CN104150873B - A kind of Longquan celadon crack glaze bottle and preparation method thereof - Google Patents

Abstract

The invention relates to a Longquan celadon cracked glaze wine bottle and a preparation method thereof. The proportions of raw materials in the blank, inner glaze and outer glaze of the wine bottle are as follows: blank: Longyan kaolin 40-55%, Longquan porcelain clay 15-25%, potassium feldspar 8-20%, quartz 7-15%, Zijin Soil 5-10%; inner glaze: glaze fruit 65-70%, glaze ash 12-25%, purple gold soil 5-10%; outer glaze: potassium feldspar 60-70%, quartz 8-15%, Longyan kaolin 8 ～13%, glaze ash 8～15%, purple gold soil 5～13%, Fe ₂ O ₃ 0.2～0.4%. On the basis of this raw material, the wet blank is made by slurrying, injection molding, and then dried, trimmed, and bisque-fired to complete the blank; finally, the inner glaze and outer glaze are applied, and the glaze firing is worthy of Longquan celadon crack glaze wine bottle. finished product. The inner glaze of this wine bottle has no lines, the outer glaze is decorated with cracks, the quality is good, the wine does not seep inside, and the preparation method has low cost and good effect.

Description

A kind of Longquan celadon crack glaze wine bottle and its preparation method

technical field

The invention belongs to the field of porcelain, and relates to a Longquan celadon cracked-glazed wine bottle, a body and a glaze preparation method and a manufacturing process of the wine bottle.

Background technique

Since ancient times, there have been two completely different decoration methods for the glazed surface of Longquan celadon. First, the glaze has no grain, and the glaze color is mainly pink green and plum green, commonly known as "di kiln". Second, the glaze is cracked as the main decoration. The effect, commonly known as "Ge Kiln", was one of the five famous kilns in the Song Dynasty. In recent years, the production scale of Longquan celadon has gradually expanded, and many technicians have carried out more research on cracked glazes, and have achieved certain results. For example, the national patent office patent number is CN200810030924's invention patent "a method for making cracked glaze for medium-temperature daily-use ceramics", which introduces lithium-containing raw materials such as spodumene to burn medium-temperature daily-use ceramic crackle glazes, but the glaze has a relatively high processing cost. Wine bottle glaze has certain limitations; another example is the invention patent of CN200910103531 "a kind of crack glaze ceramic wine bottle manufacturing process", which heats the porcelain body to 40 degrees Celsius in an oven and then applies crack glaze. It is fired at 50-150°C lower than the firing temperature. Although this method can achieve the method of no cracks in the inner glaze of the wine bottle and the decoration of outer glaze cracks, it is extremely difficult to control the thickness of the glaze layer when firing cracked glazed wine bottles with this method. Glazing defects such as glaze shrinkage, pinholes, and air bubbles are prone to occur, which has limitations.

At present, in the field of Longquan celadon production, there are cracks inside and outside the wine bottle with cracked glaze. In the case of long-term storage of wine, the liquid will penetrate into the carcass through the cracks in the inner glaze wall, causing the carcass to absorb moisture and expand. When the surface tensile coefficient is increased, the tire wall will crack, which will eventually lead to wine seepage. It can be seen that the cracked glaze wine bottles made commonly cannot meet the specific requirements of long-term wine storage.

Contents of the invention

The technical problem to be solved by the present invention is to provide a Longquan celadon cracked-glazed wine bottle with no lines in the inner glaze and decorated with cracks in the outer glaze. Cracking, good quality of inner and outer glaze;

Another technical problem to be solved by the present invention is to provide a method for preparing Longquan celadon cracked glazed wine bottles with low production cost, high yield, few glazing defects, and good overall quality of the wine bottle. This preparation method is also suitable for large-scale enterprises. Production.

In order to solve the above-mentioned technical problems to be solved, the technical scheme adopted in the present invention is as follows:

A Longquan celadon cracked glaze wine bottle, which uses mineral raw materials to prepare blanks and inner glazes, uses mineral raw materials and adds industrial chemical raw materials to prepare outer glazes, and the proportions of raw materials in the blanks, inner glazes, and outer glazes are as follows in weight percentages: (i) Blank: 40-55% of Longyan kaolin, 15-25% of Longquan porcelain clay, 8-20% of potassium feldspar, 7-15% of quartz, and 5-10% of Zijin clay; the raw material components of the blank are 100% in total; (ii) Inner glaze: 65-75% of glaze fruit, 15-25% of glaze ash, 5-10% of purple gold soil; the total raw material components of the inner glaze are 100%; (iii) Outer glaze: 60-70% of potassium feldspar %, quartz 8-15%, Longyan kaolin 5-10%, glaze ash 8-15%, purple gold clay 5-13%, Fe ₂ O ₃ 0.2-0.4%, the total of the outer glaze raw material components is 100%; and Put the billet in the slurry tank to melt the slurry, so that the ratio of material to water reaches 1:0.5-0.7, and add 0.2-0.4% of water glass and 0.02-0.05% of sodium tripolyphosphate; the wet base, After drying, billet trimming and biscuit firing processes, the billet making is completed; then the inner glaze is applied, that is, the specific gravity of the inner glaze raw material is adjusted to a mixed solution with a Baume concentration of 50-60 degrees, and the biscuit-fired wine bottle The blank is dusted, the mouth of the wine bottle is facing down, and the inner glaze is sprayed to form the inner glaze layer; then the outer glaze is applied, that is, the proportion of the outer glaze raw material of the Longquan celadon crack glaze wine bottle is adjusted to a Baume concentration of 40-50 degrees. liquid, dedust the body that has been glazed inside, and apply outer glaze to form an outer glaze layer; finally, after glaze firing, the celadon body that has been glazed inside and outside is put into a high-temperature shuttle kiln atmosphere furnace and fired for 9 to 11 hours. The temperature of the kiln is gradually raised from normal temperature to 1280-1300°C. After 30-60 minutes of heat preservation, the flame is turned off and cooled naturally to obtain the finished Longquan celadon cracked glaze wine bottle.

