CN111233324A - Electric porcelain ash glaze material, electric porcelain ash glaze and preparation thereof - Google Patents
Electric porcelain ash glaze material, electric porcelain ash glaze and preparation thereof Download PDFInfo
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- CN111233324A CN111233324A CN201811434824.4A CN201811434824A CN111233324A CN 111233324 A CN111233324 A CN 111233324A CN 201811434824 A CN201811434824 A CN 201811434824A CN 111233324 A CN111233324 A CN 111233324A
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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
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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 an electric porcelain ash glaze material, an electric porcelain ash glaze and preparation thereof. The electric porcelain ash glaze material comprises the following components in percentage by mass: 25% -27% of quartz; 36 to 39 percent of feldspar; talc powder: 8% -10%; 6-8% of limestone; 2% -4% of alumina; 2% -4% of Yunyan powder; 5% -7% of zirconium silicate; 2% -4% of lithionite; 1.5 to 3 percent of barium carbonate; 0.2 to 0.4 percent of pigment; cobalt oxide is less than 0.2%; less than 0.5% of dispersant A15; hydroxymethyl cellulose (CMC) is less than 1%. The invention controls the water content of the glaze slip to be 34-36%, the viscosity to be 20-30 Pa.s, and the granularity to be less than 10 mu m, the percentage of the glaze slip to be (73-75)%; solves the technical problems of glaze surface pinhole, glaze shrinkage and glaze high-temperature spreading.
Description
Technical Field
The invention relates to the technical field of electroceramics. More particularly, relates to an electric porcelain ash glaze material, an electric porcelain ash glaze and preparation thereof.
Background
The rapid development of Chinese economy leads users to have higher and higher quality requirements and expectations for products, so that the appearance quality of products produced by electric porcelain manufacturers cannot meet the requirements of the users, the appearance quality of the electric porcelain products is improved, the product percent of pass is increased, and the loss is reduced. Meeting the requirements of users and occupying high-end markets become the first thing that manufacturers rely on survival and development.
Because the electric porcelain is applied to the electric power industry and needs to be used under special conditions, the electric porcelain has higher requirements on mechanical properties, electrical properties, pollution resistance, cold and hot stability and the like. The surface of the electric porcelain is provided with a layer of electric porcelain glaze, which is usually gray glaze or brown glaze. Besides the decoration function, the glaze for electric porcelain has great influence on the mechanical property, pollution resistance and cold and hot stability of the electric porcelain.
However, the existing gray glaze production has the following defects:
firstly, the control of water content, viscosity and granularity is not matched when the glaze slurry is ground, and atomization is not uniform when glazing, so that glaze particles are not uniform in size.
Secondly, the thickness of the glaze layer is not uniform during glazing, so that the surface of the porcelain piece after the kiln is yellowed or glaze shrinkage is caused.
Thirdly, when the firing temperature is lowered or the time for oxygen permeation is shortened, the glaze cannot be fully melted, and overglaze, orange glaze and pinholes are generated.
Chinese patent 200810232683.8 discloses a raw material ratio of gray blue glaze and a firing method thereof, wherein the raw material ratio of the gray blue glaze is prepared from the following components in percentage by weight: quartz: 30% -35%; feldspar: 32% -38%; talc: 8-11%; clay: 2% -5%; limestone: 7.5% -9%; alumina: 3% -5%; zirconium silicate: 7.5% -9%; manganese oxide: 0.01 to 0.05 percent; iron oxide: 0.1 to 0.4 percent; chromium oxide: 0.01 to 0.05 percent; cobalt oxide: 0 to 0.3 percent; dispersing agent: 0 to 1 percent; sodium carboxymethylcellulose: 0 to 1 percent. It has the following problems: the melting point of quartz and zirconium silicate in the raw materials is high, and the melting temperature of the glaze is high at high temperature. When the fire-stopping temperature of the kiln is reduced, namely the time from melting to fire-stopping of the glaze is correspondingly shortened, the glaze cannot be fully spread, the defects of shrinkage, stacking, flowing glaze or protrusion and the like are formed, and the quality of the glaze is reduced.
The glaze slip for glaze spraying in the Chinese patent 200810232683.8 has the following water content: (32-34)%, viscosity of 30s-40s, granularity of less than 10um, and ratio of (80-83)%. Spraying glaze twice, wherein the thickness of a glaze layer is as follows: 0.6mm-0.9 mm. It has the following problems: firstly, glaze slip has low water content, high viscosity, poor fluidity, poor atomization in glaze spraying process and large particles; secondly, the glaze slip has fine particles and large glaze shrinkage degree at high temperature; thirdly, the glaze layer has insufficient thickness and uneven thickness, and the surface of the porcelain piece has yellowing phenomenon. The process comprises the following steps: in the sintering and oxygen permeation stage (1200-fire stopping temperature), enough air flow is required to be fed on the basis of weak reduction, and a certain gas flow is required to be ensured to prevent the temperature in the kiln from suddenly dropping, so that a certain amount of flow-off oxygen is contained in the kiln, the CO is required to be controlled below 1 percent, the oxygen is required to be controlled between 1 percent and 5 percent, and the process takes 4 to 5 hours. And a high-fire heat preservation stage, namely, preserving heat at a fire stopping temperature for 30 minutes to 1 hour, wherein the amount of air and fuel gas is controlled well in the high-fire heat preservation stage, and the content of oxygen is ensured to be about 5 percent. It has the following problems: under the influence of the low glass transition temperature of the raw material blank, when the firing fire-stopping temperature is reduced to 1190-1200 ℃, the oxygen permeation time is not needed, the high-temperature time is greatly reduced, and the glaze melting and spreading time is not enough.
