CN106316127A - Medium-temperature Jin Mei crystalline glaze and preparation method thereof - Google Patents
Medium-temperature Jin Mei crystalline glaze and preparation method thereof Download PDFInfo
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- CN106316127A CN106316127A CN201610675014.2A CN201610675014A CN106316127A CN 106316127 A CN106316127 A CN 106316127A CN 201610675014 A CN201610675014 A CN 201610675014A CN 106316127 A CN106316127 A CN 106316127A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
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Abstract
The invention discloses medium-temperature Jin Mei crystalline glaze and a preparation method thereof, and belongs to the technical field of ceramic glaze materials. The crystalline glaze is prepared from, by weight, 30-40 parts of potassium feldspar, 12-18 parts of quartz, 1-6 parts of calcite, 1-5 parts of calcinated zinc oxide, 1-4 parts of calcinated talc, 2-8 parts of frit, 30-38 parts of manganese carbonate and 0-10 parts of toner. The crystalline glaze is prepared mainly through the steps that manganese carbonate is supersaturated in the glaze material high-temperature melting process and crystallizes in the cooling process, and the Jin Mei crystallizne form is generated. The process is simple, and the calcinating system is easy to control; the cooling system has no special requirements, the glaze is suitable for large-scale production, stable in product property and high in heat stability, and the lead and cadmium dissolution degree, glaze surface hardness and other physical and chemical properties reach the national related household stoneware standards.
Description
Technical field
The present invention relates to ceramic glaze technical field, particularly relate to Wen Jinmei crystalline glaze and preparation method thereof in one.
Background technology
In the color glaze product that current 1250～1300 DEG C of middle temperature are burnt till, crystalline glaze class is numerous, crystallize with zinc crystallization, manganese,
Ferrum crystallization, titanium crystallization etc. are main, and also having part is ferrimanganic titanium mixed crystallization.The most popular most Products of Crystalline Glaze is with big
Area intensive Products of Crystalline Glaze, it is usually required mainly for special burning kiln or calcining system, especially at crystallization formation stages, burns till control
System requires very strict, so main, based on display art product such as vases, household china product is more rare, main inadaptable big
Large-scale production, product quality ensures to require harshness.
Generally speaking, Products of Crystalline Glaze artistry is very strong, and appreciative value is fine, is worth the highest, is deeply appreciated by consumer.But
Products of Crystalline Glaze reproducibility is poor, i.e. poor stability, and technological requirement is complicated, and especially calcining system requires harshness, thin to glaze
Degree, glazed thickness requires strict, by even base substrate is formed and all requires.
Summary of the invention
In view of this, it is an object of the invention to propose Wen Jinmei crystalline glaze and preparation method thereof in one, so that middle temperature
Gold prunus mume (sieb.) sieb.et zucc. crystalline glaze Household stoneware product does not only have complete crystal, and its physicochemical property also meets international standards, and reproducibility is good,
Can stable mass production auxiliary products.
Based on Wen Jinmei crystalline glaze in the one that the above-mentioned purpose present invention provides, in terms of parts by weight, described middle Wen Jinmei
Crystalline glaze includes potassium feldspar 30～40 parts, 12～18 parts of quartz, calcite 1～6 parts, calcining zinc oxide 1～5 parts, calcination of talc 1
～4 parts, frit 2～8 parts, manganese carbonate 30～38 parts and toner 0～10 parts.
According to Wen Jinmei crystalline glaze in the one of the present invention, described potassium feldspar is powder head, canescence；With weight fraction
Meter, dioxide-containing silica >=98% in described quartz, water content is 1～8%.
According to Wen Jinmei crystalline glaze in the one of the present invention, in terms of weight fraction, calcium oxide content in described calcite >=
53%；Described calcining zinc oxide is powder, slightly yellow tune.
According to Wen Jinmei crystalline glaze in the one of the present invention, in terms of weight fraction, content of magnesia in described calcination of talc
>=34.5%.