As a further preferred solution of the present invention, the inner glaze is applied by the pressure spray glaze method, and the thickness of the inner glaze layer is between 0.1 and 0.15mm; the outer glaze is applied by the dipping method, and the outer glaze layer The thickness is between 0.3 and 0.8mm, so that the quality of the inner and outer glazes is good.

As a further preferred solution of the present invention, the thermal expansion coefficient of the prepared outer glaze layer is 10 to 13×10 ^-6 /°C, and the thermal expansion coefficient of the inner glaze layer is 4 to 8×10 ^-6 /°C. The difference in expansion coefficient , can clearly distinguish the boundary between the inner glaze and the outer glaze, so as to more stably ensure the decorative effect of no grain in the inner glaze and cracks in the outer glaze.

As a further preferred solution of the present invention, the biscuit firing is to put the celadon body after the trimming process into a biscuit kiln for firing for 5 to 7 hours, so that the temperature of the kiln is gradually raised from normal temperature to 780 to 880 °C, and the temperature is kept After 10-20 minutes, turn off the flame and let it cool naturally.

A preparation method for Longquan celadon cracked glaze wine bottle, comprising the following steps:

A. Mold making: Make plaster molds for wine bottles, and make plaster molds, and dry them for 1 to 2 days;

B. Slurry: put the billet in the slurry tank to make the slurry, so that the ratio of material to water reaches 1:0.5-0.7, and add 0.2-0.4% water glass and 0.02-0.05% sodium tripolyphosphate;

C. Blank making: inject the melted mud into the gypsum mold through the pressure grouting pipe, pour out the excess mud after the thickness reaches 5mm-7mm, and take out the mud billet after the green body has a certain dry strength;

D. Drying: Put the mud into the drying room for 20-24 hours;

E. Blank trimming: add water to the semi-dry mud blank, scrape the sutures, and fine-tune;

F. Biscuit firing: Put the trimmed celadon body into a biscuit firing kiln and fire for 5-7 hours, so that the kiln temperature gradually rises from normal temperature to 780-880°C, keep it warm for 10-20 minutes, turn off the flame and cool naturally, that is Get Longquan celadon wine bottle bisque;

G. Apply inner glaze: adjust the specific gravity of the inner glaze of the Longquan celadon cracked glaze wine bottle to a mixture solution with a Baume concentration of 50-60 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle blank, with the mouth facing down, using The inner glaze is applied by the pressure spray glaze method, and the thickness of the inner glaze layer is 0.1-0.15mm;

H. Drying: Put the glazed wine bottle body into the drying room for 3 to 5 hours;

I. Applying the outer glaze: adjust the specific gravity of the outer glaze of the Longquan celadon cracked glaze wine bottle to a mixture solution with a Baume concentration of 40-50 degrees, use a high-pressure air pump to remove dust from the inner glazed blank, and apply the outer glaze by dipping method. The thickness of the outer glaze layer is 0.3-0.8mm;

J. Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside;

K. Glaze firing: put the celadon body with internal and external glazing into a high-temperature shuttle kiln atmosphere furnace and fire for 9-11 hours, so that the kiln temperature gradually rises from normal temperature to 1280-1300 °C, keep it warm for 30-60 minutes, turn off the flame and cool naturally , that is, the finished product is obtained.

As a preference, the blank and the inner glaze raw materials use common mineral raw materials, the outer glaze raw materials use common mineral raw materials and add a small amount of industrial chemical raw materials; the thermal expansion coefficient of the prepared outer glaze layer is 10-13×10 ^-6 /°C , the thermal expansion coefficient of the inner glaze layer is 4 to 8×10 ^-6 /°C. The difference coefficient of this expansion coefficient can clearly distinguish the boundary between the inner glaze and the outer glaze, so as to more stably ensure the formation of inner glaze without grain and outer glaze. Crackle decorative effect.

Further, step K in the above preparation method also includes the following stages:

a. Preheating stage: firing at a heating rate of 2.5-3°C/min for 2-2.5 hours to raise the kiln temperature from room temperature to 300-350°C and remove residual moisture in the green body;

b. Oxidation stage: firing at a heating rate of 4-4.5°C/min for 2.5-2.8 hours to raise the kiln temperature to 950-980°C to remove crystal water, oxidize organic matter and sulfide, decompose carbonate, and form quartz crystal change;

c. Oxidation and heat preservation stage: keep the kiln temperature stable at 980-985°C and keep it warm for 1-1.2 hours, which is helpful for the discharge of gas in the green body and inner and outer glazes;

d. Strong reduction stage: firing at a heating rate of 1.5-2°C/min for 2-2.5 hours to raise the kiln temperature to 1200-1220°C, and keep the kiln pressure at 0.03-0.04MPa, so that the ferric iron in the formula fully reduced to ferrous iron;

e. Weak reduction stage: After another 1-1.5 hours, raise the kiln temperature to 1280-1300°C to fully mature the glaze layer and fix the ferrous iron;

f. High-fire heat preservation stage: control the kiln temperature at 1280-1300°C, and stop the fire after 0.5-1 hour of heat preservation;

g. Cooling stage: adopt the natural cooling method, leave the kiln after the kiln temperature is cooled to 50-70°C, and the firing is completed, and the finished Longquan celadon cracked glaze wine bottle is obtained. Not only the quality of the bottle fired by this method is good, but also the finished product rate is better.

