CN114276015B - Tea dust glaze based on yellow river mud and preparation method of tea dust glaze - Google Patents
Tea dust glaze based on yellow river mud and preparation method of tea dust glaze Download PDFInfo
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Abstract
The invention relates to the technical field of ceramic composite materials, in particular to a tea dust glaze based on yellow river mud and a preparation method of the tea dust glaze. The tea dust glaze based on the yellow river mud comprises the following glaze raw materials: kaolin, incense ash, iron powder, potassium feldspar, quartz and CaCO 3 、MgCO 3 . The glaze color controllability of the product is greatly improved, the firing condition is stable and reliable, the operation is simple, the operability is strong, the prepared glaze is fired at high temperature, the heavy metal toxicity is avoided, the edible standard can be achieved, the color stability is obviously improved, the aesthetic value, the aesthetic space and the yield of the tea dust glaze porcelain are essentially improved, and the functionality is increased.
Description
Technical Field
The invention relates to the technical field of ceramic composite materials, in particular to a tea dust glaze based on yellow river mud and a preparation method of the tea dust glaze.
Background
The tea dust glaze originates from Tang dynasty and still gives out vitality after being deposited for thousands of years. The appearance is accidental, and according to the examination, kiln workers burn tea dust glaze unintentionally due to overfiring of black enamel. However, in the face of the firing defect, ancient kiln workers in China have keenly found the charm of the kiln workers, and the special color glaze variety with very rich decoration is created by mastering the glaze formula and the firing technology through the diligence and wisdom of the kiln workers. The tea dust glaze belongs to matt glaze, has mild glaze surface, does not make noise or stretch, and gives people a strong warm and moist feeling like Chinese jade. The tea dust glaze is a microcrystalline color glaze taking iron element as a main crystallizing agent and a coloring agent, and has yellow-green doping glaze color, green thin spots called tea and yellow small spots called dust, is fresh and natural, and has a mysterious color, so that the tea dust glaze has extremely high artistic value and economic value. This artistic effect of giving a particular visual and psychological enjoyment is why it is still favored nowadays. Because the traditional tea dust glaze formula is required to be accurate and the process is difficult to control, an extremely high kiln firing curve system is required, and the kiln transformation can be generated due to unstable firing of the tea dust glaze and temperature and flame resistance, the glaze effect is difficult to control, the firing success rate is very low, and the yield is difficult to predict.
The chemical composition of the tea dust glaze is characterized by high iron content, high calcium content and high magnesium content, wherein the magnesium content is higher than 2%, and is generally 4% of the total weight of the glaze. In the preparation process, the main problem of the tea dust glaze is that factors influencing the crystallization of the crystallized glaze, such as high temperature, impurities, uneven thickness of the glaze layer, sintering and maximum sintering temperature, are difficult to control, and complicated adjustment of the formula and preparation of the tea dust glaze is required. The invention discloses a tea dust glaze prepared from iron tailings and a preparation method thereof, wherein the tea dust glaze comprises the following components in percentage by weight: 30-86% of iron tailings, 0-4% of spodumene, 2-6% of knots, 2-15% of calcite, 1-6% of dolomite, 2-20% of feldspar, 2-8% of zinc oxide, 1-6% of quartz, 3-8% of lithium porcelain stone, 0-8% of barium carbonate, 0-3% of Yixian county soil and 0-5% of Suzhou soil. However, in the examples of this patent, the glaze is mainly obtained by firing only in an oxidizing atmosphere, and the quality of the tea dust glaze is poor.
Along with the continuous development of the process, people try to change the formula and adopt other components to prepare the tea dust glaze, for example, patent application CN2015101432416 discloses a Ru porcelain tea dust glaze and a preparation process thereof, and the invention relates to 28-32 parts of white feldspar, 12-14 parts of calcite, 8-10 parts of quartz stone, 50-53 parts of Ru medicine, 1.0-1.5 parts of bone powder and 0.5-1.0 part of talcum powder in the tea dust glaze. However, the Ru medicine used in the patent is limited to the local kaolin of python and village in Ru of Henan province, so that the practicability of the invention is greatly limited.
