CN103896633A - Method for manufacturing long afterglow fluorescent ceramic tile - Google Patents
Method for manufacturing long afterglow fluorescent ceramic tile Download PDFInfo
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- CN103896633A CN103896633A CN201410074886.4A CN201410074886A CN103896633A CN 103896633 A CN103896633 A CN 103896633A CN 201410074886 A CN201410074886 A CN 201410074886A CN 103896633 A CN103896633 A CN 103896633A
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- afterglow fluorescent
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Abstract
The invention discloses a method for manufacturing a long afterglow fluorescent ceramic tile. The method comprises the following steps: 1) weighing materials and mixing, namely weighing 10-40% of afterglow fluorescent powder, 60-90% of high-temperature calcium frit and 0-1% of glaze pigment according to the mass percent of the formula and evenly mixing, wherein the chemical formula of the long afterglow fluorescent powder is A3-x-y(PO4)2:xEu<2+>, yB, A is one or more of alkaline earth metal ions Ca<2+>, Sr<2+> or Ba<2+>, B is one or more of Dy<3+>, Nd<3+>, Ce<3+>, Pr<3+> and Tb<3+>, x is smaller than or equal to 0.3 and greater than or equal to 0 and y is smaller than or equal to 0.3 and greater than or equal to 0; 2) distributing materials, namely filtering the mixed materials in the step 1) through an 80-mesh sieve, and then distributing on a green brick through an 80-mesh material distributing net, and spraying a fixing agent to fix, wherein the distributing thickness is 2-15mm; 3) sintering, namely sintering the green brick treated in the step 2) into a kiln at 1150-1230 DEG C, wherein the sintering cycle is 90-150 minutes; and 4) edging and polishing. The method has the advantages that the process is simple, and the manufactured long afterglow fluorescent ceramic tile is high in product strength and wear resistance, long in afterglow time and the like.
Description
Technical field
The present invention relates to architectural pottery technical field, relate in particular to a kind of manufacture method of long-afterglow fluorescent ceramic tile.
Background technology
Long-afterglow fluorescent material is commonly called as luminescent powder, belongs to the one of embedded photoluminescent material, refers to the short irradiation through the light source such as daylight and long wave ultraviolet, closes after light source, still can within a very long time, continue luminous material.Long after glow luminous material, as a kind of energy storage, energy-conservation " green light source material ", is more and more subject to people's attention in today of energy worsening shortages, and especially aspect low light level illumination, demonstration, application is very extensive.At present, long after glow luminous material goods have luminous paint, paint, luminous printing ink, luminescent glaze, luminescent plastics, luminous rubber, Luminous leather, fluorescent glass, luminescent ceramic, luminous ornament stone, luminous composited aluminum and plastic decking, light-emitting workmanship etc., are widely used in the every field such as building decoration, communications and transportation, security against fire, instrument, subway tunnel, printing printing and dyeing, advertising board, bullion.
The long-afterglow fluorescent material great majority that use for secure ID on the market at present adopt the resin paste that contains transparent resinous principle and fluorescent material composition and form light-storage luminant layer, in resin paste, coordinate the transparent resinous principle of 95% weight of total amount, above-mentioned materials is as uses such as the marks of road, and wear resistant, weathering resistance, chemical resistance are all poor.
Long-afterglow fluorescent material is applied in to architectural pottery technical field and produces the ceramic tile with long-afterglow fluorescent effect and also can be used as the use of secure ID, or allow ceramic tile also can present abundant decorative effect by bright turning after dark.Conventional method has following several mode at present:
1,, in without enamel ceramic tile, directly using long-afterglow fluorescent material by a certain percentage as base substrate component, but the prepared ceramic tile cost of this kind of method is high, and effect is single;
The figure layer 2, at billet surface spraying one deck with long-afterglow fluorescent material, then burn till, but the long-afterglow fluorescent material coating forming is not wear-resisting, is easy to come off in use procedure; In addition, also can spray after long-afterglow fluorescent material, then impose layer of transparent glaze or charity clear frit, burn till rear formation protective clear layer, can alleviate like this because the problem of the long-afterglow fluorescent material coating shedding that wearing and tearing cause.