Compared with the background technology of the present invention, the raw materials in the blank, inner glaze and outer glaze of the present invention start from the field of material selection, proportioning and combined production technology, wherein: 40-55% of Longyan kaolin, 15-25% of Longquan china clay , potassium feldspar 8-20%, quartz 7-15% and purple gold clay 5-10%, the thermal expansion coefficient after firing at 1280-1300°C is 5-7×10 ^-6 /°C; The thermal expansion coefficient of the inner glaze layer after firing at 1280-1300 ℃ is 4-8×10 ^-6 /℃. ; And the outer glaze made of potassium feldspar 60-70%, quartz 8-15%, Longyan kaolin 5-10%, glaze ash 8-15%, purple gold soil 5-13% and _Fe2O3 0.2-0.4 _% The thermal expansion coefficient of the outer glaze layer after the raw materials are fired at 1280-1300°C is 10-13×10 ^-6 /°C; it can be seen that the thermal expansion coefficient of the fired outer glaze layer is larger than that of the green tire, while the thermal expansion coefficient of the inner glaze layer is The coefficient of thermal expansion is close to that of the blank, so a Longquan celadon wine bottle with no cracks in the inner glaze and cracks in the outer glaze is obtained.

At the same time, the above-mentioned preparation method of the Longquan celadon cracked glaze wine bottle is not only novel and unique, but also has low cost, is suitable for large-scale production in enterprises, and has great application prospects. It has been verified by experiments that the Longquan celadon cracked glaze wine bottle prepared by the above preparation method has a uniform thickness and good quality of the glaze layer, and will not easily produce glaze defects such as shrinkage, pinholes, and air bubbles. The raw materials and outer glaze raw materials are selected to ensure that the difference between the thermal expansion coefficient of the outer glaze layer and the inner glaze layer or body is relatively large, so that the obtained wine bottle inner glaze does not produce cracks for long-term storage. It meets the function of wine storage in wine bottles, and also has the decorative effect of celadon crack glaze.

Detailed ways

The technical solutions of the present invention will be described in further detail below through specific examples.

Example 1:

The Longquan celadon cracked glaze wine bottle of this embodiment uses mineral raw materials to prepare blanks and inner glazes, and uses mineral raw materials and adds industrial chemical raw materials to prepare outer glazes.

Specifically, the blank: the weight percentage of the formula is composed of 52% of Longyan kaolin, 20% of Longquan porcelain clay, 10% of potassium feldspar, 10% of quartz, and 8% of purple gold clay. Weigh according to the above ratio, mix the raw materials evenly, put them into a ball mill with a material:ball:water ratio of 1:2:0.6, and put them into a ball mill for 4 hours, pass the slurry through a 100-mesh sieve after being stale for 36 hours, and dehydrate, After practicing the mud process, it is made into a blank.

Inner glaze raw materials: The weight percentage of the formula is composed of glaze fruit 72%, glaze ash 20%, and purple gold soil 8%. Weigh according to the above ratio, mix the raw materials evenly, put them into a ball mill with a material: ball: water ratio of 1:2:0.6, and after 2 hours of ball milling, the fineness of the glaze will reach the sieve residue of the million-hole sieve below 0.05%.

Outer glaze raw materials: formula weight percentage is composed of potassium feldspar 65.7%, quartz 10%, Longyan kaolin 6%, glaze ash 10%, purple gold clay 8%, industrial Fe ₂ O ₃ 0.3%. Weigh according to the above ratio, after mixing the raw materials evenly, put them into the ball mill with the material: ball: water ratio of 1:2:0.6, and after 24 hours of ball milling, the fineness of the glaze will reach the sieve residue of the ten-thousand-hole sieve below 0.05%. .

After making the ingredients, follow the steps below:

1) Mold making: According to the design requirements, a plaster mold of a celadon wine bottle with a finished product capacity of 500ml is made, and a plaster mold is made, and dried for 1 day;

2) Slurrying: place the billet in the slurrying tank to make the slurry, so that the ratio of material to water reaches 1:0.5, and add 0.2% water glass and 0.03% sodium tripolyphosphate;

3) Blank making: inject the melted mud into the gypsum mold through the pressure grouting pipe, pour out the excess mud after the thickness reaches 6mm, and take out the mud billet after the green body has a certain dry strength;

4) Drying: Put the mud base into a drying room for drying for 20 hours;

5) Blank trimming: hydrating the semi-dry mud blank, scraping the sutures, finishing;

6) Biscuit firing: put the trimmed celadon body into a biscuit kiln and fire it for 6 hours, so that the temperature of the kiln gradually rises from room temperature to 800°C, keep it warm for 10 minutes, turn off the flame and let it cool naturally, and you can get the Longquan celadon wine bottle plain. Blank;

7) Applying inner glaze: adjust the specific gravity of the inner glaze of Longquan celadon cracked glaze wine bottle to the mixed solution with a Baume concentration of 50 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle blank, with the mouth facing down, using pressure spray The inner glaze is applied by the glaze method, and the thickness of the glaze layer is 0.1mm;

8) Drying: put the glazed wine bottle body into the drying room for 3 hours;

9) Exterior glaze application: adjust the specific gravity of the exterior glaze of the Longquan celadon cracked glaze wine bottle to a mixture solution with a Baume concentration of 40 degrees, remove dust from the body that has been applied with the interior glaze, and apply the exterior glaze with the glaze dipping method. The thickness of the glaze layer is 0.5 mm;

10) Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside;

11) Glaze firing: Put the celadon body with internal and external glazing into a high-temperature shuttle kiln atmosphere furnace and fire for 10.5 hours, so that the kiln temperature gradually rises from normal temperature to 1280°C, keep the temperature for 30 minutes, turn off the flame and cool naturally to obtain the finished product.