Disclosure of Invention
In order to solve at least one technical problem, the invention provides an electric porcelain gray glaze material, an electric porcelain gray glaze and preparation thereof, aiming at solving the technical problems of glaze surface pinholes, glaze shrinkage and glaze high-temperature spreading.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an electric porcelain ash glaze material which comprises the following components in percentage by mass:
25% -27% of quartz; 36 to 39 percent of feldspar; talc powder: 8% -10%; 6-8% of limestone; 2% -4% of alumina; 2% -4% of Yunyan powder; 5% -7% of zirconium silicate; 2% -4% of lithionite; 1.5 to 3 percent of barium carbonate; 0.2 to 0.4 percent of pigment; cobalt oxide is less than 0.2%; less than 0.5% of dispersant A15; hydroxymethyl cellulose (CMC) less than 1%; wherein less than or equal to means greater than 0 and less than the corresponding mass percent.
Preferably wherein the pigment comprises manganese oxide, iron oxide and chromium oxide. The pigment is directly purchased commercially or prepared according to a conventional proportion, and the formula of the pigment per se is not particularly limited.
Compared with the formula of the gray blue glaze in patent 200810232683.8, namely a method for firing gray blue glaze, the formula of the gray blue glaze disclosed by the invention is added with talcum powder, so that the content of zirconium silicate is reduced, and through determination, the high-temperature melting temperature of the glaze is reduced from 1140 ℃ to 1100 ℃, so that the glaze can be fully melted at high temperature, and pits and vacancies on the surface of a light blank can be filled. When the fire-stopping temperature of the kiln is reduced, namely the time from melting to fire-stopping of the glaze is correspondingly shortened, the glaze can be fully spread at the moment, the defects of shrinkage glaze, stacked glaze, flowing glaze or protrusion and the like are avoided, and the glaze quality is ensured.
The invention provides a preparation method of the electric porcelain gray glaze, which comprises the following steps:
s1, respectively drying the components of the electric porcelain ash glaze material;
s2, adding all the components into a ball mill according to the proportion, adding water, controlling the mass percent of the water to be 33-35%, ball-milling for 12-14 hours, and carrying out ball milling to form glaze slurry;
s3, sieving and deironing the glaze slip obtained in the step S2; sealing and storing and aging after iron is checked to be qualified;
s4, measuring and adjusting the moisture of the glaze slurry to 34-36% before glaze spraying;
and S5, carrying out glaze spraying and sintering on the blank to obtain the electric porcelain ash glaze.
In S2, a ball mill is required to process the electric porcelain ash glaze material before ball milling. Before the first preparation of the ash glaze, the ball mill needs to be cleaned. In general, the ball mill needs to be cleaned three times: adding a proper amount of quartz powder for the first time, adding water for ball milling, pouring out ground materials after grinding for 1-2 hours, and then adding water for cleaning the ball mill. The second pass repeats the above operations. And in the third time, according to the formula requirement, adding base glaze (prepared by other raw materials except pigments), grinding for 12-15 hours, pouring out the ground materials, and then adding water to clean the ball mill. Before the second and later preparation of the gray glaze, the ball mill needs to be cleaned by adding water in advance, and then the weighed raw materials are added.
Preferably, the drying in S1 controls the moisture content of quartz, clay and feldspar within 2% by mass; the moisture content of other solid components is controlled within 1 percent by mass.
Preferably, the mass percentage content of the added water in the S2 is 34-36%.
Preferably, the ball milling time of the electroceramics ash glaze material in S2 is 12-14 hours.
Preferably, the screen used for the screening described in S3 is a 200 mesh stainless steel screen. The leakage is not allowed, and the damage is found and should be replaced in time; and sieving is generally carried out not less than twice.
Preferably, the iron removing tool used for removing iron in S3 is a strong magnet bar or an iron remover.
Preferably, the iron inspection qualification in the S3 requires that a 140-mesh/inch sieve is used, and the number of iron points is not more than 2.
Preferably, the step of sealing and staling in S3 includes:
storing the glaze slurry after iron checking is qualified in a jar, adding 1-2% of water by mass percent, and covering a jar cover for ageing; the aging time is not less than one week; during the period of staleness, the glaze slip needs to be stirred for not less than half an hour every day.
In the preparation method, the step of measuring and adjusting the moisture of the glaze slurry to 34-36% before spraying glaze in S3 specifically comprises the following steps:
the glaze slip time in the glaze pot is stirred for more than or equal to 1h before glaze spraying (every day or after glaze adding). The ambient temperature of the glazing room is more than or equal to 15 ℃, and the humidity is less than or equal to 55%. And determining whether the moisture meets the process requirements. If the content is lower than the standard, adding water, blending, stirring and measuring until the standard is reached.
And the measurement and control of the moisture and the viscosity before glaze spraying are carried out so as to match the moisture, the viscosity and the granularity, and the uniform atomization during glaze application is ensured, so that the uniform particle size of the glaze surface is ensured.
