CN106673442B - A kind of preparation method with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze - Google Patents
A kind of preparation method with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze Download PDFInfo
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- CN106673442B CN106673442B CN201611218346.4A CN201611218346A CN106673442B CN 106673442 B CN106673442 B CN 106673442B CN 201611218346 A CN201611218346 A CN 201611218346A CN 106673442 B CN106673442 B CN 106673442B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
- C03C8/20—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
- C04B41/5023—Glass-ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
Abstract
A kind of preparation method with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, by quartz, potassium feldspar, albite, borax, Y2O3, Suzhou soil, after lithium carbonate ingredient in 1270-1290 DEG C of heat preservation 20-40min, taking-up is poured into water quenching and frit is made, and frit is ground to obtain A material；By A material, Y2O3、ZrO2And Suzhou soil ingredient, obtain B material；B material and dispersing agent are added to the water, stirs and evenly mixs and is configured to glaze slip；By glaze slip glazing in ceramic surface, it is fired into photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze.1. the present invention prepares ceramic glaze using the technique of firing, do not need to carry out plated film, so that the function ceramics glaze of preparation is tightly combined with ceramic matrix, Y2O3With ZrO2The photochemical catalyst Y generated during the sintering process2Zr2O7It is evenly distributed in glaze, not generating " rainbow effect " influences glaze aesthetics.
Description
Technical field
The invention belongs to the technical fields of ceramic glaze, and in particular to one kind has photo-catalysis function zirconic acid yttrium micro-crystalline ceramic
The preparation method of glaze is applied to construction sanitary ceramic and field of household ceramic.
Background technique
With the development of modern society, during Rapid-Urbanization, social contradications and environmental problem are also gradually highlighted,
Especially in recent years, air quality endure to the fullest extent the whole people denounce [Guo Shihong, it is brilliant, wait air quality and urbanization quality rapport
Research [J] ecological economy, 2015,31 (3): 25-30.].It is known that in the domestic environment being closely connected with people's life,
The air pollutants being primarily present include volatile organic matter, Air colony, CO2Deng [village know quick Indoor decoration and
Shenyang release rule research [D] of typical pollutant: Northeastern University, 2009:2-3.], and by using in people's daily life
Construction sanitary ceramic and domestic ceramics big and be seen everywhere are measured, and assigns its photocatalytic self-cleaning function, just agrees with people couple
In the health requirements and environment protection requirement of ceramic product.
The difference of this kind of new ceramics and traditional ceramics with photo-catalysis function is that the materials such as surface glaze not
Together.Not only there is photocatalysis ceramics glaze general opaque glaze the mechanical strength of product can be improved, cover body defect, prevent from seeping water
With it is ventilative, the advantages of increasing the aesthetic feeling of product [Hubei Lee family coltfoal domestic ceramics technology [M]: publishing house of Wuhan University of Technology,
1992.] the advantages of, and again combining catalysis material, under the conditions of existing for the natural light, to being adsorbed on ceramic frit surface
Organic pollutant, toxic gas molecule and bacterium degrade, to reach self-cleaning effect.
And the leitungskern as photocatalysis ceramics, zirconic acid yttrium (Y2Zr2O7) it is a kind of with visible light-responded photocatalysis
Material has excellent photocatalytic degradation effect [Yuping Tong, Panpan Xue, et al.Preparation and
characterization of Y2Zr2O7nanocrystals and their photocatalytic properties
[J].Materials Science and Engineering B,150(2008)194–198.].In addition, according to the literature,
Zirconic acid yttrium (Y2Zr2O7) simultaneously or a kind of heat barrier coat material haveing excellent performance and fluorescent material [Julie M.Drexler,
Angel L.Ortiz,et al.Composition effects of thermal barrier coating ceramics
on their interaction with molten Ca–Mg–Al–silicate(CMAS)glass.Acta
Materialia, 60 (2012) 5437-5447.], also unexpected effect can be brought for ceramic glaze performance.Photocatalysis function
The common means that prepare that can be ceramic are first is that photochemical catalyst is added in ceramic glaze, then be sintered to obtain by usual ceramic process
Self-cleaning ceramic；Second is that being coated with photocatalyst film [Liu Ping, the Dai Wen of one layer of tens nm or several hundred nm on conventional ceramic surface
Newly, On Photocatalytic Functional Ceramics and its light degradation characteristic [J] environmental science, 2004,25 (4): 109-112. are waited].Above side
The shortcomings that method, or there are photocatalysis film and matrix associativity are poor, loss easy to fall off, or there are photochemical catalysts to be distributed in glaze
Unevenly, exist " rainbow effect " the disadvantages of, directly affect ceramics aesthetics.
