CN112408791A - Firing method for high-temperature firing of bone china for daily use - Google Patents

Firing method for high-temperature firing of bone china for daily use Download PDF

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CN112408791A
CN112408791A CN202011458825.XA CN202011458825A CN112408791A CN 112408791 A CN112408791 A CN 112408791A CN 202011458825 A CN202011458825 A CN 202011458825A CN 112408791 A CN112408791 A CN 112408791A
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parts
temperature
glaze
firing
pug
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CN112408791B (en
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李冬根
彭运根
赵黎明
李朝
彭水根
杨锋
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Jiangxi Jinhaili Ceramics Co ltd
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Jiangxi Jinhaili Ceramics Co ltd
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Abstract

The invention relates to a firing method for firing bone china for daily use at high temperature, belonging to the technical field of ceramic products. The pug and glaze formula comprises the following components in parts by weight: 70-80 parts of talc, 3-4 parts of bone charcoal powder, 3-6 parts of feldspar, 4-7 parts of bentonite, 9-13 parts of kaolin and 0.2-0.5 part of sodium humate; glaze material: 55-62 parts of potassium feldspar, 9-12 parts of quartz, 9-11 parts of Longyan soil, 3-4 parts of lepidolite, 3-5 parts of zinc oxide, 9-10 parts of waste porcelain powder and 2-3 parts of bone charcoal powder, and the product is prepared by pug and glaze, molding, drying, glazing and high-temperature sintering, wherein the sintering time is 8-12 hours, and the highest sintering temperature is 1280-1320 ℃. The novel bone daily porcelain sintered by the invention has good transparency, strength and whiteness, smoothness and high ornamental value, thereby having wide application prospect.

Description

Firing method for high-temperature firing of bone china for daily use
Technical Field
The invention relates to a firing method for firing bone china for daily use at high temperature, belonging to the technical field of ceramic products.
Background
The bone china has fine and smooth porcelain quality, smooth glaze surface and soft luster, and is extremely elegant and graceful like grease. With the continuous improvement of living standard of people, higher requirements are put forward on the taste and the grade of the daily-use articles, and particularly, the daily-use ceramic articles are reflected. The bone china is the top grade of china acknowledged in the world at present, is deeply loved by consumers and has very wide market prospect.
The high white porcelain is also called high-grade white porcelain, and is carved into three golden flowers in the German porcelain together with the white porcelain and the artistic porcelain. The high-whiteness porcelain is prepared by finely processing local high-quality kaolin and other raw materials and reducing and firing at high temperature, and the glaze color of the porcelain is pure and fine. However, the traditional high-whiteness porcelain clay formula has the defects of poor mud fluidity, poor mud shaping, poor porcelain forming thermal stability, high water absorption, and unsatisfactory porcelain forming whiteness and transmittance, so that the finished product rate is low and the price is high.
The high-temperature fired bone china (the highest firing temperature is 1300 ℃) has the advantages of high strength, good whiteness and transparency, and smooth and fine glaze surface and beautiful appearance. However, the quality of the existing bone china product is difficult to control, and the main problems are low strength, poor thermal shock resistance and high lead and cadmium dissolution. With the increasing living standard of people, the requirements of consumers on daily porcelain are higher and higher, and people have high requirements on the whiteness, transparency and the like of the appearance of the daily porcelain and have higher requirements on the internal performances of lead and cadmium dissolution and thermal shock resistance. Therefore, the research on the novel bone china for daily use with better appearance, high strength, low lead and cadmium dissolution and good thermal shock resistance has great practical significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel bone china for daily use aiming at the technical defects of the existing bone china for daily use. Compared with the common high white porcelain, the novel bone daily porcelain has the advantages of low lead and cadmium dissolution amount, good thermal shock resistance, high whiteness, high transparency, smoothness, beauty, durability and high ornamental value.
