CN101786795A - Enamel glaze and preparation process thereof - Google Patents

Enamel glaze and preparation process thereof Download PDF

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Publication number
CN101786795A
CN101786795A CN200910238973A CN200910238973A CN101786795A CN 101786795 A CN101786795 A CN 101786795A CN 200910238973 A CN200910238973 A CN 200910238973A CN 200910238973 A CN200910238973 A CN 200910238973A CN 101786795 A CN101786795 A CN 101786795A
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glaze
enamel
oxide
powder
coloring
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CN101786795B (en
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刘权辉
曾学富
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Shenzhen Yong Feng Yuan Industry Co ltd
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Shenzhen Yong Feng Yuan Industry Co ltd
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Abstract

The invention discloses an enamel glaze which belongs to the technical field of ceramic materials, and the enamel glaze comprises a colored glaze basic glaze, an enamel glaze basic glaze and coloring pigments. The invention further discloses a preparation process of the enamel glaze and an application of the enamel glaze. The preparation process can improve the firing temperature of the enamel colored glaze, expand the firing range of the glaze, improve the viscosity of the enamel colored glaze and ensure that coloring metal oxides can not be diffused or the color can not be dimmed due to the flowing of the glaze by optimizing the formula of the enamel colored glaze, adopting an appropriate amount of zinc oxide for replacing heavy metal flux materials, such as lead oxide and the like, integrating the applicable color development performances of a variety of coloring materials and introducing a rare earth compound of yttrium oxide. The preparation process can further ensure that the coloring metal oxides in the enamel glaze can not be oxidized by oxygen or water vapor in the air through the way of underglaze color, thereby further ensuring that a product can not change the color or fade forever, closing heavy metals contained in the coloring oxides for avoiding solventing-out and solving the problem of heavy metal pollution.

Description

A kind of enamel glaze and preparation technology thereof
Technical field
The invention belongs to the ceramic technology field, especially relate to a kind of enamel ceramic glaze and preparation technology thereof.
Background technology
Long history is arranged, be called as " faience queen ", the enamel faience of " government porcelain kiln in the government porcelain kiln ", be to develop by cloisonne, cloisonne is to form at copper tire enamelling glaze, and the enamel faience is to fire then at porcelain body enamelling glaze to form, so the enamel faience claims " enamel painting on porcelain " again, though colour enamels has the porcelain exquisiteness, color material is dignified, bright in colour beautiful, characteristics such as painter's exquisiteness, but manufacture craft is still continued to use the low temperature over-glaze decoration technology of painting enamel glaze on traditional porcelain body at present, because of the decorative patterns pattern protrudes about glaze 1mm, be easy to the variable color that comes off through permanent friction, low because of adding fusing point in the colour enamels base glaze simultaneously, Young's modulus is big, the glass-based glaze that the coefficient of expansion is big, because of containing quartz in the glass-based glaze, quartzy melt temperature height own, up to more than 1,700 degree, in order to reduce the fusing point of glass-based glaze, will add feldspar as fusing assistant, feldspar can be introduced potassium again, sodium element, potassium, sodium can increase the coefficient of expansion of basic glaze, reduce the sticking power of enamel glaze and porcelain body, cause the enamel colored glaze to come off from porcelain body, the characteristics of enamel faience require pattern line kind to want three-dimensional feel, when the enamelling colored glaze, the glaze layer requires to reach certain thickness, and the coefficient of expansion because of porcelain body glaze and colour enamels base glaze does not match again, causes the be full of cracks of enamel colored glaze glaze, the both so-called crackle that hacks adds CaF in addition 2Reduce the viscosity of basic glaze, be easy to flow after making basic glaze fusion, because of basic glaze temperature flowing good, should not burn high temperature, cause the irregular diffusion of the painted oxidation color of part at temperature Gao Shiyi, make its dim pattern unclear, traditional colour enamels relies on the bright-coloured heavy metal of color development, such as: " arsenic ", it is deleterious material to human body and environment.Along with the raising of people's living standard, health care consciousness strengthens, and heavy metal such as lead, cadmium and toxicity of compound thereof further are familiar with, and countries in the world all propose the more and more requirement of strictness to the use that contains heavy metal material.Traditional enamel faience mostly is the detailing product of little bowl, bottle, cigarette kettle and so on, is subjected to significant limitation aspect moulding.