Disclosure of Invention
The invention provides a tea dust glaze based on yellow river mud and a preparation method of the tea dust glaze, the prepared tea dust glaze has the advantages of greatly improved color controllability, stable and reliable firing conditions, simple operation, strong operability, high-temperature firing of the glaze, no heavy metal toxicity, capability of reaching the edible standard, obvious improvement of color stability, and particularly, the glaze surface shows wood She Xiaoguo, thereby essentially improving the aesthetic value, aesthetic space and yield of the tea dust glaze porcelain and increasing the functionality, and solving the problems in the prior art.
One of the technical schemes adopted by the invention is as follows:
a tea dust glaze based on yellow river mud comprises the following glaze raw materials in parts by weight:
10-13% of kaolin, 9-10% of incense ash, 9-10% of iron powder, 38-40% of potassium feldspar, 8-10% of quartz and CaCO 3 13％-15％、MgCO 3 7％-9％。
Further, the tea dust glaze comprises the following glaze raw materials in parts by weight:
12% of kaolin, 10% of incense ash, 10% of iron powder, 39% of potassium feldspar, 9% of quartz and CaCO 3 12％、MgCO 3 8％。
The second technical scheme adopted by the invention is as follows:
the preparation method of the tea dust glaze with the tea dust glaze comprises the steps of performing low-temperature biscuit firing on pug with high iron content, and performing high-temperature firing by decoration spraying tea dust glaze with certain thickness;
the tea dust glaze comprises the following glaze raw materials in parts by weight:
10-13% of kaolin, 9-10% of incense ash, 9-10% of iron powder, 38-40% of potassium feldspar, 8-10% of quartz and CaCO 3 13％-15％、MgCO 3 7％-9％。
Further, the low temperature bisque firing temperature is 850 ℃, and the high temperature firing temperature is 1230-1260 ℃.
Further, the preparation method of the tea dust glaze further comprises the step of ball milling treatment before low-temperature bisque firing to obtain the tea dust glaze, wherein the ball milling treatment period is 25-35min.
Further, the high-temperature firing adopts a gas kiln for firing, and the internal atmosphere of the kiln is a reducing atmosphere; or the high-temperature firing adopts electric kiln firing, and the internal atmosphere of the kiln is an oxidizing atmosphere.
Further, the mud material with high iron content has a mud blank thickness of 2-3mm, and the tea dust glaze has a thickness of 1.5-2.0mm.
Further, the mud material with high iron content is yellow river mud material, long Quantie green mud material, cinnabar green mud material or purple clay mud material.
Further, the gas kiln is adopted for firing, the internal atmosphere of the kiln is a reducing atmosphere, and the operation steps comprise:
a. preheating a gasification furnace in advance;
b. and (3) a free water draining stage: opening the flashboard, firing, and completely opening the valve of the gas tank; proper pressure is given to fire guns, the pressure is 0.01, and two fire guns are symmetrically arranged; when the gun is ignited, the air valve is closed, and the air valve is regulated after ignition; controlling the air valve to adjust the blue backing flame, wherein the flame is in a jump shape instead of a straight line rising shape; after the flame is regulated, the pressure is regulated to 0.001-0.002Pa, and the temperature is controlled to be about 1 degree in 20 seconds; gun 2 are added at 200 degrees (the gun is pressurized before being added); adding more than 400 guns for 2, and keeping for 10-10 seconds and 1 degree;
c. and (3) structural water drainage stage: determining whether the free water is discharged (about 550 ℃ or more) according to the humidity of the fire observation hole, closing the door, pressurizing to 0.01, and adjusting the blue flame by a gun through an air brake;
d. and (3) heat preservation: 102, reversing the cone, entering a heat preservation stage, closing an adjusting flashboard, and keeping for 3-4 minutes at 1 degree through decompression; preserving the heat for 30-40 minutes;
e. and (3) heating: the flashboard is fully closed, pressurized by more than 0.02; adjusting the blue backing flame through an air valve; maintaining for 1 min at 1-2 deg.C; tempering easily occurs at this stage, and the problem that the firing effect is affected if the tempering is needed within 1 minute is solved;
f. when the temperature is 1100 ℃ or more, the temperature is noted whether to rise stably, and if the temperature rises slowly after pressurization, a gate is required to be opened; about 1200 degrees, observe 131 and Wen Zhui, stop fire when the awl is poured, and close the gas tank valve.
