CN102432342A - Preparation method of vanadium-titanium-iron system golden crystal glaze - Google Patents
Preparation method of vanadium-titanium-iron system golden crystal glaze Download PDFInfo
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Abstract
The invention relates to a preparation method of vanadium-titanium-iron system golden crystal glaze. A preparation method of a glaze slip comprises steps that: according to mass proportions, 38-43 parts of feldspar produced in Pingjiang, 16-20 parts of quartz produced in Fengyang, 14-18 parts of calcite produced in Xuancheng, 5-7 parts of Suzhou clay, 3-7 parts of a No.1 frit, 2-4 parts of spodumene produced in Australia, 10 parts of soil skeleton produced in Wuxi, and 5 parts of industrial pure Fe2O3 are adopted as raw materials; water is added to the raw materials, and the mixture is subject to ball milling in a ball mill, wherein the ratio of the raw materials to ballstones to water is 1:1.5:1; when the fineness of the glaze slip reaches 250 meshes, an amount of screen tailings is 0.12-0.17%; the specific gravity of the glaze slip is controlled at 1.30g/m<3>, such that the glaze slip is prepared. A glazing method comprises steps that: a base glaze is applied on stoneware or a porcelain tableware base substrate with a glazing method such as glaze spraying, glaze painting or glaze dipping; a glaze layer thickness is controlled at 0.3mm; the base glaze is dried in air; formulated surface glaze materials and water are subject to ball milling, such that surface glaze slip is produced; the surface glaze is applied on the base glaze layer on the base substrate; the sample is dried in air, and is fired, such that a finished product is obtained. With the method, the glaze surface is smooth and uniform, and has a bronze gloss. The thermal stability of the glaze is good, and the dissolution amounts of lead and cadmium are low.
Description
Technical field
The preparation method that to the present invention relates to a kind of vanadium ferrotianium be Jin Jing's glaze.
Background technology
Jin Jing's glaze is meant the crystalline glaze with metalluster, is in the crystallization glaze, to add the toner that MOX or MOX are processed, and through roasting, makes the overglaze outward appearance produce the gloss of similar certain metal.Crystalline glaze is to contain crystal material is separated out beautiful decorative pattern in hypersaturated state crystallization in the glaze; Crystalline size, shape, color are owing to the raw material and the different of firing process that add change all the time; Make and the artistic effect that has uniqueness by the ceramic product of its decoration liked by domestic and international personage.The crystallizing agent that crystalline glaze is commonly used has TiO
2, ZnO, Fe
2O
3Deng, and V
2O
5, MoO
2Deng the generation that can promote xln in the adding glaze.The existing crystalline glaze crystalline substance of Jin Jing's glaze is spent novel uniqueness, Protean characteristics, has the gloss of metalloid again, and cost is low, acid-alkali-corrosive-resisting, glaze chemical property stable, is fit to the tableware for daily use and the ceramics of multiple base substrates such as stoneware, porcelain.The report of relevant crystalline glaze, metal-lustrous glaze is many, relevant patent and report as follows:
CN101066894 disclose a kind of in high temperature sintered coarse crystalline Fe-Ti glaze and preparation method thereof, with TiO
2As crystallizing agent, introduce CaO, Fe
2O
3With TiO
2Form stable xln, still have crystallization effect preferably, reduced the glaze cost again widely to guarantee high temperature.The technical recipe of glaze with the mass fraction proportioning is: 45 parts of feldspars; Quartzy 15～20 parts; 12～18 parts in calcite; 5～8 parts of white titanium pigments; 2～5 parts in talcum; 5～10 parts of iron oxide reds; 5～10 parts of kaolin.By the various starting material of the accurate weighing of technical recipe requirement, the ratio of material, ballstone, water is strict to be carried out by 1: 1.6: 0.6., again raw materials such as white titanium pigment, iron oxide red are added earlier, continued ball milling 6-8 hour mineral ball millings such as feldspar, quartz, calcite, talcum, kaolin 5-9 hour; Glaze slip behind the ball milling is sieved with 10000-hole sieve, and the 10000-hole sieve screen over-size is controlled at 0.03～0.08%; Glaze slip after sieving is added water be modulated into 40～49Be °, impose on the green compact after sieving, go into kiln after the drying, 1250 ℃～1350 ℃ are burnt till.