Summary of the invention
One of purpose of the present invention is to provide a kind of enamel glaze, solves the defective that prior art exists.
For achieving the above object, the present invention adopts following technical scheme:
A kind of enamel glaze comprises coloured glaze basis glaze, enamel glaze basis glaze and tinting pigment, and the component and the content (weight percent wt%) of described coloured glaze basis glaze are: SiO 240～60%, Al 2O 35～10%, CaO5～12%, MgO0～5%, P 2O 51～5%, SrO0.5～5%, ZnO2～8%, K 2O1～7%, Na 2O1～5%, Li 2O0.5～5%, B 2O 31～8%, ZrO 20～4%; The component and the content (weight percent wt%) of described enamel glaze basis glaze are SiO 244～63%, Al 2O 37～12%, CaO5～12%, MgO0～5%, P 2O 50～5%, SrO0.5～5%, ZnO3～8%, K 2O1～6.5%, Na 2O1～5%, Li 2O0.5～5%, B 2O 31～8%, ZrO 20～4%, Y 2O 30.2～4%.
Preferred scheme is: the firing range of described coloured glaze basis glaze is 1080 ℃～1180 ℃, high fiery soaking time 10～120min; Described enamel glaze basis glaze firing range is 1050 ℃～1200 ℃, high fiery soaking time 10～120min.
More preferred scheme is: described tinting pigment is one or several mixtures in ferric oxide, chromic oxide, cupric oxide, weisspiessglanz, nickel oxide, cobalt oxide, stannic oxide, the manganese oxide; Perhaps be one or several mixtures that form with the grinding of low temperature flux mixed calcining in the described coloring oxide.Coloring metal oxide compound and low temperature flux mixed calcining grind the mixture that forms, and the more single coloring metal oxide compound of color development is more stable.
Two of purpose of the present invention is to provide a kind of technology for preparing enamel glaze, adopts following technical scheme:
A kind of technology for preparing enamel glaze comprises the steps:
(A) preparation of color glaze:
(A1) preparation of the basic glaze of color glaze: get the silica powder 20～45% that 325 orders or thinner mesh screen sieve, get the feldspar in powder 20～40% that 325 orders or thinner mesh screen sieve,, borax 2～20%, zinc oxide 2～7%, zirconium silicate 0～5%, lime carbonate 6～16%, magnesiumcarbonate 0～8%, Vanadium Pentoxide in FLAKES 1～5%, Strontium carbonate powder 0.5～6%, Quilonum Retard 2～10%;
(A2) above-mentioned raw materials is mixed after, 1350 ℃～1500 ℃ fusings, put into the cold water shrend and make frit;
(A3) frit is packed in the ball mill, add water, high alumina ballstone and add and get the kaolin 0～12% that 325 orders or thinner mesh screen sieve and grind to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 70～100 ℃ of oven dry, and make powder and cross 250 mesh sieves or thinner, with dry powder and the coloring oxide tinting pigment mixing of making, and adding (40～70%) water mixing and stirring can be used;
(B) preparation of enamel glaze basis glaze:
(B 1) gets the silica powder 25～45% that 325 orders or thinner mesh screen sieve, get the nepheline powder 20～40% that 325 orders or thinner mesh screen sieve, borax 2～20%, zinc oxide 2～7%, zirconium silicate 0～5%, yttrium oxide 0.1～3%, lime carbonate 6～16%, magnesiumcarbonate 0～8%, Vanadium Pentoxide in FLAKES 0～5%, Strontium carbonate powder 0.5～6%, Quilonum Retard 2～10%;
(B2) above-mentioned raw materials is mixed after, 1360 ℃～1480 ℃ fusings, put into the cold water shrend and make frit;
(B3) frit is packed in the ball mill, add the kaolin that water, high alumina ballstone and 0～15%325 order or thinner mesh screen sieve, or other glaze slip properties modifier grinds to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 80～100 ℃ of oven dry, and make that powder is crossed 250 orders or thinner mesh screen makes enamel color ceramic glaze basis glaze.