According to Wen Jinmei crystalline glaze in the one of the present invention, described frit is common boron, calcium, zinc frit, and block is granular, white
Band Blues.
According to Wen Jinmei crystalline glaze in the one of the present invention, described toner is coloring oxide.
The preparation method of the middle Wen Jinmei crystalline glaze of a kind of present invention, comprises the steps:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, ballstone are ground together with water, prepares glaze slip standby；
B. glazing: Shi porcelain mold glazing, glazed thickness are controlled at 0.10～0.25 millimeter by glaze slip standby in step a；
C. fire: by the glazing Shi porcelain mold of gained in step b at a temperature of 50～60 DEG C be dried 1.5～2.5 hours, so
Laggard klining becomes；Firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 3～4 DEG C/min, with 5～6
DEG C/min is warming up to 760 DEG C, is warming up to 1170 DEG C with 8～10 DEG C/min, is warming up to 1250～1270 DEG C with 1～3 DEG C/min, protect
Temperature 20～30min, is cooled to 700 DEG C with 24～26 DEG C/min, is cooled to 530 DEG C with 7～8 DEG C/min, drops with 1～2 DEG C/min
Temperature, to 450 DEG C, is cooled to 38 DEG C with 8～10 DEG C/min；
Or, firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 4～5 DEG C/min, with 19～
20 DEG C/min is warming up to 950 DEG C, is warming up to 980 DEG C with 1～2 DEG C/min, is warming up to 1150 DEG C with 7～8 DEG C/min, with 1～2
DEG C/min is warming up to 1280～1300 DEG C, be incubated 20～30min, be cooled to 750 DEG C with 23～25 DEG C/min, with 9～10 DEG C/
Min is cooled to 530 DEG C, is cooled to 450 DEG C with 1～2 DEG C/min, is cooled to 38 DEG C with 8～10 DEG C/min.
The manufacture method of a kind of middle Wen Jinmei crystalline glaze according to the present invention, in terms of parts by weight, described raw material, ballstone,
The ratio of water is 1:(2～2.5): (0.6～0.8).
The manufacture method of a kind of middle Wen Jinmei crystalline glaze according to the present invention, the concentration of described glaze slip is 30～60 Baumes
Degree.
The manufacture method of a kind of middle Wen Jinmei crystalline glaze according to the present invention, described glaze slip fineness controls to sieve at 250 mesh sieves
Surplus is 0.01～0.03%.
The potassium length used in Wen Jinmei crystalline glaze formula in the present invention originates from Hubei Province's Pingjiang County；Quartz originates from Liling, in
Fine sand shape；Calcite originates from Guangxi；Calcining zinc oxide originates from zhuzhou,hunan；Manganese carbonate is that industrial chemical is pure, originates from Shanghai；Forge
Burn Talcum and originate from Guangxi；Frit originates from Liling, commercially available；Toner is coloring oxide, and other colorants are easily hidden by manganese color development
And do not develop the color.
In the present invention, Wen Jinmei crystalline glaze formula combination is of entirely key, indispensable, so being adapted in process
Extensively, i.e. can burn till by middle temperature oxidizing flame, again can middle temperature firing with reductive flame.With potassium feldspar, quartz as backbone in formula, composition
Glaze slip matrix；Frit, calcite, calcining zinc oxide, calcination of talc are flux, ensure that glaze firing temperature reaches or remains institute
The firing temperature needed and crystallization temperature.Crystallization is had in amount ranges described herein by calcining zinc oxide and calcination of talc
Facilitation, exceed this amount ranges to crystallization counterproductive, i.e. be unfavorable for crystallization formation or crystallization continue to grow up.Carbonic acid
Manganese decomposites manganese dioxide in pyroprocess, and the manganese dioxide decomposited is than individually adding manganese dioxide activity more preferably purity more
High；It is molten state that glaze formula always forms when high temperature, and the manganese dioxide of excess is dissolved in glaze liquation in high temperature, is lowering the temperature
Cheng Zhong, oversaturated manganese dioxide separates out crystal in glaze layer condensation process, forms gold prunus mume (sieb.) sieb.et zucc. crystalline glaze.