Summary of the invention
It is an object of the invention to propose a kind of preparation method with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, the pottery
Glaze through by the way of glaze spraying glazing evenly dispersed micron order photocatalysis can be formed in ceramic glaze layer in ceramic surface
Object phase.The glaze of preparation had both had preferable glazing effect, while frit surface has good photocatalytic self-cleaning effect again.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, includes the following steps:
1) firstly, by quartz, potassium feldspar, albite, borax, Y2O3, Suzhou soil, lithium carbonate SiO in mass ratio2: Al2O3:
B2O3: Y2O3: Li2O:Na2O:K2O=(57-59): (4-6): (22-24): (2-4): (5-7): (2-4): (1-3) carries out ingredient；
2) powder after ingredient is dry-mixed and grind, sieving obtains mixture, and mixture is kept the temperature at 1270-1290 DEG C
20-40min, taking-up are poured into water quenching and frit are made, and frit is ground to obtain A material；
3) by A material, Y2O3、ZrO2And Suzhou soil is expected according to mass ratio A: Y2O3: ZrO2: Suzhou soil=(82-86):
(4.6-5): (5-5.4): the proportion of (5-7) carries out ingredient, and grinding obtains B material；
4) B material and dispersing agent are added to the water, stir and evenly mix and is configured to glaze slip；
5) glaze slip glazing is burnt into after dry through roller kilns oxidizing flame, firing temperature 1100-1140 in ceramic surface
DEG C, firing period is 40-50 minutes, and soaking time is 6-8 minutes under firing temperature, is obtained micro- with photo-catalysis function zirconic acid yttrium
Brilliant ceramic glaze.
A further improvement of the present invention lies in that grinding is carried out in ball grinder in step 2) and step 3, and frit:
Ball: water quality ratio is 1:1:0.8, and milling time is 3-5 hours.
A further improvement of the present invention lies in that the mass content of water is 44-50% in glaze slip in step 4).
A further improvement of the present invention lies in that the mass content of dispersing agent is 0.05-0.15% in glaze slip.
A further improvement of the present invention lies in that dispersing agent is sodium carboxymethylcellulose in step 4).
A further improvement of the present invention lies in that carrying out glazing using glaze spraying mode in step 5).
A further improvement of the present invention lies in that glazing is in step 5) with a thickness of 0.2-0.4mm.
A further improvement of the present invention lies in that temperature dry in step 5) is 60-80 DEG C.
A further improvement of the present invention lies in that firing atmosphere is oxidizing atmosphere in step 5).
Compared with prior art, the invention has the benefit that
1. the present invention prepares ceramic glaze using the technique of firing, do not need to carry out plated film, so that the function pottery of preparation
Glaze is tightly combined with ceramic matrix, Y2O3With ZrO2The photochemical catalyst Y generated during the sintering process2Zr2O7Divide in glaze
Cloth is uniform, and not generating " rainbow effect " influences glaze aesthetics.
2. the photochemical catalyst Y generated in the present invention through firing2Zr2O7Special appearance can be quickly formed in frit surface
The brilliant flower of crystallization, has good surface decoration effect, and glossiness is good, and chemical property is stablized.
3. raw material uses Suzhou soil, contain a small amount of TiO in ingredient2, be conducive to the absorption benefit for promoting glaze to ultraviolet light
With rate.Glaze prepared by the present invention has photo-catalysis function in addition to the basic function with ceramic glaze.Ceramic glaze energy
It is enough that there is catalyticing decomposition action to organic pollutant after 8 hours under illumination condition, it is anti-using BL-GHX-V type photochemistry
Ying Yi carries out photocatalysis effect test to glaze layer, and test result shows that the resolution ratio to dyestuffs such as rhodamine B and methylene blues can
To reach 85%.
4. glaze prepared by the present invention has the spy in visible light wave range high absorptivity and the high-transmission rate to infrared light
Point, photocatalytic ingredient have good visible light-responded.
Detailed description of the invention
Fig. 1 is 1 glaze layer surface X-ray diffraction analysis figure of embodiment.
Fig. 2 is the Y that 1 glaze layer surface of embodiment is precipitated2Zr2O7Crystalline substance flower SEM figure.
Fig. 3 is 1 glaze layer photocatalytic degradation rhodamine B efficiency chart of embodiment.
Specific embodiment
Present invention will now be described in detail with reference to the accompanying drawings..
In the present invention in Suzhou soil based on mass percentage, containing 37%~39% Al2O3, 46%~48% SiO2。
Embodiment 1
1) firstly, by quartz, potassium feldspar, albite, borax, Y2O3, Suzhou soil, lithium carbonate is according to following quality chemistry group
Distribution ratio carries out ingredient.SiO2: Al2O3: B2O3: Y2O3: Li2O:Na2O:K2O=57:4:22:4:7:4:3.