In order to calculate the coefficient of thermal expansion better, its chemical composition of the above-mentioned raw materials that the embodiment of the present invention adopts is as shown in Table 1 below:

Table 1: Chemical composition of the above-mentioned raw materials Unit: %

Example 2:

The Longquan celadon cracked glaze wine bottle of this embodiment uses mineral raw materials to prepare blanks and inner glazes, and uses mineral raw materials and adds industrial chemical raw materials to prepare outer glazes.

Specifically, the blank: the weight percentage of the formula is composed of 46% of Longyan kaolin, 20% of Longquan porcelain clay, 14% of potassium feldspar, 10% of quartz, and 10% of purple gold clay. After weighing the raw materials according to the billet formula and mixing them evenly, put them into a ball mill with a material:ball:water ratio of 1:2:0.6 and mill them for 4 hours. Pass the slurry through a 100-mesh sieve after aging for 36 hours. After the process, it is made into a blank.

Inner glaze raw materials: The weight percentage of the formula is composed of glaze fruit 74%, glaze ash 18%, and purple gold soil 8%. Weigh according to the above ratio, mix the raw materials evenly, put them into a ball mill with a material: ball: water ratio of 1:2:0.6, and after 2 hours of ball milling, the fineness of the glaze will reach the sieve residue of the million-hole sieve below 0.05%.

Outer glaze raw materials: formula weight percentage is composed of 64.8% of potassium feldspar, 11% of quartz, 5% of Longyan kaolin, 9% of glaze ash, 10% of purple gold clay, and 0.2% _of industrial _Fe2O3 . Weigh according to the above ratio, after mixing the raw materials evenly, put them into the ball mill with the material: ball: water ratio of 1:2:0.6, and after 24 hours of ball milling, the fineness of the glaze will reach the sieve residue of the ten-thousand-hole sieve below 0.05%. .

After making the ingredients, follow the steps below:

1) Mold making: According to the design requirements, a plaster mold of a celadon wine bottle with a finished product capacity of 500ml is made, and a plaster mold is made, and dried for 1 day;

2) Slurrying: place the billet in the slurrying tank to make the slurry, so that the ratio of material to water reaches 1:0.5, and add 0.2% water glass and 0.03% sodium tripolyphosphate;

3) Blank making: inject the melted mud into the gypsum mold through the pressure grouting pipe, pour out the excess mud after the thickness reaches 6mm, and take out the mud billet after the green body has a certain dry strength;

4) Drying: Put the mud base into a drying room for drying for 20 hours;

5) Blank trimming: hydrating the semi-dry mud blank, scraping the sutures, finishing;

6) Biscuit firing: put the trimmed celadon body into a biscuit kiln and fire it for 6 hours, so that the temperature of the kiln gradually rises from room temperature to 800°C, keep it warm for 10 minutes, turn off the flame and let it cool naturally, and you can get the Longquan celadon wine bottle plain. Blank;

7) Applying inner glaze: adjust the specific gravity of the inner glaze of Longquan celadon cracked glaze wine bottle to the mixed solution with a Baume concentration of 50 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle blank, with the mouth facing down, using pressure spray The inner glaze is applied by the glaze method, and the thickness of the glaze layer is 0.1mm;

8) Drying: put the glazed wine bottle body into the drying room for 3 hours;

9) Exterior glaze application: adjust the specific gravity of the exterior glaze of the Longquan celadon cracked glaze wine bottle to a mixture with a Baume concentration of 40 degrees, use a high-pressure air pump to remove dust from the inner glazed blank, and apply the exterior glaze by dipping glaze. The thickness is 0.5mm;

10) Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside;

11) Glaze firing: Put the celadon body with internal and external glazing into a high-temperature shuttle kiln atmosphere furnace and fire for 10.5 hours, so that the kiln temperature gradually rises from normal temperature to 1280°C, keep the temperature for 30 minutes, turn off the flame and cool naturally to obtain the finished product.

Example 3:

The Longquan celadon cracked glaze wine bottle of this embodiment uses mineral raw materials to prepare blanks and inner glazes, and uses mineral raw materials and adds industrial chemical raw materials to prepare outer glazes.

Specifically, the blank: the weight percentage of the formula is composed of 46% of Longyan kaolin, 17% of Longquan porcelain clay, 15% of potassium feldspar, 12% of quartz, and 10% of purple gold clay. After weighing the raw materials according to the billet formula and mixing them evenly, put them into a ball mill with a material:ball:water ratio of 1:2:0.6 and mill them for 4 hours. Pass the slurry through a 100-mesh sieve after aging for 36 hours. After the process, it is made into a blank.

Inner glaze raw materials: The weight percentage of the formula is composed of glaze fruit 70%, glaze ash 20%, and purple gold soil 10%. Weigh according to the above ratio, mix the raw materials evenly, put them into a ball mill with a material: ball: water ratio of 1:2:0.6, and after 2 hours of ball milling, the fineness of the glaze will reach the sieve residue of the million-hole sieve below 0.05%.

Outer glaze raw materials: formula weight percentage is composed of potassium feldspar 67.6%, quartz 10%, Longyan kaolin 8%, glaze ash 8%, purple gold clay 6%, industrial Fe ₂ O ₃ 0.4%. Weigh according to the above ratio, after mixing the raw materials evenly, put them into the ball mill with the material: ball: water ratio of 1:2:0.6, and after 24 hours of ball milling, the fineness of the glaze will reach the sieve residue of the ten-thousand-hole sieve below 0.05%. .