The invention provides a slip glaze formula for high-temperature-fired bone domestic porcelain, which comprises the following components in parts by weight:
the pug comprises: 70-80 parts of talc, 3-4 parts of bone charcoal powder, 3-6 parts of feldspar, 4-7 parts of bentonite, 9-13 parts of kaolin and 0.2-0.5 part of sodium humate;
the glaze material comprises: 55-62 parts of potash feldspar, 9-12 parts of quartz, 9-11 parts of Longyan soil, 3-4 parts of lepidolite, 3-5 parts of zinc oxide, 9-10 parts of waste porcelain powder and 2-3 parts of bone charcoal powder.
In the process of firing the daily bone china at high temperature, both the pug and the glaze on the pug expand and contract to a certain extent, so that for the daily bone china fired at high temperature, the pug and the glaze of the daily bone china fired at high temperature need to meet the requirements at the same time, and the expansion coefficients of the pug and the glaze need to be adapted to ensure that the china cannot deform, bubble, crack and the like in the firing process.
Further, the pug comprises: 74 parts of talcum, 4 parts of bone charcoal powder, 5 parts of feldspar, 6 parts of bentonite, 11 parts of Datong soil and 0.3 part of sodium humate.
Further, the feldspar is albite or potassium feldspar.
Further, the glaze comprises: 58 parts of potassium feldspar, 9 parts of quartz, 11 parts of Longyan soil, 3 parts of lepidolite, 5 parts of zinc oxide, 10 parts of waste porcelain powder and 3 parts of bone charcoal powder.
Further, the preparation process of the pug comprises the following steps: weighing the raw materials according to the formula of the pug, adding water until the water content of the pug is 40-45%, loading into ball milling equipment for ball milling, sieving the milled mud to remove iron, dehydrating, pugging and aging to obtain the pug.
Further, the preparation process of the glaze material comprises the following steps: weighing the raw materials according to the formula of the glaze, adding water until the water content of the glaze is 45-50%, putting the glaze into ball milling equipment for ball milling, and sieving the milled glaze slurry to remove iron to obtain the finished product.
Further, the pug is 10 times of the weight of the glaze.
The invention also aims to provide a firing method for high-temperature firing of the bone domestic porcelain, which comprises the following steps:
1) preparing raw materials: respectively preparing pug and glaze for high-temperature firing of the bone domestic porcelain;
2) and (3) mechanical pressing and forming: finishing the manufacture of a blank body by adopting the pug, and glazing after drying the blank body to obtain a glaze blank;
3) first-stage oxidation impurity removal: after the glaze blank is dried, placing the dried glaze blank into a furnace kiln for oxidation impurity removal firing, wherein the oxidation impurity removal firing method comprises the steps of heating the temperature in the furnace kiln to 975-985 ℃ from room temperature for 3-4h and keeping the temperature for 20-40 min;
4) and (3) second-stage weak reduction: raising the temperature of the furnace from 975-985 ℃ to 1200-1240 ℃ for 2-2.5h when the temperature of the furnace is used, and carrying out weak reduction firing on the oxidized, impurity-removed and fired glaze blank;
5) three-stage high-temperature sintering: the temperature of the furnace is increased from 1200-1240 ℃ to 1280-1320 ℃ for 2.5-3.5h, and the glaze blank after the weak reduction firing is sintered at high temperature and is kept for 20-40 min.
Further, the oxidizing impurity removal firing method comprises the steps of heating the temperature in the kiln from room temperature to 980 ℃ for 3.5 hours and preserving the temperature for 30 min.
Further, the weak reduction firing method is that the temperature of the furnace is increased from 980 ℃ to 1200 ℃ for 2.5h, and the glaze blank after oxidation impurity removal firing is subjected to weak reduction firing.
Further, the high-temperature firing method is that the temperature of the furnace is increased from 1200 ℃ to 1300 ℃ for 2.5h, and the glaze blank after the weak reduction firing is subjected to high-temperature firing, and then the temperature is kept for 30 min.
Further, the kiln is an automatic energy-saving shuttle kiln.
The invention adopts a three-section type firing process to fire the high-temperature fired bone domestic porcelain, and specifically, the oxidation impurity removal firing aims at removing carbon, crystal water, sulfur oxide, organic impurities and the like in a glaze blank; the reduction firing aims at reducing Fe in the glaze blank at high temperature so as to improve the whiteness of the porcelain; the high temperature firing aims to impart high transparency to the porcelain by imparting a higher glass phase to the porcelain at high temperature.