In the present invention in Wen Jinmei crystalline glaze manufacture method, time prepared by step a glaze slip, during grinding add ballstone have greatly,
Middle or small three kinds, big ballstone a diameter of 25-35 millimeter, middle ballstone a diameter of 15-25 millimeter, little ballstone a diameter of 8-15 millimeter, greatly
Ballstone, middle ballstone, the ratio of little ballstone are 2:5:3.When step b is to Shi porcelain mold glazing, first glaze slip is crossed 120 targets accurate
Sieve, is possible to prevent in slurry goes out ball process to introduce impurity, such as little broken granules such as the ballstone in ball mill and ball milling liners, and
The impurity particle etc. that ball mill discharging mouth brings.According to different types, add water regulation concentration of glaze slip, add electrolyte regulation
Ensure that glaze slip thixotropy reaches optimum, it is ensured that after glazing, the glazed thickness of base substrate is between 0.1～0.25 millimeter；Glaze slip touches
When degeneration reaches optimum, glaze is easy to use, and does not produce such as glaze planar defects such as excess glaze, glaze muscle.Glazed thickness exceedes this
Poor effect during 0.1～0.25 millimeter of scope described in invention, if glazed thickness is less than 0.1 millimeter, occurs almost without crystallization,
If glazed thickness is more than 0.25 millimeter, excessively, glaze seems coarse can't bear because being full crystallization in crystallization.Step c burns till employing oxygen
During activating QI atmosphere, when being warming up to 180 DEG C by 80 DEG C primarily to water vapor discharging, by 530 DEG C be cooled to 450 DEG C use 1～2 DEG C/
Min is carried out, and is primarily due to quartz crystal transformation body change and carries out at this temperature stage, so wanting slow cooling in order to avoid bursting；Burn till
When using reducing atmosphere, also it is primarily to water vapor discharging when being warming up to 180 DEG C by 80 DEG C, is warming up to 1150 DEG C by 950 DEG C
Mainly complete the oxidizing atmosphere transformation to reducing atmosphere, by 530 DEG C be cooled to 450 DEG C use 1～2 DEG C/min carry out former
Cause, is because quartz crystal transformation change in volume equally and carries out at this temperature stage, so wanting slow cooling in order to avoid bursting.
From above, it can be seen that advantages of the present invention and providing the benefit that:
(1) the middle Wen Jinmei Products of Crystalline Glaze of the present invention belongs to manganese crystalline glaze category, and temperature adaptation width both can be the highest
Firing temperature reaches in the firing period of 1250～1270 DEG C, and oxidizing flame atmosphere is burnt till；1280 can be reached again at maximum sintering temperature
～in the firing period of 1300 DEG C, reducing flame atmosphere is burnt till, sintering curve requires loose, it is not necessary to special crystallization holding stage,
Existing common middle temperature roller kilns can be made full use of produce, be suitable for large-scale production.
(2) in the present invention crystallization flower effect of Wen Jinmei crystalline glaze be outer ring be the reddest haloing of yellow, be yellow slightly within,
Middle is golden speckle, has the sense of slight projection, and hands Chu feels, and golden sense by force, as gold Flos Mume, therefore is named Jin Mei for whole
Crystalline glaze.Ingot diameter is between 0.5 millimeter to 3.5 millimeter, more dense at glaze thickness, and thin place is dilute.Background glaze is metal light
Pool glaze, sub-light, quality is like rustless steel.
(3) in the present invention, Wen Jinmei crystalline glaze is mainly manganese carbonate supersaturation during glaze high-temperature fusion, in cooling
During occur that crystallization produces gold prunus mume (sieb.) sieb.et zucc. crystalline, technique is simple, and calcining system is easy to control.