Three of purpose of the present invention is to provide a kind of colour enamels, burns for the described enamel glaze baking of the arbitrary technical scheme of one of goal of the invention to form.
Four of purpose of the present invention is to provide a kind of technology for preparing colour enamels, adopts following technical scheme:
A kind of technology for preparing colour enamels comprises the steps:
(1) on smart base of pottery or low temperature biscuit, dips in and apply the skeleton diagram that a kind of material water-proof material that can stop the base substrate sucking forms required pattern;
(2) at (red, yellow, blue, green, black etc.) of two described prepared of smart base of described pottery or low temperature biscuit outside surface last layer goal of the invention coloured glaze;
(3) throw off or after low temperature burns the material water-proof material of before having painted, form colourless in the position that scribbles material water-proof material originally or do not have the pattern contour figure of glaze, carrying out enamel glaze on no glaze pattern contour figure decorates, after product decoration is good, send kiln high temperature to burn till product, firing temperature is controlled at 1200 ℃～1300 ℃, execute one deck coloured glaze basis glaze in the above through after the assay was approved through the product that burns till, sending kiln to carry out glaze firing, the temperature of glaze firing is controlled at 1080 ℃～1180 ℃, can be fired into enamel faience under the glaze.
Preferred scheme, described material water-proof material is tearable glue, perhaps oils, perhaps paraffin, perhaps plastics, perhaps waterproofing agent etc.
The present invention compared with prior art has following advantage and beneficial effect:
The present invention is by paint enamel glaze on smart base of pottery or biscuit, burn till through 1200 ℃～1300 ℃ oxydizing flame porcelainization then, enamel glaze or pattern were by firm being fixed on the porcelain base after the process pate dureization was burnt till, last one deck basis glaze of on the porcelain body that burns till through porcelainization, executing again, the firing temperature of glaze burns till for low 80 ℃～150 ℃ than the temperature of burning till for the first time, allow under the glaze enamel colored glaze stablize color development and do not flow or diffusion, make its feature that not only has traditional colour enamels, also have the characteristics of under glazed.
Colour enamels porcelain products by method manufacturing of the present invention, have characteristics such as bright-colored, pure, full, no diffusion, no color differnece, embossment sense be strong, increased the sticking power of enamel glaze and porcelain body simultaneously, adjusted the coefficient of expansion of porcelain body and colour enamels base glaze, make it suitable mutually, the enamel colored glaze is difficult for coming off from porcelain body; The mode that belongs under glazed by the enamel faience of this invention manufacturing, color in the enamel glaze and air insulated, coloring metal oxide compound in the enamel glaze can be by airborne oxygen or steam oxidation, thereby guarantee that product is will never change colour or fade, contained heavy metal is enclosed under the glaze by cover-coat enamel in the coloring oxide simultaneously, can dissolved not come out, solved the problem of heavy metal contamination, thereby guarantee the edible safety of product; This method can be achieved on any type product of pottery, can only be in the limitation of the enterprising luggage decorations of smallclothes products such as little bowl, bottle, cigarette kettle thereby solved traditional enamel faience.