Current disclosed scheme; the long-afterglow fluorescent material that adopts is to be obtained after rear-earth-doped by the spinel of aluminate, silicate, aluminosilicate, metatitanic acid alkali; it is not suitable for high temperature and burns till (being generally no more than 950 ℃); therefore be difficult to adopt single firing process to prepare this series products; and under so low firing temperature; protective clear layer hardness at long-afterglow fluorescent material coatingsurface is low, not wear-resisting, is easy in actual use scratch.
Summary of the invention
The object of the invention is to propose one and the object of the present invention is to provide a kind of long-afterglow fluorescent ceramic tile and manufacture method thereof, be intended to solve existing long-afterglow fluorescent material and be only suitable for easy fired, cannot form high, the anti abrasive long-afterglow fluorescent ceramic tile of intensity.
For reaching this object, the present invention by the following technical solutions:
A kind of long-afterglow fluorescent ceramic tile, it comprises green body layer and is compounded in the long-afterglow fluorescent glass coating in green body layer, wherein said long-afterglow fluorescent glass coating is by long-afterglow fluorescent material sintering after distributing technique charity is in green body layer is made, the formula of described long-afterglow fluorescent material by mass percentage, comprise 10～40% long persistence luminescent powder, 60～90% high temperature calcium base frit and 0～1% glaze stain, described long persistence luminescent powder has following chemical formula composition: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ca
2+, Sr
2+or Ba
2+one or more; B is Dy
3+, Nd
3+, Ce
3+, Pr
3+, Tb
3+in one or more combination, and 0<x≤0.3,0≤y≤0.3.
Preferably, in such scheme, the firing temperature of described sintering is 1150 ℃～1230 ℃.
Preferably, allow long-afterglow fluorescent material coating have better quality, the fineness of described high temperature calcium base frit is 100～200 orders.
Further, in order to allow long-afterglow fluorescent material coating there is better quality, fineness≤800 order of described long persistence luminescent powder.
Preferably, in order to obtain longer time of persistence, described alkaline-earth metal ions is Sr
2+or Ba
2+or both combinations.
Further, in above-mentioned long-afterglow fluorescent ceramic tile, also comprise the printed layer between green body layer and long-afterglow fluorescent glass coating.
For printed layer pattern can be presented preferably, further, in above-mentioned long-afterglow fluorescent ceramic tile, the formula of described long-afterglow fluorescent material by mass percentage, comprises 10～20% long persistence luminescent powder, 80～90% high temperature calcium base clear frit.Long persistence luminescent powder add-on exceedes 20% transparent glass layer that can make high temperature calcium base clear frit form and becomes muddy, makes printed layer dim pattern unclear.
The present invention also provides a kind of manufacture method of long-afterglow fluorescent ceramic tile, and it comprises the steps:
Step 1) weighing mixes; By prescription quality per-cent, take 10～40% long persistence luminescent powder, 60～90% high temperature calcium base frit and 0～1% glaze stain, and mix, the chemical formula of wherein said long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ca
2+, Sr
2+or Ba
2+one or more; B is Dy
3+, Nd
3+, Ce
3+, Pr
3+, Tb
3+in one or more combination, and 0<x≤0.3,0≤y≤0.3;
Step 2) cloth; Compound mixed step 1) is crossed to 80 mesh sieves, then execute in adobe by 80 order cloth screen cloths, and spray fixing agent and fix, charity thickness is advisable with 2～15mm;
Step 3) is burnt till; By step 2) adobe after cloth burns till in kiln, and firing temperature is 1150 ℃～1230 ℃, and firing period is 90～150min;
The polishing of step 4) edging; Goods after step 3) is burnt till carry out edging polishing and obtain finished product.
Preferably, allow long-afterglow fluorescent material coating have better quality, in aforesaid method, the fineness of described high temperature calcium base frit is 100～200 orders.
Further, in order to allow long-afterglow fluorescent material coating there is better quality, in aforesaid method, fineness≤800 order of described long persistence luminescent powder.
Preferably, in order to obtain longer time of persistence, in aforesaid method, described alkaline-earth metal ions is Sr
2+or Ba
2+or both combinations.
Further, in aforesaid method, in step 2) in the adobe surface that uses there is the printed layer forming by screen printing, rotary printing or ink-jet printed technique.