CN101935232A discloses a kind of hot metal bright glaze and preparation method thereof; It is to contain Orthophosphoric acid Ferrum and ceramic base glaze; Orthophosphoric acid Ferrum: ceramic base glaze=0.5～1:1, the composition of ceramic base glaze is by weight being albite: quartz: Wingdale: kaolin is 15～35: 10～30: 2～6: 3～10.Hot metal bright glaze raw material type of the present invention is few, and wide material sources are cheap, and manufacture craft is identical with common cover-coat enamel, and the glaze cost is low; Method of use is simple, and once-firing gets final product, and firing temperature is low, helps energy-conserving and environment-protective; Ratio through the adjustment glaze can burn out the product with different colours metalluster, like golden yellow, and silvery white, golden red, black-and-blue, reach various design requirementss, use range is extensive.
CN101462895 discloses a kind of flavous metal-lustrous glaze and preparation method thereof, and it is mixed by ceramic glaze and golden yellow pearly pigment, and its weight percent is: ceramic glaze 40～90%, golden yellow pearly pigment 10～60%; This product adds golden yellow pearly pigment in ceramic glaze, the nacreous mica powder thermostability in the yellow pearly pigment of security deposit is brought up to more than 1100 ℃, thereby can present beautiful golden yellow at 1000～1200 ℃ of high temperature once-fired wares.
2008 the 01st phases of periodical " Chinese pottery " have been reported the preparation and the research of Ferrious material glaze; Adopting red oxide of iron, manganese oxide, cupric oxide, nickel oxide, titanium oxide etc. is raw material, has inquired into the preparation, glazing, firing temperature of the Ferrious material glaze influence to glaze.The result shows: the optimum burning temperature-forming of Ferrious material glaze is 1150～1180 ℃, high-temperature holding time 30min, in the roller kiln 1180 ℃～1220 ℃, high-temperature holding time 15min.
2010 the 10th phases of periodical " pottery " have been reported the preparation of ferrotitanium crystalline glaze; With potassium felspar sand, quartz, Wingdale, talcum, bone ash, red stone, titanium oxide is that main raw material has been manufactured experimently out the ferrotianium crystalline glaze; Set about from prescription and technology, through single factor experiment method inquired into that prescription is formed and technological factor to ferrotianium crystalline glaze Effect on Performance.
Periodical " Chinese pottery industry " the 04th phase in 2010 has been reported low-cost TiO
2The development of crystalline glaze, having introduced a kind of is main flux with glass powder with low cost, composition simple T iO
2The method of production of crystalline glaze, and provide crystalline substance and spend full crystalline glaze prescription to be: glass powder 71.8%, feldspar 9.6%, TiO
218.7%.Also inquired into the generation of the crystalline glaze quality factor that influences simultaneously.
Do not find at present report as yet about bronze-colored metalluster crystalline glaze.
Summary of the invention
The objective of the invention is:The preparation method that to aim to provide a kind of vanadium ferrotianium be Jin Jing's glaze, this Jin Jing's glaze has the bronze-colored metalluster of micro-crystallization state, simultaneously glaze moisten full, Heat stability is good, plumbous quantity of cadmium release is very low, is applicable to the decoration of porcelain, stoneware tableware and artwork.
Technical scheme of the present invention is:Technology such as mainly comprise material choice, proportioning, glaze slip processing, glazing and burn till.
This Jin Jing's glaze preparation is divided into ground-coat enamel glaze layer and cover-coat enamel glaze layer, the ZnO in the raw material, TiO
2Need at 1200 ℃～1300 ℃ following roasting 16～18h.
