CN102010126A - Lead-free frit for glass color ceramic glaze and preparation method thereof - Google Patents

Lead-free frit for glass color ceramic glaze and preparation method thereof Download PDF

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Publication number
CN102010126A
CN102010126A CN2009101952167A CN200910195216A CN102010126A CN 102010126 A CN102010126 A CN 102010126A CN 2009101952167 A CN2009101952167 A CN 2009101952167A CN 200910195216 A CN200910195216 A CN 200910195216A CN 102010126 A CN102010126 A CN 102010126A
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glass
lead
colored glaze
less glasses
bao
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CN2009101952167A
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李胜春
郑庆云
武荣丽
王亮
李辉
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SHANGHAI GELING NEW MATERIAL SCIENCE AND TECHNOLOGY Co Ltd
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SHANGHAI GELING NEW MATERIAL SCIENCE AND TECHNOLOGY Co Ltd
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Priority to CN2009101952167A priority Critical patent/CN102010126A/en
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Abstract

The invention relates to a lead-free frit for a glass color ceramic glaze and a preparation method thereof. The lead-free frit comprises the following raw materials in percentages by weight: 20-40% of SiO2, 10-30% of B2O3, 10-20% of ZnO, 5-20% of Bi2O3, 5-15% of Na2O and Li2O, 1-10% of TiO2 and 1-10% of BaO. The invention can be applied to glass products, such as bottles, cups, and the like for surface decoration and the lead-free frit for the glass color ceramic glaze for making a trademark, and has the advantages of low melting point, innocuity and no pollution. The lead-free glass can be sealed with various kinds of glass, ceramics and metals consistent with the temperature and an expansion coefficient.

Description

A kind of glass colored glaze lead-less glasses material and preparation method thereof
[technical field]
The present invention relates to glass art, concrete is a kind of glass colored glaze lead-less glasses material and preparation method thereof.
[background technology]
Colored glazed glass uses as a kind of finishing material, has had decades abroad, and the history of recent two decades is also arranged at home.Colored glazed glass has become a kind of sophisticated glass processing product, and its use is very extensive and general.The gold glass is released colored glazed glass, existing so far very years.The most outstanding characteristics of colored glazed glass are its decoration functions that have, and are widely used in architectural decoration, for high building adds lustre, for mansion adds coloured silk.Use colored glazed glass at other field, also can make dull glass become the colorful world, beautified people's life.Below will be from glaze, technology, products characteristics, standard, different aspects such as application are described, and this product of colored glazed glass is used by people better.
The glaze glass industry uses inorganic glaze to be mainly used in and makes building colored glazed glass, vehicle glass, Bottle ﹠ Can and other ambettis such as boiler face kitchen range glass, microwave oven backplate, aspects such as refrigerator electrical equipment glass.Colored glaze material sub-oxide glaze and precious metal glaze, wherein building the most frequently used in the colored glaze is the inorganic non-metallic glaze.Glaze for building mostly is silk screen printing or roller printing because of the process of glazing, so its glaze is called printing ink again.Printing ink has three big moietys: colorant, frit, finish.Mostly colorant is metal oxide, covers glass surface behind the printing sintering, forms opaque colored layer (indivedual colored glazes are transparent or semitransparent), has brought into play the color development function of colored glaze.Frit itself is exactly a glassy substances, and the colorant that can bond behind the sintering produces peculiar gloss.Frit is adjusted the effect of the glazed colour layer coefficient of expansion in addition in addition, and different colours glazed colour layer and glass substrate thermal expansivity are complementary, thereby avoids glazed colour layer cracking, and phenomenon such as come off.Finish is used for regulating the sliminess of printing ink, makes printing ink be applicable to different typography modes.
