CN115745404A - High-solid-content glaze suitable for direct-writing 3D printing and preparation method thereof - Google Patents
High-solid-content glaze suitable for direct-writing 3D printing and preparation method thereof Download PDFInfo
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- CN115745404A CN115745404A CN202211499066.0A CN202211499066A CN115745404A CN 115745404 A CN115745404 A CN 115745404A CN 202211499066 A CN202211499066 A CN 202211499066A CN 115745404 A CN115745404 A CN 115745404A
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Abstract
The invention provides a high-solid-content glaze suitable for direct-writing 3D printing, which is prepared by adding an auxiliary agent into a raw material for ceramic glaze, deionizing and uniformly mixing; the invention also provides a preparation method of the high-solid-content glaze suitable for direct-writing 3D printing, which comprises the steps of uniformly mixing the raw materials for the ceramic glaze, the added auxiliary agent and deionized water to obtain a high-solid-content glaze paste; obtaining a 3D printing high-solid-content glaze paste after vacuumizing and defoaming treatment; the method comprises the steps of adding the high-solid-content glaze paste into a 3D printer, printing on a blank based on a set model, directly writing and extruding through a printing head of the 3D printer, overlapping the high-solid-content glaze paste layer by layer to obtain a 3D printing graph on the blank, drying and sintering.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to a high-solid-content glaze suitable for direct-writing 3D printing and a preparation method thereof.
Background
The glaze is a silicate compound and is a layer of vitreous thin layer adhered to the surface of the ceramic body after high temperature action. Ceramics generally fall into three broad categories: domestic ceramics, artistic ceramics and industrial ceramics, and the industrial ceramics also comprise building-sanitary ceramics. According to different ceramic types, glazing methods on ceramic blanks are different, and artificial glazing (glaze spraying, glaze dipping, glaze pouring, glaze swinging), screen printing, roller printing, ink-jet printing and the like are adopted. The problems that the artificial glazing is high in cost, long in manufacturing period and the like are solved, an ink-jet printing picture is lost in the production process of technologies such as ink-jet printing and printing, after a pattern is printed on a blank of a ground glaze, the pattern becomes fuzzy and unclear, and sometimes due to the color of the blank, the pattern cannot achieve a very ideal effect in the gradation, the bonding performance with the blank is not good, the sufficient thickness cannot be met and the like are solved, and the Chinese patent publication No. CN114634349A discloses an ink-jet decorative ceramic tile, a blank thereof and a preparation method thereof.
The direct-writing 3D printing technology is a relatively novel preparation method, the technology develops rapidly abroad, the direct-writing 3D printing technology extrudes slurry from a needle nozzle by pneumatic or mechanical power to form linear fluid, the linear fluid is molded on a substrate according to a designed three-dimensional structure, the linear fluid is molded from a first layer, and the linear fluid moves in a three-dimensional space and moves in a Z-axis direction according to a modeling path design to form an integral physical model layer by layer. The direct-writing 3D printing technology researched by the invention has the advantages that the printing line width is controlled to be 0.8mm or more, the single-layer thickness can be controlled to be less than 1mm, the printing speed can be adjusted at any time, the simple equipment structure and the good slurry compatibility can be better utilized in daily production, and the production can be realized efficiently, quickly and individually. With the continuous updating of materials, an active design of multi-component raw materials can be formed. At present, in domestic researches on ceramic direct-writing 3D printing, the research on related glaze is less, so that the high-solid-content glaze for the direct-writing 3D printer is prepared based on the development and the use of a direct-writing 3D printing technology.
Disclosure of Invention
The invention aims to provide a high-solid-content glaze suitable for direct-writing 3D printing and a preparation method thereof, which are used for solving the problems.