Further, an electric kiln is adopted for firing, and the kiln atmosphere is an oxidizing atmosphere. The components of the tea dust glaze in the preparation method are suitable for two atmospheres of an electric kiln and a gas kiln.
The invention has the beneficial effects that:
the tea dust glaze with the wood leaf effect is obtained accidentally in the process of burning glaze, on the basis of obvious formula difference with the existing tea dust glaze, the mud with high iron content is adopted, and the specific burning method and the specific burning condition are matched, so that the tea dust glaze with the wood leaf is obtained, the glaze color controllability is greatly improved, the burning condition is stable and reliable, the operation is simple, the operability is strong, the prepared glaze is burnt at high temperature, the heavy metal toxicity is avoided, the color stability is obviously improved, and the aesthetic value, the aesthetic space and the yield of the tea dust glaze porcelain are essentially improved, and the functionality is increased. The tea dust glaze prepared by the invention has new breakthroughs from the aspects of edible safety and aesthetic value.
Drawings
FIG. 1 is a graph of the temperature rise during kiln firing according to the present invention;
FIG. 2 is a graph showing the effect of the tea dust glaze in example 1 of the present invention;
FIG. 3 is a graph showing the effect of the tea dust glaze in example 2 of the present invention;
fig. 4 is a graph showing the effect of the tea dust glaze in example 3 of the present invention;
fig. 5 is a graph showing the effect of the tea dust glaze in example 4 of the present invention;
FIG. 6 is a graph showing the effect of the tea dust glaze in example 5 of the present invention;
FIG. 7 is a graph showing the effect of the tea dust glaze in example 6 of the present invention;
FIG. 8 is a graph showing the effect of the tea dust glaze in example 7 of the present invention;
fig. 9 is a graph showing the effect of the tea dust glaze in example 8 of the present invention.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
The tea dust glaze based on the yellow river mud comprises the following glaze raw materials in parts by weight:
12% of kaolin, 10% of incense ash, 10% of iron powder, 39% of potassium feldspar, 9% of quartz and CaCO 3 12％、MgCO 3 8%. The method for manufacturing the tea dust glaze by adopting the tea dust glaze based on the yellow river mud comprises the following operation steps:
(1) In a ball mill, putting the components of the tea dust glaze and water into the ball mill for ball milling according to the weight ratio of 1:0.7; the balls in the ball milling tank cannot exceed half of the volume of the tank, the ball milling time is about 30min, and the ball milling particles can pass through a screen with 120 meshes to obtain tea dust glaze; standby;
(2) Selecting yellow river mud, preparing mud blank with thickness of 2-3mm, performing biscuit firing at 850 ℃, and spraying tea dust glaze with thickness of 1-2mm on the local decoration of glaze tyre;
(3) And (3) placing the glaze tyre prepared in the step (2) on the upper layer of a kiln, and firing the glaze tyre by using a gas kiln at a high temperature of 1260 ℃.
