temperature and boiling temperature of described coloring metal.Also for the performance (such as thermal shock resistance etc.) ensureing gained pottery, it is more preferred to, the temperature of described contact is not higher than the sintering temperature of described pottery.Especially, if but can close to or up the temperature of the boiling point of described coloring metal when the Contact Temperature adopted is not higher than the sintering temperature of described pottery, it is possible to obtain more sufficient steam.In this respect, therefore the present invention can preferably employ again such boiling point coloring metal lower than ceramic sintering temperature, for instance metallic zinc.
According to the present invention, although the preparation method of the colored ceramic of the present invention is not particularly limited, however, to ensure that the tinctorial quality of coloring metal and utilization rate, the present invention carries out preferably in airtight reaction vessel.In order to prevent other gas reactions of described coloring metal and reaction vessel, reaction vessel can be carried out evacuation process or add noble gas air-out, but also for reducing the temperature of described contact, under preferable case, described contact carries out in a vacuum, thus the present invention can just reach more than the melting temperature of described coloring metal at lower temperature.It is highly preferred that the absolute pressure of this vacuum environment is 10-1-10-5Pa, more preferably 10-3-10-5Pa。
In the present invention, it is preferred to described contact adopts the mode that heats stage by stage, for instance be 10 in above-mentioned absolute pressure-1-10-5When Pa, for the metallic aluminium of coloring metal specifically preferred according to the invention, magnesium metal, manganese metal and metal zirconium and alloy thereof, the condition of this mode heated stage by stage includes: heat up through 30-60min (being preferably 40-50min) to 400-550 DEG C (being preferably 450-500 DEG C) from 20-50 DEG C, after insulation 8-30min (is preferably 10-15min), being warming up to 700-1100 DEG C (being preferably 850-950 DEG C) then through 30-100min (being preferably 60-80min), insulation 20-120min (is preferably 60-90min).
It is particularly preferred that for metallic aluminium, this mode heated stage by stage includes: heat up through 30-50min to 400-550 DEG C from 20-50 DEG C, after insulation 10-20min, it is warming up to 700-900 DEG C then through 50-60min, is incubated 30-120min.
It is particularly preferred that for magnesium metal, this mode heated stage by stage includes: heat up through 30-50min to 500-550 DEG C from 20-50 DEG C, after insulation 10-30min, it is warming up to 700-1000 DEG C then through 30-60min, is incubated 30-90min.
It is particularly preferred that for manganese metal, this mode heated stage by stage includes: heat up through 30-50min to 500-550 DEG C from 20-50 DEG C, after insulation 8-30min, it is warming up to 900-1100 DEG C then through 50-90min, is incubated 30-90min.
It is particularly preferred that for metal zirconium and alloy thereof, this mode heated stage by stage includes: heat up through 30-50min to 500-550 DEG C from 20-50 DEG C, after insulation 8-30min, it is warming up to 900-1050 DEG C then through 30-100min, is incubated 20-60min.
After the heat treated of the present invention, cooling gained pottery, preferably the pottery after cooling is processed by shot blasting, particularly adopt be partially separated and in complete unseparated situation, process and be more uniformly distributed bright colored ceramic with greater need for carrying out surface finish obtaining surface colour.
Present invention also offers the colored ceramic prepared by the preparation method of above-mentioned colored ceramic.
Hereinafter will be described the present invention by embodiment.
In following example and comparative example,
Fracture toughness test is to test according to the Single edge notch beam recorded in GBT23806；
Colourity test is by adopting color difference analysis instrument to be contrasted by the blackout standard sample of the colored ceramic sheet of following example and comparative example gained Yu white carbon black, and wherein, the Δ L of definition white carbon black is 0；Value of chromatism Δ L be on the occasion of, represent partially whiter than white carbon black；Δ L is negative value, represents partially more black than white carbon black.
Preparation example 1
Claiming 20g white oxide zirconium powder to fill to mould, pressurize about 40s under pressure 10MPa, mould unloading takes out ceramic body.Being placed in high temperature furnace by gained ceramic body and be sintered, the condition of sintering processes includes: is incubated 1h at 600 DEG C, then is incubated 1.5h at 1200 DEG C, then is incubated 2h at 1450 DEG C.After sintering, the pottery of gained is white oxide zircon ceramic.
Preparation example 2
The alumina powder claiming 20g is filled to mould, pressurize about 35s under pressure 10MPa, and mould unloading takes out ceramic body.Being placed in high temperature furnace by gained ceramic body and be sintered, the condition of sintering processes includes: 1.5h under being incubated at 600 DEG C, then is incubated 3h at 1550 DEG C.The pottery of sintering gained is white alumina pottery.
Embodiment 1
The present embodiment is for colored ceramic that the present invention is described and preparation method thereof.
