A black-based blue-spotted glaze with earthworm-like patterns and its preparation method

By using specific raw material formulas and process steps, a black-based blue-spotted glaze with earthworm-like patterns was prepared, solving the problem of insufficient mechanical properties of glazes in existing technologies and achieving a high yield and improved artistic decorative effect.

CN118271119BActive Publication Date: 2026-05-26SHAANXI UNIV OF SCI & TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
SHAANXI UNIV OF SCI & TECH
Filing Date
2024-04-03
Publication Date
2026-05-26

AI Technical Summary

Technical Problem

There are no reports in the existing technology on black-based blue-spotted glazes with earthworm-like patterns and their preparation methods, and the existing glazes are insufficient in terms of mechanical properties and artistic decorative effect.

Method used

Using specific raw material formulas and process steps, including a combination of black base glaze and blue speckled glaze, the worm-like texture is formed through wet ball milling, bisque firing, glazing, and oxidation-reduction firing. Components such as calcium borate, barium carbonate, and talc are added to improve the transparency, wear resistance, and mechanical properties of the glaze layer.

Benefits of technology

A black-based blue-spotted glaze with a unique metallic luster, smooth and delicate texture, and natural and vivid earthworm-like patterns was prepared. It has strong mechanical properties, high yield, and environmentally friendly raw materials.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention discloses a black-based blue-spotted glaze with an earthworm-like pattern and its preparation method. The glaze consists of a body, a black base glaze, and a blue-spotted glaze from the inside out. The raw materials for the black base glaze are: feldspar, calcite, calcium borate, dolomite, talc, barium carbonate, quartz, bentonite, zirconium silicate, rutile, cobalt oxide, manganese oxide, and iron oxide. The raw materials for the blue-spotted glaze are: feldspar, limestone, alumina, talc, barium sulfate, Datong clay, zinc oxide, quartz, and titanium dioxide. The preparation method includes: 1. Wet ball milling the black base glaze raw materials to obtain a black base glaze slurry; 2. Wet ball milling the blue-spotted glaze raw materials to obtain a blue-spotted glaze slurry; 3. Bisque firing the body; 4. Applying the black base glaze slurry to the body and drying it; 5. Applying the blue-spotted glaze slurry to the body and drying it; 6. Oxidation firing and reduction firing of the body, followed by natural cooling to obtain the black-based blue-spotted glaze. The raw material formula of this invention is reasonable and environmentally friendly, which can improve the mechanical properties of the glaze; the preparation method is simple and the yield is high.
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Description

Technical Field

[0001] This invention relates to the field of porcelain glaze preparation technology, specifically to a black-based blue-spotted glaze with earthworm-like patterns and its preparation method. Background Technology

[0002] Floral porcelain, also known as "Tang Jun," originated in the Tang Dynasty. It features regular or irregular sky-blue or moon-white spots on black, yellowish-brown, or tea-dust glazes, creating a milky, shimmering, and dazzling effect, possessing extremely high artistic and aesthetic value. Floral porcelain is considered the earliest phase-separated glaze in Chinese ceramic history. Its appearance and some of its techniques originated from the Tang Sancai (three-color glaze) of Gongxian kiln, laying the foundation for the development of Song Dynasty Jun porcelain. It can be considered the ancestor of multi-colored glaze and kiln-transformed glaze porcelain.

[0003] "Earthworm tracks" refers to a natural pattern on the surface of ceramic glaze that resembles the tracks left by earthworms. It is vivid, lively, and highly decorative. Its formation is mainly due to technological factors. One reason is that finer glazes tend to develop irregular natural cracks after drying on the ceramic body. When a top glaze is applied, some of these cracks are filled. During firing, the difference in composition between the cracks and the surrounding glaze layer creates the "earthworm tracks" pattern. Another reason is that cracks may form in the glaze layer during the early stages of firing. When a certain temperature is reached, the lower-melting-temperature top glaze can penetrate these cracks, creating the "earthworm tracks" pattern.