The present invention is by optimizing the colour enamels glaze formula, adopted an amount of zinc oxide heavy metal flux material such as plumbous oxide as an alternative, taken into account applicable performance to various colorant color developments, by introducing the rare earth compound yttrium oxide, improve the firing temperature of enamel colored glaze, widened the firing range of glaze, improved the viscosity of enamel colored glaze, guaranteed that the coloring metal oxide compound does not spread because of glaze is mobile or color becomes dim.Mode by under glazed again, guarantee that the coloring metal oxide compound in the enamel glaze can be by airborne oxygen or steam oxidation, thereby guarantee that product is will never change colour or fade that contained heavy metal is closed insoluble separating out in the coloring oxide, has solved the problem of heavy metal contamination.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further details:
Raw materials used main chemical constitution weight percent among table 1 embodiment
Embodiment 1: on the smart base of 480mm sclerotin porcelain vase, dip in tearable glue with writing brush and be coated with the outline figure of dragon and phoenix that draws, again at the golden yellow coloured glaze of the outside surface last layer of the smart base of 480mm sclerotin porcelain vase, golden yellow coloured glaze according to following formulation with 25 parts of silica powders (325 order), feldspar in powder (325 order): 25 parts, 10 parts of kaolin, 12 parts of boraxs, 5 parts in zinc oxide, 1 part of zirconium silicate, 11 parts in lime carbonate, 5 parts of Vanadium Pentoxide in FLAKESs, 1 part of Strontium carbonate powder, 5 parts of Quilonum Retards.After above-mentioned raw materials mixed,, put into the cold water shrend and make frit 1400 ℃～1450 ℃ fusings.Frit is packed in the ball mill, add water, high alumina ballstone and add 6% kaolin and grind to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 70～100 ℃ of oven dry, and make powder and cross 250 mesh sieves, basic glaze and the tinting pigment of making (wrapping up golden yellow colorant) carried out batch mixes according to 7: 10 weight ratios, add entry in the material that will mix again, according to material: the ratio of water=10: 7 adds, and mixing and stirring can be used.
After throwing off the tearable glue of before scribbling up, on the position that scribbles tearable glue originally, form the dragon of no glaze and the outline figure of phoenix pattern, carry out the enamel glaze decoration on the imperial and phoenix pattern contour figure at no glaze by the painter again: enamel glaze according to following formulation with 38 parts of silica powders (325 order), nepheline powder (325 order): 25 parts, 12 parts of boraxs, 3 parts in zinc oxide, 2 parts of zirconium silicates, 2 parts of yttrium oxides, 6 parts in lime carbonate, 3 parts in magnesiumcarbonate, 2 parts of Vanadium Pentoxide in FLAKESs, 3 parts of Strontium carbonate powders, 4 parts of Quilonum Retards.After above-mentioned raw materials mixed,, put into the cold water shrend and make frit 1390 ℃～1430 ℃ fusings.Frit is packed in the ball mill, add water, high alumina ballstone and add 10% kaolin and grind to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 80～100 ℃ of oven dry, and make powder and cross 250 mesh sieves, with the basic glaze made and coloring oxide (ferric oxide) the ratio batching according to 1: 2, again according to material: the ratio of water=50: 33 adds entry, and outer doping (PVA polyvinyl alcohol 0.5%) mixing and stirring promptly can be used for enamel colored drawing under the ceramic glaze.
After product decoration is good, send kiln high temperature to burn till product, firing temperature is controlled at 1250 ℃～1270 ℃, 100 minutes high temperature constant temperature time, burning is done 16 hours cycles, the product that process is burnt till is through after the assay was approved, execute one deck color basis glaze in the above, then through 80～100 ℃ of oven dry, and make powder and cross 250 mesh sieves, sending kiln to carry out glaze firing, the temperature of glaze firing is controlled at 1130 ℃～1150 ℃, 60 minutes high temperature constant temperature time, burn and do 8 hours cycles, can be fired into colour enamels porcelain vase under the 480mm sclerotin enamel.