A high-solid-content glaze suitable for direct-writing 3D printing comprises the following raw materials in percentage by weight: 71.5 to 85.75 percent of raw material for ceramic glaze, 2.25 to 8.5 percent of additive and 12 to 20 percent of deionized water are evenly mixed to prepare the ceramic glaze;
the raw materials for the ceramic glaze comprise 23-52% of potash feldspar, 15-27% of quartz, 13-20% of kaolin, 6-24% of limestone, 4-10% of talcum and 1-4% of zirconium silicate, and the raw materials are uniformly mixed, subjected to wet ball milling with deionized water according to the proportion of 1.
The additive comprises 2-6% of binder, 0.1-0.5% of surfactant and 0.15-2% of dispersant.
The high-solid-content glaze material has the solid content of 73-80% and the particle size of 4-11 mu m, and is suitable for most ceramic biscuit firing blanks.
The binder is one or more of polyvinyl alcohol, sodium carboxymethylcellulose and acacia.
The surfactant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and stearic acid.
The dispersing agent is one or more of 3-mercaptopropionic acid, poly-4-styrene sulfonic acid, sodium polyacrylate and sodium hexametaphosphate.
The invention also discloses a preparation method of the high-solid-content glaze suitable for direct-writing 3D printing, and the preparation method of the high-solid-content glaze suitable for direct-writing 3D printing comprises the following steps:
s1, uniformly mixing raw materials for ceramic glaze, an additive and deionized water to obtain a high-solid-content glaze paste;
s2, filling the high-solid-content paste obtained in the step S1 into a charging barrel, and performing vacuumizing and defoaming treatment to obtain a 3D printing high-solid-content glaze paste;
s3, adding the high-solid-content glaze paste body obtained in the step S2 into a 3D printer, printing on the blank body based on a set model, directly writing and extruding through a printing head of the 3D printer, overlapping the high-solid-content glaze paste body layer by layer, and obtaining a 3D printing graph on the blank body;
and S4, drying and sintering the 3D printed graphic product obtained in the step S3.
The direct-write forming conditions in the step S3 are as follows: the air pressure is 0.3-0.6Mpa, the diameter of the printing needle is 0.86-3mm, the printing speed is 3-12mm/s, the printing interval is 0.9-3.2mm, and the single-layer thickness is 0.1-0.6mm.
The blank in the step S3 is a ceramic biscuit firing blank.
The firing conditions in the step S4 are as follows:
the first stage is as follows: the temperature interval is normal temperature to 300 ℃, and the glaze firing time is 60 to 90 minutes;
and a second stage: the temperature interval is 300-920 ℃, and the glaze firing time is 120-150 minutes;
and a third stage: the temperature interval is 920-1050 ℃, and the glaze firing time is 60-80 minutes;
a fourth stage: the temperature range is 1050-1280 ℃, and the glaze firing time is 180-210 minutes;
the fifth stage: the temperature range is 1280 ℃ to normal temperature, and the natural cooling is carried out.
The high-solid-content glaze suitable for direct-writing 3D printing and the preparation method thereof have the beneficial effects that:
(1) The preparation of the high solid content glaze paste is mainly to regulate and control the high solid content and the rheological property of the paste by adjusting the proportion of the ceramic glaze powder, the binder, the surfactant and the dispersant, and the extruded lines are uniform, well combined with the surface of a ceramic biscuit firing body and not easy to crack and fall off.
(2) The raw materials selected in the invention are common raw materials, the obtaining is simple, the price is low, the high-temperature performance in the blank glaze firing process is not influenced, the bonding performance of the intermediate layer of the generated blank glaze is good, and the yield is high.
(3) The invention utilizes the direct-writing 3D printing technology, can control the size and the thickness of the pattern through the principle of layer-by-layer stacking, has the advantages of controlling the printing line width to be 0.8mm or more, controlling the single-layer thickness to be less than 1mm, adjusting the printing speed at any time and the like, can be more utilized in daily production due to simple equipment structure and good slurry compatibility, can realize production efficiently, quickly and individually, and can change the pattern style at any time through 3D modeling, thereby realizing free patterns on a blank body. The direct-writing 3D printing high-solid-content glaze makes up for the defect that no related research is available in China.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic diagram of a biscuit in a process of 3D printing a graphic product in embodiment 1 of the present invention.