[0004] However, in the existing technology, there has been no report on the black-based blue-spotted glaze with earthworm-like patterns and its preparation method. Summary of the Invention

[0005] The purpose of this invention is to provide a black-based blue-spotted glaze with earthworm-like patterns and its preparation method. The raw material formula of this invention is reasonable and environmentally friendly, and can improve the mechanical properties of the glaze; the preparation method is simple and has a high yield.

[0006] To achieve the above objectives, the technical solution of the present invention is a black-based blue-spotted glaze with earthworm-track patterns and its preparation method, comprising a black-based blue-spotted glaze, wherein the glaze body consists of a body, a black base glaze, and a blue-spotted glaze from the inside out.

[0007] The black base glaze is prepared from the following raw materials in parts by weight: feldspar 30-40 parts, calcite 8-10 parts, calcium borate 4-6 parts, dolomite 3-7 parts, talc 12-20 parts, barium carbonate 6-8 parts, quartz 10-20 parts, bentonite 4-6 parts, zirconium silicate 11-19 parts, rutile 16-24 parts, cobalt oxide 2-4 parts, manganese oxide 1-3 parts, and iron oxide 3-6 parts.

[0008] The blue-spotted glaze is prepared from the following raw materials in parts by weight: 26-34 parts feldspar, 12-16 parts limestone, 2-5 parts alumina, 3-6 parts talc, 7-12 parts barium sulfate, 5-9 parts Datong clay, 3-5 parts zinc oxide, 20-30 parts quartz, and 4-10 parts titanium dioxide.

[0009] A method for preparing a black-based blue-spotted glaze with earthworm-track patterns, characterized by comprising the following steps:

[0010] Step 1: Wet ball mill the black base glaze raw material to achieve a glaze concentration of 60-65%, and then pass it through a 150-300 mesh sieve to obtain a black base glaze slurry for later use.

[0011] Step 2: Wet ball mill the blue-spotted glaze raw material to achieve a glaze concentration of 50-55%, and then pass it through a 100-150 mesh sieve to obtain the blue-spotted glaze slurry for later use.

[0012] Step 3: bisque-fire the green body. During bisque-firing, the temperature is raised evenly to 950-1000℃ and then cooled naturally to room temperature to obtain a bisque-fired green body.

[0013] Step 4: Apply a black base glaze slurry to the bisque-fired body to a thickness of 1.3-1.6 mm, and let it stand and dry to obtain a black base glaze body;

[0014] Step 5: Apply blue-spotted glaze slurry to the black-glazed body to a thickness of 0.8-1.2mm, and let it stand and dry to obtain a black-based blue-spotted body;

[0015] Step Six: The black-based blue-spotted body is oxidized and fired. During oxidation firing, the temperature is raised evenly to 900-960℃ and held. Then, it is reduced and fired. During reduction firing, the temperature is raised evenly to 1280-1290℃. Finally, it is naturally cooled to room temperature to obtain a black-based blue-spotted glaze.

[0016] Furthermore, in step one, the wet ball milling speed is 300-400 r / min, and the time is 60-80 min.

[0017] Furthermore, in step two, the wet ball milling speed is 200-300 r / min, and the time is 40-60 min.

[0018] Furthermore, the time for uniform heating in step three is 8-9 hours.

[0019] Further, in step four, the specific steps for applying the black base glaze are to apply 3-4 layers of black base glaze.

[0020] Further, the specific steps for applying the blue-spotted glaze slurry in step five are to apply 1-2 layers of blue-spotted glaze slurry.

[0021] Furthermore, the atmosphere used for oxidative firing in step six is ​​an oxidizing atmosphere.

[0022] Furthermore, in step six, the uniform heating time for oxidation firing is 6-7 hours, and the holding time is 2-3 hours.