The preparation of ground-coat enamel and glazing: earlier feldspar 38～43 is produced in the Pingjiang River, quartz 16～20 is produced in Fengyang, and calcite 14～18 is produced in the Xuancheng, 5～7, No. 1 frit 3～7 of Suzhou soil, and triphane 2～4 is produced in Australia, and native bone 10～13, technical pure Fe are produced in the Wuxi
2O
3Be that 5～7 raw materials such as grade add water ball milling in ball mill, raw material, ballstone and water ratio are 1: 1.5: 1, when the glaze slip fineness reach 250 mesh sieves tail over be 0.12～0.17%, control glaze slip proportion is 1.30～1.36 g/m
3Get final product.Adopt glaze spraying, oiling or soak enameling method such as glaze ground-coat enamel is imposed on stoneware or porcelain dinner-ware (or artwork) the biscuiting base substrate, the glaze layer thickness is 0.3～0.5mm, dries.
The crystallizing agent TiO that adopts in the glaze
2With generation micro-crystallization crystalline crystallization promoter V
2O
5, TiO
2Also with tinting material Fe
2O
3Effect makes glaze generate bronze-colored metalluster.
The preparation of cover-coat enamel and glazing: earlier feldspar 22～27 is produced in the Pingjiang River, calcite 12～16 is produced in the Xuancheng, 5～7, No. 1 frit 8～12 of Suzhou soil, and bone carbon 5～7, zirconium English powder 8～12, technical pure V are produced in Yixing
2O
5Be 0.1～0.4, technical pure TiO
2Be 9～12, technical pure Fe
2O
3Be 3～5; Technical pure ZnO is that 15～17 raw materials such as (being mass parts) add water ball milling in ball mill; Its raw material, ballstone and water ratio are 1: 1.5: 1, when the glaze slip fineness reach 250 mesh sieves tail over be 0.1～0.13%, control glaze slip proportion is 1.38～1.45 g/m
3Get final product.Adopt glaze spraying, oiling or soak that enameling method such as glaze imposed on ground-coat enamel with cover-coat enamel and on air dried stoneware or porcelain dinner-ware (or artwork) the biscuiting base substrate, the glaze layer thickness is 0.2～0.3mm, dries.
Calcining system: the temperature rise period rises to 500 ± 10 ℃ with 1.7～2.6 ℃/min speed by room temperature with the base substrate after the glazing in the kiln earlier; Rise to 950～1000 ℃, insulation 15～20min with 0.7～1.4 ℃/min speed then, then rise to 1230 ± 10 ℃, be incubated 20～30min again with the phase same rate; Colling stages is cooled fast to 1130 ± 10 ℃, insulation 20～30min with 0.9～1.3 ℃/min speed earlier; Be cooled fast to 850 ± 10 ℃ with 2.5～3.7 ℃/min speed then; Then be cooled to 600 ± 20 ℃ with 1.3～2.7 ℃/min speed again; Naturally cool to room temperature at last and obtain product, and product is detected.
The invention has the beneficial effects as follows:The Jin Jing's glaze that makes is fine and close interlacing tiny needle-like rutile crystal, and refraction of light is strong, and glaze moistens evenly; Has copper-colored metalluster; Heat stability is good, deleterious lead, quantity of cadmium release are very low, are applicable to the decoration of porcelain, stoneware tableware and artwork.
Description of drawings
Fig. 1 vanadium ferrotianium is the 11 inch ceramic discs that Jin Jing's glaze is modified.
Embodiment
1, makes the biscuiting base substrate of stoneware tableware
Blank is by 45.0～55.8 middle mountain products kaolin, and china clay is produced in 20.8～25.7 Xuancheng, and Fengyang of 10.5～20.1 is produced quartzy, and feldspar is produced in 1.4～3.5 the Pingjiang River, and Wuhu of 1.1～3.7 is produced porcelain stone and formed.Raw material is added water carry out ball milling, practice system then, be made into the base substrate shape that needs again, drying is burnt till under specific system at last, and top temperature is 1210 ± 20 ℃, and the control water-intake rate is 2.0%～3.5%, obtains the biscuiting base substrate.Chemical constitution is (mass parts): SiO
2Be 60～75, Al
2O
3Be 18～30, Fe
2O
3Be 1.0～2.0, CaO is 0.1～0.8, and MgO is 0.1～0.7, K
2O is 1.0～3.0, Na
2O is 0.1～0.8, and other are 5～15 years old.