The technology colored glazed glass is by silk screen printing (or roller etc.) inorganic glaze to be printed on glass surface, again through oven dry, after the thermal treatment, forms the permanent firmly glassy product of glaze layer at glass surface.The colored glazed glass production technique generally includes to produce and prepares, glazing, oven dry, four key links of thermal treatment.Production wherein prepares to differ huge because of the different printing mode, and particularly the making of the half tone of silk-screen is comparatively loaded down with trivial details and professional, has formed a little sector coil, so skip at this.Glazing can be adopted silk screen printing, and modes such as roller printing realize, even available spraying or the glazing of Freehandhand-drawing mode.Oven dry is usually immediately following carrying out continuously in the back of glazing.The purpose of oven dry is to make finish to volatilize gradually, avoids the generation blistering of directly heating.The glaze layer is thick more, and fraction of coverage is high more, and the effect of oven dry is more obvious and necessary.Thermal treatment comprises tempering, and generally between 650～750 ℃, too high then color shoals for half tempered, different heat treatment modes such as hot bending, colored glazed glass sintering temperature, and low excessively then thawing is not thorough, lacks gloss.
The characteristics of colored glazed glass are that the rich color pattern is various, its color, and pattern all can be customized by customer requirement, and use range is extensive, and its color and luster is stable, and is ageing-resistant, and antiacid alkali is colour-fast, and decorative effect is outstanding.Can also absorb simultaneously, the reflecting part solar thermal energy, shaded effects are obvious.Select different heat treatment can obtain the glassy product of difference in functionality.Colored glazed glass also can further carry out plated film, interlayer, Compound Machining such as hollow, additional greater functionality and effect.Not merely have only the plane colored glaze, also can produce the colored glazed glass of bending.
The glazed colour layer of using on the colored glazed glass in fact also is the vitreum of the densification behind the sintering, within it the painted mineral microparticle of part cloth.Colorant is distributed in the situation in the glaze layer, and situation about being distributed in the cement concrete with stone is similar, and just the glaze layer is transparent, and outside surface is slightly rough and uneven in surface.Colored glazed glass is coated with glaze by the surface and has tangible decoration function, belongs to the scope of glass surface processing and decorative kind in glass deep processing classification.Colored glaze toughened glass can be regarded toughened glass as and equally use, and has just increased decorative effect.The colored glaze surface can't influence the further Compound Machining of other operations, thus colored glaze laminated glass, colored glaze hollow, kind glass such as colored glaze plated film are also very general, are used in a large number already, and this has greatly enlarged the use range of colored glazed glass.Colored glazed glass not only has decoration function, also has the function of sunshade, and the shading coefficient of ordinary white silk-screen colored glazed glass can reach about 0.32, and such colored glazed glass has been equivalent to the shaded effects of solar control film glass.
The lead borosilicate glass material that adopt carried out surface decoration and made trade mark glassworks such as bottle and cups as glass glaze more past, but in recent years owing to plumbous toxicity problem comes into one's own, the development research of unleaded type frit is extensively carried out, many lead-less glasses materials have appearred, but at firing temperature, the coefficient of expansion, still there is room for improvement aspects such as alkali resistance, alkali resistance particularly, glaze layer downgrade after soda lye wash repeatedly do not reach the level of lead borosilicate glass material.
The lead-less glasses material alkali resistance that the special fair 4-19704 of Japan's wild pharmaceutical industry difficult to understand (strain) proposes is good, and frit composition quality per-cent consists of: SiO 2Be 45～50%, ZnO is 20～25%, B 2O 3Be 8～12%, K 2O+Na 2O+Li 2O is 5～10%, and CaO is 3～6%, ZrO 2Be 1～5%, F is 1～4%, and this frit nontoxicity is mainly used in the surface decoration of Foods or drinks packing bottle, and as printing trade mark, firing temperature is below 640 ℃, the coefficient of expansion 85 * 10 -7/ ℃ below.
The special public clear 47-33051 of Japan's wild pharmaceutical industry difficult to understand (strain) proposes a class and the non-discoloring glass colored glaze of sulfide effect lead-less glasses material, proposes to replace PbO with BaO+ZnO, and its compositing range mass percent is SiO 2Be 26～32%, B 2O 3Be 15～20%, TiO 2Be 3～8%, Na 2O+Li 2O is 7～12%, and ZnO is 14～19%, and BaO is 17～22%.Utilize BaO+ZnO to replace PbO, red color development is easy, can add selenium ruby, cobalt blue, heat-resisting mineral dye such as cadmium yellow.Because do not contain PbO, under gas effects such as hydrogen sulfide and sulfurous gas, can not turn black.