For printed layer pattern can be presented preferably, further, in aforesaid method, the formula of described long-afterglow fluorescent material by mass percentage, 10～20% long persistence luminescent powder, 80～90% high temperature calcium base clear frit.Long persistence luminescent powder add-on exceedes 20% transparent glass layer that can make high temperature calcium base clear frit form and becomes muddy, makes printed layer dim pattern unclear.
Compared to the prior art, tool of the present invention has the following advantages: the spinel that steady persistence long persistence luminescent powder that ceramic tile adopts provided by the invention is phosphate base is through rear-earth-doped acquisition, it is more high temperature resistant, therefore can under the hot conditions more than 1150 ℃, burn till, prepared like this ceramic tile goods base substrate part has been sintered to porcelain, intensity is higher, and high as the long-afterglow fluorescent glass coating of basic material formation has intensity through the rear-earth-doped long persistence luminescent powder obtaining take high temperature calcium base frit and phosphate base spinel, wear-resistant, the advantages such as time of persistence is long, and can only need once-firing, green body layer and long-afterglow fluorescent glass coating can complete in a high temperature burns till, and simplify technique, save energy.
Embodiment
Further illustrate technical scheme of the present invention below by embodiment.Following table 1 is the formula table of embodiment of the present invention 1-10, wherein long persistence luminescent powder is by setting proportioning according to it, select corresponding raw mineral materials under reducing atmosphere, to calcine acquisition, the domestic application for a patent for invention document that corresponding preparation technology can be 201110324833.X with reference to number of patent application, high temperature calcium base frit and glaze stain are architectural pottery and produce conventional raw material in addition, all can buy in common colour glaze company, the above two kinds of raw materials that use in the embodiment of the present invention are to buy and obtain from three Shui great Hong enamel frit makeing company limiteds of Foshan City.
Table 1: formula table
| Numbering | Long persistence luminescent powder (wt%) | High temperature calcium base frit (wt%) | Glaze stain (wt%) |
| 1 | 10 | 90 | ? |
| 2 | 20 | 80 | ? |
| 3 | 30 | 70 | ? |
| 4 | 40 | 60 | ? |
| 5 | 35 | 64.5 | 0.5 |
| 6 | 39.3 | 60 | 0.7 |
| 7 | 29 | 70 | 1 |
| 8 | 12 | 88 | ? |
| 9 | 15 | 85 | ? |
| 10 | 18 | 82 | ? |
Upper table 1 is the formula table of embodiment 1-10.
In embodiment 1, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ca
2+; B is Dy
3+, and x is that 0.05, y is 0.1.
In embodiment 2, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Sr
2+; B is Pr
3+x is that 0.1, y is 0.1.
In embodiment 3, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Sr
2+and Ba
2+; B is Nd
3+and Tb
3+, x is that 0.12, y is 0.15.
In embodiment 4, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ca
2+and Ba
2+; B is Ce
3+and Pr
3+, x is that 0.07, y is 0.09.
In embodiment 5, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is Sr
2+; B is Ce
3+, x is that 0.3, y is 0.12; Glaze stain is praseodymium yellow.
In embodiment 6, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions and Sr
2+; B is Pr
3+and Tb
3+, x is that 0.1, y is 0.3; Glaze stain is peacock blue.
In embodiment 7, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ca
2+; B is Tb
3+, x is that 0.15, y is 0.05; Glaze stain is manganese red.
In embodiment 8, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ba
2+, B is Nd
3+, x is that 0.03, y is 0.09; Wherein high temperature calcium base frit is high temperature calcium base clear frit.
In embodiment 9, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Sr
2+and Ba
2+; B is Tb
3+, x is that 0.12, y is 0.15; Wherein high temperature calcium base frit is high temperature calcium base clear frit.
In embodiment 10, the chemical formula of long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Sr
2+and Ba
2+; B is Ce
3+and Pr
3+, x is that 0.09, y is 0.18; Wherein high temperature calcium base frit is high temperature calcium base clear frit.
The manufacture method of embodiment 1-7 is as follows:
Step 1) weighing mixes; Take raw material according to various material rates listed in table 1, then in dry method vibrating ball mill, vibration mixes, and mixes rear formation compound for subsequent use, and wherein the fineness of high temperature calcium base frit is 100～200 orders, long-afterglow fluorescent powder fineness≤800 order.