(4) product cooling system of the present invention does not has particular/special requirement, is suitable for large-scale production, and product property is stable, and heat is steady
The physicochemical properties such as qualitative good, Lead and cadmium degree and hardness of glaze surface reach the relevant Household stoneware standard of country.
Accompanying drawing explanation
Fig. 1 is the middle temperature oxidizing flame sintering curve of the embodiment of the present invention；
Fig. 2 is the middle temperature firing with reductive flame curve of the embodiment of the present invention.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.
Embodiment 1
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 30 parts, 12 parts of quartz, 6 parts of calcite, calcining
Zinc oxide 5 parts, calcination of talc 4 parts, frit 2 parts, manganese carbonate 38 parts, without any toner.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.01%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2:0.7, big ballstone, middle ballstone, little ballstone in high alumina ballstone
Ratio be 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 30 Baume degrees, adds
Enter 0.08% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness control
At 0.10 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 2.5 hours at a temperature of 50 DEG C, then enters middle temperature
Oxidizing flame roller kilns burn till, and firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 4 DEG C/min, with 5
DEG C/min is warming up to 760 DEG C, is warming up to 1170 DEG C with 10 DEG C/min, is warming up to 1260 DEG C with 3 DEG C/min, is incubated 30min, with 24
DEG C/min is cooled to 700 DEG C, it is cooled to 530 DEG C with 8 DEG C/min, is cooled to 450 DEG C with 1 DEG C/min, be cooled to 10 DEG C/min
38 DEG C, fire.Specifically, seeing middle temperature oxidizing flame sintering curve Fig. 1, wherein maximum sintering temperature is up to 1250～1270
℃。
Embodiment 2
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 40 parts, 18 parts of quartz, 1 part of calcite, calcining
Zinc oxide 1 part, calcination of talc 1 part, frit 8 parts, manganese carbonate 30 parts, toner 8 parts, toner is cobalt oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.03%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2.5:0.6, big ballstone, middle ballstone, bead in high alumina ballstone
The ratio of stone is 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 60 Baume degrees, adds
Enter 0.1% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness controls
0.25 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 1.5 hours at a temperature of 60 DEG C, then enters shuttle-type
Klining becomes, and firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 5 DEG C/min, heats up with 20 DEG C/min
To 950 DEG C, it is warming up to 980 DEG C with 1 DEG C/min, is warming up to 1150 DEG C with 8 DEG C/min, be warming up to 1290 DEG C with 2 DEG C/min, insulation
20min, is cooled to 750 DEG C with 23 DEG C/min, is cooled to 530 DEG C with 10 DEG C/min, is cooled to 450 DEG C with 1 DEG C/min, with 10
DEG C/min is cooled to 38 DEG C, fire.Specifically, see middle temperature firing with reductive flame curve chart 2, wherein maximum sintering temperature up to
1280～1300 DEG C.
Embodiment 3
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 35 parts, 15 parts of quartz, 4 parts of calcite, calcining
Zinc oxide 3 parts, calcination of talc 2 parts, frit 5 parts, manganese carbonate 34 parts, toner 8 parts, toner is cobalt oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.02%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2.3:0.8, big ballstone, middle ballstone, bead in high alumina ballstone
The ratio of stone is 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 45 Baume degrees, adds
Enter 0.09% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness control
At 0.18 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 2 hours at a temperature of 55 DEG C, then enters middle temperature oxygen
Change flame roller kilns burn till, firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 3 DEG C/min, with 6 DEG C/
Min is warming up to 760 DEG C, is warming up to 1170 DEG C with 8 DEG C/min, is warming up to 1270 DEG C with 3 DEG C/min, be incubated 20min, with 26 DEG C/
Min is cooled to 700 DEG C, is cooled to 530 DEG C with 7 DEG C/min, is cooled to 450 DEG C with 2 DEG C/min, is cooled to 38 DEG C with 8 DEG C/min,
Fire.Specifically, seeing middle temperature oxidizing flame sintering curve Fig. 1, wherein maximum sintering temperature is up to 1250～1270 DEG C.
