CN110590327B - Method for firing photoluminescence fluorescent glazed ceramic through roller kiln - Google Patents
Method for firing photoluminescence fluorescent glazed ceramic through roller kiln Download PDFInfo
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- 238000005424 photoluminescence Methods 0.000 title claims abstract description 51
- 239000000919 ceramic Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000010304 firing Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 34
- 238000000498 ball milling Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 14
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 14
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010453 quartz Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 239000010459 dolomite Substances 0.000 claims abstract description 7
- 229910000514 dolomite Inorganic materials 0.000 claims abstract description 7
- 229910001940 europium oxide Inorganic materials 0.000 claims abstract description 7
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000010433 feldspar Substances 0.000 claims abstract description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 7
- 239000000454 talc Substances 0.000 claims abstract description 7
- 229910052623 talc Inorganic materials 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000748 compression moulding Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000008602 contraction Effects 0.000 description 4
- 238000002211 ultraviolet spectrum Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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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
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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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
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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- 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
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- 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
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention provides a method for firing photoluminescence fluorescent glazed ceramics by a roller kiln, belonging to the technical field of production of architectural ceramics and comprising the following steps: mixing dolomite, quartz, europium oxide, yttrium oxide and aluminum hydroxide, adding water, performing ball milling, drying and calcining to obtain photoluminescence fluorescent powder, mixing kaolin, talc, pyrophyllite, medium-temperature frit and photoluminescence fluorescent powder, adding water, and performing ball milling to obtain fluorescent glaze; mixing kaolin, feldspar and quartz, adding water, and performing ball milling, drying, pulverizing and compression molding to obtain a blank; and finally, applying the fluorescent glaze material on the green body, and sintering the photoluminescent glaze ceramic at high temperature in a roller kiln. The glaze material in the photoluminescence emission fluorescent glazed ceramic produced by the method has good compatibility with a blank body, emits red fluorescence, can regulate and control the fluorescence intensity, and can meet the requirements of the fields of anti-counterfeiting marks, real-time display and photoresponse.
Description
Technical Field
The invention provides a method for firing photoluminescence fluorescent glazed ceramics by a roller kiln, belonging to the technical field of production of architectural ceramics.
Background
With the development of society, people pursue higher and higher quality of building ceramics. While excellent decorative properties are considered, functional elements are also of interest, such as real-time fluorescent ceramics with optical properties including long persistence, light storage, or photoluminescence, have recently received attention from researchers, manufacturers, and consumers. The material selected for the long afterglow ceramic glaze is mainly obtained by doping aluminate, silicate, aluminosilicate or titanate based spinel material with rare earth, is not suitable for high temperature firing (generally not more than 950 ℃), and cannot be used in the production of roller kilns of building ceramics. Patent ZL201410074886.4 mentions that the long afterglow ceramic tile is produced by 10-40% of long afterglow fluorescent powder, 60-90% of high temperature calcium base medium temperature frit and 0-1% of glaze pigment, and the chemical composition of the long afterglow fluorescent powder is A3-x-y（PO4）2:xEu2+And yB, A is alkaline earth metal ion Ca2+、Sr2+、Ba2+B is Dy3+、Nd3+、Ce3+、Pr3+、Tb3+The luminescent ceramic produced by the scheme belongs to the category of photoluminescence, the long afterglow fluorescent powder is large in dosage, the afterglow time is more than 3 hours, and the problem of light pollution is caused when the luminescent ceramic is applied indoors.
The photoluminescence can be used for real-time display, and after the excitation light source is turned off, the luminescence phenomenon is less than 10-4The fluorescent material disappears in seconds, and is widely applied to fields which do not need long-time luminescence, such as anti-counterfeiting marks, instant display and photoresponse fields. Patent ZL201210053502.1 mentions that the effect of emitting red light under the irradiation of a blue fluorescent pen is obtained by applying fluorescent powder and low-temperature glaze on the surface of ceramic and firing at 800 ℃. CN201810339976.X discloses a method for firing ceramic tiles with fluorescent anti-counterfeiting marks in a 1200 ℃ high-temperature roller kiln after glazing for multiple times by using ZnO: Zn as a fluorescent substance, wherein the ceramic tiles structurally comprise a bottom blank layer, a bottom glaze layer, a bottom glass layer, a fluorescent powder layer and a glass layer, and the glazing process is repeatedThe purpose is to ensure that the ZnO, Zn fluorescent powder exists in the form of crystal clusters and does not react with a blank body and a glaze layer, thereby ensuring the effect of photoluminescence green light; in addition, the production of the fluorescent powder ZnO-Zn is obtained by producing ZnO and ZnS in a reducing atmosphere, and the requirement on production equipment is high.