Step 2) cloth; Compound mixed step 1) is crossed to 80 mesh sieves, then execute in adobe by 80 order cloth screen cloths, and spray fixing agent and fix, charity thickness is advisable with 2～15mm.The fixing agent spraying is viscosity organic solution, the aqueous solution of for example dextrin or methylcellulose gum, here the saturated aqueous solution that the fixing agent of selecting is carboxymethyl cellulose, the adobe that used is in addition unsintered moulded pottery not yet put in a kiln to bake after impact briquetting is also dry, certainly select the base substrate after sintering also can realize the present invention, but that can additionally increase operation and improve energy consumption.
Step 3) is burnt till; By step 2) adobe after cloth burns till in kiln, and firing temperature is 1150 ℃～1230 ℃, and firing period is 90～150min; The kiln using is wide roller kiln.
The polishing of step 4) edging; Goods after step 3) is burnt till carry out edging polishing and obtain finished product.
The manufacture method of embodiment 8-10 is as follows:
Step 1) weighing mixes; Take raw material according to various material rates listed in table 1, then in dry method vibrating ball mill, vibration mixes, mix rear formation compound for subsequent use, wherein the fineness of high temperature calcium base frit is 100～200 object high temperature calcium base clear frits, long-afterglow fluorescent powder fineness≤800 order.
Step 2) cloth; Compound mixed step 1) is crossed to 80 mesh sieves, then execute in adobe by 80 order cloth screen cloths, and spray fixing agent and fix, charity thickness is advisable with 2～15mm.The fixing agent spraying is viscosity organic solution, the aqueous solution of for example dextrin or methylcellulose gum, here the saturated aqueous solution that the fixing agent of selecting is carboxymethyl cellulose, the adobe that used is in addition unsintered moulded pottery not yet put in a kiln to bake after impact briquetting is also dry, and its surface has the printed layer through screen printing, rotary printing, ink-jet printed formation, certainly select the base substrate after sintering also can realize the present invention in its surface formation printed layer, but that can additionally increase operation and improve energy consumption.
Step 3) is burnt till; By step 2) adobe after cloth burns till in kiln, and firing temperature is 1150 ℃～1230 ℃, and firing period is 90～150min; The kiln using is wide roller kiln.
The polishing of step 4) edging; Goods after step 3) is burnt till carry out edging polishing and obtain finished product.
Test the performance of above embodiment goods, the Mohs' hardness of its surperficial long-afterglow fluorescent glass coating is 6, and intensity is high, wear-resistant; And the time of persistence that the long-afterglow fluorescent ceramic tile prepared of the above embodiment incandescent light that is 100 watts at power irradiated after 30 minutes be all greater than 3 hours, that wherein time of persistence is the longest is embodiment 3 and embodiment 6, is about 6 hours time of persistence.
Know-why of the present invention has below been described in conjunction with specific embodiments.These are described is in order to explain principle of the present invention, and can not be interpreted as by any way limiting the scope of the invention.Based on explanation herein, those skilled in the art does not need to pay performing creative labour can associate other embodiment of the present invention, within these modes all will fall into protection scope of the present invention.
Claims (6)
1. a manufacture method for long-afterglow fluorescent ceramic tile, it comprises the steps:
Step 1) weighing mixes; By prescription quality per-cent, take 10～40% long persistence luminescent powder, 60～90% high temperature calcium base frit and 0～1% glaze stain, and mix, the chemical formula of wherein said long persistence luminescent powder consists of: A
3-x-y(PO
4)
2: xEu
2+, yB, wherein A is alkaline-earth metal ions Ca
2+, Sr
2+or Ba
2+one or more; B is Dy
3+, Nd
3+, Ce
3+, Pr
3+, Tb
3+in one or more combination, and 0<x≤0.3,0≤y≤0.3;
Step 2) cloth; Compound mixed step 1) is crossed to 80 mesh sieves, then execute in adobe by 80 order cloth screen cloths, and spray fixing agent and fix, charity thickness is 2～15mm;
Step 3) is burnt till; By step 2) adobe after cloth burns till in kiln, and firing temperature is 1150 ℃～1230 ℃, and firing period is 90～150min;
The polishing of step 4) edging; Goods after step 3) is burnt till carry out edging polishing and obtain finished product.