Fig. 2 is a 3D printed graphic product in embodiment 1 of the present invention.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and examples, and the following examples are only used to more clearly illustrate the technical solutions of the present invention, and therefore are only used as examples, and the protection scope of the present invention is not limited thereby.
Example 1
1. Printing stock preparation
A high solid content glaze suitable for direct-writing 3D printing is prepared through proportionally mixing raw materials for glaze, ball grinding, proportionally adding assistant and water, and preparing.
a. Ball milling: the glaze material consists of potash feldspar 52 wt%, quartz 15 wt%, kaolin 20 wt%, limestone 6 wt%, talc 4 wt% and zirconium silicate 3 wt%. The glaze raw materials are as follows: ball stones: water =1:2:1 for 30 minutes, sieving, drying, and making into glaze A.
b. Preparation: according to the weight percentage, the 3D printing raw material comprises 85.75 percent of glaze A, 1.5 percent of polyvinyl alcohol, 0.5 percent of sodium carboxymethyl cellulose, 0.1 percent of sodium dodecyl benzene sulfonate, 0.15 percent of 3-mercaptopropionic acid and 12 percent of deionized water. The raw materials are uniformly mixed to prepare the glaze paste with high solid content.
2. Printed graphic product
And (2) filling the high-solid-content glaze paste prepared in the step (1) into a charging barrel, removing bubbles in a vacuum device for 2 hours, and then assembling the high-solid-content glaze paste on a printer, wherein the printing parameters are set as follows: the air pressure is 0.3-0.6Mpa, the diameter of a printing needle is 3mm, the printing speed is 12mm/s, the printing interval is 3.2mm, and the single-layer thickness is 0.6mm. And printing according to a set program to obtain a pattern product biscuit.
3. Firing into
Firing the biscuit product according to the following curve:
the first stage is as follows: the temperature interval is normal temperature to 300 ℃, and the glaze firing time is 60 to 90 minutes;
and a second stage: the temperature interval is 300-920 ℃, and the glaze firing time is 120-150 minutes;
and a third stage: the temperature interval is 920-1050 ℃, and the glaze firing time is 60-80 minutes;
a fourth stage: the temperature interval is 1050-1280 ℃, and the glaze firing time is 180-210 minutes;
and a fifth stage: the temperature range is 1280 ℃ to normal temperature, and the natural cooling is carried out.
In each sintering stage, the free water evaporation stage is carried out before 300 ℃, the temperature rise is not suitable to be too fast, and a line is reserved at a kiln door to facilitate the escape of water vapor. The temperature of 300-920 ℃ is the evaporation stage of the crystal water, the temperature rising speed is slowed down from 920 ℃ to 1050 ℃ in order to avoid the escape of carbon, sulfur-containing gas and harmful impurities and the generation of pinholes and bubbles of finished products. In the firing process of 1050-1280 ℃, the blank body is vitrified, the glaze layer is vitrified, the shrinkage is large, the uniform heating of the product is ensured, the high-temperature reaction is consistent, the temperature rise is slow, and the kiln temperature is promoted to be balanced. And (5) firing, and naturally cooling to finally obtain the 3D printing graphic product.
Example 2
1. Printing stock preparation
A high solid content glaze material suitable for direct-writing 3D printing is prepared by mixing raw materials for glaze according to a proportion, ball-milling, and adding an auxiliary agent and water according to a proportion.
a. Ball milling: the glaze material consists of potash feldspar 23 wt%, quartz 26 wt%, kaolin 13 wt%, limestone 24 wt%, talc 10 wt% and zirconium silicate 4 wt%. The glaze raw materials are as follows: ball stone: water =1:2:1 for 30 minutes, sieving, drying and preparing powder which is marked as glaze A.
b. Preparation: according to the weight percentage content, the 3D printing raw material comprises 71.5% of glaze A, 2% of Arabic gum, 4% of sodium carboxymethylcellulose, 0.5% of sodium dodecyl benzene sulfate, 2% of sodium polyacrylate and 20% of deionized water. The raw materials are uniformly mixed to prepare the glaze paste with high solid content.