The internal atmosphere of the kiln fired by the gas kiln is a reducing atmosphere, and the specific operation steps are as follows:
a, preheating a gasification furnace in advance for half an hour;
b stage of draining free water: the flashboard is opened, the fire is started, and the valve of the gas tank is completely opened. Proper pressure is given to fire guns, the pressure is about 0.01, the fire guns with too small pressure can be extinguished, and the two fire guns are symmetrically ignited; when the gun is ignited, the air valve is closed firstly, and then the air valve is regulated after ignition; the control air valve regulates the blue backing flame, and the flame is in a jump shape instead of a straight rising shape. After the flame is adjusted, the pressure is adjusted to about 0.001-0.002Pa, and the temperature is controlled to about 1 degree (3-4 degrees for 1 minute) for about 20 seconds; gun 2 are added at about 200 degrees or more (the gun is pressurized before being added); adding more than 400 guns for 2, and keeping for 10-10 seconds and more than 1 degree;
c, structural water stage: determining whether the free water is discharged (about 550 ℃ or more) according to the humidity of the fire observation holes, closing the door, pressurizing to about 0.01, and adjusting full blue flame by opening a damper when the gun is added (the rest);
d, heat preservation: 102, reversing the cone, entering a heat preservation stage, closing an adjusting flashboard, and keeping for 3-4 minutes at 1 degree (more than 2 minutes and 1 degree) through decompression; preserving the heat for 30-40 minutes;
and e, heating: the flashboard is fully closed, pressurized to be more than about 0.02; adjusting the blue backing flame through an air valve; maintaining for 1 min at 1-2 deg.C; tempering easily occurs at this stage, and the problem that the firing effect is affected if the tempering is needed within 1 minute is solved;
if the temperature rises slowly after pressurization, a gate needs to be opened; about 1200 degrees, observe 131 Wen Zhui, stop fire when the awl is tipped over, close the gas canister valve.
The firing temperature-time curve is shown in FIG. 1.
In the firing process, attention is paid to whether the internal pressure of the kiln is normal or not, when the kiln door is closed (about 500), the normal condition is micro negative pressure, the kiln door is closed to 1020 degrees and micro negative pressure is also generated (when a flame is tried from a flame viewing port by a flame gun, the flame can go into the kiln), the heat preservation stage (after the cone of 102 is inverted and before strong reduction), the pressure is flat, the strong reduction is carried out in the firing kiln, and flame ejection (positive pressure, flat pressure and negative pressure are all the pressure in the kiln) is carried out in the flame viewing hole.
Example 2 (the amounts of the components used are the same as in example 1, firing temperature was varied in the preparation method)
The tea dust glaze is the same as the tea dust glaze of the example 1, and the preparation method comprises the following operation steps:
(1) In a ball mill, putting the components of the tea dust glaze and water into the ball mill for ball milling according to the weight ratio of 1:0.7; the balls in the ball milling tank cannot exceed half of the volume of the tank, the ball milling time is about 30min, and the ball milling particles can pass through a screen with 120 meshes to obtain tea dust glaze; standby;
(2) Selecting purple clay pug, preparing a mud blank with the thickness of 2-3mm, performing biscuit firing at the low temperature of 850 ℃, and spraying tea dust glaze with the thickness of 1-2mm on the local decoration of a glaze blank;
(3) And (3) placing the glaze embryo prepared in the step (2) on the upper layer of a kiln, firing by using a gas kiln, and firing at a high temperature of 1280 ℃.
The firing operation in the gas kiln was the same as that in example 1.
Example 3
The tea dust glaze comprises the following glaze raw materials in parts by weight:
11% of kaolin, 9% of incense ash, 10% of iron powder, 38% of potassium feldspar, 9% of quartz and CaCO 3 15％、MgCO 3 8％。
The method for manufacturing the tea dust glaze by using the tea dust glaze and the firing method are the same as those of the preparation method and the firing method of the embodiment 1, except that the mud material is Longquan mud material.
Example 4
The tea dust glaze comprises the following glaze raw materials in parts by weight:
12% of kaolin, 10% of incense ash, 9% of iron powder, 38% of potassium feldspar, 8% of quartz and CaCO 3 14％、MgCO 3 9％。
The method for manufacturing the tea dust glaze by using the tea dust glaze and the firing method are the same as the preparation method and the firing method of the example 1.