2) above-mentioned powder is dry-mixed and grind, it crosses 60 meshes and obtains mixture, be fitted into crucible, be put into electric furnace 1270
DEG C heat preservation 20min, taking-up be poured into water quenching be made frit.Frit is taken out from water, be put into after drying it is levigate in ball grinder,
Control material (frit): ball: water quality ratio is 1:1:0.8, crosses 250 meshes after grinding 3 hours, is dried for standby.The powder is denoted as A
Material.
3) above-mentioned A is expected and Y2O3、ZrO2And Suzhou soil is A material: Y according to mass ratio2O3: Suzhou soil=82:5:7 matches
Than carrying out ingredient, and Y2O3With ZrO2The ratio of amount of substance meet Y2Zr2O7In stoichiometric ratio, be uniformly mixed and in ball milling
Levigate in tank, control material: ball: water quality ratio is 1:1:0.8, crosses 250 meshes after grinding 3 hours, is dried for standby.The powder is denoted as
B material.
4) B material and dispersing agent are added to the water, stir and evenly mix and be configured to glaze slip, the mass content of water is in glaze slip
44%, the mass content of dispersing agent is 0.05%, and dispersing agent is sodium carboxymethylcellulose.
5) use the glazing of glaze spraying mode in ceramic surface above-mentioned prepared glaze slip, glazing is with a thickness of 0.4mm, at 60 DEG C
Under the conditions of it is dry after be burnt into through roller kilns oxidizing flame, firing temperature is 1100 DEG C, and firing period is 40 minutes, is protected under firing temperature
The warm time is 6 minutes, is obtained with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze.
Fig. 1 is the glaze layer surface XRD spectrum prepared under the conditions of embodiment 1, as can be seen from the figure Y2Zr2O7Photocatalysis
The preparation that ingredient is succeeded.
Fig. 2 is the SEM figure that crystallite is precipitated in the glaze layer surface prepared under the conditions of embodiment 1, as can be seen from the figure
Y2Zr2O7The microscopic appearance of photocatalytic ingredient is flower-like structure.Average-size is at 3 μm or so.
Fig. 3 is rhdamine B of degrading under the glaze layer surface simulation visible light conditions prepared under the conditions of embodiment 1,
Middle to use 1000W xenon lamp simulated visible light, the rhodamine B that degradation concentration is 3mg/L, after irradiation in 8 hours, degradation efficiency reaches
85%.
Embodiment 2
1) firstly, by quartz, potassium feldspar, albite, borax, Y2O3, Suzhou soil, lithium carbonate is according to following quality chemistry group
Distribution ratio carries out ingredient.SiO2: Al2O3: B2O3: Y2O3: Li2O:Na2O:K2O=58:5:23:3:6:3:2.
2) above-mentioned powder is dry-mixed and grind, it crosses 60 meshes and obtains mixture, be fitted into crucible, be put into electric furnace 1280
DEG C heat preservation 30min, taking-up be poured into water quenching be made frit.Frit is taken out from water, be put into after drying it is levigate in ball grinder,
Control material (frit): ball: water quality ratio is 1:1:0.8, crosses 250 meshes after grinding 4 hours, is dried for standby.The powder is denoted as A
Material.
3) above-mentioned A is expected and Y2O3、ZrO2And Suzhou soil is A material: Y according to mass ratio2O3: Suzhou soil=84:4.8:6
Proportion carries out ingredient, and Y2O3With ZrO2The ratio of amount of substance meet Y2Zr2O7In stoichiometric ratio, be uniformly mixed and in ball
Levigate in grinding jar, control material: ball: water quality ratio is 1:1:0.8, crosses 250 meshes after grinding 4 hours, is dried for standby.Powder note
For B material.
4) B material and dispersing agent are added to the water, stir and evenly mix and be configured to glaze slip, the mass content of water is in glaze slip
47%, the mass content of dispersing agent is 0.10%, and dispersing agent is sodium carboxymethylcellulose.
5) use the glazing of glaze spraying mode in ceramic surface above-mentioned prepared glaze slip, glazing is with a thickness of 0.3mm, at 70 DEG C
Under the conditions of it is dry after be burnt into through roller kilns oxidizing flame, firing temperature is 1120 DEG C, and firing period is 45 minutes, is protected under firing temperature
The warm time is 7 minutes, is obtained with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze.
Embodiment 3
1) firstly, by quartz, potassium feldspar, albite, borax, Y2O3, Suzhou soil, the raw materials such as lithium carbonate are according to following quality
Chemical constituent proportion carries out ingredient.SiO2: Al2O3: B2O3: Y2O3: Li2O:Na2O:K2O=59:6:24:2:5:2:1.