[0023] Furthermore, the uniform heating time for reduction firing in step six is ​​8-10 hours.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] (1) In this invention, calcium borate is added to the black base glaze raw material, which can improve the transparency, wear resistance and chemical resistance of the glaze layer and extend its service life; barium carbonate, as a sintering agent, can reduce the sintering temperature of the glaze and increase the sintering density, making it more shock resistant, inhibiting cracking and enhancing its mechanical properties; bentonite can improve the adhesion, smoothness and toughness of the ingredients and improve the overall quality of ceramic products; zirconium silicate additive can improve the mechanical properties of ceramics, improve insulation properties, promote color stability and improve corrosion resistance; rutile has good melting and chemical stability, can be compatible with other glaze components, can improve the color, gloss and hardness of the glaze layer, and improve its durability and corrosion resistance; manganese oxide can improve the flow properties of the glaze slurry, making the rheological characteristics of the glaze slurry better, so that the glaze is more evenly distributed on the surface and the glaze surface is smoother and more delicate; cobalt oxide and iron oxide, as colorants, give the black base glaze a metallic luster, add its layered texture, and also play a role in enhancing the crystal network structure of the glaze surface, thereby preventing the glaze surface from peeling off or breaking.

[0026] (2) In this invention, talc is added to the raw material of blue speckled glaze. Talc can fill the pores in the ceramic and improve its density, thereby improving the strength and toughness of the ceramic products. Talc can also form finer grains in the ceramic, so that the grain boundaries of the ceramic are arranged in an orderly manner, enhancing its mechanical properties. Barium sulfate forms a dense and bright film on the surface of the glaze, increases the reflectivity of the glaze, improves its gloss, and makes the glaze surface smoother, more delicate, and crystal clear. Adding zinc oxide will reduce the tension of the glaze layer, which can lower the sintering temperature and save energy and time. Titanium dioxide can increase the smoothness and transparency of the glaze layer, and also improve its surface stain resistance.

[0027] (3) The preparation method of the present invention is that irregular natural cracks are easily generated after the black base glaze slurry with a larger fineness is dried on the body. When the blue spot glaze slurry is applied, some of the cracks will be filled. During firing, the cracks and the surrounding glaze layer are different in composition, and then a black base blue spot glaze with earthworm pattern is formed. The preparation method is simple and easy to operate.

[0028] (4) This invention combines earthworm mud pattern and black base with blue spots glaze for the first time to create a new artistic glaze color. The raw material formula is reasonable and environmentally friendly, which improves the mechanical properties of the glaze. The preparation method is simple and the yield can reach more than 80%. Detailed Implementation

[0029] The present invention will be further described in detail below with reference to specific embodiments.

[0030] Example 1: A method for preparing a black-based blue-spotted glaze with earthworm-track patterns, comprising the following raw material formula:

[0031] Black base glaze: 35g feldspar, 8g calcite, 4g calcium borate, 6g dolomite, 14g talc, 6g barium carbonate, 14g quartz, 5g bentonite, 12g zirconium silicate, 20g rutile, 2g cobalt oxide, 2g manganese oxide, 6g iron oxide.

[0032] Blue Spotted Glaze: Feldspar 30g, Limestone 12g, Alumina 3g, Talc 4g, Barium Sulfate 8g, Datong Clay 6g, Zinc Oxide 3g, Quartz 25g, Titanium Dioxide 4g;

[0033] The specific steps are as follows:

[0034] Step 1: Mix the black base glaze raw material with 250g of pebbles of different particle sizes, add deionized water and wet ball mill at 400r / min for 80min to make the glaze concentration reach 65%, and then pass it through a 300-mesh sieve to obtain the black base glaze slurry for later use.

[0035] Step 2: Mix the blue-spotted glaze raw material with 150g of pebbles of different particle sizes, add deionized water and wet-mill at 200r / min for 50min to make the glaze concentration reach 50%, and then pass it through a 120-mesh sieve to obtain the blue-spotted glaze slurry for later use.

[0036] Step 3: Firing the green body into a bisque. During bisque firing, the temperature is raised evenly to 950℃ over 8-9 hours, and then cooled naturally to room temperature to obtain a bisque fired green body.

[0037] Step 4: Apply 3 layers of black base glaze to the bisque-fired body to achieve a thickness of 1.5mm, and let it stand and dry to obtain a black base glaze body;

[0038] Step 5: Apply a layer of blue-spotted glaze slurry to the black-glazed body, making the thickness 1mm. After letting it stand and dry, a black-based blue-spotted body is obtained.