Wherein, the step of spraying glaze and sintering the blank to obtain the electric porcelain ash glaze in S4 specifically comprises the following steps:
glaze spraying: the present invention improves the glaze spraying method, firstly, the spray gun keeps the upper part or the lower part of the umbrella sprayed in one direction, then the spray gun changes the lower part or the upper part of the umbrella sprayed in the other direction, and the glaze spraying is generally in the tangential direction with the circumference of the section of the blank. And after the first spraying of the blank with the main body diameter larger than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out. And directly glazing the blank with the main body diameter less than 160mm for the second time after the first glaze spraying, and glazing for the second time totally. And (3) opening a hot air blower beside the spraying device to blow hot air while spraying the primary glaze and the secondary glaze. After each glaze spraying, the surface is dried by hot air.
The glazing should be carried out on hot blanks, for which purpose the blanks on each shelf should be preheated twice, alternately glazed, in order to maintain the temperature of the blank.
Soot blowing is required to be carried out on the blank before the glaze is sprayed for the first time and the second time. In order to prevent the bowl scraps generated during the lifting of the product, when the glaze is sprayed for the first time, the glaze is uniformly sprayed on the neck.
And (3) firing: the firing is mainly divided into a small fire heating stage, an oxidation stage, a middle fire heat preservation stage, a reduction stage, a high fire heat preservation stage and a cooling stage; the parameters of each stage are as follows:
a small fire heating stage: the temperature is raised from room temperature to 300 ℃, and the temperature raising speed in the stage is 10 ℃/h.
And (3) an oxidation stage: the temperature is increased from 300 ℃ to 950 ℃, and the temperature increasing speed is 25-45 ℃/h.
And (3) a medium-fire heat preservation stage: the temperature is raised from 950 ℃ to 960 ℃, and the oxygen content in the kiln is controlled to be 8-12% in the stage under the condition of ensuring the temperature to be stable.
And (3) reduction stage: raising the temperature from 970 ℃ to a high-preservation temperature, wherein the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2-4 hours, the temperature is 1200-fire stopping temperature, enough air is required to be introduced on the basis of weak reduction, a certain gas flow is ensured to prevent sudden temperature drop in the kiln, the free oxygen is ensured to be contained in the kiln, the volume content of CO in the kiln is controlled to be below 1%, and the volume content of the oxygen is controlled to be 1-3%.
And (3) high-fire heat preservation stage: keeping the temperature at the fire-stopping temperature for 0.2-0.5 h, and controlling the amount of air and fuel gas at this stage to ensure that the oxygen content is about 2.8-3.8%.
And (3) a cooling stage: namely the fire stopping temperature is-room temperature, and the whole process takes 30-45 hours; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
The invention improves the sintering process as follows:
the first stage is an oxidation stage: namely, the temperature is raised from 300 ℃ to 950 ℃, and the temperature raising speed is kept at 25-45 ℃/h and is gradually raised; the tail end temperature is reduced, the heating time can be reduced, and the energy consumption is reduced.
Secondly, a medium-fire heat preservation stage: namely, the temperature is increased from 950 ℃ to 960 ℃, and the content of oxygen in the kiln is controlled to be 8-12% in the stage under the condition of ensuring the temperature to be stable; by reducing the heat preservation temperature and increasing the oxygen content, the green body can be fully oxidized in the kiln, the generation of low-oxygen defects is avoided, and a foundation is laid for the subsequent glaze surface melting. If the oxidation is insufficient, the blank continues to react in the subsequent reduction stage, which can cause bubbles to be generated on the glaze surface.
Thirdly, a reduction stage: namely, the temperature is increased from 970 ℃ to a high-temperature preservation temperature, and the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; finally, the gray glazed porcelain piece with uniform color and smooth surface is formed.
The third aspect of the invention provides the electric porcelain ash glaze obtained by the preparation method. The electric porcelain ash glaze porcelain has stable quality and good appearance, can be produced in batch, and improves the satisfaction degree of users.
The invention solves the technical problem of glaze pinholes by adjusting the moisture and the viscosity of glaze slip. The water content of the glaze slip is adjusted to 34-36% from 32-34% in the prior art, and the viscosity is correspondingly adjusted to 20-30 Pa.s from 30-40 Pa.s. The technical problem of glaze shrinkage is solved by adjusting the granularity of the glaze slip. The materials are mixed according to the formula and put into a ball mill for ball milling, and the ball milling time before adjustment is from 18-20 hours to 12-14 hours in the prior art. Corresponding particle analysis: the granularity is less than 10 mu m, and the proportion is adjusted from (80-83)% to (73-75)%. By adjusting the formula of the glaze, the problem of high-temperature spread of the glaze is solved. The solution of the above technical problems can be achieved not only by simple adjustment but also by the improvement of the glaze spraying method and the firing process of the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
Firstly, preparing the following components in percentage by weight:
26% of quartz; 37% of feldspar; talc powder: 10 percent; 8% of limestone; 4% of aluminum oxide; 2% of Zuoyun powder; 6% of zirconium silicate; 2% of lithiumate; 3% of barium carbonate; 0.2 to 0.4 percent of pigment (manganese oxide, ferric oxide and chromium oxide); less than 0.2% of cobalt oxide, dispersant A15: less than 0.5%; CMC: less than 1%.
Then, respectively putting the solid raw material components into a drying room for drying, wherein the water content of quartz and feldspar is controlled within 2% by mass; the moisture content of other solid raw material components is controlled within 1 percent by mass.
Adding all the raw material components into a ball mill one by one according to the raw material ratio, adding water, wherein the mass percentage content of the water is required to be controlled at 34-36%, ball milling for 12-14 hours to form glaze slurry, and then sieving the glaze slurry with a 200-mesh sieve; and (3) removing iron from the sieved glaze slurry by using a magnet rod, then checking iron by using a 140-mesh/inch screen, and removing iron again if the number of iron points is more than 2 until the number of the iron points is not more than 2, and determining that the glaze slurry is qualified.