The photoluminescent glaze applied to architectural ceramics needs to overcome the following difficulties: (1) the material is high temperature resistant, namely, the fluorescent material is not decomposed at the high temperature of 1150-1230 ℃ in the roller kiln; (2) the compatibility with the green body layer is high, namely, the green body layer does not generate physical and chemical reactions, the sintering shrinkage rate is kept consistent, and the defects of bubbles and the like do not occur in the glaze surface; (3) the amount used is as low as possible to ensure the feasibility of economic costs. To date, no report has been made on glazed architectural ceramics that photo-emit red fluorescence.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for firing photoluminescence fluorescent glazed ceramics by a roller kiln, which is characterized by comprising the following steps:
(1) preparing the following materials in percentage by mass: 36.25% of dolomite, 27.18% of quartz, 5.58% of europium oxide, 3.81% of yttrium oxide and 27.18% of aluminum hydroxide, and adding water to ensure that the mass ratio of the materials to the water is 100:80, ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, drying the slurry at 110 ℃, and then calcining for 15 minutes at 1175 ℃ to obtain the photoluminescence fluorescent powder; mixing the prepared photoluminescence fluorescent powder with other raw materials according to the mass percentage: 7.04-7.69% of kaolin, 11.27-12.31% of talc, 3.07-11.27% of pyrophyllite, 56.34-61.54% of intermediate-temperature frit and 14.08-15.39% of light-induced emission fluorescent powder, wherein the chemical composition of the intermediate-temperature frit is 1.77% of Na2O、2.00%MgO、5.97%Al2O3、61.59%SiO2、5.61%K2Adding water into O, 8.63% of CaO, 11.7% of ZnO and 2.73% of BaO, enabling the mass ratio of the materials to the water to be 100:80, and carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour to produce the fluorescent glaze;
(2) preparing the following materials in percentage by mass: 50% of kaolin, 20% of feldspar and 30% of quartz, adding water to ensure that the mass ratio of the materials to the water is 100:80, carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour, drying slurry at 110 ℃ to obtain blank powder, and pressing at 200MPa to obtain a blank;
(3) applying the fluorescent glaze produced in the step (1) on the green body produced in the step (2), wherein the glazing amount is 372.2-482.4 g/m2And sintering in a roller kiln at 1175 ℃ for 50min to obtain the photoluminescence glaze ceramic.
Wherein, the fluorescence luminous intensity of the photoluminescence emission fluorescent ceramic can be changed by changing the adding amount of the photoluminescence emission fluorescent powder in the step (1) and the glazing amount in the step (3). The wavelength of the absorption peak of the photoluminescence ceramic can be changed with the addition amount of the materials in the step (1).
The invention has the beneficial effects that:
1. the raw materials selected by the method are mostly mineral materials, the cost is low, the process is simple, and the industrial production is easy to realize;
2. the photoluminescence fluorescent glaze produced by the method has good compatibility with the blank, does not generate physical and chemical reactions, has consistent shrinkage at the joint of the blank and the glaze, has no air holes and has no deformation of the blank;
3. the fluorescence wavelength of the photoluminescence fluorescence glaze ceramic produced by the method is in the red light range, and the fluorescence luminous intensity can be regulated and controlled by the production process, so that the requirements of the fields of anti-counterfeiting marks, real-time display and photoresponse can be met.
Drawings
In the attached fig. 1, (a), (b), (C) and (d) are the absorption spectra of the fluorescent glazes (obtained by drying at 110 ℃ for 2 hours) produced by the step (1) of examples 1, 2, 3 and 4, respectively.