[0039] Step Six: The black-based blue-spotted body is oxidized and fired in an oxidizing atmosphere. During the oxidizing firing, the temperature is uniformly raised to 900℃ over 6-7 hours and held for 2-3 hours. Then, a reduction firing is carried out. During the reduction firing, the temperature is uniformly raised to 1280℃ over 8-10 hours. Finally, it is naturally cooled to room temperature to obtain a black-based blue-spotted glaze.

[0040] By using a reasonable ratio of raw materials and firing temperature and atmosphere, the prepared black glaze has a unique metallic luster, while the blue spotted glaze is full of color, smooth and delicate, stable with a natural and vivid earthworm-track texture, and the glaze layer has strong mechanical properties.

[0041] Comparative Example 1

[0042] The raw material formula is as follows:

[0043] Black base glaze: 35g feldspar, 8g calcite, 4g calcium borate, 6g dolomite, 14g talc, 6g barium carbonate, 14g quartz, 5g bentonite, 12g zirconium silicate, 20g rutile, 2g cobalt oxide, 2g manganese oxide, 6g iron oxide.

[0044] Blue Spotted Glaze: Feldspar 30g, Limestone 12g, Alumina 3g, Talc 4g, Datong Clay 6g, Zinc Oxide 3g, Quartz 25g, Titanium Dioxide 4g;

[0045] The preparation method is the same as the specific steps in Example 1.

[0046] Compared with Example 1, Comparative Example 1 did not use barium sulfate in the raw materials. The black-based blue-spotted glaze with earthworm-like patterns produced by this example had a dull luster, a rougher glaze surface, and was not delicate and lustrous enough. The yield was only about 40%.

[0047] Comparative Example 2

[0048] The raw material formula is the same as in Example 1;

[0049] The preparation method is the same as in Example 1, except that the step of passing through a 300-mesh sieve in step one is changed to a 100-mesh sieve.

[0050] Compared with Example 1, Comparative Example 2 obtained a black base glaze slurry after wet ball milling and passing it through a 100-mesh sieve. Because the glaze slurry was not fine enough, it was not easy for irregular natural cracks to occur after being applied to the body and dried. When the blue spot glaze slurry was applied, it did not flow much with the black base glaze and was not easy to form earthworm-like patterns.

[0051] Comparative Example 3

[0052] The raw material formula is as follows:

[0053] Black base glaze: 35g feldspar, 8g calcite, 4g calcium borate, 6g dolomite, 14g talc, 6g barium carbonate, 14g quartz, 5g bentonite, 12g zirconium silicate, 20g rutile, 2g manganese oxide, 6g iron oxide.

[0054] Blue Spotted Glaze: Feldspar 30g, Limestone 12g, Alumina 3g, Talc 4g, Barium Sulfate 8g, Datong Clay 6g, Zinc Oxide 3g, Quartz 25g, Titanium Dioxide 4g;

[0055] The preparation method is the same as the specific steps in Example 1.

[0056] Compared with Example 1, Comparative Example 3 did not use cobalt oxide in its raw materials, resulting in a black glaze that lacked depth and smoothness, had no metallic luster, and exhibited poor wear resistance.

[0057] Example 2: A method for preparing a black-based blue-spotted glaze with earthworm-track patterns, comprising the following raw material formula:

[0058] Black base glaze: feldspar 35g, calcite 10g, calcium borate 4g, dolomite 6g, talc 16g, barium carbonate 6g, quartz 18g, bentonite 5g, zirconium silicate 16g, rutile 18g, cobalt oxide 2g, manganese oxide 2g, iron oxide 4g.

[0059] Blue Spotted Glaze: Feldspar 30g, Limestone 14g, Alumina 4g, Talc 4g, Barium Sulfate 10g, Datong Clay 6g, Zinc Oxide 4g, Quartz 25g, Titanium Dioxide 7g;

[0060] The specific steps are as follows:

[0061] Step 1: Mix the black base glaze raw material with 250g of pebbles of different particle sizes, add deionized water and wet ball mill at 350r / min for 60min to make the glaze concentration reach 60%, and then pass it through a 200-mesh sieve to obtain the black base glaze slurry for later use.