In the invention, strong reduction firing is changed into weak reduction firing, in the process of strong reduction firing, the firing temperature needs to reach more than 1260 ℃, and the firing time needs to reach 3.5h so as toSo that Fe in the glaze blank3+All reduced to Fe2+And the obtained finished product is white and green, and in the invention, the Fe in the glaze blank is sintered for 2-2.5h at 1200-1240 DEG C3+Partially reduced to Fe2+In the process, the whiteness of the finished product is natural and soft, the energy consumption is saved, the discharged sintering waste gas contains less sulfur and harmful substances, the process is more environment-friendly, and the prepared porcelain product has higher strength, higher transparency and softer color and luster by matching the formula of the invention and the sintering process.
Compared with the prior art, the invention has the following beneficial effects:
the bone china for daily use developed and debugged by the formula of the slip glaze has the advantages of low lead and cadmium dissolution, good thermal shock resistance, high strength whiteness, high transparency, smoothness, beauty, durability and high ornamental value, and compared with the original old china (high white porcelain), the new china of the invention has the advantages of increased cost by about 10%, increased selling price by about 25% and direct economic benefit by about 15%.
The adaptability of the slip glaze material of the forming process is upgraded, the slip casting process is suitable, the operation of a full-automatic intelligent forming production line is also suitable, and the requirements are completely met after the slip glaze material is put into mass production.
The firing curve is adjusted, full-automatic energy-saving shuttle kiln firing is taken as a subject, the original strong reducing flame firing is adjusted into weak reducing flame firing, so that about 20 percent of natural gas is saved, and the produced ceramic product is more transparent, bright, clean, fine, high in strength and whiteness, smooth in color and has jade texture.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The daily bone china fired at high temperature comprises the following components in parts by weight:
pug: 74 parts of talc, 4 parts of bone charcoal powder, 5 parts of feldspar, 6 parts of bentonite, 11 parts of Datong soil and 0.3 part of sodium humate;
glaze material: 58 parts of potassium feldspar, 9 parts of quartz, 11 parts of Longyan soil, 3 parts of lepidolite, 5 parts of zinc oxide, 10 parts of waste porcelain powder and 3 parts of bone charcoal powder;
the preparation method comprises the following steps:
1) preparing mud materials: weighing the raw materials according to the formula of the pug, adding water until the water content of the pug is 40-45%, loading into ball milling equipment for ball milling, sieving the milled mud to remove iron, dehydrating, pugging and aging for later use.
2) Preparing glaze: weighing the raw materials according to the formula of the glaze, adding water until the moisture content of the glaze is 45-50%, placing the glaze into ball milling equipment for ball milling, and sieving the milled glaze slurry to remove iron for later use.
3) After the pug prepared in the step 1) is put into a gypsum mold for molding, applying the glaze prepared in the step 2) on the surface of a pug after the pug is dried, wherein the used pug is 10 times of the weight of the glaze, and a three-stage high-temperature firing process is adopted for a glazed blank body, and the specific firing step is as follows:
first-stage oxidation impurity removal: drying the glaze blank, and then placing the dried glaze blank into a furnace kiln for oxidation impurity removal firing, wherein the oxidation impurity removal firing method comprises the steps of heating the temperature in the furnace kiln from room temperature to 980 ℃ for 3.5 hours and preserving the temperature for 30min to remove carbon, crystal water, sulfur oxide, organic impurities and the like in the blank;
and (3) second-stage weak reduction: raising the temperature of the furnace from 980 ℃ to 1200 ℃ for 2.5h, and carrying out weak reduction firing on the glaze blank subjected to oxidation impurity removal firing to obtain Fe in the blank3+Reduction to Fe2+
Three-stage high-temperature sintering: heating the furnace kiln from 1200 ℃ to 1300 ℃ for 2.5h, sintering the weakly reduced and sintered glaze blank at high temperature, and keeping the temperature for 30min to enable the blank body to generate a glass phase; and finally, extinguishing the kiln and naturally cooling to room temperature.