2, glaze and processing
The glaze raw material is: feldspar is produced in the Pingjiang River, and Fengyang is produced quartzy, and calcite is produced in the Xuancheng, Suzhou soil, and No. 1 frit, triphane is produced in Australia, and native bone, technical pure Fe are produced in the Wuxi
2O
3, bone carbon, zirconium English powder, technical pure V are produced in Yixing
2O
5, technical pure TiO
2, technical pure Fe
2O
3Be 3～5, technical pure ZnO etc.
The pre-treatment of raw material: with the ZnO in the raw material, TiO
2At 1200 ℃～1300 ℃ following roasting 16～18h.
3, the preparation of ground-coat enamel and glazing: earlier feldspar 38～43 is produced in the Pingjiang River, quartz 16～20 is produced in Fengyang, and calcite 14～18 is produced in the Xuancheng, 5～7, No. 1 frit 3～7 of Suzhou soil, and triphane 2～4 is produced in Australia, and native bone 10～13, technical pure Fe are produced in the Wuxi
2O
3Be that 5～7 raw materials such as grade add water ball milling in ball mill, its raw material, ballstone and water ratio are 1: 1.5: 1, when the glaze slip fineness reach 250 mesh sieves tail over be 0.12～0.17%, control glaze slip proportion is 1.30～1.36 g/m
3Get final product.Adopt glaze spraying, oiling or soak enameling method such as glaze ground-coat enamel is imposed on stoneware or porcelain dinner-ware (or artwork) the biscuiting base substrate, the glaze layer thickness is 0.3～0.5mm, dries.
4, the preparation of cover-coat enamel and glazing: earlier feldspar 22～27 is produced in the Pingjiang River, calcite 12～16 is produced in the Xuancheng, 5～7, No. 1 frit 8～12 of Suzhou soil, and bone carbon 5～7, zirconium English powder 8～12, technical pure V are produced in Yixing
2O
5Be 0.1～0.4, technical pure TiO
2Be 9～12, technical pure Fe
2O
3Be 3～5, technical pure ZnO is that 15～17 raw materials such as grade add water ball milling in ball mill, and its raw material, ballstone and water ratio are 1: 1.5: 1, when the glaze slip fineness reach 250 mesh sieves tail over be 0.1～0.13%, control glaze slip proportion is 1.38～1.45 g/m
3Get final product.Adopt glaze spraying, oiling or soak that enameling method such as glaze imposed on ground-coat enamel with cover-coat enamel and on air dried stoneware or porcelain dinner-ware (or artwork) the biscuiting base substrate, the glaze layer thickness is 0.2～0.3mm, dries.The present invention is at technical pure TiO
2Be 9～12, technical pure Fe
2O
3Be 3～5, technical pure ZnO is Jin Jing's glaze that all can obtain similar accompanying drawing in 15～17 the scope.
The present invention mainly is main raw material prescription with the cover-coat enamel, but ground-coat enamel of the present invention and cover-coat enamel belong to homologous series, and it is a little to be used better effects if on the whole.As adopting the ground-coat enamel prescription of the daily porcelain of the applicant, Jin Jing's effect of glaze is slightly poor.
5, calcining system: the temperature rise period rises to 500 ± 10 ℃ with 1.7～2.6 ℃/min speed by room temperature with the base substrate after the glazing in the kiln earlier; Rise to 950～1000 ℃, insulation 15～20min with 0.7～1.4 ℃/min speed then, then rise to 1230 ± 10 ℃, be incubated 20～30min again with the phase same rate; Colling stages is cooled fast to 1130 ± 10 ℃, insulation 20～30min with 0.9～1.3 ℃/min speed earlier; Be cooled fast to 850 ± 10 ℃ with 2.5～3.7 ℃/min speed then; Then be cooled to 600 ± 20 ℃ with 1.3～2.7 ℃/min speed again; Naturally cool to room temperature at last and obtain product, and product is detected.