In the attached figure 2, (a), (b), (c) and (d) are absorption spectra of the photoluminescence glaze ceramic produced by the examples 1, 2, 3 and 4 respectively.
In the attached figure 3, (a), (b), (C) and (d) are photoluminescence spectra (excitation light wavelength is 532 nm) of the fluorescent glazes (obtained by drying at 110 ℃ for 2 hours) produced in the steps (1) of examples 1, 2, 3 and 4, respectively.
FIG. 4 is a photoluminescence fluorescence spectrum (excitation wavelength 532 nm) of a photoluminescence glazed ceramic produced in example 1.
Detailed Description
Example 1
(1) Preparing the following materials in percentage by mass: 36.25% of dolomite, 27.18% of quartz, 5.58% of europium oxide, 3.81% of yttrium oxide and 27.18% of aluminum hydroxide, and adding water to ensure that the mass ratio of the materials to the water is 100:80, ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, drying the slurry at 110 ℃, and then calcining for 15 minutes at 1175 ℃ to obtain the photoluminescence fluorescent powder; mixing the prepared photoluminescence fluorescent powder with other raw materials according to the mass percentage: 7.46% of kaolin, 11.94% of talc, 5.97% of pyrophyllite, 59.70% of intermediate-temperature frit and 14.93% of photoluminescence phosphor powder, wherein the chemical composition of the intermediate-temperature frit is 1.77% of Na2O、2.00%MgO、5.97%Al2O3、61.59%SiO2、5.61%K2Adding water into O, 8.63% of CaO, 11.7% of ZnO and 2.73% of BaO, enabling the mass ratio of the materials to the water to be 100:80, and carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour to produce the fluorescent glaze;
(2) preparing the following materials in percentage by mass: 50% of kaolin, 20% of feldspar and 30% of quartz, adding water to ensure that the mass ratio of the materials to the water is 100:80, carrying out ball milling in a planetary ball mill at the speed of 400 rpm for 1 hour, drying the slurry at 110 ℃ to obtain blank powder, and pressing under 200MPa to obtain a blank;
(3) applying the fluorescent glaze material produced in the step (1) on the green body produced in the step (2), wherein the glazing amount is 399.7g/m2And placing the ceramic into a roller kiln, and sintering at 1175 ℃ for 50min to obtain the photoluminescence fluorescence glaze ceramic.
The test shows that the absorption peaks of the fluorescent glaze and the photoluminescence ceramic are respectively positioned at 305.9 nm and 296.6 nm (attached figures 1 and 2), and belong to the ultraviolet spectrum region. The fluorescent glaze and the photoluminescence emission fluorescent ceramic have high luminous intensity, the peak values of the strongest fluorescence are 46315.3 and 40603.5 (shown in figures 3 and 4), and the corresponding fluorescence wavelengths all belong to the red light range. The produced photoluminescence fluorescence glazed ceramic has smooth glaze surface, no air holes, consistent contraction of the blank and the glaze layer, and no cracks and deformation of the blank.
Example 2
(1) Preparing the following components in percentage by mass: 36.25% of dolomite, 27.18% of quartz, 5.58% of europium oxide, 3.81% of yttrium oxide and 27.18% of aluminum hydroxide, and adding water to ensure that the mass ratio of the materials to the water is 100:80, ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, drying the slurry at 110 ℃, and then calcining for 15 minutes at 1175 ℃ to obtain the photoluminescence fluorescent powder; mixing the prepared photoluminescence fluorescent powder with other raw materials according to the mass percentage: 7.69% of kaolin, 12.31% of talc, 3.07% of pyrophyllite, 61.54% of intermediate-temperature frit and 15.39% of photoluminescence phosphor powder, wherein the chemical composition of the intermediate-temperature frit is 1.77% of Na2O、2.00%MgO、5.97%Al2O3、61.59%SiO2、5.61%K2Adding water into O, 8.63% of CaO, 11.7% of ZnO and 2.73% of BaO, enabling the mass ratio of the materials to the water to be 100:80, and carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour to produce the fluorescent glaze;
(2) preparing the following materials in percentage by mass: 50% of kaolin, 20% of feldspar and 30% of quartz, adding water to ensure that the mass ratio of the materials to the water is 100:80, carrying out ball milling in a planetary ball mill at the speed of 400 rpm for 1 hour, drying the slurry at 110 ℃ to obtain blank powder, and pressing under 200MPa to obtain a blank;
(3) applying the fluorescent glaze material produced in the step (1) on the green body produced in the step (2), wherein the glazing amount is 482.4 g/m2And placing the ceramic into a roller kiln, and sintering at 1175 ℃ for 50min to obtain the photoluminescence fluorescence glaze ceramic.