Example 2
The daily bone china fired at high temperature comprises the following components in parts by weight:
pug: 74 parts of talc, 4 parts of bone charcoal powder, 5 parts of feldspar, 6 parts of bentonite, 11 parts of Datong soil and 0.3 part of sodium humate;
glaze material: 58 parts of potassium feldspar, 9 parts of quartz, 11 parts of Longyan soil, 3 parts of lepidolite, 5 parts of zinc oxide, 10 parts of waste porcelain powder and 3 parts of bone charcoal powder;
the preparation method comprises the following steps:
1) preparing mud materials: weighing the raw materials according to the formula of the pug, adding water until the water content of the pug is 40-45%, loading into ball milling equipment for ball milling, sieving the milled mud to remove iron, dehydrating, pugging and aging for later use.
2) Preparing glaze: weighing the raw materials according to the formula of the glaze, adding water until the moisture content of the glaze is 45-50%, placing the glaze into ball milling equipment for ball milling, and sieving the milled glaze slurry to remove iron for later use.
3) After the pug prepared in the step 1) is put into a gypsum mold for molding, applying the glaze prepared in the step 2) on the surface of a pug after the pug is dried, wherein the used pug is 10 times of the weight of the glaze, and a three-stage high-temperature firing process is adopted for a glazed blank body, and the specific firing step is as follows:
first-stage oxidation impurity removal: drying the glaze blank, and then placing the dried glaze blank into a furnace kiln for oxidation impurity removal firing, wherein the oxidation impurity removal firing method comprises the steps of heating the temperature in the furnace kiln from room temperature to 980 ℃ for 3.5 hours and preserving the temperature for 30min to remove carbon, crystal water, sulfur oxide, organic impurities and the like in the blank;
and (3) second-stage weak reduction: increasing the temperature of the furnace from 980 ℃ to 1240 ℃ for 2.5h, and weakly reducing and firing the oxidized and impurity-removed fired glaze blank to obtain Fe in the blank3+Reduction to Fe2+
Three-stage high-temperature sintering: heating the furnace kiln from 1240 ℃ to 1320 ℃ for 2.5h, sintering the weakly reduced and sintered glaze blank at high temperature, and keeping the temperature for 30min to ensure that the blank body generates a glass phase; and finally, extinguishing the kiln and naturally cooling to room temperature.
Example 3
The daily bone china fired at high temperature comprises the following components in parts by weight:
pug: 78 parts of talc, 3 parts of bone charcoal powder, 3 parts of feldspar, 5 parts of bentonite, 9 parts of Datong soil and 0.5 part of sodium humate;
glaze material: 60 parts of potash feldspar, 11 parts of quartz, 9 parts of Longyan soil, 4 parts of lepidolite, 4 parts of zinc oxide, 9 parts of waste porcelain powder and 2 parts of bone charcoal powder;
the preparation method comprises the following steps:
1) preparing mud materials: weighing the raw materials according to the formula of the pug, adding water until the water content of the pug is 40-45%, loading into ball milling equipment for ball milling, sieving the milled mud to remove iron, dehydrating, pugging and aging for later use.
2) Preparing glaze: weighing the raw materials according to the formula of the glaze, adding water until the moisture content of the glaze is 45-50%, placing the glaze into ball milling equipment for ball milling, and sieving the milled glaze slurry to remove iron for later use.
3) After the pug prepared in the step 1) is put into a gypsum mold for molding, applying the glaze prepared in the step 2) on the surface of a pug after the pug is dried, wherein the used pug is 10 times of the weight of the glaze, and a three-stage high-temperature firing process is adopted for a glazed blank body, and the specific firing step is as follows:
first-stage oxidation impurity removal: drying the glaze blank, and then placing the dried glaze blank into a furnace kiln for oxidation impurity removal firing, wherein the oxidation impurity removal firing method comprises the steps of heating the temperature in the furnace kiln from room temperature to 980 ℃ for 3.5 hours and preserving the temperature for 30min to remove carbon, crystal water, sulfur oxide, organic impurities and the like in the blank;
and (3) second-stage weak reduction: raising the temperature of the furnace from 980 ℃ to 1200 ℃ for 2.5h, and carrying out weak reduction firing on the glaze blank subjected to oxidation impurity removal firing to obtain Fe in the blank3+Reduction to Fe2+
Three-stage high-temperature sintering: heating the furnace kiln from 1200 ℃ to 1300 ℃ for 2.5h, sintering the weakly reduced and sintered glaze blank at high temperature, and keeping the temperature for 30min to enable the blank body to generate a glass phase; and finally, extinguishing the kiln and naturally cooling to room temperature.