Storing the qualified glaze slip into a jar, adding 1-2% of water by mass percent, and covering a jar cover for ageing, wherein the ageing time of the glaze slip is not less than one week; and adjusting the water content of the aged glaze slip to 34-36% by mass.
And opening a spray gun to spray glaze on the green body, drying the surface of the green body by using a hot air blower after the first glaze spraying is finished, and then spraying glaze for the second time, wherein the hot air blowers blow hot air beside the two glaze spraying processes. There is no specific requirement for the rod diameter of the product. The glaze spraying method is improved in the patent: the spraying gun is firstly kept to spray the upper part or the lower part of the umbrella in one direction, then the spraying gun is changed to spray the lower part or the upper part of the umbrella in the other direction, and the glaze spraying is generally in the tangential direction with the circumference of the section of the product. And after the first spraying of the blank with the main body diameter larger than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out. And (4) directly glazing the blank with the main body diameter less than 160mm after the glazing is sprayed for the first time, and then glazing for the second time, wherein the glazing for the second time is carried out for the second time. And (3) opening a hot air blower beside the spraying device to blow hot air while spraying the primary glaze and the secondary glaze. After each glaze spraying, the surface is dried by hot air.
The glazing should be carried out on hot blanks, for which purpose the blanks on each shelf should be preheated twice, alternately glazed, in order to maintain the temperature of the blank.
Soot blowing is required to be carried out on the blank before the glaze is sprayed for the first time and the second time. In order to prevent the bowl scraps generated during the lifting of the product, when the glaze is sprayed for the first time, the glaze is uniformly sprayed on the neck.
Putting the blank body sprayed with the glaze slip into a drying room, and drying for 4-6 hours; then loading the materials from a drying room into a drawer kiln for sintering: in the existing firing process, firing is mainly divided into a small-fire heating stage, an oxidation stage, a middle-fire heat preservation stage, a reduction stage, a high-fire heat preservation stage and a cooling stage; the parameters of each stage are as follows:
a small fire heating stage: the temperature is increased from room temperature to 300 ℃, and the temperature increasing speed is 10 ℃/h in the stage.
And (3) an oxidation stage: namely, the temperature is increased from 300 ℃ to 950 ℃, and the temperature increasing speed is kept between 25 and 45 ℃/h.
And (3) a medium-fire heat preservation stage: namely, the temperature is increased from 950 ℃ to 960 ℃, and the content of oxygen in the kiln is controlled to be 8-12% in the stage under the condition of ensuring the temperature to be stable;
and (3) reduction stage: namely, the temperature is increased from 970 ℃ to a high-temperature preservation temperature, and the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2-4 hours, the temperature is from 1200 ℃ to the fire stopping temperature, enough air is required to be introduced on the basis of weak reduction, a certain gas flow is ensured to prevent sudden temperature drop in the kiln, the flowing-away oxygen is ensured to be contained in the kiln, the volume content of CO in the kiln is controlled to be below 1%, and the volume content of the oxygen is controlled to be 1-3%.
And (3) high-fire heat preservation stage: keeping the temperature at the fire-stopping temperature for 0.2-0.5 h, and controlling the amount of air and fuel gas at this stage to ensure that the oxygen content is about 2.8-3.8%.
And (3) a cooling stage: namely the fire stopping temperature is-room temperature, and the whole process takes 30-45 hours; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
Example 2
Firstly, preparing the following components in percentage by weight:
25% of quartz; 38% of feldspar; talc powder: 9 percent; 9% of limestone; 3% of aluminum oxide; 3% of Zuoyun powder; 6% of zirconium silicate; 3% of lithium limestone; 3% of barium carbonate; 0.2 to 0.4 percent of pigment (manganese oxide, ferric oxide and chromium oxide); less than 0.2% of cobalt oxide, dispersant A15: less than 0.5%; CMC: less than 1%.
Then, respectively putting the solid raw material components into a drying room for drying, wherein the water content of quartz and feldspar is controlled within 2% by mass; the moisture content of other solid raw material components is controlled within 1 percent by mass.
Adding all the raw material components into a ball mill one by one according to the raw material ratio, adding water, wherein the mass percentage content of the water is required to be controlled at 34-36%, ball milling for 12-14 hours to form glaze slurry, and then sieving the glaze slurry with a 200-mesh sieve; and (3) removing iron from the sieved glaze slurry by using a magnet rod, then checking iron by using a 140-mesh/inch screen, and removing iron again if the number of iron points is more than 2 until the number of the iron points is not more than 2, and determining that the glaze slurry is qualified.
And storing the qualified glaze slip into a cylinder, adding 1-2% of water by mass percent, and covering a cylinder cover for ageing, wherein the ageing time of the glaze slip is not less than one week. And adjusting the water content of the aged glaze slip to 34-36% by mass.
And opening a spray gun to spray glaze on the green body, drying the surface of the green body by using a hot air blower after the first glaze spraying is finished, and then spraying glaze for the second time, wherein the hot air blowers blow hot air beside the two glaze spraying processes. There is no specific requirement for the rod diameter of the product. The glaze spraying method is improved in the patent: the spraying gun is firstly kept to spray the upper part or the lower part of the umbrella in one direction, then the spraying gun is changed to spray the lower part or the upper part of the umbrella in the other direction, and the glaze spraying is generally in the tangential direction with the circumference of the section of the product. And after the first spraying of the blank with the main body diameter larger than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out. And (4) directly glazing the blank with the main body diameter less than 160mm after the glazing is sprayed for the first time, and then glazing for the second time, wherein the glazing for the second time is carried out for the second time. And (3) opening a hot air blower beside the spraying device to blow hot air while spraying the primary glaze and the secondary glaze. After each glaze spraying, the surface is dried by hot air.