2. manufacture method as claimed in claim 1, is characterized in that, the fineness of described high temperature calcium base frit is 100～200 orders.
3. manufacture method as claimed in claim 1, is characterized in that fineness≤800 order of described long persistence luminescent powder.
4. manufacture method as claimed in claim 1, is characterized in that, described alkaline-earth metal ions is Sr
2+or Ba
2+or both combinations.
5. manufacture method as claimed in claim 1, is characterized in that, in described step 2) in the adobe surface that uses there is the printed layer forming by screen printing, rotary printing or ink-jet printed technique.
6. manufacture method as claimed in claim 5, is characterized in that, the formula of described long-afterglow fluorescent material by mass percentage, 10～20% long persistence luminescent powder, 80～90% high temperature calcium base clear frit.
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|---|---|---|---|
| CN201410074886.4A CN103896633B (en) | 2014-03-03 | 2014-03-03 | A kind of manufacture method of long-afterglow fluorescent ceramic tile |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410074886.4A CN103896633B (en) | 2014-03-03 | 2014-03-03 | A kind of manufacture method of long-afterglow fluorescent ceramic tile |
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| Publication Number | Publication Date |
|---|---|
| CN103896633A true CN103896633A (en) | 2014-07-02 |
| CN103896633B CN103896633B (en) | 2015-08-12 |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108238819A (en) * | 2017-03-11 | 2018-07-03 | 肇庆乐华陶瓷洁具有限公司 | A kind of high texture Antique Imitation Tiles with fluorescence and preparation method thereof |
| CN109336471A (en) * | 2018-10-11 | 2019-02-15 | 深圳大学 | A kind of fluorescence soft ceramic tile and preparation method thereof |
| CN109627053A (en) * | 2019-01-24 | 2019-04-16 | 信益陶瓷(中国)有限公司 | A kind of light-accumulated luminous Imitation Rock Porcelain Tiles and its manufacturing method |
| CN112010673A (en) * | 2020-10-26 | 2020-12-01 | 佛山市东鹏陶瓷发展有限公司 | Luminous ceramic tile and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1775902A (en) * | 2005-12-16 | 2006-05-24 | 中国科学院长春应用化学研究所 | Alkaline earth phosphate long afterglow luminous material and its preparing method |
| CN102775074A (en) * | 2012-08-13 | 2012-11-14 | 广东金牌陶瓷有限公司 | Method for producing microcrystal glass ceramics composite board |
-
2014
- 2014-03-03 CN CN201410074886.4A patent/CN103896633B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1775902A (en) * | 2005-12-16 | 2006-05-24 | 中国科学院长春应用化学研究所 | Alkaline earth phosphate long afterglow luminous material and its preparing method |
| CN102775074A (en) * | 2012-08-13 | 2012-11-14 | 广东金牌陶瓷有限公司 | Method for producing microcrystal glass ceramics composite board |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108238819A (en) * | 2017-03-11 | 2018-07-03 | 肇庆乐华陶瓷洁具有限公司 | A kind of high texture Antique Imitation Tiles with fluorescence and preparation method thereof |
| CN109336471A (en) * | 2018-10-11 | 2019-02-15 | 深圳大学 | A kind of fluorescence soft ceramic tile and preparation method thereof |
| CN109627053A (en) * | 2019-01-24 | 2019-04-16 | 信益陶瓷(中国)有限公司 | A kind of light-accumulated luminous Imitation Rock Porcelain Tiles and its manufacturing method |
| CN112010673A (en) * | 2020-10-26 | 2020-12-01 | 佛山市东鹏陶瓷发展有限公司 | Luminous ceramic tile and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103896633B (en) | 2015-08-12 |
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Inventor after: Lin Qingsheng Inventor before: Fan Xinhui |
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Effective date of registration: 20170614 Address after: 526000 Bei Shui Economic Development Zone, Yongan Town, Dinghu District, Guangdong, Zhaoqing Patentee after: Guangdong Zhonghong exhibition Ceramics Co. Ltd Address before: 528000 Guangdong, Chancheng Province, No. Wei Road, room 5, room 6, No. 208 Patentee before: Fan Xinhui |