And place the billet in the slurry tank to melt the slurry, so that the ratio of material to water reaches 1:0.6, and add 0.4% water glass and 0.04% sodium tripolyphosphate; the wet billet is obtained by injection molding, and then dried, repaired Billet and biscuit firing process to complete billet making. Among them, biscuit firing is to put the celadon body after the trimming process into a biscuit kiln and fire it for 7 hours, so that the temperature of the kiln gradually rises from normal temperature to 800 ° C, and after 10 to 20 minutes of heat preservation, the flame is turned off and naturally cooled. Then apply the inner glaze, that is, adjust the specific gravity of the inner glaze raw material to a mixed solution with a Baume concentration of 55 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle. The inner glaze is applied by the method, and the thickness of the inner glaze layer is 0.14mm. After applying the outer glaze, the specific gravity of the outer glaze raw materials described in the Longquan celadon cracked glaze wine bottle is adjusted to a mixed solution with a Baume concentration of 44 degrees. The inner glazed blank is dedusted with a high-pressure air pump, and the outer glaze is applied by dipping glaze method. , The thickness of the outer glaze layer is 0.8mm. Finally, after glaze firing, the celadon body that is glazed inside and outside is put into a high-temperature shuttle kiln atmosphere furnace and fired for 10 hours, so that the kiln temperature gradually rises from normal temperature to 1300°C, and after 50 minutes of heat preservation, the flame is turned off and naturally cooled to obtain Longquan celadon cracks. Finished glaze wine bottle.

Example 4:

The Longquan celadon cracked glaze wine bottle of this embodiment uses mineral raw materials to prepare blanks and inner glazes, and uses mineral raw materials and adds industrial chemical raw materials to prepare outer glazes.

Specifically, the blank: the weight percentage of the formula is composed of 50% of Longyan kaolin, 20% of Longquan china clay, 12% of potassium feldspar, 10% of quartz, and 8% of purple gold clay. After weighing the raw materials according to the billet formula and mixing them evenly, put them into a ball mill with a material:ball:water ratio of 1:2:0.6 and mill them for 4 hours. Pass the slurry through a 100-mesh sieve after aging for 36 hours. After the process, it is made into a blank.

Inner glaze raw materials: The weight percentage of the formula is composed of glaze fruit 69%, glaze ash 22%, and purple gold soil 9%. Weigh according to the above ratio, mix the raw materials evenly, put them into a ball mill with a material: ball: water ratio of 1:2:0.6, and after 2 hours of ball milling, the fineness of the glaze will reach the sieve residue of the million-hole sieve below 0.05%.

Outer glaze raw materials: formula weight percentage is composed of potassium feldspar 64%, quartz 10%, Longyan kaolin 6%, glaze ash 10%, purple gold clay 9.6%, industrial Fe ₂ O ₃ 0.4%. Weigh according to the above ratio, after mixing the raw materials evenly, put them into the ball mill with the material: ball: water ratio of 1:2:0.6, and after 24 hours of ball milling, the fineness of the glaze will reach the sieve residue of the ten-thousand-hole sieve below 0.05%. .

And place the billet in the pulp tank to make the pulp, make the ratio of material to water reach 1:0.7, and add 0.2% water glass and 0.05% sodium tripolyphosphate; injection mold the wet billet, then dry, repair Billet and biscuit firing process to complete billet making. Among them, biscuit firing is to put the celadon body after the trimming process into a bisque firing kiln and fire it for 7 hours, so that the temperature of the kiln gradually rises from normal temperature to 780 ° C, and after 10 to 20 minutes of heat preservation, the flame is turned off and naturally cooled. Then, after applying the inner glaze, the specific gravity of the inner glaze raw material is adjusted to a mixed solution with a Baume concentration of 55 degrees, and the biscuit-fired wine bottle is dedusted, and the mouth of the wine bottle is facing downward, and the inner glaze is applied by the pressure spray glaze method. Glaze, the thickness of the inner glaze layer is 0.1mm. After applying the outer glaze, the specific gravity of the outer glaze raw materials described in the Longquan celadon cracked glaze wine bottle is adjusted to a mixed solution with a Baume concentration of 44 degrees. Layer thickness to 0.5mm. Finally, after glaze firing, the celadon body that is glazed inside and outside is put into a high-temperature shuttle kiln atmosphere furnace and fired for 11 hours, so that the kiln temperature gradually rises from normal temperature to 1290°C, and after 45 minutes of heat preservation, the flame is turned off and naturally cooled to obtain Longquan celadon cracks. Finished glaze wine bottle.

Example 5:

What this embodiment provides is a kind of preparation method of Longquan celadon crack glaze wine bottle, and this preparation method comprises the following steps:

1) Mold making: According to the design requirements, make a gypsum mold of a celadon wine bottle with a finished product capacity of 1500ml, and make a gypsum mold, and dry it for 2 days.

2) Slurrying: place the billet in the pulping tank to make the slurry, so that the ratio of material to water reaches 1:0.6, and add 0.4% water glass and 0.02% sodium tripolyphosphate;

3) Blank making: inject the melted mud into the gypsum mold through the pressure pipe, pour out the excess mud after the thickness reaches 5mm-7mm, and take out the mud billet after the green body has a certain drying strength.

