CN108358604B - Manufacturing method of colored nixing pottery - Google Patents

Manufacturing method of colored nixing pottery Download PDF

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CN108358604B
CN108358604B CN201810272234.XA CN201810272234A CN108358604B CN 108358604 B CN108358604 B CN 108358604B CN 201810272234 A CN201810272234 A CN 201810272234A CN 108358604 B CN108358604 B CN 108358604B
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nixing pottery
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曾谊
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Guangxi Qinzhou City Pinyitang Nixing Ceramics Co ltd
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Guangxi Qinzhou City Pinyitang Nixing Ceramics Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
    • C04B33/13Compounding ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00Clay-wares
    • C04B33/32Burning methods
    • C04B33/34Burning methods combined with glazing
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5036Ferrites
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The invention discloses a manufacturing method of a colored nixing pottery, which comprises the following steps: 1) reacting ZnCl2、FeCl3Dissolving with deionized water to prepare a metal salt solution; 2) weighing (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution; 3) slowly adding a metal salt solution into the ammonium oxalate solution, and uniformly mixing to obtain yellow precipitate; 4) washing the yellow precipitate with water, drying, mixing with ruthenium dioxide with the weight of 0.01-0.05% of the weight of the dried yellow precipitate, and calcining at the temperature of 400-500 ℃ under 500-800 MPa to obtain yellow powder; 5) diluting the yellow powder, and then drawing and decorating the nixing pottery blank; 6) and drying the decorated blank, and then feeding the blank into a kiln for firing to obtain the color nixing pottery. The zinc ferrite yellow used in the invention has the advantages of pure and uniform color and luster after being modified, and can resist being fired at 1200 ℃ without color change.