Example 5 (MgCO) 3 The amounts used were below the minimum amounts and the amounts of the other ingredients were the same as in example 1)
The tea dust glaze comprises the following glaze raw materials in parts by weight:
12% of kaolin, 10% of incense ash, 10% of iron powder, 39% of potassium feldspar, 9% of quartz and CaCO 3 15％、MgCO 3 5％。
The method for manufacturing the tea dust glaze by using the tea dust glaze and the firing method are the same as the preparation method and the firing method of the example 1.
Example 6 (MgCO) 3 The amount is higher than the highest amount
The tea dust glaze comprises the following glaze raw materials in parts by weight:
10% of kaolin, 10% of incense ash, 10% of iron powder, 38% of potassium feldspar, 9% of quartz and CaCO 3 13％、MgCO 3 10％。
The method for manufacturing the tea dust glaze by using the tea dust glaze and the firing method are the same as the preparation method and the firing method of the example 1.
Example 7 (MgCO) 3 The amount is higher than in example 6
The tea dust glaze comprises the following glaze raw materials in parts by weight:
11% of kaolin, 9% of incense ash, 9% of iron powder, 39% of potassium feldspar, 8% of quartz and CaCO 3 12％、MgCO 3 12％。
The method for manufacturing the tea dust glaze by using the tea dust glaze and the firing method are the same as the preparation method and the firing method of the example 1.
Example 8 (MgCO) 3 The recommended usage of the traditional tea dust glaze firing is adopted
The tea dust glaze comprises the following glaze raw materials in parts by weight:
13% of kaolin, 10% of incense ash, 9% of iron powder, 40% of potassium feldspar, 9% of quartz and CaCO 3 15％、MgCO 3 4％。
The method for manufacturing the tea dust glaze by using the tea dust glaze and the firing method are the same as the preparation method and the firing method of the example 1.
The glaze effect experiment is tested as follows:
1. ball-milling glaze and test piece test
The gram weights of the raw materials are accurately weighed according to 1: specific gravity of 0.7 the ingredients and water were put into a ball mill for ball milling. The balls in the ball milling tank can not exceed half of the volume of the tank, the ball milling time is about 25-2100min, and the ball milling particles can pass through a screen with 120 meshes.
Three groups of test pieces are manufactured by using the glaze material of the embodiment 1 of the invention and are respectively placed on different positions of the upper layer, the middle layer and the lower layer of the kiln so as to observe whether the color development of the glaze material has stability and the position with the best firing effect. The glazing thickness of each test piece is divided into thin and thick, and only the upper half part of the test piece is glazed, so that the color development and the flowing property of the glaze with different thicknesses can be conveniently observed. The notches with different depths are carved on each test piece by a tool so as to observe the effect of the deposited glaze with different layering degrees.
2. Compared with low-temperature metal glaze, the safety performance detection of the tea dust glaze prepared by the invention
Glaze treatment temperature: 850 ℃ and 1260 DEG C
Sample: 200g of low-temperature metal glaze alpha and 200g of tea dust glaze are melted and ball-milled into powder.
a (low temperature metal glaze before lead precipitation), b (low temperature metal glaze after lead precipitation), c (tea powder glaze of the invention of example 1 before lead precipitation), d (tea powder glaze of the invention of example 1 after lead precipitation), e (tea powder glaze of the invention of example 3 before lead precipitation), f (tea powder glaze of the invention of example 3 after lead precipitation), g (tea powder glaze of the invention of example 4 before lead precipitation), h (tea powder glaze of the invention of example 4 after lead precipitation).
The device comprises: ball mill, scanning electron microscope (philips, netherlands), energy spectrometer (idax, usa);
the results of the detection are shown in tables 1 and 2 below.
TABLE 1 comparison of lead precipitation from Low temperature Metal glaze samples
| Name of the name | Pb |
| a | 65.6 |
| b | 71.1 |
TABLE 2 comparison of lead precipitation from tea dust glaze samples of the invention
| Name of the name | Pb |
| c | 0 |
| d | 0 |
| e | 0 |
| f | 0 |
| g | 0 |
| h | 0 |
The detection result shows that the tea dust glaze prepared by the invention can be fired at high temperature to ensure that no lead element is harmful to the health of a user. It is evident from Table 1 that the glaze material a itself before lead precipitation contains very high lead, and the lead content becomes higher after the treatment.