Comparative example 1
The high-white porcelain fired at high temperature comprises the following components in parts by weight:
pug: 80 parts of kaolin, 10 parts of feldspar, 7 parts of waste porcelain powder and 3 parts of sodium humate;
glaze material: 62 parts of feldspar, 20 parts of quartz, 5 parts of calcium carbonate, 5 parts of zinc oxide and 8 parts of kaolin;
the preparation method comprises the following steps:
1) preparing mud materials: weighing the raw materials according to the formula of the pug, adding water until the water content of the pug is 40-45%, loading into ball milling equipment for ball milling, sieving the milled mud to remove iron, dehydrating, pugging and aging for later use.
2) Preparing glaze: weighing the raw materials according to the formula of the glaze, adding water until the moisture content of the glaze is 45-50%, placing the glaze into ball milling equipment for ball milling, and sieving the milled glaze slurry to remove iron for later use.
3) After the pug prepared in the step 1) is put into a gypsum mold for molding, applying the glaze prepared in the step 2) on the surface of a pug after the pug is dried, wherein the used pug is 10 times of the weight of the glaze, and a three-stage high-temperature firing process is adopted for a glazed blank body, and the specific firing step is as follows:
first-stage oxidation impurity removal: drying the glaze blank, and then placing the dried glaze blank into a furnace kiln for oxidation impurity removal firing, wherein the oxidation impurity removal firing method comprises the steps of raising the temperature in the furnace kiln to 980 ℃ from room temperature within 4 hours and preserving the temperature for 30min so as to remove carbon, crystal water, sulfur oxide, organic impurities and the like in the blank;
and (3) second-stage weak reduction: the temperature of the furnace is increased from 980 ℃ to 1260 ℃ for 3.5h, the oxidized and impurity-removed fired glaze blank is subjected to weak reduction firing, and Fe in the blank body is obtained3+Reduction to Fe2+
Three-stage high-temperature sintering: heating the furnace kiln from 1260 ℃ to 1350 ℃ for 4.5h, sintering the weakly reduced and sintered glaze blank at high temperature, and keeping the temperature for 30min to enable the blank body to generate a glass phase; and finally, extinguishing the kiln and naturally cooling to room temperature.
The quality test was carried out on the fired samples of examples 1-3 and comparative example 1, wherein the thermal shock resistance was measured according to the method specified in GB/T3298-;
the detection basis of the whiteness is QB/T1503-2011;
the detection basis of the lead migration amount is GB 31604.34-2016;
the detection basis of the cadmium migration amount is GB 31604.24-2016;
the detection basis of the water absorption is GB/T3299-2011;
the detection basis of the bending strength is GB/T4741-1999;
the results are shown in table 1:
TABLE 1
National standard Example 1 Example 2 Example 3 Comparative example 1
Thermal shock resistance - Not cracked Not cracked Not cracked Not cracked
Whiteness (%) ≧55 87 83 86 74
Migration amount of lead (mg/L) - Not detected out Not detected out Not detected out Not detected out
Migration volume of cadmium (mg/L) - Not detected out Not detected out Not detected out Not detected out
Water absorption (E/%) ≦0.5 0.02 0.03 0.02 0.11
Flexural strength (MPa) - 132 126 130 111
Percentage of finished product (%) - 96.5 95.9 96.3 92.4
As can be seen from the data in Table 1, the bone domestic porcelain fired by the invention has extremely low lead-cadmium dissolution rate and water absorption rate, good thermal shock resistance and bending strength resistance and high whiteness, and compared with the original fired porcelain (high white porcelain), the internal performance and the appearance of the bone domestic porcelain are obviously improved, thereby meeting the high requirements of people on the domestic porcelain nowadays.