The test shows that the absorption peaks of the fluorescent glaze and the photoluminescence emission ceramic are respectively positioned at 304.5 nm and 303.7 nm (attached figures 1 and 2), and belong to the ultraviolet spectrum region. The fluorescent glaze has high luminous intensity, the peak value of the strongest fluorescence is 37973.3 (figure 3), and the corresponding fluorescence wavelength belongs to the red light range. The produced photoluminescence fluorescence glaze ceramics emits red light under the irradiation of an ultraviolet lamp with the wavelength of 365 nm. The photoluminescent glazed ceramic has smooth glaze surface, no air holes, homogeneous contraction between the blank and the glaze layer, no crack and no deformation.
Example 3
(1) Preparing the following materials in percentage by mass: 36.25% of dolomite, 27.18% of quartz, 5.58% of europium oxide, 3.81% of yttrium oxide and 27.18% of aluminum hydroxide, and adding water to ensure that the mass ratio of the materials to the water is 100:80, ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, drying the slurry at 110 ℃, and then calcining for 15 minutes at 1175 ℃ to obtain the photoluminescence fluorescent powder; mixing the prepared photoluminescence fluorescent powder with other raw materials according to the mass percentage: 7.25% of kaolin, 11.59% of talc, 8.7% of pyrophyllite, 57.97% of intermediate temperature frit and 14.49% of light-induced emission fluorescent powder, wherein the chemical composition of the intermediate temperature frit is 1.77% of Na2O、2.00%MgO、5.97%Al2O3、61.59%SiO2、5.61%K2Adding water into O, 8.63% of CaO, 11.7% of ZnO and 2.73% of BaO, enabling the mass ratio of the materials to the water to be 100:80, and carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour to produce the fluorescent glaze;
(2) preparing the following materials in percentage by mass: 50% of kaolin, 20% of feldspar and 30% of quartz, adding water to ensure that the mass ratio of the materials to the water is 100:80, carrying out ball milling in a planetary ball mill at the speed of 400 rpm for 1 hour, drying the slurry at 110 ℃ to obtain blank powder, and pressing under 200MPa to obtain a blank;
(3) applying the fluorescent glaze material produced in the step (1) on the green body produced in the step (2), wherein the glazing amount is 399.7g/m2And placing the ceramic into a roller kiln, and sintering at 1175 ℃ for 50min to obtain the photoluminescence fluorescence glaze ceramic.
The test shows that the absorption peaks of the fluorescent glaze and the photoluminescence emission ceramic are respectively positioned at 304.2 nm and 297.0 nm (attached figures 1 and 2), and belong to the ultraviolet spectrum region. The fluorescent glaze has high luminous intensity, the peak value of the strongest fluorescence is 30587.1 (figure 3), and the corresponding fluorescence wavelength belongs to the red light range. The produced photoluminescence fluorescence glaze ceramics emits red light under the irradiation of an ultraviolet lamp with the wavelength of 365 nm. The photoluminescent glazed ceramic has smooth glaze surface, no air holes, homogeneous contraction between the blank and the glaze layer, no crack and no deformation.