Embodiment 4
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 35 parts, 15 parts of quartz, 4 parts of calcite, calcining
Zinc oxide 3 parts, calcination of talc 2 parts, frit 5 parts, manganese carbonate 34 parts, toner 10 parts, toner is cobalt oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.03%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2.5:0.6, big ballstone, middle ballstone, bead in high alumina ballstone
The ratio of stone is 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 60 Baume degrees, adds
Enter 0.1% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness controls
0.25 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 1.5 hours at a temperature of 60 DEG C, then enters middle temperature
Reducing flame roller kilns burn till, and firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 4 DEG C/min, with 19
DEG C/min is warming up to 950 DEG C, it is warming up to 980 DEG C with 2 DEG C/min, is warming up to 1150 DEG C with 7 DEG C/min, be warming up to 1 DEG C/min
1280 DEG C, it is incubated 30min, is cooled to 750 DEG C with 25 DEG C/min, is cooled to 530 DEG C with 9 DEG C/min, be cooled to 2 DEG C/min
450 DEG C, it is cooled to 38 DEG C with 8 DEG C/min, has fired.Specifically, middle temperature firing with reductive flame curve chart 2, hyperpyrexia are seen
Become temperature up to 1280～1300 DEG C.
Embodiment 5
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 32 parts, 13 parts of quartz, 5 parts of calcite, calcining
Zinc oxide 4 parts, calcination of talc 3 parts, frit 3 parts, manganese carbonate 36 parts, toner 2 parts, toner is nickel oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.01%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2:0.7, big ballstone, middle ballstone, little ballstone in high alumina ballstone
Ratio be 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 30 Baume degrees, adds
Enter 0.08% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness control
At 0.10 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 2.5 hours at a temperature of 50 DEG C, then enters middle temperature
Oxidizing flame roller kilns burn till, and firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 3 DEG C/min, with 6
DEG C/min is warming up to 760 DEG C, is warming up to 1170 DEG C with 8 DEG C/min, is warming up to 1250 DEG C with 1 DEG C/min, is incubated 30min, with 26
DEG C/min is cooled to 700 DEG C, it is cooled to 530 DEG C with 7 DEG C/min, is cooled to 450 DEG C with 2 DEG C/min, be cooled to 38 with 8 DEG C/min
DEG C, fire.Specifically, seeing middle temperature oxidizing flame sintering curve Fig. 1, wherein maximum sintering temperature is up to 1250～1270 DEG C.
Embodiment 6
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 38 parts, 16 parts of quartz, 2 parts of calcite, calcining
Zinc oxide 2 parts, calcination of talc 2 parts, frit 6 parts, manganese carbonate 32 parts, toner 4 parts, toner is chromium oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.03%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2:0.7, big ballstone, middle ballstone, little ballstone in high alumina ballstone
Ratio be 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 60 Baume degrees, adds
Enter 0.1% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness controls
0.25 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 1.5 hours at a temperature of 60 DEG C, then enters middle temperature
Reducing flame roller kilns burn till, and firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 5 DEG C/min, with 20
DEG C/min is warming up to 950 DEG C, it is warming up to 980 DEG C with 1 DEG C/min, is warming up to 1150 DEG C with 8 DEG C/min, be warming up to 2 DEG C/min
1300 DEG C, it is incubated 20min, is cooled to 750 DEG C with 23 DEG C/min, is cooled to 530 DEG C with 10 DEG C/min, be cooled to 1 DEG C/min
450 DEG C, it is cooled to 38 DEG C with 10 DEG C/min, has fired.Specifically, middle temperature firing with reductive flame curve chart 2, hyperpyrexia are seen
Become temperature up to 1280～1300 DEG C.