Embodiment:According to above-mentioned to the vanadium ferrotianium be Jin Jing's glaze embodiment made stoneware 8 inch square positions, 220ml coffee cup and 8 inch bowls each 100, its salient features and index are following:
1, the Jin Jing's glaze that makes is fine and close interlacing tiny needle-like rutile crystal, and refraction of light is strong, and glaze moistens evenly, has copper-colored metalluster.
2, glaze Heat stability is good does not ftracture National standard at 1 glaze layer of 180～20 ℃ of heat exchanges.
3, plumbous, quantity of cadmium release is respectively less than 0.226mg/ml and 0.5mg/ml, reaches the strict standard regulation in the world, and is safe in utilization.
4, the chemical constitution of the ground-coat enamel of crystalline glaze (mass parts) is: Na
2O is 0.93～1.51, K
2O is 5.02～5.92, Li
2O is 9.46～10.63, and CaO is 8.46～9.78, and MgO is 0.21～0.44, and BaO is 0.03～0.08, Al
2O
3Be 10.23～11.59, B
2O
3Be 0.23～0.63, MnO
2Be 0.46～0.88, Fe
2O
3Be 6.85～7.56, SiO
2Be 61.22～64.74, other component≤0.7; The chemical constitution of cover-coat enamel (mass parts) is: Na
2O is 0.42～0.76, K
2O is 2.56～4.42, and CaO is 4.21～6.09, and MgO is 0.0.4～0.07, and BaO is 0.03～0.07, and ZnO is 14.23～17.35, Al
2O
3Be 9.12～11.89, Fe
2O
3Be 11.45～15.39, ZrO
2Be 12.35～16.39, SiO
2Be 13.53～17.67, B
2O
3Be 0.86～1.34, TiO
2Be 8.21～10.53, P
2O
5Be 6.95～9.98, V
2O
5Be 0.86～1.36, other component≤0.7.
Claims (5)
1. the vanadium ferrotianium is the preparation method of Jin Jing's glaze, it is characterized in that the preparation and the glazing of cover-coat enamel glaze slip: earlier feldspar 22～27 is produced in the Pingjiang River, calcite 12～16 is produced in the Xuancheng, 5～7, No. 1 frit 8～12 of Suzhou soil, and bone carbon 5～7, zirconium English powder 8～12, technical pure V are produced in Yixing
2O
5Be 0.1～0.4, technical pure TiO
2Be 9～12, technical pure Fe
2O
3Be 3～5, technical pure ZnO is that 15～17 (mass parts) raw material adds water ball milling in ball mill, and raw material, ballstone and water ratio are 1: 1.5: 1, when the glaze slip fineness reach 250 mesh sieves tail over be 0.1～0.13%, control glaze slip proportion is 1.38～1.45 g/m
3Get final product; Adopt glaze spraying, oiling or soak that enameling method such as glaze imposed on ground-coat enamel with cover-coat enamel and on air dried stoneware or porcelain dinner-ware or the artwork biscuiting base substrate, the glaze layer thickness is 0.2～0.3mm, dries.
2. the vanadium ferrotianium is the preparation method of Jin Jing's glaze, it is characterized in that the preparation and the glazing of ground-coat enamel glaze slip: earlier feldspar 38～43 is produced in the Pingjiang River, Fengyang produces quartzy 16～20; Calcite 14～18 is produced in the Xuancheng, 5～7, No. 1 frit 3～7 of Suzhou soil; Triphane 2～4 is produced in Australia, and native bone 10～13, technical pure Fe are produced in the Wuxi
2O
3The raw material that is 5～7 parts (mass parts) adds water ball milling in ball mill, and raw material, ballstone and water ratio are 1: 1.5: 1, when the glaze slip fineness reach 250 mesh sieves tail over be 0.12～0.17%, control glaze slip proportion is 1.30～1.36 g/m
3Get final product; Adopt glaze spraying, oiling or soak enameling method such as glaze ground-coat enamel is imposed on stoneware or porcelain dinner-ware or the artwork biscuiting base substrate, the glaze layer thickness is 0.3～0.5mm, dries.