The glazing should be carried out on hot blanks, for which purpose the blanks on each shelf should be preheated twice, alternately glazed, in order to maintain the temperature of the blank.
Soot blowing is required to be carried out on the blank before the glaze is sprayed for the first time and the second time. In order to prevent the bowl scraps generated during the lifting of the product, when the glaze is sprayed for the first time, the glaze is uniformly sprayed on the neck.
Putting the blank body sprayed with the glaze slip into a drying room, and drying for 4-6 hours; then loading the materials from a drying room into a drawer kiln for sintering: in the existing firing process, firing is mainly divided into a small-fire heating stage, an oxidation stage, a middle-fire heat preservation stage, a reduction stage, a high-fire heat preservation stage and a cooling stage; the parameters of each stage are as follows:
a small fire heating stage: the temperature is increased from room temperature to 300 ℃, and the temperature increasing speed is 10 ℃/h in the stage.
And (3) an oxidation stage: namely, the temperature is increased from 300 ℃ to 950 ℃, and the temperature increasing speed is kept at 25-45 ℃/h; and (3) a medium-fire heat preservation stage: namely, the temperature is increased from 950 ℃ to 960 ℃, and the oxygen content in the kiln is controlled to be 8-12% at the stage under the condition of ensuring the temperature to be stable.
And (3) reduction stage: namely, the temperature is increased from 970 ℃ to a high-temperature preservation temperature, and the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2-4 hours, the temperature is from 1200 ℃ to the fire stopping temperature, enough air is required to be introduced on the basis of weak reduction, a certain gas flow is ensured to prevent sudden temperature drop in the kiln, the flowing-away oxygen is ensured to be contained in the kiln, the volume content of CO in the kiln is controlled to be below 1%, and the volume content of the oxygen is controlled to be 1-3%.
And (3) high-fire heat preservation stage: keeping the temperature at the fire-stopping temperature for 0.2-0.5 h, and controlling the amount of air and fuel gas at this stage to ensure that the oxygen content is about 2.8-3.8%.
And (3) a cooling stage: namely the fire stopping temperature is-room temperature, and the whole process takes 30-45 hours; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
Example 3
Firstly, preparing the following components in percentage by weight:
27% of quartz; 36 percent of feldspar; talc powder: 10 percent; 7% of limestone; 2% of alumina; 4% of Zuoyun powder; 7% of zirconium silicate; 2% of lithiumate; 1.5 percent of barium carbonate; 0.2 to 0.4 percent of pigment (manganese oxide, ferric oxide and chromium oxide); less than 0.2% of cobalt oxide, dispersant A15: less than 0.5%; CMC: less than 1%.
Then, respectively putting the solid raw material components into a drying room for drying, wherein the water content of quartz and feldspar is controlled within 2% by mass; the moisture content of other solid raw material components is controlled within 1 percent by mass.
Adding all the raw material components into a ball mill one by one according to the raw material ratio, adding water, wherein the mass percentage content of the water is required to be controlled at 34-36%, ball milling for 12-14 hours to form glaze slurry, and then sieving the glaze slurry with a 200-mesh sieve; and (3) removing iron from the sieved glaze slurry by using a magnet rod, then checking iron by using a 140-mesh/inch screen, and removing iron again if the number of iron points is more than 2 until the number of the iron points is not more than 2, and determining that the glaze slurry is qualified.
Storing the qualified glaze slip into a jar, adding 1-2% of water by mass percent, and covering a jar cover for ageing, wherein the ageing time of the glaze slip is not less than one week; and adjusting the water content of the aged glaze slip to 34-36% by mass.
And opening a spray gun to spray glaze on the green body, drying the surface of the green body by using a hot air blower after the first glaze spraying is finished, and then spraying glaze for the second time, wherein the hot air blowers blow hot air beside the two glaze spraying processes. There is no specific requirement for the rod diameter of the product. The glaze spraying method is improved in the patent: the spraying gun is firstly kept to spray the upper part or the lower part of the umbrella in one direction, then the spraying gun is changed to spray the lower part or the upper part of the umbrella in the other direction, and the glaze spraying is generally in the tangential direction with the circumference of the section of the product. And after the first spraying of the blank with the main body diameter larger than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out. And (4) directly glazing the blank with the main body diameter less than 160mm after the glazing is sprayed for the first time, and then glazing for the second time, wherein the glazing for the second time is carried out for the second time. And (3) opening a hot air blower beside the spraying device to blow hot air while spraying the primary glaze and the secondary glaze. After each glaze spraying, the surface is dried by hot air.
The glazing should be carried out on hot blanks, for which purpose the blanks on each shelf should be preheated twice, alternately glazed, in order to maintain the temperature of the blank.
Soot blowing is required to be carried out on the blank before the glaze is sprayed for the first time and the second time. In order to prevent the bowl scraps generated during the lifting of the product, when the glaze is sprayed for the first time, the glaze is uniformly sprayed on the neck.