2) above-mentioned powder is dry-mixed and grind, it crosses 40 meshes and obtains mixture, be fitted into crucible, be put into electric furnace 1290
DEG C heat preservation 40min, taking-up be poured into water quenching be made frit.Frit is taken out from water, be put into after drying it is levigate in ball grinder,
Control material (frit): ball: water quality ratio is 1:1:0.8, crosses 250 meshes after grinding 3 hours, is dried for standby.The powder is denoted as A
Material.
3) above-mentioned A is expected and Y2O3、ZrO2And Suzhou soil is A material: Y according to mass ratio2O3: Suzhou soil=86:4.6:5
Proportion carries out ingredient, and Y2O3With ZrO2The ratio of amount of substance meet Y2Zr2O7In stoichiometric ratio, be uniformly mixed and in ball
Levigate in grinding jar, control material: ball: water quality ratio is 1:1:0.8, crosses 250 meshes after grinding 5 hours, is dried for standby.Powder note
For B material.
4) B material and dispersing agent are added to the water, stir and evenly mix and be configured to glaze slip, the mass content of water is in glaze slip
50%, the mass content of dispersing agent is 0.15%, and dispersing agent is sodium carboxymethylcellulose.
5) use the glazing of glaze spraying mode in ceramic surface above-mentioned prepared glaze slip, glazing is with a thickness of 0.2mm, at 80 DEG C
Under the conditions of it is dry after be burnt into through roller kilns oxidizing flame, firing temperature is 1140 DEG C, and firing period is 50 minutes, is protected under firing temperature
The warm time is 8 minutes, is obtained with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze.
The present invention may be implemented directly to synthesize the crystallite with photo-catalysis function simultaneously during prepared by glaze, and light is urged
Agent can be prepared with glaze and while uniformly generate, and can after glazing to ceramic matrix beautiful decoration ceramic watch
Face can effectively overcome the problems, such as that above method exists.Therefore it has broad application prospects.
Claims (8)
1. a kind of preparation method with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which comprises the steps of:
1) firstly, by quartz, potassium feldspar, albite, borax, Y2O3, Suzhou soil, lithium carbonate SiO in mass ratio2: Al2O3: B2O3:
Y2O3: Li2O:Na2O:K2O=(57-59): (4-6): (22-24): (2-4): (5-7): (2-4): (1-3) carries out ingredient；
2) powder after ingredient is dry-mixed and grind, sieving obtains mixture, by mixture in 1270-1290 DEG C of heat preservation 20-
40min, taking-up are poured into water quenching and frit are made, and frit is ground to obtain A material；
3) by A material, Y2O3、ZrO2And Suzhou soil is expected according to mass ratio A: Y2O3: ZrO2: Suzhou soil=(82-86): (4.6-5):
(5-5.4): the proportion of (5-7) carries out ingredient, and grinding obtains B material；
4) B material and dispersing agent are added to the water, stir and evenly mix and is configured to glaze slip；
5) glaze slip glazing is burnt into after dry through roller kilns oxidizing flame in ceramic surface, firing temperature is 1100-1140 DEG C, is burnt
It is 40-50 minutes at the period, soaking time is 6-8 minutes under firing temperature, obtains making pottery with photo-catalysis function zirconic acid yttrium crystallite
Enamel.
2. the preparation method according to claim 1 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which is characterized in that
Grinding is carried out in ball grinder in step 2) and step 3, and frit: ball: water quality ratio is 1:1:0.8, and milling time is
3-5 hours.
3. the preparation method according to claim 1 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which is characterized in that
The mass content of water is 44-50% in glaze slip in step 4).
4. the preparation method according to claim 1 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which is characterized in that
The mass content of dispersing agent is 0.05-0.15% in glaze slip.
5. the preparation method according to claim 1 or 4 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, feature exist
In dispersing agent is sodium carboxymethylcellulose in step 4).
6. the preparation method according to claim 1 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which is characterized in that
Glazing is carried out using glaze spraying mode in step 5).
7. the preparation method according to claim 1 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which is characterized in that
Glazing is in step 5) with a thickness of 0.2-0.4mm.
8. the preparation method according to claim 1 with photo-catalysis function zirconic acid yttrium micro-crystalline ceramic glaze, which is characterized in that
Dry temperature is 60-80 DEG C in step 5).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001303276A (en) * | 2000-04-28 | 2001-10-31 | Kawasaki Steel Corp | Enamel material |
| CN101067207A (en) * | 2007-06-08 | 2007-11-07 | 东华大学 | Method for producing photo catalytic self-cleaning enamel |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001303276A (en) * | 2000-04-28 | 2001-10-31 | Kawasaki Steel Corp | Enamel material |
| CN101067207A (en) * | 2007-06-08 | 2007-11-07 | 东华大学 | Method for producing photo catalytic self-cleaning enamel |
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