3. vanadium ferrotianium according to claim 1 and 2 is the preparation method of Jin Jing's glaze; It is characterized in that adopting the glaze firing curve to be: the temperature rise period rises to 500 ± 10 ℃ with 1.7～2.6 ℃/min speed by room temperature with the base substrate after the glazing in the kiln earlier; Rise to 950～1000 ℃, insulation 15～20min with 0.7～1.4 ℃/min speed then, then rise to 1230 ± 10 ℃, be incubated 20～30min again with the phase same rate; Colling stages is cooled fast to 1130 ± 10 ℃, insulation 20～30min with 0.9～1.3 ℃/min speed earlier; Be cooled fast to 850 ± 10 ℃ with 2.5～3.7 ℃/min speed then; Then be cooled to 600 ± 20 ℃ with 1.3～2.7 ℃/min speed again; Naturally cool to room temperature at last and obtain product, and product is detected.
4. vanadium ferrotianium according to claim 1 is the preparation method of Jin Jing's glaze, it is characterized in that ZnO, TiO in the raw material
2All need be at 1200 ℃～1300 ℃ following roasting 16～18h.
5. vanadium ferrotianium according to claim 1 is the preparation method of Jin Jing's glaze, it is characterized in that the chemical constitution (mass parts) of ground-coat enamel is: Na
2O is 0.93～1.51, K
2O is 5.02～5.92, Li
2O is 9.46～10.63, and CaO is 8.46～9.78, and MgO is 0.21～0.44, and BaO is 0.03～0.08, Al
2O
3Be 10.23～11.59, B
2O
3Be 0.23～0.63, MnO
2Be 0.46～0.88, Fe
2O
3Be 6.85～7.56, SiO
2Be 61.22～64.74, other component≤0.7; The chemical constitution of cover-coat enamel (mass parts) is: Na
2O is 0.42～0.76, K
2O is 2.56～4.42, and CaO is 4.21～6.09, and MgO is 0.0.4～0.07, and BaO is 0.03～0.07, and ZnO is 14.23～17.35, Al
2O
3Be 9.12～11.89, Fe
2O
3Be 11.45～15.39, ZrO
2Be 12.35～16.39, SiO
2Be 13.53～17.67, B
2O
3Be 0.86～1.34, TiO
2Be 8.21～10.53, P
2O
5Be 6.95～9.98, V
2O
5Be 0.86～1.36, other component≤0.7.
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| CN108314321A (en) * | 2018-02-25 | 2018-07-24 | 醴陵嘉华瓷业制造有限公司 | The double-deck glaze and preparation method thereof that reaction glaze is combined with metal glaze |
| CN108328926A (en) * | 2018-03-28 | 2018-07-27 | 福建省德化县艺韵陶瓷有限公司 | A kind of starry sky series glaze formula |
| CN111018350A (en) * | 2019-12-18 | 2020-04-17 | 江苏宜翔陶瓷科技有限公司 | Stereoscopic matt orange red frosted black glaze ceramic container and preparation method thereof |
| CN111204978A (en) * | 2020-01-23 | 2020-05-29 | 福建省德化县尚品陶瓷有限公司 | Ceramic glaze with non-cracking glaze surface and glazing method thereof |
| CN111453991A (en) * | 2020-03-14 | 2020-07-28 | 湖南陶润会文化传播有限公司 | Golden crystal glaze and preparation method thereof |
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| CN112499970A (en) * | 2020-12-31 | 2021-03-16 | 卡罗比亚(中国)高新材料有限公司 | Production process of ceramic tile with decorative glaze with golden bright metal cracks |
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Application publication date: 20120502 |