Putting the blank body sprayed with the glaze slip into a drying room, and drying for 4-6 hours; then loading the materials from a drying room into a drawer kiln for sintering: in the existing firing process, firing is mainly divided into a small-fire heating stage, an oxidation stage, a middle-fire heat preservation stage, a reduction stage, a high-fire heat preservation stage and a cooling stage; the parameters of each stage are as follows:
a small fire heating stage: the temperature is increased from room temperature to 300 ℃, and the temperature increasing speed is 10 ℃/h in the stage.
And (3) an oxidation stage: namely, the temperature is increased from 300 ℃ to 950 ℃, and the temperature increasing speed is kept at 25-45 ℃/h; and (3) a medium-fire heat preservation stage: namely, the temperature is increased from 950 ℃ to 960 ℃, and the oxygen content in the kiln is controlled to be 8-12% at the stage under the condition of ensuring the temperature to be stable.
And (3) reduction stage: namely, the temperature is increased from 970 ℃ to a high-temperature preservation temperature, and the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2-4 hours, the temperature is from 1200 ℃ to the fire stopping temperature, enough air is required to be introduced on the basis of weak reduction, a certain gas flow is ensured to prevent sudden temperature drop in the kiln, the flowing-away oxygen is ensured to be contained in the kiln, the volume content of CO in the kiln is controlled to be below 1%, and the volume content of the oxygen is controlled to be 1-3%.
And (3) high-fire heat preservation stage: keeping the temperature at the fire-stopping temperature for 0.2-0.5 h, and controlling the amount of air and fuel gas at this stage to ensure that the oxygen content is about 2.8-3.8%.
And (3) a cooling stage: namely the fire stopping temperature is-room temperature, and the whole process takes 30-45 hours; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
Example 4
Firstly, preparing the following components in percentage by weight:
25% of quartz; 39% of feldspar; talc powder: 8 percent; 8% of limestone; 2% of alumina; 2% of Zuoyun powder; 6% of zirconium silicate; 2% of lithiumate; 2% of barium carbonate; 0.2 to 0.4 percent of pigment (manganese oxide, ferric oxide and chromium oxide); less than 0.2% of cobalt oxide, dispersant A15: less than 0.5%; CMC: less than 1%.
Then, respectively putting the solid raw material components into a drying room for drying, wherein the water content of quartz and feldspar is controlled within 2% by mass; the moisture content of other solid raw material components is controlled within 1 percent by mass.
Adding all the raw material components into a ball mill one by one according to the raw material ratio, adding water, wherein the mass percentage content of the water is required to be controlled at 34-36%, ball milling for 12-14 hours to form glaze slurry, and then sieving the glaze slurry with a 200-mesh sieve; and (3) removing iron from the sieved glaze slurry by using a magnet rod, then checking iron by using a 140-mesh/inch screen, and removing iron again if the number of iron points is more than 2 until the number of the iron points is not more than 2, and determining that the glaze slurry is qualified.
Storing the qualified glaze slip into a jar, adding 1-2% of water by mass percent, and covering a jar cover for ageing, wherein the ageing time of the glaze slip is not less than one week; and adjusting the water content of the aged glaze slip to 34-36% by mass.
And opening a spray gun to spray glaze on the green body, drying the surface of the green body by using a hot air blower after the first glaze spraying is finished, and then spraying glaze for the second time, wherein the hot air blowers blow hot air beside the two glaze spraying processes. There is no specific requirement for the rod diameter of the product. The glaze spraying method is improved in the patent: the spraying gun is firstly kept to spray the upper part or the lower part of the umbrella in one direction, then the spraying gun is changed to spray the lower part or the upper part of the umbrella in the other direction, and the glaze spraying is generally in the tangential direction with the circumference of the section of the product. And after the first spraying of the blank with the main body diameter larger than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out. And (4) directly glazing the blank with the main body diameter less than 160mm after the glazing is sprayed for the first time, and then glazing for the second time, wherein the glazing for the second time is carried out for the second time. And (3) opening a hot air blower beside the spraying device to blow hot air while spraying the primary glaze and the secondary glaze. After each glaze spraying, the surface is dried by hot air.
The glazing should be carried out on hot blanks, for which purpose the blanks on each shelf should be preheated twice, alternately glazed, in order to maintain the temperature of the blank.
Soot blowing is required to be carried out on the blank before the glaze is sprayed for the first time and the second time. In order to prevent the bowl scraps generated during the lifting of the product, when the glaze is sprayed for the first time, the glaze is uniformly sprayed on the neck.
Putting the blank body sprayed with the glaze slip into a drying room, and drying for 4-6 hours; then loading the materials from a drying room into a drawer kiln for sintering: in the existing firing process, firing is mainly divided into a small-fire heating stage, an oxidation stage, a middle-fire heat preservation stage, a reduction stage, a high-fire heat preservation stage and a cooling stage; the parameters of each stage are as follows:
a small fire heating stage: the temperature is increased from room temperature to 300 ℃, and the temperature increasing speed is 10 ℃/h in the stage.
And (3) an oxidation stage: namely, the temperature is increased from 300 ℃ to 950 ℃, and the temperature increasing speed is kept at 25-45 ℃/h; and (3) a medium-fire heat preservation stage: namely, the temperature is increased from 950 ℃ to 960 ℃, and the oxygen content in the kiln is controlled to be 8-12% at the stage under the condition of ensuring the temperature to be stable.