Description

Manufacturing method of colored nixing pottery
Technical Field
The invention belongs to a manufacturing method of nixing ceramics, and particularly relates to a manufacturing method of colored nixing ceramics.
Background
The Qinzhou nixing pottery, Jiangsu Yixing purple clay pottery, Yunnan Jianshui pottery, Sichuan Rongchang pottery famous-column of the four major pottery in China, the reputations of China. In the history of the examination of nixing pottery, no exact name exists in the middle leaf period of Qing dynasty, until Qing dynasty, Xinzhou pottery develops a great deal, and the nixing ware is widely used, so the name of nixing is obtained. Nixing pottery products are various in types, fine in manufacture and long in history, are elegant artware, have high practical value and are deeply popular with collectors at home and abroad. The preparation process of the traditional Qinzhou nixing pottery mainly comprises the following steps: 1) preparing a blank: the blank is made of pottery clay material, and the unique east and west mud of Qinzhou local is selected as raw material. The east clay is clay traversing east region of Qinjiang in Qinzhou city, mostly exists in low-lying region, is dense and soft, is soft clay, is yellow-white in color, and contains trace quartz sand. The west mud is soil traversing the west region of the Qinjiang city in Qinzhou, the storage land is mainly a hillside, the soil is compact block-shaped, contains a small amount of K2O, Na2O, CaO, MgO, Fe2O3, TiO2, SiO2 and MnO2, is purple mud stone with high iron content, is purple red in color, has a small amount of iron on the surface layer, is hard clay, and has poorer plasticity and binding property than east mud. Mixing 40-60% of east mud and 60-40% of west mud by weight percent, and carrying out the existing and commonly used blank preparation method of nixing ceramics: making into blank by plastic method and slip casting method; 2) molding: making various blank bodies of different shapes from the blank; 3) trimming: trimming the blank body to meet the design requirement; 4) drying the blank: drying the green body to discharge the moisture of the green body; for example, by room drying, air drying, sun drying or other currently available and feasible drying methods; 5) decorating the green body: the nixing pottery is not added with any pigment, glazed or painted with any coloring material to draw colors and patterns on the blank during the manufacturing process, the nixing pottery is made to have unpredictable and uncontrollable colors only by means of occasional kiln changes, and the blank is decorated by using an engraving process. The carving process uses a sharp steel knife to carve characters and patterns on a blank body, and generally adopts a plain carving process and a relief carving process. The flat carving is carried out on a semi-dry and slightly wet clay blank by techniques such as line carving, engraving, sculpture, inlaying and the like. The embossing is carried out on a fully dried blank, and techniques such as high embossing, low embossing and the like are provided. In order to more clearly highlight the decorative pattern, white mud can be filled in the carved pattern, the white mud is slightly faint yellow after being fired and has the same warm tone with the pottery color, the clay pottery has the effect of gold tracing in a distant view, and the overall tone of the nixing pottery can be improved. 6) Firing: firing the decorated green body in a kiln; in order to achieve higher firing rate and improve kiln rate, the highest firing temperature of the green body is controlled to be 1100-1200 ℃, the firing time is 10 hours, and the nixing pottery is obtained after the firing and the discharging from the kiln.
The zinc ferrite yellow is heat-resistant iron yellow, has stable chemical properties and good pigment characteristics, but the pigment is easy to turn red, even blacken and darken at the temperature of over 500 ℃, and the blank body of the nixing pottery is brownish red, so that the coloring capability is lost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for manufacturing a color nixing pottery, which can solve the problem that the firing temperatures of the nixing pottery and zinc ferrite yellow are inconsistent, and the fired color nixing pottery is bright and beautiful in color.
The technical scheme provided by the invention is a manufacturing method of a color nixing pottery, which is characterized by comprising the following steps: the method comprises the following steps:
1) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+Concentration of0.15 to 0.3mol/L, Fe3+The concentration is 0.3-0.8 mol/L, and a metal salt solution is prepared;
2) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
3) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 60-70 ℃, and reacting for 3-5 hours to obtain yellow precipitate;
4) washing the yellow precipitate with water, drying, mixing with ruthenium dioxide with the weight of 0.01-0.05% of the weight of the dried yellow precipitate, and calcining at the temperature of 400-500 ℃ under 500-800 MPa to obtain yellow powder;
5) diluting the yellow powder, and then drawing and decorating the nixing pottery blank;
6) and drying the decorated blank, and then feeding the blank into a kiln for firing to obtain the color nixing pottery.
In the step 3), the temperature of the mixed solution is adjusted to 60-65 ℃.
In the step 4), the yellow precipitate is dried for 10-12 hours at 120-150 ℃.
In the step 4), the calcination time is 0.1-0.3 h.
In the step 6), the firing temperature is 1100-1200 ℃, and the firing time is 8-12 h.
Ruthenium is a strong compatible element of zinc ferrite spinel under the oxidation condition, therefore, under the conditions of high temperature and high pressure, ruthenium can enter the zinc ferrite crystal lattice to form a strong ionic bond with 0 atom, the vacancy in the zinc ferrite crystal lattice is filled, the zinc ferrite crystal structure is promoted to be more saturated, the existence of Ru-O can balance the Zn-O, Fe-O, Zn-O electrostatic bond strength, the thermal shock stability, the chemical erosion resistance and the wear resistance of the crystal are greatly improved on the premise that the zinc ferrite crystal lattice is not changed, the zinc ferrite yellow can resist the high-temperature roasting at 1200 ℃ and is not discolored or darkened, the long-time coloring effect is good, and the color is not easy to fade.
Moreover, the addition of ruthenium dioxide is also helpful to promote zinc oxide to replace water in the crystal lattice of iron oxide yellow to form zinc ferrite, thereby greatly improving the growth of zinc ferrite crystals, shortening the calcination time and saving energy.
Detailed Description
The following specific examples further illustrate the invention but are not intended to limit the invention thereto.
Example 1
1) Mixing Dong mud and West mud according to the weight ratio of 6: 4, mixing, preparing a blank by a conventional method, and drying for later use;
2) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+Concentration of 0.15mol/L, Fe3+The concentration is 0.3mol/L, and the metal salt solution is prepared;
3) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
4) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 60 ℃, and reacting for 3 hours to obtain yellow precipitate;
5) washing yellow precipitate with water, drying at 120 deg.C for 10 hr, mixing with ruthenium dioxide 0.01 wt% of the yellow precipitate, and calcining at 400 deg.C under 500MPa for 0.1 hr to obtain yellow powder;
6) diluting the yellow powder, and then drawing and decorating on the green body;
7) and drying the decorated blank, then feeding the dried blank into a kiln, firing the blank at 1100 ℃ for 8h, cooling the blank, and taking the blank out of the kiln to obtain the color nixing pottery. The decorative area of the blank body is bright yellow through visual observation.
Example 2
1) Mixing Dong mud and West mud according to the weight ratio of 6: 4, mixing, preparing a blank by a conventional method, and drying for later use;
2) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+Concentration of 0.3mol/L, Fe3+The concentration is 0.8mol/L, and the metal salt solution is prepared;
3) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
4) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 70 ℃, and reacting for 5 hours to obtain yellow precipitate;
5) washing the yellow precipitate with water, drying at 150 deg.C for 12h, mixing with ruthenium dioxide 0.05% of the weight of the yellow precipitate, and calcining at 500 deg.C under 800MPa for 0.3h to obtain yellow powder;
6) diluting the yellow powder, and then drawing and decorating on the green body;
7) and drying the decorated green body, then feeding the dried green body into a kiln, firing the dried green body for 12 hours at 1200 ℃, cooling, and taking the green body out of the kiln to obtain the color nixing pottery. The decorative area of the blank body is bright yellow through visual observation.
Example 3
1) Mixing Dong mud and West mud according to the weight ratio of 6: 4, mixing, preparing a blank by a conventional method, and drying for later use;
2) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+Concentration of 0.2mol/L, Fe3+The concentration is 0.6mol/L, and the metal salt solution is prepared;
3) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
4) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 65 ℃, and reacting for 4 hours to obtain yellow precipitate;
5) washing the yellow precipitate with water, drying at 140 deg.C for 11h, mixing with ruthenium dioxide 0.03% of the weight of the yellow precipitate, and calcining at 600MPa and 450 deg.C for 0.2h to obtain yellow powder;
6) diluting the yellow powder, and then drawing and decorating on the green body;
7) and drying the decorated blank, then feeding the dried blank into a kiln, firing the blank at 1150 ℃ for 10h, cooling and taking the blank out of the kiln to obtain the color nixing pottery. The decorative area of the blank body is bright yellow through visual observation.
Example 4
1) Mixing Dong mud and West mud according to the weight ratio of 6: 4, mixing, preparing a blank by a conventional method, and drying for later use;
2) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+Concentration of 0.15mol/L, Fe3+The concentration is 0.8mol/L, and the metal salt solution is prepared;
3) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
4) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 60 ℃, and reacting for 5 hours to obtain yellow precipitate;
5) washing yellow precipitate with water, drying at 120 deg.C for 12 hr, mixing with ruthenium dioxide 0.01 wt% of the yellow precipitate, and calcining at 400 deg.C under 800MPa for 0.3 hr to obtain yellow powder;
6) diluting the yellow powder, and then drawing and decorating on the green body;
7) and drying the decorated blank, then feeding the dried blank into a kiln, firing the blank at 1100 ℃ for 12h, cooling the blank, and taking the blank out of the kiln to obtain the color nixing pottery. The decorative area of the blank body is bright yellow through visual observation.
Comparative example 1
1) Mixing Dong mud and West mud according to the weight ratio of 6: 4, mixing, preparing a blank by a conventional method, and drying for later use;
2) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+Concentration of 0.15mol/L, Fe3+The concentration is 0.3mol/L, and the metal salt solution is prepared;
3) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
4) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 60 ℃, and reacting for 3 hours to obtain yellow precipitate;
5) washing the yellow precipitate with water, drying at 120 deg.C for 10h, and calcining at 500MPa and 400 deg.C for 2h to obtain yellow powder;
6) diluting the yellow powder, and then drawing and decorating on the green body;
7) and drying the decorated blank, then feeding the dried blank into a kiln, firing the blank at 1100 ℃ for 8h, cooling the blank, and taking the blank out of the kiln to obtain the color nixing pottery. And through visual observation, the color of the decorative area of the blank is dark and black, and is integrated with the color of the blank, so that decorative traces can not be seen.