Zirconia ceramics in preparation example 1 is shaped to surface area is 3320mm2The potsherd of (upper and lower surface sum), thickness 1.6mm, and by this potsherd and 0.5g aluminium powder (analytical pure, granularity is 75 μm, purchased from Shanghai crystalline substance pure reagent company limited) it is placed in airtight vacuum drying oven, and this potsherd and aluminium powder are discontiguous；Then vacuum drying oven is carried out evacuation, be 10 to absolute pressure-3Start to warm up during Pa and rise to 500 DEG C from room temperature (20 DEG C) through 50min, after insulation 10min, 900 DEG C are risen to through 60min again from 500 DEG C, insulation 1.5h, then natural cooling gained potsherd carry out plain grinding polishing, it is painted bright uniform, thus obtaining the colored ceramic C1 of the present invention, the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 2
The present embodiment is for colored ceramic that the present invention is described and preparation method thereof.
Zirconia ceramics in preparation example 1 is shaped to surface area is 3320mm2The potsherd of (upper and lower surface sum), thickness 1.6mm, and by this potsherd and 1g aluminium powder (analytical pure, granularity is 75 μm, purchased from Shanghai crystalline substance pure reagent company limited) it is placed in airtight vacuum drying oven, and aluminium powder is sprinkled upon on this potsherd uniformly；Then carry out evacuation, be 10 to absolute pressure-3Start to warm up during Pa and rise to 500 DEG C from room temperature (20 DEG C) through 50min, after insulation 10min, 900 DEG C are risen to through 80min again from 500 DEG C, insulation 1.5h, then natural cooling gained potsherd carry out plain grinding polishing, thus obtaining the colored ceramic C2 of the present invention, it is painted bright uniform, and the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 3
The present embodiment is for colored ceramic that the present invention is described and preparation method thereof.
According to the method described in embodiment 2, institute the difference is that, adopt the manganese powder (analytical pure of 0.5g, granularity is 100 μm, purchased from Tianjin Kermel Chemical Reagent Co., Ltd.) replace aluminium powder, and with embodiment 2 also to some extent the difference is that its final holding temperature is 1100 DEG C, thus obtaining the colored ceramic C3 of the present invention, it is painted bright uniform, and the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 4
The present embodiment is for colored ceramic that the present invention is described and preparation method thereof.
According to the method described in embodiment 3, institute the difference is that, be 0.5h wait being warming up to the time of insulation after 1100 DEG C, thus obtaining the colored ceramic C4 of the present invention, its painted bright uniformly, the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 5
The present embodiment is for colored ceramic that the present invention is described and preparation method thereof.
Zirconia ceramics in preparation example 1 is shaped to surface area is 3320mm2The potsherd of (upper and lower surface sum), thickness 1.6mm, and by this potsherd and 2.5g magnesium powder (analytical pure, granularity is 150 μm, purchased from Xilong Chemical Co., Ltd) it is placed in airtight vacuum drying oven, and this potsherd and magnesium powder are discontiguous；Then carry out evacuation, be 0.5 × 10 to absolute pressure-4Start to warm up during Pa and rise to 400 DEG C from room temperature (20 DEG C) through 40min, after insulation 8min, 850 DEG C are risen to through 60min again from 400 DEG C, insulation 2h, then natural cooling gained potsherd carry out plain grinding polishing, thus obtaining the colored ceramic C5 of the present invention, it is painted bright uniform, and the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 6
The present embodiment is for colored ceramic that the present invention is described and preparation method thereof.
Zirconia ceramics in preparation example 1 is shaped to surface area is 3320mm2The potsherd of (upper and lower surface sum), thickness 1.6mm, and (chemical formula is Zr by this potsherd and 0.6g zirconium alloy powder65Al20Ni15, analytical pure, granularity is 100 μm, purchased from Biyadi Co Ltd) be placed in airtight vacuum drying oven, and this potsherd and magnesium powder are discontiguous；Then carry out evacuation, be 1 × 10 to absolute pressure-4Start to warm up during Pa and rise to 500 DEG C from room temperature (20 DEG C) through 50min, after insulation 10min, 950 DEG C are risen to through 80min again from 500 DEG C, insulation 1h, then natural cooling gained potsherd carry out plain grinding polishing, thus obtaining the colored ceramic C6 of the present invention, it is painted bright uniform, and the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 7
According to the method described in embodiment 2, institute the difference is that, adopt alumina ceramic plate to replace zirconia ceramics sheet, thus obtaining the colored ceramic C7 of the present invention, its painted comparatively bright uniformity is not high, and the test of its fracture toughness and colourity test result are in Table 1.
Embodiment 8
According to the method described in embodiment 2, institute the difference is that, zinc metal powder is adopted to replace aluminium powder, wherein, owing to the boiling point of this metal is relatively low, therefore, with embodiment 2 also to some extent the difference is that its final holding temperature is 800 DEG C, thus obtaining the colored ceramic C8 of the present invention, its painted comparatively bright uniformity is not high, and the test of its fracture toughness and colourity test result are in Table 1.