Comparative example 1
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 45 parts, 20 parts of quartz, 0.5 part of calcite, forges
Burning zinc oxide 6 parts, calcination of talc 0.5 part, frit 1 part, manganese carbonate 28 parts, toner 8 parts, toner is cobalt oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.02%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2.3:0.8, big ballstone, middle ballstone, bead in high alumina ballstone
The ratio of stone is 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 45 Baume degrees, adds
Enter 0.09% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness control
At 0.15 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 2 hours at a temperature of 55 DEG C, then enters middle temperature oxygen
Change flame roller kilns burn till, firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 4 DEG C/min, with 5 DEG C/
Min is warming up to 760 DEG C, is warming up to 1170 DEG C with 10 DEG C/min, is warming up to 1260 DEG C with 3 DEG C/min, be incubated 30min, with 24 DEG C/
Min is cooled to 700 DEG C, is cooled to 530 DEG C with 8 DEG C/min, is cooled to 450 DEG C with 1 DEG C/min, is cooled to 38 with 10 DEG C/min
DEG C, fire.Specifically, seeing middle temperature oxidizing flame sintering curve Fig. 1, wherein maximum sintering temperature is up to 1250～1270 DEG C.
Comparative example 2
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 25 parts, 10 parts of quartz, 7 parts of calcite, calcining
Zinc oxide 0.5 part, calcination of talc 5 parts, frit 10 parts, manganese carbonate 40 parts, toner 4 parts, toner is chromium oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.03%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2:0.7, big ballstone, middle ballstone, little ballstone in high alumina ballstone
Ratio be 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 60 Baume degrees, adds
Enter 0.1% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness controls
0.25 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 1.5 hours at a temperature of 60 DEG C, then enters middle temperature
Reducing flame roller kilns burn till, and firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 5 DEG C/min, with 20
DEG C/min is warming up to 950 DEG C, it is warming up to 980 DEG C with 2 DEG C/min, is warming up to 1150 DEG C with 8 DEG C/min, be warming up to 2 DEG C/min
1300 DEG C, it is incubated 20min, is cooled to 750 DEG C with 23 DEG C/min, is cooled to 530 DEG C with 10 DEG C/min, be cooled to 1 DEG C/min
450 DEG C, it is cooled to 38 DEG C with 10 DEG C/min, has fired.Specifically, middle temperature firing with reductive flame curve chart 2, hyperpyrexia are seen
Become temperature up to 1280～1300 DEG C.
Comparative example 3
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 40 parts, 18 parts of quartz, 1 part of calcite, calcining
Zinc oxide 1 part, calcination of talc 1 part, frit 8 parts, manganese carbonate 30 parts, toner 8 parts, toner is cobalt oxide.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.03%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2.5:0.6, big ballstone, middle ballstone, bead in high alumina ballstone
The ratio of stone is 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 60 Baume degrees, adds
Enter 0.1% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness controls
0.30 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 1.5 hours at a temperature of 60 DEG C, then enters shuttle-type
Klining becomes, and firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 4 DEG C/min, heats up with 19 DEG C/min
To 950 DEG C, it is warming up to 980 DEG C with 1 DEG C/min, is warming up to 1150 DEG C with 7 DEG C/min, be warming up to 1280 DEG C with 1 DEG C/min, insulation
30min, is cooled to 750 DEG C with 25 DEG C/min, is cooled to 530 DEG C with 9 DEG C/min, is cooled to 450 DEG C with 2 DEG C/min, with 8 DEG C/
Min is cooled to 38 DEG C, has fired.Specifically, see middle temperature firing with reductive flame curve chart 2, wherein maximum sintering temperature up to
1280～1300 DEG C.
Comparative example 4
Wen Jinmei crystalline glaze in one, its formula composition includes: potassium feldspar 30 parts, 12 parts of quartz, 6 parts of calcite, calcining
Zinc oxide 5 parts, calcination of talc 4 parts, frit 2 parts, manganese carbonate 38 parts, without any toner.