Example 4
(1) Preparing the following materials in percentage by mass: 36.25% of dolomite, 27.18% of quartz, 5.58% of europium oxide, 3.81% of yttrium oxide and 27.18% of aluminum hydroxide, and adding water to ensure that the mass ratio of the materials to the water is 100:80, ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, drying the slurry at 110 ℃, and then calcining for 15 minutes at 1175 ℃ to obtain the photoluminescence fluorescent powder; mixing the prepared photoluminescence fluorescent powder with other raw materials according to the mass percentage: 7.04% of kaolin, 11.27% of talc, 11.27% of pyrophyllite, 56.34% of intermediate temperature frit and 14.08% of photoluminescence phosphor powder, wherein the chemical composition of the intermediate temperature frit is 1.77% of Na2O、2.00%MgO、5.97%Al2O3、61.59%SiO2、5.61%K2Adding water into O, 8.63% of CaO, 11.7% of ZnO and 2.73% of BaO, enabling the mass ratio of the materials to the water to be 100:80, and carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour to produce the fluorescent glaze;
(2) preparing the following materials in percentage by mass: 50% of kaolin, 20% of feldspar and 30% of quartz, adding water to ensure that the mass ratio of the materials to the water is 100:80, carrying out ball milling in a planetary ball mill at the speed of 400 rpm for 1 hour, drying the slurry at 110 ℃ to obtain blank powder, and pressing under 200MPa to obtain a blank;
(3) applying the fluorescent glaze produced in the step (1) on the green body produced in the step (2), wherein the glazing amount is 372.2 g/m2And placing the ceramic in a roller kiln, sintering at 1175 ℃ for 50min to obtain the photoluminescence fluorescence glaze ceramic.
The test shows that the absorption peaks of the fluorescent glaze and the photoluminescence emission ceramic are respectively positioned at 306.9 nm and 294.5 nm (attached figures 1 and 2), and belong to the ultraviolet spectrum region. The fluorescent glaze has high luminous intensity, the peak value of the strongest fluorescence is 35578.1 (figure 3), and the corresponding fluorescence wavelength belongs to the red light range. The produced photoluminescence fluorescence glaze ceramics emits red light under the irradiation of an ultraviolet lamp with the wavelength of 365 nm. The photoluminescent glazed ceramic has smooth glaze surface, no air holes, homogeneous contraction between the blank and the glaze layer, no crack and no deformation.
Claims (1)
1. A method for firing photoluminescence fluorescence glazed ceramics by a roller kiln is characterized by comprising the following steps:
step 1, preparing the following materials in percentage by mass: 36.25% of dolomite, 27.18% of quartz, 5.58% of europium oxide, 3.81% of yttrium oxide and 27.18% of aluminum hydroxide, and adding water to ensure that the mass ratio of the materials to the water is 100:80, ball milling for 1 hour at the speed of 400 revolutions per minute in a planetary ball mill, drying the slurry at 110 ℃, and then calcining for 15 minutes at 1175 ℃ to obtain the photoluminescence fluorescent powder; mixing the prepared photoluminescence fluorescent powder with other raw materials according to the mass percentage: 7.04-7.69% of kaolin, 11.27-12.31% of talc, 3.07-11.27% of pyrophyllite, 56.34-61.54% of intermediate-temperature frit and 14.08-15.39% of light-induced emission fluorescent powder, wherein the chemical composition of the intermediate-temperature frit is 1.77% of Na2O、2.00%MgO、5.97%Al2O3、61.59%SiO2、5.61%K2Adding water into O, 8.63% of CaO, 11.7% of ZnO and 2.73% of BaO, enabling the mass ratio of the materials to the water to be 100:80, and carrying out ball milling in a planetary ball mill at the speed of 400 revolutions per minute for 1 hour to produce the fluorescent glaze;
step 2, preparing the following materials in percentage by mass: 50% of kaolin, 20% of feldspar and 30% of quartz, adding water to ensure that the mass ratio of the materials to the water is 100:80, carrying out ball milling in a planetary ball mill at the speed of 400 rpm for 1 hour, drying the slurry at 110 ℃ to obtain blank powder, and pressing under 200MPa to obtain a blank;
step 3, applying the fluorescent glaze material produced in the step 1 on the green body produced in the step 2, wherein the glazing amount is 372.2-482.4 g/m2And placing the ceramic into a roller kiln, and sintering at 1175 ℃ for 50min to obtain the photoluminescence fluorescence glaze ceramic.
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| CN115849953B (en) * | 2022-12-13 | 2023-11-07 | 福建省德化县美景礼品有限公司 | Photochromic ceramic glaze and preparation method thereof |
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