Embodiment 2: on the smart base in 400mm hard-paste square position, dip in the outline figure that paraffin is coated with the Tree Peony flower of drawing with writing brush, again the outside surface last layer large red coloured glaze of smart base in 400mm hard-paste square position, the large red coloured glaze according to following formulation with 44 parts of silica powders (325 order), nepheline powder (325 order): 20 parts, 6 parts of kaolin, 8 parts of boraxs, 6 parts in zinc oxide, 1 part of yttrium oxide, 9 parts in lime carbonate, 2 parts in magnesiumcarbonate, 2 parts of Strontium carbonate powders, 2 parts of Quilonum Retards.After above-mentioned raw materials mixed,, put into the cold water shrend and make frit 1450 ℃ of fusings.Frit is packed in the ball mill, add water, high alumina ballstone and add 10% kaolin and grind to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 80 ℃ of oven dry, and make powder and cross 250 mesh sieves, basic glaze and the tinting pigment of making (wrapping up bright red colorant) carried out batch mixes according to 1: 2 weight ratio, add entry in the material that will mix again, according to material: the ratio of water=2: 1 adds, and mixing and stirring can be used.
To spray the product of color after 400 ℃ temperature baking, paraffin is burnt the outline figure that forms the Tree Peony flower pattern of no glaze on the position that scribbles paraffin originally, carrying out enamel glaze by the painter on no glaze Tree Peony flower pattern contour figure again decorates: enamel glaze according to following formulation with 38 parts of silica powders (325 order), nepheline powder (325 order): 25 parts, 12 parts of boraxs, 3 parts in zinc oxide, 2 parts of zirconium silicates, 2 parts of yttrium oxides, 6 parts in lime carbonate, 3 parts in magnesiumcarbonate, 2 parts of Vanadium Pentoxide in FLAKESs, 3 parts of Strontium carbonate powders, 4 parts of Quilonum Retards.After above-mentioned raw materials mixed,, put into the cold water shrend and make frit 1400 ℃ of fusings.Frit is packed in the ball mill, add water, high alumina ballstone and add 2% kaolin and grind to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 100 ℃ of oven dry, and make powder and cross 250 mesh sieves, with the basic glaze made and coloring oxide (cupric oxide) the ratio batching according to 1: 2, again according to material: the ratio of water=5: 3 adds entry, and outer doping (carboxymethyl cellulose 0.8%) mixing and stirring promptly can be used for enamel colored drawing under the ceramic glaze.
After product decoration is good, send kiln high temperature to burn till product, burn till at 1280 ℃～1300 ℃ reducing flames, 40 minutes high temperature constant temperature time, burn and do 6 hours cycles, the product that process is burnt till is through after the assay was approved, execute one deck color basis glaze in the above, then through 100 ℃ of oven dry, and make powder and cross 250 mesh sieves, sending kiln to carry out glaze firing, the temperature of glaze firing is controlled at 1180 ℃, 60 minutes high temperature constant temperature time, burn and do 8 hours cycles, can be fired into enamel faience square position under the 400mm hard enamel.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to the protection domain of inventing type.

Claims (7)

1. enamel glaze is characterized in that: comprise coloured glaze basis glaze, enamel glaze basis glaze and tinting pigment, the component and the content (weight percent wt%) of described coloured glaze basis glaze are: SiO 240～60%, Al 2O 35～10%, CaO 5～12%, and MgO 0～5%, P 2O 51～5%, SrO 0.5～5%, and ZnO 2～8%, K 2O 1～7%, Na 2O 1～5%, Li 2O0.5～5%, B 2O 31～8%, ZrO 20～4%; The component and the content (weight percent wt%) of described enamel glaze basis glaze are SiO 244～63%, Al 2O 37～12%, CaO 5～12%, and MgO 0～5%, P 2O 50～5%, SrO 0.5～5%, ZnO3～8%, K 2O 1～6.5%, Na 2O1～5%, Li 2O0.5～5%, B 2O 31～8%, ZrO 20～4%, Y 2O 30.2～4%.
2. enamel glaze as claimed in claim 1 is characterized in that: the firing range of described coloured glaze basis glaze is 1080 ℃～1180 ℃, high fiery soaking time 10～120min; Described enamel glaze basis glaze firing range is 1050 ℃～1200 ℃, high fiery soaking time 10～120min.