4) Drying: Put the mud base into the drying room for drying for 24 hours;

5) Blank trimming: hydrating the semi-dry mud blank, scraping the sutures, finishing;

6) Biscuit firing: put the trimmed celadon body into a biscuit firing kiln and fire it for 8 hours, so that the temperature of the kiln gradually rises from room temperature to 850°C, keep it warm for 20 minutes, turn off the flame and let it cool naturally, and you can get the Longquan celadon wine bottle plain. Blank;

7) Inner glaze application: adjust the specific gravity of the inner glaze raw materials to a mixed solution with a Baume concentration of 60 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle, with the mouth facing down, and apply the inner glaze with the pressure spray glaze method , the thickness of the glaze layer is 0.15mm;

8) Drying: put the glazed wine bottle body into the drying room for drying for 5 hours;

9) Exterior glaze application: the specific gravity of the exterior glaze raw materials is adjusted to a mixed solution with a Baume concentration of 45 degrees, and the base that has been applied with interior glaze is dedusted by a high-pressure air pump, and the exterior glaze is applied by the glaze dipping method, and the thickness of the glaze layer is 0.8 mm;

10) Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside;

11) Glaze firing: Put the celadon body glazed inside and outside into a high-temperature shuttle kiln atmosphere furnace and fire for 10.1 hours, so that the kiln temperature gradually rises from room temperature to 1285°C, keep the temperature for 60 minutes, turn off the flame and cool naturally to obtain the finished product.

The specific operation process in the step 11) includes: a. Preheating stage: firing at a heating rate of 2.5°C/min for 2 hours, so that the kiln temperature rises from normal temperature to 300°C, and removes residual moisture in the green body; b. Oxidation Stage: firing at a heating rate of 4°C/min for 2.7 hours to raise the kiln temperature to 950°C to remove crystal water, oxidize organic matter and sulfide, decompose carbonate, and transform quartz crystal form; c. Oxidation and heat preservation stage: make The kiln temperature is stabilized at 980°C and kept for 1 hour, which is helpful for the discharge of gas in the green body and inner and outer glazes; d. Strong reduction stage: firing at a heating rate of 1.5°C/min for 2.4 hours to raise the kiln temperature to 1200°C, And keep the kiln air pressure at 0.03Mpa, so that the ferric iron in the formula can be fully reduced to ferrous iron; e. Weak reduction stage: after another 1 hour, the kiln temperature will be raised to 1285°C, so that the glaze layer is fully mature, and the ferrous iron Fixed; f. High-fire heat preservation stage: control the kiln temperature at 1285°C, and stop the fire after heat preservation for 1 hour; g. Cooling stage: adopt natural cooling method, and leave the kiln after the kiln temperature is cooled to 50-70°C, and the firing is completed , that is, the finished product of Longquan celadon cracked glaze wine bottle. Not only the quality of the bottle fired by this method is good, but also the finished product rate is better.

Embodiment 6:

What this embodiment provides is a kind of preparation method of Longquan celadon crack glaze wine bottle, and this preparation method comprises the following steps:

1) Mold making: According to the design requirements, make a gypsum mold of a celadon wine bottle with a finished product capacity of 1500ml, and make a gypsum mold, and dry it for 1.5 days.

2) Slurrying: place the billet in the slurrying tank to make the slurry, so that the ratio of material to water reaches 1:0.5, and add 0.2% water glass and 0.03% sodium tripolyphosphate;

3) Blank making: inject the melted mud into the gypsum mold through the pressure pipe, pour out the excess mud after the thickness reaches 7mm, and take out the mud billet after the green body has a certain dry strength.

4) Drying: Put the mud base into the drying room for drying for 22 hours;

5) Blank trimming: hydrating the semi-dry mud blank, scraping the sutures, finishing;

6) Biscuit firing: put the trimmed celadon body into a biscuit kiln and fire it for 6 hours, so that the temperature of the kiln gradually rises from room temperature to 850°C, keep it warm for 18 minutes, turn off the flame and cool it naturally, and you can get the Longquan celadon wine bottle plain. Blank;

7) Applying the inner glaze: adjust the specific gravity of the inner glaze raw materials to a mixed solution with a Baume concentration of 57 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle, with the mouth facing down, and apply the inner glaze by using the pressure spray glaze method , the thickness of the glaze layer is 0.12mm;

8) Drying: put the glazed wine bottle body into the drying room for 3 hours;

9) Exterior glaze application: the specific gravity of the exterior glaze raw materials is adjusted to a mixed solution with a Baume concentration of 42 degrees, and the base that has been applied with interior glaze is dedusted by a high-pressure air pump, and the exterior glaze is applied by the glaze dipping method, and the thickness of the glaze layer is 0.6mm;

10) Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside;

11) Glaze firing: Put the celadon body glazed inside and outside into a high-temperature shuttle kiln atmosphere furnace and fire for 10.8 hours, so that the kiln temperature gradually rises from normal temperature to 1290°C, keep the temperature for 60 minutes, turn off the flame and cool naturally, and the finished product is obtained.

The specific operation process in the step 11) includes: a. Drying stage: firing at a heating rate of 3°C/min for 2.5 hours to make the kiln temperature rise to 440°C; b. Oxidation stage: firing at a heating rate of about 4°C/min The heating rate is fired for 2 hours to raise the kiln temperature to 977°C, so that the water vapor and oxidative decomposition gas products are fully volatilized, and the organic matter and sulfide are oxidized, the carbonate is decomposed, and the quartz crystal form is transformed; c. Holding stage: to stabilize the kiln temperature At 980°C, keep warm for 1.3 hours, which is helpful for the discharge of gas in the tire (i.e. green body) and glaze; d. Strong reduction stage: firing at a heating rate of 1.2°C/min for 3 hours to raise the kiln temperature to 1200°C, And keep the kiln air pressure at 0.04Mpa, so that the ferric iron in the formula can be fully reduced to ferrous iron; e. Weak reduction stage: after 2.5 hours, raise the kiln temperature to 1285°C, so that the glaze layer is fully mature, and the ferrous iron Fixed; f. heat preservation stage: control the kiln temperature at 1285 ℃, and stop the fire after 1 hour of heat preservation; g. cooling stage: adopt natural cooling method, and leave the kiln after the kiln temperature is cooled to 50 ℃, and the firing is completed, that is, the product Invented Longquan celadon crack glaze wine bottle. Not only the quality of the bottle fired by this method is good, but also the finished product rate is better.