[summary of the invention]
The objective of the invention is to overcome the deficiency of existing glass colored glaze with lead-less glasses material, a kind of glass colored glaze lead-less glasses material that glassworks such as bottle and cup carry out surface decoration and make trade mark that is applied to is provided, has low melting point, nontoxic, free of contamination advantage, this glass can with all glass that conforms to the coefficient of expansion in this temperature, pottery, the crown glass of metal sealing.
The objective of the invention is to be achieved through the following technical solutions:
A kind of glass colored glaze lead-less glasses material, described frit consists of by weight percentage, SiO 2Be 20～40%, B 2O 3Be 10～30%, ZnO is 10～20%, Bi 2O 3Be 5～20%, Na 2O+Li 2O is 5～15%, TiO 2Be 1～10%, BaO is 1～10%.
Described SiO 2Be preferably 26%～36%; Described B 2O 3Be preferably 15%～25%; Described ZnO is preferably 10%～15%.
Described SiO 2The best is 36%; Described B 2O 3The best is 20%; Described ZnO the best is 12%.
Described Bi 2O 3Be preferably 12%～18%; Described Na 2O+Li 2O is preferably 10%～14%.
Described Bi 2O 3The best is 15%; Described Na 2O+Li 2O the best is 12%.
Described TiO 2Be preferably 1%～5%; Described BaO is preferably 1%～4%.
Described TiO 2The best is 3%; Described BaO the best is 2%.
A kind of glass colored glaze of the present invention comprises the following steps: with lead-less glasses material and preparation method thereof
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing, make compound;
(3) quartz crucible being put into temperature is 1300 ℃～1450 ℃ electric furnace, preheating 15 minutes;
(4) compound is added in the quartz crucible, under 1300 ℃～1450 ℃ glass melting temperature, found, be incubated 2～5 hours;
(5) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
(6) ball milling sieves, and detects packing.
Described glass colored glaze with lead-less glasses material can with all glass that conforms to the coefficient of expansion in this temperature, pottery, metal sealing.
A kind of glass colored glaze of the present invention with the positively effect of lead-less glasses material is: have low melting point, and nontoxic, free of contamination advantage.
[embodiment]
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
The invention provides a kind of glass colored glaze lead-less glasses material that glassworks such as bottle and cup carry out surface decoration and make trade mark that is applied to, have low melting point, nontoxic, free of contamination advantage, this glass can with all glass that conforms to the coefficient of expansion in this temperature, pottery, the crown glass of metal sealing.
Wherein, described a kind of glass colored glaze comprises following by weight the component of forming: SiO with lead-less glasses material 2Be 20～40%, B 2O 3Be 10～30%, ZnO is 10～20%, Bi 2O 3Be 5～20%, Na 2O+Li 2O is 5～15%, TiO 2Be 1～10%, BaO is 1～10%.
In order to improve alkali resistance, add an amount of SiO in the glass ingredient 2Content, and introduce regulation percentage of T iO 2, because the coefficient of expansion that these compositions cause reduces and the raising of firing temperature, also increase B in order to suppress in right amount 2O 3, ZnO, Na 2O and BaO, and introduce Li 2O.TiO 2Can improve alkali resistance, but TiO 2It is too high to surpass 5% firing temperature, Na 2O, BaO and Li 2O can reduce firing temperature, increases the coefficient of expansion of frit simultaneously.Behind the batch melting, pour tabletting machine into and be pressed into thin slice or pour shrend in the cold water into, pulverize by wet-type ball mill again, drying, glass frit powder is made in screening, and is identical with common glass colored glaze method for making, uses with slurry or ink form.Glass powder can with titanium white, cobalt blue, chrome green, heat-resisting mineral dye such as cologne earth mixes, and adds the mixing slurry type glaze of making of silk screen wet goods organic carrier again, perhaps with the mixing thermoplastics type's glaze of making of paraffin.To the glasswork glazing, as utilize method for printing screen by usual method, burn till at 530～580 ℃ then the bottle printing, form alkali proof, the painted epithelium of surface luster.