2. Printed graphic product
Filling the glaze paste with high solid content prepared in the step 1 into a charging barrel, removing bubbles in a vacuum device for 2 hours, and then assembling the glaze paste on a printer, wherein the printing parameters are set as follows: the air pressure is 0.3-0.6Mpa, the diameter of the printing needle is 0.86mm, the printing speed is 3mm/s, the printing interval is 0.9mm, and the single-layer thickness is 0.1mm. And printing according to a set program to obtain a pattern product biscuit.
3. Firing into
Firing the biscuit product according to the following curve:
the first stage is as follows: the temperature interval is normal temperature to 300 ℃, and the glaze firing time is 60 to 90 minutes;
and a second stage: the temperature interval is 300-920 ℃, and the glaze firing time is 120-150 minutes;
and a third stage: the temperature interval is 920-1050 ℃, and the glaze firing time is 60-80 minutes;
a fourth stage: the temperature range is 1050-1280 ℃, and the glaze firing time is 180-210 minutes;
the fifth stage: the temperature range is 1280 ℃ to normal temperature, and the natural cooling is carried out.
In each sintering stage, the free water evaporation stage is carried out before 300 ℃, the temperature rise is not suitable to be too fast, and a line is reserved at a kiln door to facilitate the escape of water vapor. The temperature of 300-920 ℃ is a crystal water evaporation stage, the temperature rising speed is slowed down from 920 ℃ to 1050 ℃, so that carbon, sulfur-containing gas and harmful impurities escape, and the generation of pinholes and bubbles of finished products is avoided. In the firing process of 1050-1280 ℃, the blank body is vitrified, the glaze layer is vitrified, the shrinkage is large, the uniform heating of the product is ensured, the high-temperature reaction is consistent, the temperature rise is slow, and the kiln temperature is promoted to be balanced. And (5) firing, and naturally cooling to finally obtain the 3D printing graphic product.
Example 3
1. Printing stock preparation
A high solid content glaze suitable for direct-writing 3D printing is prepared through proportionally mixing raw materials for glaze, ball grinding, proportionally adding assistant and water, and preparing.
a. Ball milling: the glaze material comprises 45% of potassium feldspar, 20% of quartz, 15% of kaolin, 13% of limestone, 6% of talc and 1% of zirconium silicate according to weight percentage. The glaze raw materials are as follows: ball stones: water =1:2:1 for 30 minutes, sieving, drying, and making into glaze A.
b. Preparation: according to the weight percentage, the 3D printing raw material comprises 76.26 percent of glaze A, 4 percent of sodium carboxymethyl cellulose, 0.4 percent of stearic acid, 0.04 percent of poly 4-styrene sulfonic acid, 1.3 percent of sodium hexametaphosphate and 18 percent of deionized water. The raw materials are uniformly mixed to prepare the glaze paste with high solid content.
2. Printed graphic product
Filling the glaze paste with high solid content prepared in the step 1 into a charging barrel, removing bubbles in a vacuum device for 2 hours, and then assembling the glaze paste on a printer, wherein the printing parameters are set as follows: the air pressure is 0.3-0.6Mpa, the diameter of a printing needle is 1.26mm, the printing speed is 5mm/s, the printing interval is 1.32mm, and the single-layer thickness is 0.2mm. And printing according to a set program to obtain a pattern product biscuit.
3. Firing into
The biscuit product is placed in an electric kiln, and the firing system (temperature rise curve) is as follows:
the first stage is as follows: the temperature interval is normal temperature to 300 ℃, and the glaze firing time is 60 to 90 minutes;
and a second stage: the temperature interval is 300-920 ℃, and the glaze firing time is 120-150 minutes;
and a third stage: the temperature interval is 920-1050 ℃, and the glaze firing time is 60-80 minutes;
a fourth stage: the temperature range is 1050-1280 ℃, and the glaze firing time is 180-210 minutes;
the fifth stage: the temperature range is 1280 ℃ to normal temperature, and the natural cooling is carried out.