And (3) reduction stage: namely, the temperature is increased from 970 ℃ to a high-temperature preservation temperature, and the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2-4 hours, the temperature is from 1200 ℃ to the fire stopping temperature, enough air is required to be introduced on the basis of weak reduction, a certain gas flow is ensured to prevent sudden temperature drop in the kiln, the flowing-away oxygen is ensured to be contained in the kiln, the volume content of CO in the kiln is controlled to be below 1%, and the volume content of the oxygen is controlled to be 1-3%.
And (3) high-fire heat preservation stage: keeping the temperature at the fire-stopping temperature for 0.2-0.5 h, and controlling the amount of air and fuel gas at this stage to ensure that the oxygen content is about 2.8-3.8%.
And (3) a cooling stage: namely the fire stopping temperature is-room temperature, and the whole process takes 30-45 hours; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
Example 5
Firstly, preparing the following components in percentage by weight:
26% of quartz; 37% of feldspar; talc powder: 10 percent; 8% of limestone; 2% of alumina; 3% of Zuoyun powder; 5% of zirconium silicate; 2% of lithiumate; 1.5 percent of barium carbonate; 0.2 to 0.4 percent of pigment (manganese oxide, ferric oxide and chromium oxide); less than 0.2% of cobalt oxide, dispersant A15: less than 0.5%; CMC: less than 1%.
Then, respectively putting the solid raw material components into a drying room for drying, wherein the water content of quartz and feldspar is controlled within 2% by mass; the moisture content of other solid raw material components is controlled within 1 percent by mass.
Adding all the raw material components into a ball mill one by one according to the raw material ratio, adding water, wherein the mass percentage content of the water is required to be controlled at 34-36%, ball milling for 12-14 hours to form glaze slurry, and then sieving the glaze slurry with a 200-mesh sieve; and (3) removing iron from the sieved glaze slurry by using a magnet rod, then checking iron by using a 140-mesh/inch screen, and removing iron again if the number of iron points is more than 2 until the number of the iron points is not more than 2, and determining that the glaze slurry is qualified.
Storing the qualified glaze slip into a jar, adding 1-2% of water by mass percent, and covering a jar cover for ageing, wherein the ageing time of the glaze slip is not less than one week; and adjusting the water content of the aged glaze slip to 34-36% by mass.
And opening a spray gun to spray glaze on the green body, drying the surface of the green body by using a hot air blower after the first glaze spraying is finished, and then spraying glaze for the second time, wherein the hot air blowers blow hot air beside the two glaze spraying processes. There is no specific requirement for the rod diameter of the product. The glaze spraying method is improved in the patent: the spraying gun is firstly kept to spray the upper part or the lower part of the umbrella in one direction, then the spraying gun is changed to spray the lower part or the upper part of the umbrella in the other direction, and the glaze spraying is generally in the tangential direction with the circumference of the section of the product. And after the first spraying of the blank with the main body diameter larger than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out. And (4) directly glazing the blank with the main body diameter less than 160mm after the glazing is sprayed for the first time, and then glazing for the second time, wherein the glazing for the second time is carried out for the second time. And (3) opening a hot air blower beside the spraying device to blow hot air while spraying the primary glaze and the secondary glaze. After each glaze spraying, the surface is dried by hot air.
The glazing should be carried out on hot blanks, for which purpose the blanks on each shelf should be preheated twice, alternately glazed, in order to maintain the temperature of the blank.
Soot blowing is required to be carried out on the blank before the glaze is sprayed for the first time and the second time. In order to prevent the bowl scraps generated during the lifting of the product, when the glaze is sprayed for the first time, the glaze is uniformly sprayed on the neck.
Putting the blank body sprayed with the glaze slip into a drying room, and drying for 4-6 hours; then loading the materials from a drying room into a drawer kiln for sintering: in the existing firing process, firing is mainly divided into a small-fire heating stage, an oxidation stage, a middle-fire heat preservation stage, a reduction stage, a high-fire heat preservation stage and a cooling stage; the parameters of each stage are as follows:
a small fire heating stage: the temperature is increased from room temperature to 300 ℃, and the temperature increasing speed is 10 ℃/h in the stage.
And (3) an oxidation stage: namely, the temperature is increased from 300 ℃ to 950 ℃, and the temperature increasing speed is kept at 25-45 ℃/h; and (3) a medium-fire heat preservation stage: namely, the temperature is increased from 950 ℃ to 960 ℃, and the oxygen content in the kiln is controlled to be 8-12% at the stage under the condition of ensuring the temperature to be stable.
And (3) reduction stage: namely, the temperature is increased from 970 ℃ to a high-temperature preservation temperature, and the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2-4 hours, the temperature is from 1200 ℃ to the fire stopping temperature, enough air is required to be introduced on the basis of weak reduction, a certain gas flow is ensured to prevent sudden temperature drop in the kiln, the flowing-away oxygen is ensured to be contained in the kiln, the volume content of CO in the kiln is controlled to be below 1%, and the volume content of the oxygen is controlled to be 1-3%.
And (3) high-fire heat preservation stage: keeping the temperature at the fire-stopping temperature for 0.2-0.5 h, and controlling the amount of air and fuel gas at this stage to ensure that the oxygen content is about 2.8-3.8%.
And (3) a cooling stage: namely the fire stopping temperature is-room temperature, and the whole process takes 30-45 hours; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
The raw material proportion and the firing method thereof adopt the traditional equipment in the firing process of the electric porcelain gray glaze, completely meet the requirement of batch production, can greatly improve the appearance quality and glaze surface performance of porcelain pieces, can ensure high qualification rate of products, and have good economic benefit.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (10)
1. The electric porcelain ash glaze material is characterized by comprising the following components in percentage by mass:
25% -27% of quartz; 36 to 39 percent of feldspar; talc powder: 8% -10%; 6-8% of limestone; 2% -4% of alumina; 2% -4% of Yunyan powder; 5% -7% of zirconium silicate; 2% -4% of lithionite; 1.5 to 3 percent of barium carbonate; 0.2 to 0.4 percent of pigment; cobalt oxide is less than 0.2%; less than 0.5% of dispersant A15; less than 1% of hydroxymethyl cellulose.