The manufacture method of middle Wen Jinmei crystalline glaze is as follows:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1,
Raw material, high alumina ballstone are put in ball mill together with water and be ground, until 250 mesh standard sieve screen over-sizes are 0.01%, system
Obtain glaze slip standby；Wherein raw material, high alumina ballstone, the ratio of water are 1:2:0.7, big ballstone, middle ballstone, little ballstone in high alumina ballstone
Ratio be 2:5:3.
B. glazing: glaze slip standby in step a is crossed 120 mesh standard sieves, addition water regulation concentration of glaze slip, to 30 Baume degrees, adds
Enter 0.08% sodium tripolyphosphate regulation glaze slip thixotropy to optimum state, then to Shi porcelain mold glazing, glazed thickness control
At 0.05 millimeter；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 2.5 hours at a temperature of 50 DEG C, then enters middle temperature
Oxidizing flame roller kilns burn till, and firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 3 DEG C/min, with 6
DEG C/min is warming up to 760 DEG C, is warming up to 1170 DEG C with 8 DEG C/min, is warming up to 1270 DEG C with 3 DEG C/min, is incubated 20min, with 26
DEG C/min is cooled to 700 DEG C, it is cooled to 530 DEG C with 7 DEG C/min, is cooled to 450 DEG C with 2 DEG C/min, be cooled to 38 with 8 DEG C/min
DEG C, fire.Specifically, seeing middle temperature oxidizing flame sintering curve Fig. 1, wherein maximum sintering temperature is up to 1250～1270 DEG C.
Detection embodiment
The Shi porcelain mold with middle Wen Jinmei crystalline glaze embodiment 1 to 6 and comparative example 1 to 4 prepared, carries out thermally-stabilised
Property, the detection of lead-indium alloy, presentation quality, hardness of glaze surface, and carry out dish-washing machine test.
Heat stability testing method: detect with reference to BSEN1183:1997, Method B.
Lead and cadmium weight testing method: detect with reference to ISO6486-1:1999.
Hardness of glaze surface detection method: delineate at glaze with knife and fork, checks that glaze delineates vestige.
Dish-washing machine equivalence method of testing: after aqueous alkali 100 DEG C soaks 4 hours, observes glaze change.
Testing result is shown in Table 1.
Table 1.
The frit and the colorant that use in the present invention are all strict with, the containing for only denier or do not contain lead cadmium of employing
Frit and colorant, thus ensure that in goods, lead cadmium content is extremely low；By using each component to ensure that glaze in glaze composition of raw materials
Thermal coefficient of expansion mates with base substrate thermal coefficient of expansion, it is ensured that the overall good heat stability of porcelain body；Glaze composition of raw materials is adopted
Potassium feldspar ensure that under identical cooling-down effect, glaze can have bigger hardness, and glaze has golden prunus mume (sieb.) sieb.et zucc. crystallization, knot
Brilliant hardness is very big, further increases hardness of glaze surface.
Those of ordinary skill in the field are it is understood that the discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, and there is the different aspect of the present invention as above
Other change of many, in order to simple and clear they do not provide in details.Therefore, all within the spirit and principles in the present invention,
Any omission of being made, amendment, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. Wen Jinmei crystalline glaze in a kind, it is characterised in that in terms of parts by weight, described middle Wen Jinmei crystalline glaze includes potassium feldspar
30～40 parts, 12～18 parts of quartz, calcite 1～6 parts, calcining zinc oxide 1～5 parts, calcination of talc 1～4 parts, frit 2～8
Part, manganese carbonate 30～38 parts and toner 0～10 parts.
Wen Jinmei crystalline glaze in one the most according to claim 1, it is characterised in that described potassium feldspar is powder head, ash
White；In terms of weight fraction, dioxide-containing silica >=98% in described quartz, water content is 1～8%.