Embodiment 7:

What this embodiment provides is a kind of preparation method of Longquan celadon crack glaze wine bottle, and this preparation method comprises the following steps:

1) Mold making: According to the design requirements, make a gypsum mold of a celadon wine bottle with a finished product capacity of 1500ml, and make a gypsum mold, and dry it for 1.5 days.

2) Slurrying: place the billet in the slurrying tank to make the slurry, so that the ratio of material to water reaches 1:0.4, and add 0.2% water glass and 0.04% sodium tripolyphosphate;

3) Blank making: inject the melted mud into the gypsum mold through the pressure pipe, pour out the excess mud after the thickness reaches 5mm-7mm, and take out the mud billet after the green body has a certain drying strength.

4) Drying: Put the mud base into a drying room for drying for 20 hours;

5) Blank trimming: watering and finishing the semi-dried mud blank;

6) Biscuit firing: Put the trimmed celadon body into a biscuit kiln and fire it for 6 hours, so that the temperature of the kiln gradually rises from room temperature to 800°C, keep it warm for 15 minutes, turn off the flame and cool it naturally, and you can get the plain celadon wine bottle of Longquan. Blank;

7) Inner glaze application: adjust the specific gravity of the inner glaze raw materials to a mixed solution with a Baume concentration of 52 degrees, and dedust the biscuit-fired wine bottle blank, with the mouth facing down, apply the inner glaze by the pressure spray glaze method, and the glaze layer The thickness is 0.11mm;

8) Drying: Put the glazed wine bottle body into the drying room for 4 hours;

9) Exterior glaze application: adjust the specific gravity of the exterior glaze raw materials to a mixed solution with a Baume concentration of 45 degrees, remove dust from the body that has been applied with the interior glaze, and apply the exterior glaze with the glaze dipping method, and the thickness of the glaze layer is 0.8mm;

10) Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside;

11) Glaze firing: Put the celadon body glazed inside and outside into a high-temperature shuttle kiln atmosphere furnace and fire it for 12 hours, so that the kiln temperature gradually rises from normal temperature to 1280 ° C, keep it warm for 45 minutes, turn off the flame and cool it naturally, and the finished product is obtained.

The specific operation process in the above step 11) includes: a. Drying stage: firing at a heating rate of 2.6°C/min for 2.8 hours to make the kiln temperature rise to 445°C; b. Oxidation stage: heating at a heating rate of about 4.2°C/min Fire at a speed of 2 hours to raise the kiln temperature to 980°C, so that the water vapor and oxidative decomposition gas products are fully volatilized, and organic matter and sulfide are oxidized, carbonate is decomposed, and the crystal form of quartz is transformed; c. Holding stage: the kiln temperature is stabilized at 983°C, heat preservation for 1.3 hours, which is helpful for the discharge of gas in the tire (i.e. green body) and glaze; d. Strong reduction stage: firing at a heating rate of 1.4°C/min for 3 hours to raise the kiln temperature to 1200°C, and Keep the kiln air pressure at 0.04Mpa to fully reduce the ferric iron in the formula to ferrous iron; e. Weak reduction stage: After 2.5 hours, raise the kiln temperature to 1285°C to fully mature the glaze layer and fix the ferrous iron; f. heat preservation stage: control the kiln temperature at 1280 ℃, and stop the fire after 1 hour of heat preservation; g. cooling stage: adopt natural cooling method, and leave the kiln after the kiln temperature is cooled to 68 ℃, and the firing is completed to obtain the kiln of the present invention. Finished Longquan celadon wine bottle with cracked glaze. Not only the quality of the bottle fired by this method is good, but also the finished product rate is better.

The green body and the inner glaze layer used in the above preparation method are prepared from ordinary mineral raw materials, while the outer glaze layer is prepared from ordinary mineral raw materials and a small amount of industrial chemical raw materials. The industrial Fe ₂ O ₃ is industrial chemical raw materials, not natural minerals.

Claims (7)