2. The electric porcelain ash glaze material according to claim 1, wherein the pigment comprises manganese oxide, iron oxide and chromium oxide.
3. The preparation method of the electric porcelain ash glaze is characterized by comprising the following steps:
s1, respectively drying the components of the electric porcelain ash glaze material of claim 1 or 2;
s2, adding all the components into a ball mill according to the proportion, adding water, and performing ball milling to form glaze slurry;
s3, sieving and deironing the glaze slip obtained in the step S2; sealing and storing and aging after iron is checked to be qualified;
s4, measuring and adjusting the moisture of the glaze slurry to 34-36% before glaze spraying;
and S5, carrying out glaze spraying and sintering on the blank to obtain the electric porcelain ash glaze.
4. The preparation method according to claim 3, wherein the drying in S1 controls the moisture content of the quartz and feldspar within 2% by mass; the moisture content of other solid components is controlled within 1 percent by mass.
5. The preparation method according to claim 3, wherein the water is added to S2 in a mass percent of 34-36%;
preferably, the ball milling time of the electroceramics ash glaze material in S2 is 12-14 hours.
6. The method according to claim 3, wherein the screen used for the screening in S3 is a 200-mesh stainless steel screen;
preferably, the iron removing tool used for removing iron in S3 is a strong magnet bar or an iron remover;
preferably, the iron inspection qualification in the S3 requires the use of a 140-mesh/inch sieve, and the number of iron points is not more than 2;
preferably, the step of sealing and staling in S3 includes:
storing the glaze slurry after iron checking is qualified in a jar, adding 1-2% of water by mass percent, and covering a jar cover for ageing; the aging time is not less than one week; during the period of staleness, the glaze slip needs to be stirred for not less than half an hour every day.
7. The method according to claim 3, wherein the step of "S4, measuring and adjusting the moisture content of the glaze slurry to 34-36%" before glaze spraying specifically comprises:
the time for stirring the glaze slip before glaze spraying is more than or equal to 1 h; the ambient temperature of the glazing room is more than or equal to 15 ℃, and the humidity is less than or equal to 55 percent; determining whether the moisture meets the process requirements;
adding water when the water content is lower than the standard, blending, stirring, and measuring until the water content reaches the standard; when the moisture content is higher than the standard, the water-soluble organic silicon compound is mixed with the low moisture content for use.
8. The method according to claim 3, wherein the glaze spraying comprises:
firstly, enabling a spray gun to keep the upper part or the lower part of the umbrella sprayed in one direction, then, replacing the spray gun with the lower part or the upper part of the umbrella sprayed in the other direction, and enabling the glaze spraying to form a tangential direction with the circumference of the section of the blank;
after the first spraying of the blank with the main body diameter being more than or equal to 160mm, pulling the blank into a drying room, drying, and then glazing for the second time, wherein the glazing for the second time is carried out for the second time; directly glazing a blank with the main body diameter less than 160mm after the first glazing, and glazing for the second time; when the primary glaze and the secondary glaze are sprayed, a hot air blower beside the primary glaze and the secondary glaze is opened to blow hot air; after each glaze spraying, the surface is dried by hot air.
9. The production method according to claim 3, wherein the firing includes:
a small fire heating stage: heating the mixture from room temperature to 300 ℃ at a heating speed of 10 ℃/h;
and (3) an oxidation stage: heating from 300 ℃ to 950 ℃ at a heating speed of 25-45 ℃/h;
and (3) a medium-fire heat preservation stage: raising the temperature from 950 ℃ to 960 ℃, and controlling the oxygen content in the kiln to be 8-12%;
and (3) reduction stage: raising the temperature from 970 ℃ to a high-preservation temperature, wherein the stage is divided into a strong reduction period, a weak reduction period and an oxygen permeation period in sequence; the strong reduction period takes 10 to 13 hours, the temperature is raised from 970 ℃ to 1130 ℃, and the volume content of CO in the kiln is controlled to be 4.4 to 2 percent; the weak reduction period takes 4 to 5 hours, the temperature is raised from 1130 ℃ to 1200 ℃, and the volume content of CO in the kiln is controlled to be 2.2 to 0.2 percent; the oxygen permeation period takes 2 to 4 hours, the volume content of CO in the kiln is controlled to be below 1 percent and the volume content of oxygen is controlled to be 1 to 3 percent from 1200 ℃ to the fire stopping temperature;
and (3) high-fire heat preservation stage: keeping the temperature at the fire stopping temperature for 0.2 to 0.5 hour to ensure that the oxygen content is between 2.8 and 3.8 percent;
and (3) a cooling stage: stopping fire at room temperature for 30-45 hr; and after the cooling stage is finished, the electric porcelain gray glaze can be fired.
10. An electric porcelain gray glaze prepared by the preparation method of any one of claims 3 to 9.
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| CN114656149A (en) * | 2022-04-19 | 2022-06-24 | 德化县京隆堂陶瓷有限责任公司 | Aurora green fiber glaze ceramic and preparation method thereof |
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Application publication date: 20200605 |