Embodiment 1
(1) the raw material composition is by weight percentage:
SiO 2Be 27%, B 2O 3Be 24%, ZnO is 20%, Bi 2O 3Be 13%, Na 2O+Li 2O is 12%, TiO 2Be 2%, BaO is 2%.
(2) preparation method:
1. the weight percent according to each component takes by weighing each raw material;
2. with the raw material thorough mixing that is taken by weighing, make compound;
3. quartz crucible is put into temperature and is 1340 ℃ electric furnace, preheating 15 minutes;
4. compound is added in the quartz crucible, under 1340 ℃ glass melting temperature, found, be incubated 2 hours;
5. the glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
6. ball milling sieves, and detects packing.
(3) product performance:
The coefficient of expansion (0～300 ℃): 87 * 10 -7/ ℃
Softening temperature: 484 ℃
Heat-resisting mineral dye adds: 5～15%
Firing temperature: 530～580 ℃
Have or not be full of cracks: do not have
Embodiment 2
(1) the raw material composition is by weight percentage:
SiO 2Be 29%, B 2O 3Be 24%, ZnO is 13%, Bi 2O 3Be 14%, Na 2O+Li 2O is 13%, TiO 2Be 2%, BaO is 5%.
(2) preparation method:
1. the weight percent according to each component takes by weighing each raw material;
2. with the raw material thorough mixing that is taken by weighing, make compound;
3. quartz crucible is put into temperature and is 1350 ℃ electric furnace, preheating 15 minutes;
4. compound is added in the quartz crucible, under 1350 ℃ glass melting temperature, found, be incubated 2 hours;
5. the glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
6. ball milling sieves, and detects packing.
(3) product performance:
The coefficient of expansion (0～300 ℃): 88 * 10 -7/ ℃
Softening temperature: 478 ℃
Heat-resisting mineral dye adds: 5～15%
Firing temperature: 530～580 ℃
Have or not be full of cracks: do not have
Embodiment 3
(1) the raw material composition is by weight percentage:
SiO 2Be 32%, B 2O 3Be 21%, ZnO is 16%, Bi 2O 3Be 10%, Na 2O+Li 2O is 9%, TiO 2Be 3%, BaO is 9%.
(2) preparation method:
1. the weight percent according to each component takes by weighing each raw material;
2. with the raw material thorough mixing that is taken by weighing, make compound;
3. quartz crucible is put into temperature and is 1420 ℃ electric furnace, preheating 15 minutes;
4. compound is added in the quartz crucible, under 1420 ℃ glass melting temperature, found, be incubated 4 hours;
5. the glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
6. ball milling sieves, and detects packing.
(3) product performance:
The coefficient of expansion (0～300 ℃): 89 * 10 -7/ ℃
Softening temperature: 470 ℃
Heat-resisting mineral dye adds: 5～15%
Firing temperature: 530～580 ℃
Have or not be full of cracks: do not have
Embodiment 4
(1) the raw material composition is by weight percentage:
SiO 2Be 36%, B 2O 3Be 20%, ZnO is 12%, Bi 2O 3Be 15%, Na 2O+Li 2O is 12%, TiO 2Be 3%, BaO is 2%.
(2) preparation method:
1. the weight percent according to each component takes by weighing each raw material;
2. with the raw material thorough mixing that is taken by weighing, make compound;
3. quartz crucible is put into temperature and is 1440 ℃ electric furnace, preheating 15 minutes;
4. compound is added in the quartz crucible, under 1440 ℃ glass melting temperature, found, be incubated 4 hours;
5. the glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
6. ball milling sieves, and detects packing.