1. A Longquan celadon crackle glaze wine bottle, which adopts mineral raw materials to prepare blank and inner glaze, adopts mineral raw materials and adds industrial chemical raw materials to prepare outer glaze, is characterized in that: the proportioning of raw materials in its blank, inner glaze and outer glaze is respectively In terms of weight percentage, it is as follows: (i) Blank: 40-55% of Longyan kaolin, 15-25% of Longquan porcelain clay, 8-20% of potassium feldspar, 7-15% of quartz, and 5-10% of Zijin clay; the raw material components of the blank are 100% in total; (ii) Inner glaze: 65-75% of glaze fruit, 15-25% of glaze ash, 5-10% of purple gold soil; the total of the raw material components of the inner glaze is 100%; (iii) Outer glaze: potassium feldspar 60-70%, quartz 8-15%, Longyan kaolin 5-10%, glaze ash 8-15%, purple gold clay 5-13%, Fe ₂ O ₃ 0.2-0.4%; The raw material components of the outer glaze add up to 100%; And place the billet in the slurry tank to melt the slurry, so that the ratio of material to water reaches 1:0.5-0.7, and add 0.2-0.4% of water glass and 0.02-0.05% of sodium tripolyphosphate; the wet base is obtained by injection molding , After drying, billet trimming and biscuit firing processes, the billet making is completed; Then apply the inner glaze, that is, adjust the specific gravity of the inner glaze raw material to a mixed solution with a Baume concentration of 50-60 degrees, and dedust the biscuit-fired wine bottle, with the mouth of the wine bottle facing down, spray the inner glaze to form inner glaze layer; After applying the outer glaze, the specific gravity of the outer glaze raw materials described in the Longquan celadon cracked glaze wine bottle is adjusted to a mixed solution with a Baume concentration of 40-50 degrees. ; Finally, after glaze firing, the celadon body that is glazed inside and outside is put into a high-temperature shuttle kiln atmosphere furnace and fired for 9 to 11 hours, so that the temperature of the kiln gradually rises from normal temperature to 1280-1300°C, and the flame is turned off after 30-60 minutes of heat preservation. After cooling, the finished Longquan celadon crack glaze wine bottle is obtained. 2. A Longquan celadon cracked glaze wine bottle according to claim 1, characterized in that: said inner glaze is applied by pressure spray glaze method, and the thickness of the inner glaze layer is between 0.1-0.15 mm; The outer glaze is applied by the glaze dipping method, and the thickness of the outer glaze layer is between 0.5 and 1 mm. 3. A Longquan celadon cracked glaze wine bottle according to claim 2, characterized in that: the thermal expansion coefficient of the prepared outer glaze layer is 10～13×10 ^-6 /°C, and the thermal expansion coefficient of the inner glaze layer is 4～ 8×10 ^-6 /°C. 4. A Longquan celadon cracked glaze wine bottle according to claim 1, characterized in that: the biscuit firing is to put the celadon body after the trimming process into a biscuit firing kiln for firing for 5-7 hours, Make the kiln temperature gradually rise from normal temperature to 780-880°C, keep warm for 10-20 minutes, then turn off the flame and cool naturally. 5. a kind of preparation method of Longquan celadon crackle glaze wine bottle as claimed in claim 1, it is characterized in that: comprise the following steps: A. Mold making: Make plaster molds for wine bottles, and make plaster molds, and dry them for 1 to 2 days; B. Slurry: put the billet in the slurry tank to make the slurry, so that the ratio of material to water reaches 1:0.5-0.7, and add 0.2-0.4% water glass and 0.02-0.05% sodium tripolyphosphate; C. Blank making: inject the melted mud into the gypsum mold through the pressure grouting pipe, pour out the excess mud after the thickness reaches 5mm-7mm, and take out the mud billet after the green body has a certain dry strength; D. Drying: Put the mud into the drying room for 20-24 hours; E. Blank trimming: add water to the semi-dry mud blank, scrape the sutures, and fine-tune; F. Biscuit firing: Put the trimmed celadon body into a biscuit firing kiln and fire for 5-7 hours, so that the kiln temperature gradually rises from normal temperature to 780-880°C, keep it warm for 10-20 minutes, turn off the flame and cool naturally, that is Get Longquan celadon wine bottle biscuit; G. Apply inner glaze: adjust the specific gravity of the inner glaze of the Longquan celadon cracked glaze wine bottle to a mixture solution with a Baume concentration of 50-60 degrees, and use a high-pressure air pump to remove dust from the biscuit-fired wine bottle blank, with the mouth facing down, using The inner glaze is applied by the pressure spray glaze method, and the thickness of the inner glaze layer is 0.1-0.15mm; H. Drying: Put the glazed wine bottle body into the drying room for 3 to 5 hours; I. Applying the outer glaze: adjust the specific gravity of the outer glaze of the Longquan celadon cracked glaze wine bottle to a mixture solution with a Baume concentration of 40-50 degrees, use a high-pressure air pump to remove dust from the inner glazed blank, and apply the outer glaze by dipping method. The thickness of the outer glaze layer is 0.3-0.8mm; J. Scrape the bottom foot: scrape off the glaze on the bottom foot of the Longquan celadon cracked glaze wine bottle that has been glazed inside and outside; K. Glaze firing: put the celadon body with internal and external glazing into a high-temperature shuttle kiln atmosphere furnace and fire for 9-11 hours, so that the kiln temperature gradually rises from normal temperature to 1280-1300 °C, keep it warm for 30-60 minutes, turn off the flame and cool naturally , that is, the finished product is obtained. 6. A method for preparing a Longquan celadon wine bottle according to claim 5, characterized in that: the outer glaze raw material adopts common mineral raw materials and adds a small amount of industrial chemical raw materials; the thermal expansion coefficient of the outer glaze layer prepared is 10- 13×10 ^-6 /℃, and the thermal expansion coefficient of the inner glaze layer is 4～8×10 ^-6 /℃. 7. a kind of Longquan celadon wine bottle preparation method according to claim 5 is characterized in that: step K also comprises the following stages: a. Preheating stage: firing at a heating rate of 2.5-3°C/min for 2-2.5 hours to raise the kiln temperature from room temperature to 300-350°C and remove residual moisture in the green body; b. Oxidation stage: firing at a heating rate of 4-4.5°C/min for 2.5-2.8 hours to raise the kiln temperature to 950-980°C; c. Oxidation and heat preservation stage: keep the kiln temperature stable at 980-985°C, and keep heat for 1-1.2 hours; d. Strong reduction stage: firing at a heating rate of 1.5-2°C/min for 2-2.5 hours to raise the kiln temperature to 1200-1220°C and keep the kiln pressure at 0.03-0.04Mpa; e. Weak reduction stage: After another 1-1.5 hours, raise the kiln temperature to 1280-1300°C; f. High-fire heat preservation stage: control the kiln temperature at 1280-1300°C, and stop the fire after 0.5-1 hour of heat preservation; g. Cooling stage: adopt the natural cooling method, leave the kiln after the kiln temperature is cooled to 50-70°C, and the firing is completed, and the finished Longquan celadon cracked glaze wine bottle is obtained.