[0062] Step 2: Mix the blue-spotted glaze raw material with 150g of pebbles of different particle sizes, add deionized water and wet ball mill at 240r / min for 40min to make the glaze concentration reach 52%, and then pass it through a 100-mesh sieve to obtain the blue-spotted glaze slurry for later use.

[0063] Step 3: Firing the green body into a bisque. During bisque firing, the temperature is raised evenly to 980℃ over 9 hours, and then cooled naturally to room temperature to obtain a bisque fired green body.

[0064] Step 4: Apply three layers of black base glaze to the bisque-fired body to achieve a thickness of 1.3mm. After letting it stand and dry, a black base glaze body is obtained.

[0065] Step 5: Apply two layers of blue-spotted glaze slurry to the black-glazed body, making the thickness 1.2mm. After letting it stand and dry, a black-based blue-spotted body is obtained.

[0066] Step Six: The black-based blue-spotted body is oxidized and fired in an oxidizing atmosphere. During the oxidizing firing, the temperature is uniformly raised to 940℃ over 7 hours and held for 2 hours. Then, a reduction firing is carried out. During the reduction firing, the temperature is uniformly raised to 1290℃ over 10 hours. Finally, it is naturally cooled to room temperature to obtain a black-based blue-spotted glaze.

[0067] Example 3: A method for preparing a black-based blue-spotted glaze with earthworm-track patterns, comprising the following raw material formula:

[0068] Black base glaze: feldspar 40g, calcite 8g, calcium borate 4g, dolomite 6g, talc 18g, barium carbonate 6g, quartz 10g, bentonite 5g, zirconium silicate 14g, rutile 18g, cobalt oxide 2g, manganese oxide 3g, iron oxide 6g.

[0069] Blue Spotted Glaze: Feldspar 30g, Limestone 16g, Alumina 4g, Talc 6g, Barium Sulfate 10g, Datong Clay 6g, Zinc Oxide 4g, Quartz 30g, Titanium Dioxide 4g;

[0070] The specific steps are as follows:

[0071] Step 1: Mix the black base glaze raw material with 250g of pebbles of different particle sizes, add deionized water and wet ball mill at 300r / min for 70min to make the glaze concentration reach 62%, and then pass it through a 150-mesh sieve to obtain the black base glaze slurry for later use.

[0072] Step 2: Mix the blue-spotted glaze raw material with 150g of pebbles of different particle sizes, add deionized water and wet ball mill at 300r / min for 60min to make the glaze concentration reach 55%, and then pass it through a 150-mesh sieve to obtain the blue-spotted glaze slurry for later use.

[0073] Step 3: Firing the green body into a bisque. During bisque firing, the temperature is raised evenly to 1000℃ over 8 hours, and then cooled naturally to room temperature to obtain a bisque fired green body.

[0074] Step 4: Apply 4 layers of black base glaze to the bisque-fired body to achieve a thickness of 1.6mm, and let it stand and dry to obtain a black base glaze body;

[0075] Step 5: Apply a layer of blue-spotted glaze slurry to the black-glazed body, making the thickness reach 0.8mm. After letting it stand and dry, a black-based blue-spotted body is obtained.

[0076] Step Six: The black-based blue-spotted body is oxidized and fired in an oxidizing atmosphere. During the oxidizing firing, the temperature is uniformly raised to 960℃ over 6.5 hours and held for 2.5 hours. Then, a reduction firing is carried out. During the reduction firing, the temperature is uniformly raised to 1285℃ over 8 hours. Finally, it is naturally cooled to room temperature to obtain a black-based blue-spotted glaze.

[0077] The raw material formulas for the black-based blue-spotted glaze with earthworm-track patterns provided in Examples 4-23 of this invention are shown in Tables 1-4, with units of g. The preparation method is the same as the specific steps in Example 1.