(3) product performance:
The coefficient of expansion (0～300 ℃): 89 * 10 -7/ ℃
Softening temperature: 462 ℃
Heat-resisting mineral dye adds: 5～15%
Firing temperature: 530～580 ℃
Have or not be full of cracks: do not have
Embodiment 5
(1) the raw material composition is by weight percentage:
SiO 2Be 37%, B 2O 3Be 20%, ZnO is 14%, Bi 2O 3Be 17%, Na 2O+Li 2O is 10%, TiO 2Be 1%, BaO is 1%.
(2) preparation method:
1. the weight percent according to each component takes by weighing each raw material;
2. with the raw material thorough mixing that is taken by weighing, make compound;
3. quartz crucible is put into temperature and is 1440 ℃ electric furnace, preheating 15 minutes;
4. compound is added in the quartz crucible, under 1440 ℃ glass melting temperature, found, be incubated 5 hours;
5. the glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
6. ball milling sieves, and detects packing.
(3) product performance:
The coefficient of expansion (0～300 ℃): 86 * 10 -7/ ℃
Softening temperature: 469 ℃
Heat-resisting mineral dye adds: 5～15%
Firing temperature: 530～580 ℃
Have or not be full of cracks: do not have
Embodiment 6
(1) the raw material composition is by weight percentage:
SiO 2Be 33%, B 2O 3Be 18%, ZnO is 17%, Bi 2O 3Be 19%, Na 2O+Li 2O is 11%, TiO 2Be 1%, BaO is 1%.
(2) preparation method:
1. the weight percent according to each component takes by weighing each raw material;
2. with the raw material thorough mixing that is taken by weighing, make compound;
3. quartz crucible is put into temperature and is 1400 ℃ electric furnace, preheating 15 minutes;
4. compound is added in the quartz crucible, under 1400 ℃ glass melting temperature, found, be incubated 3 hours;
5. the glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
6. ball milling sieves, and detects packing.
(3) product performance:
The coefficient of expansion (0～300 ℃): 85 * 10 -7/ ℃
Softening temperature: 476 ℃
Heat-resisting mineral dye adds: 5～15%
Firing temperature: 530～580 ℃
Have or not be full of cracks: do not have.

Claims (8)

1. a glass colored glaze lead-less glasses material is characterized in that described frit consists of by weight percentage, SiO 2Be 20～40%, B 2O 3Be 10～30%, ZnO is 10～20%, Bi 2O 3Be 5～20%, Na 2O+Li 2O is 5～15%, TiO 2Be 1～10%, BaO is 1～10%.
2. a kind of glass colored glaze lead-less glasses material according to claim 1 is characterized in that described SiO2 is 26%～36%; Described B 2O 3Be 15%～25%; Described ZnO is 10%～15%.
3. a kind of glass colored glaze lead-less glasses material according to claim 2 is characterized in that described SiO 2Be 36%; Described B 2O 3Be 20%; Described ZnO is 12%.
4. a kind of glass colored glaze lead-less glasses material according to claim 1 is characterized in that described Bi 2O 3Be 12%～18%; Described Na 2O+Li 2O is 10%～14%.
5. a kind of glass colored glaze lead-less glasses material according to claim 4 is characterized in that described Bi 2O 3Be 15%; Described Na 2O+Li 2O is 12%.
6. a kind of glass colored glaze lead-less glasses material according to claim 1 is characterized in that described TiO 2Be 1%～5%; Described BaO is 1%～4%.
7. a kind of glass colored glaze lead-less glasses material according to claim 6 is characterized in that described TiO 2Be 3%; Described BaO is 2%.
8. a kind of glass colored glaze according to claim 1 is characterized in that with the preparation method of lead-less glasses material, comprises the following steps:
(1) weight percent according to each component takes by weighing each raw material;
(2) with the raw material thorough mixing that is taken by weighing, make compound;
(3) quartz crucible being put into temperature is 1300 ℃～1450 ℃ electric furnace, preheating 15 minutes;
(4) compound is added in the quartz crucible, under 1300 ℃～1450 ℃ glass melting temperature, found, be incubated 2～5 hours;
(5) glass metal after will melting is poured tabletting machine into and is pressed into thin slice or pours shrend in the cold water into;
(6) ball milling sieves, and detects packing.