3. enamel glaze as claimed in claim 2, it is characterized in that: described tinting pigment is a coloring oxide, and described coloring oxide is one or several mixtures in ferric oxide, chromic oxide, cupric oxide, weisspiessglanz, nickel oxide, cobalt oxide, stannic oxide, the manganese oxide; Perhaps be one or several mixtures that form with the grinding of low temperature flux mixed calcining in the described coloring oxide.
4. a technology for preparing enamel glaze comprises the steps:
(A) preparation of color glaze:
(A1) preparation of the basic glaze of color glaze: get the silica powder 20～45% that 325 orders or thinner mesh screen sieve, get the feldspar in powder 20～40% that 325 orders or thinner mesh screen sieve,, borax 2～20%, zinc oxide 2～7%, zirconium silicate 0～5%, lime carbonate 6～16%, magnesiumcarbonate 0～8%, Vanadium Pentoxide in FLAKES 1～5%, Strontium carbonate powder 0.5～6%, Quilonum Retard 2～10%;
(A2) above-mentioned raw materials is mixed after, 1350 ℃～1500 ℃ fusings, put into the cold water shrend and make frit;
(A3) frit is packed in the ball mill, add water, high alumina ballstone and add and get the kaolin 0～12% that 325 orders or thinner mesh screen sieve and grind to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 70～100 ℃ of oven dry, and make powder and cross 250 mesh sieves or thinner, with dry powder and the coloring oxide tinting pigment mixing of making, and adding (40～70%) water mixing and stirring can be used;
(B) preparation of enamel glaze basis glaze:
(B1) get the silica powder 25～45% that 325 orders or thinner mesh screen sieve, get the nepheline powder 20～40% that 325 orders or thinner mesh screen sieve, borax 2～20%, zinc oxide 2～7%, zirconium silicate 0～5%, yttrium oxide 0.1～3%, lime carbonate 6～16%, magnesiumcarbonate 0～8%, Vanadium Pentoxide in FLAKES 0～5%, Strontium carbonate powder 0.5～6%, Quilonum Retard 2～10%;
(B2) above-mentioned raw materials is mixed after, 1360 ℃～1480 ℃ fusings, put into the cold water shrend and make frit;
(B3) frit is packed in the ball mill, add the kaolin that water, high alumina ballstone and 0～15%325 order or thinner mesh screen sieve, or other glaze slip properties modifier grinds to form glaze slip, it is surplus less than 0.03% that fineness is controlled at 10000-hole sieve, then through 80～100 ℃ of oven dry, and make that powder is crossed 250 orders or thinner mesh screen makes enamel color ceramic glaze basis glaze.
5. a colour enamels forms for each described enamel glaze of claim 1～3 dries by the fire to burn.
6. a technology for preparing colour enamels comprises the steps:
(1) on smart base of pottery or low temperature biscuit, dips in and apply the skeleton diagram that a kind of material water-proof material that can stop the base substrate sucking forms required pattern;
(2) at the smart base of described pottery or low temperature biscuit outside surface last layer coloured glaze as prepared as described in the claim 4;
(3) throw off or after low temperature burns the material water-proof material of before having painted, form colourless in the position that scribbles material water-proof material originally or do not have the pattern contour figure of glaze, carrying out enamel glaze on no glaze pattern contour figure decorates, after product decoration is good, send kiln high temperature to burn till product, firing temperature is controlled at 1200 ℃～1300 ℃, execute one deck coloured glaze basis glaze in the above through after the assay was approved through the product that burns till, sending kiln to carry out glaze firing, the temperature of glaze firing is controlled at 1080 ℃～1180 ℃, can be fired into enamel faience under the glaze.
7. the technology of preparation colour enamels as claimed in claim 6, described material water-proof material are tearable glue, perhaps oils, perhaps paraffin, perhaps plastics, perhaps waterproofing agent.
CN200910238973.8A 2009-12-31 2009-12-31 Enamel glaze and preparation process thereof Active CN101786795B (en)

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