The above-described embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications can be made by one skilled in the art, and any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The firing method for the high-temperature fired bone china for daily use is characterized by comprising the following steps of:
1) preparing raw materials: respectively preparing pug and glaze for high-temperature firing of the bone domestic porcelain;
2) and (3) mechanical pressing and forming: finishing the manufacture of a blank body by adopting the pug, and glazing after drying the blank body to obtain a glaze blank;
3) first-stage oxidation impurity removal: after the glaze blank is dried, placing the dried glaze blank into a furnace kiln for oxidation impurity removal firing, wherein the oxidation impurity removal firing method comprises the steps of heating the temperature in the furnace kiln to 975-985 ℃ from room temperature for 3-4h and keeping the temperature for 20-40 min;
4) and (3) second-stage weak reduction: raising the temperature of the furnace from 975-985 ℃ to 1200-1240 ℃ for 2-2.5h when the temperature of the furnace is used, and carrying out weak reduction firing on the oxidized, impurity-removed and fired glaze blank;
5) three-stage high-temperature sintering: the temperature of the furnace is increased from 1200-1240 ℃ to 1280-1320 ℃ for 2.5-3.5h, and the glaze blank after the weak reduction firing is sintered at high temperature and is kept for 20-40 min.
2. The firing method of the high-temperature fired bone china for daily use according to claim 1, wherein the pug comprises the following components in parts by weight: 70-80 parts of talc, 3-4 parts of bone charcoal powder, 3-6 parts of feldspar, 4-7 parts of bentonite, 9-13 parts of Datong soil and 0.2-0.5 part of sodium humate.
3. The firing method of the high-temperature fired bone china for daily use according to claim 1, wherein the glaze comprises the following components in parts by weight: 55-62 parts of potash feldspar, 9-12 parts of quartz, 9-11 parts of Longyan soil, 3-4 parts of lepidolite, 3-5 parts of zinc oxide, 9-10 parts of waste porcelain powder and 2-3 parts of bone charcoal powder.
4. The firing method of the high-temperature fired bone china for daily use according to claim 2, characterized in that the pug comprises 74 parts of talc, 4 parts of bone charcoal powder, 5 parts of feldspar, 6 parts of bentonite, 11 parts of kaolin and 0.3 part of sodium humate;
preferably, the feldspar is albite or potassium feldspar.
5. The firing method of the high-temperature fired bone china for daily use according to claim 3, wherein the glaze comprises: 58 parts of potassium feldspar, 9 parts of quartz, 11 parts of Longyan soil, 3 parts of lepidolite, 5 parts of zinc oxide, 10 parts of waste porcelain powder and 3 parts of bone charcoal powder.
6. The firing method of the high-temperature fired bone china for daily use according to any one of claims 1 to 5, characterized in that the preparation process of the pug is: weighing the raw materials according to the formula of the pug, adding water until the water content of the pug is 40-45%, putting the pug into ball milling equipment for ball milling, sieving the obtained grinding mud to remove iron, dehydrating, pugging and aging to obtain the pug.
7. The firing method of the high-temperature fired bone china for daily use according to any one of claims 1 to 5, characterized in that the glaze preparation process comprises: weighing the raw materials according to the formula of the glaze, adding water until the water content of the glaze is 45-50%, putting the glaze into ball milling equipment for ball milling, and sieving the milled glaze slurry to remove iron to obtain the finished product.
8. The firing method of the high-temperature fired bone china for daily use according to claim 1, wherein the oxidation impurity removal firing method comprises the steps of raising the temperature in a kiln from room temperature to 980 ℃ for 3.5 hours and keeping the temperature for 30 min.
9. The firing method of the high-temperature fired bone china for daily use according to claim 1, wherein the weak reduction firing method comprises the step of increasing the kiln temperature from 980 ℃ to 1200 ℃ for 2.5 hours to conduct weak reduction firing on the oxidized impurity-removed fired glaze blank.
10. The firing method of a high-temperature-fired bone china for daily use according to claim 1, wherein the firing method comprises the steps of raising the kiln temperature from 1200 ℃ to 1300 ℃ for 2.5 hours, firing the weakly-reduced and fired glaze blank at a high temperature, and then holding the temperature for 30 minutes.
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