[0078] Table 1 Raw material formulations for Examples 4-8

[0079]

[0080]

[0081] Table 2 Raw material formulations for Examples 9-13

[0082]

[0083]

[0084] Table 3 Raw material formulations for Examples 14-18

[0085]

[0086] Table 4 Raw material formulations for Examples 19-23

[0087]

[0088]

[0089] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A black base blue spot glaze with earthworm tracks, characterized in that: The glaze consists of the body, black base glaze, and blue-spotted glaze from the inside out. ​ The black base glaze is prepared from the following raw materials in parts by weight: feldspar 30-40 parts, calcite 8-10 parts, calcium borate 4-6 parts, dolomite 3-7 parts, talc 12-20 parts, barium carbonate 6-8 parts, quartz 10-20 parts, bentonite 4-6 parts, zirconium silicate 11-19 parts, rutile 16-24 parts, cobalt oxide 2-4 parts, manganese oxide 1-3 parts, and iron oxide 3-6 parts. The blue-spotted glaze is prepared from the following raw materials in parts by weight: 26-34 parts feldspar, 12-16 parts limestone, 2-5 parts alumina, 3-6 parts talc, 7-12 parts barium sulfate, 5-9 parts Datong clay, 3-5 parts zinc oxide, 20-30 parts quartz, and 4-10 parts titanium dioxide. The preparation of the black-based blue-spotted glaze includes the following steps: Step 1: Wet ball mill the black base glaze raw material to achieve a glaze concentration of 60-65%, and then pass it through a 150-300 mesh sieve to obtain a black base glaze slurry for later use. Step 2: Wet ball mill the blue-spotted glaze raw material to achieve a glaze concentration of 50-55%, and then pass it through a 100-150 mesh sieve to obtain the blue-spotted glaze slurry for later use. Step 3: bisque-fire the green body. During bisque-firing, the temperature is raised evenly to 950-1000℃ and then cooled naturally to room temperature to obtain a bisque-fired green body. Step 4: Apply a black base glaze slurry to the bisque-fired body to a thickness of 1.3-1.6 mm, and let it stand and dry to obtain a black base glaze body; Step 5: Apply blue-spotted glaze slurry to the black-glazed body to a thickness of 0.8-1.2mm, and let it stand and dry to obtain a black-based blue-spotted body; Step Six: The black-based blue-spotted body is oxidized and fired. During oxidation firing, the temperature is raised evenly to 900-960℃ and held. Then, it is reduced and fired. During reduction firing, the temperature is raised evenly to 1280-1290℃. Finally, it is naturally cooled to room temperature to obtain a black-based blue-spotted glaze.

2. A black base blue spot glaze with earthworm tracks according to claim 1, characterized in that: In step one, the wet ball milling speed is 300-400 r / min, and the time is 60-80 min.

3. The black base blue spot glaze with earthworm tracks according to claim 1, characterized in that: In step two, the wet ball milling speed is 200-300 r / min, and the time is 40-60 min.

4. The black base blue spot glaze with earthworm tracks according to claim 1, characterized in that: The time for uniform heating in step three is 8-9 hours.

5. The black base blue spot glaze with earthworm tracks according to claim 1, characterized in that: The specific steps for applying the black base glaze in step four are to apply 3-4 layers of black base glaze.

6. A black-based blue-spotted glaze with earthworm-track patterns as described in claim 1, characterized in that: The specific steps for applying the blue-spotted glaze in step five are to apply 1-2 layers of blue-spotted glaze.

7. A black-based blue-spotted glaze with earthworm-track patterns as described in claim 1, characterized in that: The atmosphere used for oxidative firing in step six is ​​an oxidizing atmosphere.

8. A black-based blue-spotted glaze with earthworm-track patterns as described in claim 1, characterized in that: In step six, the uniform heating time for oxidation firing is 6-7 hours, and the holding time is 2-3 hours.

9. A black-based blue-spotted glaze with earthworm-track patterns as described in claim 1, characterized in that: The uniform heating time for reduction firing in step six is ​​8-10 hours.