3. Influence of kiln position on the glaze effect of the tea dust glaze of the invention
Kiln: electric kiln
Test piece: six groups of test pieces, 3 pieces each
TABLE 3 tea dust glaze effect
From the results of table 3 above, it can be seen that by comparing the firing effects at different kiln positions, the firing effect is better at the position closer to the kiln wire, and the coloring effect is better when the kiln is placed on the upper layer of the kiln than when the kiln is placed on the lower layer.
4. The tea powder glaze product of the invention is compared with the traditional tea powder glaze
Kiln: electric kiln
Kiln temperature: 1260 DEG C
Test piece: seven groups of 20 pieces each
Numbering: inventive example 1 product A, conventional tea dust glaze B, inventive example 3 product C, inventive example 4 product D
TABLE 4 comparison of inventive product with conventional tea dust glaze
As shown in the results of the firing experiment IV in Table 4, compared with the traditional tea dust glaze, the novel tea dust glaze provided by the invention has the advantages of stable glaze color, high edible safety and high yield.
5. Different MgCOs in examples 3 Glazed character of tea dust glaze product
TABLE 5
As is clear from Table 5, mgCO in the tea dust glaze of the present invention 3 The content of (2) plays an important role in the glaze characteristics of the tea dust glaze and is shown in MgCO 3 When the content of (C) is changed, the same preparation method and firing process have obvious appearance differences of color development, crystal density, luster and the like of the glaze effect. Along with MgCO 3 The content of (2) exceeds 9%, the appearance is reduced, and the composition is prepared in MgCO 3 The content is increased to 12%, and compared with 10%, the glaze surface characteristic effect is poorer. If the prior tea dust glaze with the magnesium content of 4 percent is adopted for the invention, the glazeThe complexion is biased to green brown, and the rare and local crystals are not seen. In addition, the firing temperature also has a certain influence on the glaze effect, and the glaze of example 2 declines after the firing temperature exceeds 1260 ℃.
The above embodiments are not to be taken as limiting the scope of the invention, and any alternatives or modifications to the embodiments of the invention will be apparent to those skilled in the art and fall within the scope of the invention.
The present invention is not described in detail in the present application, and is well known to those skilled in the art.
Claims (4)
1. A preparation method of tea dust glaze is characterized by comprising the steps of performing low-temperature biscuit firing at 850 ℃ on yellow river mud material, performing decoration spraying tea dust glaze with certain thickness, and performing high-temperature firing at 1260 ℃;
the raw materials of the tea dust glaze comprise the following components in parts by weight:
10-13% of kaolin, 9-10% of incense ash, 9-10% of iron powder, 38-40% of potassium feldspar, 8-10% of quartz and CaCO 3 13％-15％、MgCO 3 7％-9％。
2. The method for preparing tea dust glaze according to claim 1, further comprising the step of ball milling the tea dust glaze before low-temperature biscuit firing, wherein the ball milling period is 25-35min.
3. The method for preparing tea dust glaze according to claim 1 or 2, wherein the high-temperature firing adopts a gas kiln firing, and the atmosphere inside the kiln is a reducing atmosphere; or the high-temperature firing adopts electric kiln firing, and the internal atmosphere of the kiln is an oxidizing atmosphere.
4. The method for preparing the tea dust glaze according to claim 1, wherein the yellow river mud is mud blank with the thickness of 2-3mm, and the thickness of the tea dust glaze is 1.5-2.0mm.
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| CN116003103A (en) * | 2022-12-19 | 2023-04-25 | 齐鲁工业大学 | High-temperature ceramic material based on yellow river mud and preparation method and application thereof |
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| CN111320458A (en) * | 2020-03-02 | 2020-06-23 | 福建省德化县昱晟工艺品有限责任公司 | Preparation method of tea dust glaze light porcelain |
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