Claims (5)

1. The manufacturing method of the color nixing pottery is characterized by comprising the following steps: the method comprises the following steps:
1) reacting ZnCl2、FeCl3Dissolving with deionized water to regulate Zn2+A concentration of 0.15 to 0.3mol/L, Fe3+The concentration is 0.3-0.8 mol/L, and a metal salt solution is prepared;
2) according to C2O4 2-The molar ratio of the metal ions to the metal ions is 1:1 (NH)4)2C2O4·H2Adding deionized water to dissolve to obtain an ammonium oxalate solution;
3) slowly adding a metal salt solution into the ammonium oxalate solution, uniformly mixing, adjusting the temperature of the mixed solution to 60-70 ℃, and reacting for 3-5 hours to obtain yellow precipitate;
4) washing the yellow precipitate with water, drying, mixing with ruthenium dioxide with the weight of 0.01-0.05% of the weight of the dried yellow precipitate, and calcining at the temperature of 400-500 ℃ under 500-800 MPa to obtain yellow powder;
5) diluting the yellow powder, and then drawing and decorating the nixing pottery blank;
6) and drying the decorated blank, and then feeding the blank into a kiln for firing to obtain the color nixing pottery.
2. The manufacturing method of the colored nixing pottery according to claim 1, characterized in that: in the step 3), the temperature of the mixed solution is adjusted to 60-65 ℃.
3. The manufacturing method of the colored nixing pottery according to claim 1, characterized in that: in the step 4), the drying is to dry the yellow precipitate at 120-150 ℃ for 10-12 h.
4. The manufacturing method of the colored nixing pottery according to claim 1, characterized in that: in the step 4), the calcination time is 0.1-0.3 h.
5. The manufacturing method of the colored nixing pottery according to claim 1, characterized in that: in the step 6), the firing temperature is 1100-1200 ℃, and the firing time is 8-12 h.
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CN101555131A (en) * 2008-04-07 2009-10-14 山东理工大学 Preparation method of zinc ferrite desulfurization porous ceramic
CN104787803A (en) * 2015-04-04 2015-07-22 天津大学 Method for preparing nano-sized zinc ferrite from zinc-contained steel pickling waste liquid
CN106745302A (en) * 2017-02-27 2017-05-31 陕西科技大学 A kind of coralloid zinc ferrite powder of three-dimensional network and preparation method thereof

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