CN2009101952167A 2009-09-07 2009-09-07 Lead-free frit for glass color ceramic glaze and preparation method thereof Pending CN102010126A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826757A (en) * 2012-09-29 2012-12-19 湖南泉湘陶瓷有限公司 Manufacturing method of silicon-zinc crystal glaze
CN104891810A (en) * 2015-06-04 2015-09-09 禹金库 Glass glaze coloring composite material, glaze coloring glass plate and application of glass glaze coloring composite material
CN109574502A (en) * 2018-12-04 2019-04-05 咸阳盈和电子材料有限公司 A kind of automobile back windshield half matt crown glass body powder and preparation method thereof
CN109626825A (en) * 2019-01-17 2019-04-16 北京汉能光伏投资有限公司 Inorganic glaze and preparation method thereof, colored glazed glass and preparation method thereof
CN109717738A (en) * 2019-01-31 2019-05-07 王德平 Cook nonmetallic heating device
CN110099873A (en) * 2017-11-30 2019-08-06 法国圣戈班玻璃厂 Coated with stack of thin and with the glass plate of glaze layer
CN110436780A (en) * 2019-08-06 2019-11-12 北京工业大学 A kind of inorganic brilliant color painting of 3D printing for surface of plate glass decoration
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CN113024124A (en) * 2020-09-02 2021-06-25 深圳市百柔新材料技术有限公司 Glass powder and preparation method thereof
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CN113754274A (en) * 2021-08-19 2021-12-07 天珵新材料(嘉兴)有限公司 Lead-free glass powder, glass black glaze and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826757A (en) * 2012-09-29 2012-12-19 湖南泉湘陶瓷有限公司 Manufacturing method of silicon-zinc crystal glaze
CN104891810A (en) * 2015-06-04 2015-09-09 禹金库 Glass glaze coloring composite material, glaze coloring glass plate and application of glass glaze coloring composite material
CN110099873A (en) * 2017-11-30 2019-08-06 法国圣戈班玻璃厂 Coated with stack of thin and with the glass plate of glaze layer
CN109574502A (en) * 2018-12-04 2019-04-05 咸阳盈和电子材料有限公司 A kind of automobile back windshield half matt crown glass body powder and preparation method thereof
CN109626825A (en) * 2019-01-17 2019-04-16 北京汉能光伏投资有限公司 Inorganic glaze and preparation method thereof, colored glazed glass and preparation method thereof
CN111150304A (en) * 2019-01-31 2020-05-15 王德平 Nonmetal heating device is used in culinary art
CN111067351A (en) * 2019-01-31 2020-04-28 王德平 Nonmetal heating device is used in culinary art
CN109717738A (en) * 2019-01-31 2019-05-07 王德平 Cook nonmetallic heating device
CN111166188A (en) * 2019-01-31 2020-05-19 王德平 Metal body and heating plate suitable for food utensil
CN111166188B (en) * 2019-01-31 2021-09-17 王德平 Metal body and heating plate suitable for food utensil
CN111067351B (en) * 2019-01-31 2021-09-17 王德平 Nonmetal heating device is used in culinary art
CN111150304B (en) * 2019-01-31 2022-03-04 王德平 Nonmetal heating device is used in culinary art
CN110436780A (en) * 2019-08-06 2019-11-12 北京工业大学 A kind of inorganic brilliant color painting of 3D printing for surface of plate glass decoration
CN113024124A (en) * 2020-09-02 2021-06-25 深圳市百柔新材料技术有限公司 Glass powder and preparation method thereof
CN113620606A (en) * 2021-08-12 2021-11-09 醴陵陶润实业发展有限公司 Silver metallic luster frit and preparation method thereof
CN113754274A (en) * 2021-08-19 2021-12-07 天珵新材料(嘉兴)有限公司 Lead-free glass powder, glass black glaze and preparation method thereof

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Application publication date: 20110413