Table 1
| Potsherd | Fracture toughness (MPa m1/2) | Colourity Δ L |
| C1 | 5 | 24.41 |
| C2 | 5 | 20.18 |
| C3 | 5.5 | 25.33 |
| C4 | 5.5 | 33.05 |
| C5 | 5 | 36.63 |
| C6 | 5 | 19.36 |
| C7 | 5 | 41.55 |
| C8 | 5.5 | 60.53 |
| The zirconia ceramics of preparation example 1 | 5.5 | 87.67 |
The preferred embodiment of the present invention described in detail above; but, the present invention is not limited to the detail in above-mentioned embodiment, in the technology concept of the present invention; technical scheme can being carried out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that, each concrete technical characteristic described in above-mentioned detailed description of the invention, in reconcilable situation, it is possible to be combined by any suitable mode, in order to avoid unnecessary repetition, various possible compound modes are no longer illustrated by the present invention separately.
Additionally, can also carry out combination in any between the various different embodiment of the present invention, as long as it is without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the preparation method of a colored ceramic, it is characterised in that the method includes: being contacted with the melt of coloring metal and/or the steam of coloring metal by pottery, the temperature of described contact is more than the melting temperature of described coloring metal.
2. method according to claim 1, wherein, the temperature of described contact is in the temperature range between the melting temperature and boiling temperature of described coloring metal.
3. method according to claim 1, wherein, described coloring metal is one or more in metallic aluminium and alloy, magnesium metal and alloy, manganese metal and alloy thereof and metal zirconium and alloy thereof, it is preferred to metallic aluminium, magnesium metal, manganese metal and metal zirconium and one or more in alloy thereof.
4. method according to claim 3, wherein, described contact adopts the mode heated stage by stage, the condition of the described mode heated stage by stage includes: heat up through 30-60min to 400-550 DEG C from 20-50 DEG C, after insulation 8-30min, it is warming up to 700-1100 DEG C then through 30-100min, is incubated 20-120min.
5. method according to claim 4, wherein, the condition of the described mode heated stage by stage includes: heat up through 40-50min to 450-500 DEG C from 20-50 DEG C, after insulation 10-15min, is warming up to 850-950 DEG C then through 60-80min, is incubated 60-90min.
6. method according to claim 1, wherein, described contact carries out in a vacuum, and the absolute pressure of vacuum is 10-1-10-5Pa。
7. the method according to claim 1 or 3, wherein, relative to every mm2The surface area of described pottery, the consumption 0.1-1mg of described coloring metal.
8. the method according to any one in claim 1-7, wherein, described pottery is zirconia ceramics and/or aluminium oxide ceramics.
9. method according to claim 8, wherein, described pottery is zirconia ceramics.
10. the colored ceramic that the method described in any one in claim 1-9 prepares.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108129169A (en) * | 2016-12-01 | 2018-06-08 | 比亚迪股份有限公司 | A kind of ceramic-metal combination and preparation method thereof |
| TWI774516B (en) * | 2021-08-13 | 2022-08-11 | 吳興昌 | Ceramic sticking method |
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| CN1450193A (en) * | 2003-05-08 | 2003-10-22 | 上海交通大学 | High-energy ultrasonic metal coating method for ceramic surface |
| CN103342584A (en) * | 2013-07-03 | 2013-10-09 | 哈尔滨工业大学 | Ultrasonic-assisted local metallizing method on surface of ceramic |
| CN104119095A (en) * | 2013-04-27 | 2014-10-29 | 比亚迪股份有限公司 | Metal-ceramic composite product and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1052473A (en) * | 1988-12-14 | 1991-06-26 | 李周雄 | Ceramic-metal bonding |
| CN1450193A (en) * | 2003-05-08 | 2003-10-22 | 上海交通大学 | High-energy ultrasonic metal coating method for ceramic surface |
| CN104119095A (en) * | 2013-04-27 | 2014-10-29 | 比亚迪股份有限公司 | Metal-ceramic composite product and preparation method thereof |
| CN103342584A (en) * | 2013-07-03 | 2013-10-09 | 哈尔滨工业大学 | Ultrasonic-assisted local metallizing method on surface of ceramic |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108129169A (en) * | 2016-12-01 | 2018-06-08 | 比亚迪股份有限公司 | A kind of ceramic-metal combination and preparation method thereof |
| CN108129169B (en) * | 2016-12-01 | 2021-01-19 | 比亚迪股份有限公司 | Metal ceramic product and preparation method thereof |
| TWI774516B (en) * | 2021-08-13 | 2022-08-11 | 吳興昌 | Ceramic sticking method |
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Application publication date: 20160629 |