Wen Jinmei crystalline glaze in one the most according to claim 1, it is characterised in that in terms of weight fraction, described side solves
Calcium oxide content >=53% in stone；Described calcining zinc oxide is powder, slightly yellow tune.
Wen Jinmei crystalline glaze in one the most according to claim 1, it is characterised in that in terms of weight fraction, described calcining
Content of magnesia >=34.5% in Talcum.
Wen Jinmei crystalline glaze in one the most according to claim 1, it is characterised in that described frit is common boron, calcium, zinc
Frit, block is granular, white band Blues.
Wen Jinmei crystalline glaze in one the most according to claim 1, it is characterised in that described toner is coloring oxide.
7. the preparation method of a middle Wen Jinmei crystalline glaze as claimed in claim 1, it is characterised in that comprise the steps:
A. prepared by glaze slip: in terms of mass fraction, weighs middle Wen Jinmei crystalline glaze formula material as claimed in claim 1, by former
Material, ballstone grind together with water, prepare glaze slip standby；
B. glazing: Shi porcelain mold glazing, glazed thickness are controlled at 0.10～0.25 millimeter by glaze slip standby in step a；
C. fire: the glazing Shi porcelain mold of gained in step b is dried 1.5～2.5 hours at a temperature of 50～60 DEG C, then enters
Klining becomes；Firing atmosphere is oxidizing atmosphere, and 80 DEG C is initial temperature, is warming up to 245 DEG C with 3～4 DEG C/min, with 5～6 DEG C/min
Be warming up to 760 DEG C, be warming up to 1170 DEG C with 8～10 DEG C/min, be warming up to 1250～1270 DEG C with 1～3 DEG C/min, insulation 20～
30min, is cooled to 700 DEG C with 24～26 DEG C/min, is cooled to 530 DEG C with 7～8 DEG C/min, is cooled to 450 with 1～2 DEG C/min
DEG C, it is cooled to 38 DEG C with 8～10 DEG C/min；
Or, firing atmosphere is reducing atmosphere, and 80 DEG C is initial temperature, is warming up to 500 DEG C with 4～5 DEG C/min, with 19～20
DEG C/min is warming up to 950 DEG C, be warming up to 980 DEG C with 1～2 DEG C/min, be warming up to 1150 DEG C with 7～8 DEG C/min, with 1～2 DEG C/
Min is warming up to 1280～1300 DEG C, is incubated 20～30min, is cooled to 750 DEG C with 23～25 DEG C/min, drops with 9～10 DEG C/min
Temperature, to 530 DEG C, is cooled to 450 DEG C with 1～2 DEG C/min, is cooled to 38 DEG C with 8～10 DEG C/min.
The manufacture method of a kind of middle Wen Jinmei crystalline glaze the most according to claim 7, it is characterised in that with parts by weight
Meter, described raw material, ballstone, the ratio of water are 1:(2～2.5): (0.6～0.8).
The manufacture method of a kind of middle Wen Jinmei crystalline glaze the most according to claim 7, it is characterised in that described glaze slip dense
Degree is 30～60 Baume degrees.
The manufacture method of a kind of middle Wen Jinmei crystalline glaze the most according to claim 7, it is characterised in that described glaze slip is thin
Degree controls at 250 mesh sieve screen over-sizes to be 0.01～0.03%.
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| CN111410425A (en) * | 2020-03-31 | 2020-07-14 | 景德镇市乐陶陶瓷原料有限公司 | Medium-temperature bright red glaze and preparation method thereof |
| CN111718122A (en) * | 2019-03-21 | 2020-09-29 | 梅州市林海陶瓷有限公司 | Glaze formula of novel crystal glaze ceramic product |
| CN112408797A (en) * | 2020-12-04 | 2021-02-26 | 湖南华联瓷业股份有限公司 | Crystalline glaze and preparation method thereof |
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