In each sintering stage, the free water evaporation stage is carried out before 300 ℃, the temperature rise is not suitable to be too fast, and a line is reserved at a kiln door to facilitate the escape of water vapor. The temperature of 300-920 ℃ is a crystal water evaporation stage, the temperature rising speed is slowed down from 920 ℃ to 1050 ℃, so that carbon, sulfur-containing gas and harmful impurities escape, and the generation of pinholes and bubbles of finished products is avoided. In the firing process of 1050 ℃ -1280 ℃, a blank body is vitrified, a glaze layer is vitrified, the shrinkage is large, the uniform heating of a product is ensured, the high-temperature reaction is consistent, the temperature rise is slow, and the kiln temperature is promoted to be balanced. And (5) firing, and naturally cooling to finally obtain the 3D printing graphic product.
The above embodiments are described in further detail to solve the technical problems, technical solutions and advantages of the present invention, and it should be understood that the above embodiments are only examples of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The high-solid-content glaze suitable for direct-writing 3D printing is characterized by comprising the following raw materials in percentage by weight: 71.5 to 85.75 percent of raw material for ceramic glaze, 2.25 to 8.5 percent of additive and 12 to 20 percent of deionized water are evenly mixed to prepare the ceramic glaze;
the raw materials for the ceramic glaze comprise 23-52% of potash feldspar, 15-27% of quartz, 13-20% of kaolin, 6-24% of limestone, 4-10% of talcum and 1-4% of zirconium silicate, and the raw materials are uniformly mixed, subjected to wet ball milling with deionized water according to the proportion of 1.
2. The high-solid-content glaze suitable for direct-write 3D printing according to claim 1, wherein the additive comprises 2% -6% of binder, 0.1% -0.5% of surfactant and 0.15% -2% of dispersant.
3. The high solid content glaze suitable for direct-write 3D printing according to claim 1 or 2, wherein the high solid content glaze has a solid content of 73-80% and a particle size of 4-11 μm.
4. The high-solid-content glaze suitable for direct-writing 3D printing according to claim 2, wherein the binder is one or more of polyvinyl alcohol, sodium carboxymethylcellulose and acacia gum.
5. The high-solid-content glaze suitable for direct-writing 3D printing according to claim 4, wherein the surfactant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and stearic acid.
6. The high-solid-content glaze suitable for direct-writing 3D printing according to claim 5, wherein the dispersant is one or more of 3-mercaptopropionic acid, poly-4-styrenesulfonic acid, sodium polyacrylate and sodium hexametaphosphate.
7. A method of preparing a high solids glaze suitable for direct write 3D printing using a high solids glaze suitable for direct write 3D printing as claimed in any one of claims 1 to 7, comprising the steps of:
s1, uniformly mixing a raw material for ceramic glaze, an additive and deionized water to obtain a high-solid-content glaze paste;
s2, filling the high-solid-content paste obtained in the step S1 into a charging barrel, and performing vacuumizing and defoaming treatment to obtain a 3D printing high-solid-content glaze paste;
s3, adding the high-solid-content glaze paste body obtained in the step S2 into a 3D printer, printing on the blank body based on a set model, directly writing and extruding through a printing head of the 3D printer, overlapping the high-solid-content glaze paste body layer by layer, and obtaining a 3D printing graph on the blank body;
and S4, drying and sintering the 3D printing graphic product obtained in the step S3.
8. The method for preparing high solid content glaze suitable for direct-write 3D printing according to claim 7, wherein the direct-write molding conditions in step S3 are as follows: the air pressure is 0.3-0.6Mpa, the diameter of the printing needle is 0.86-3mm, the printing speed is 3-12mm/s, the printing interval is 0.9-3.2mm, and the single-layer thickness is 0.1-0.6mm.
9. The method for preparing a high solid content glaze suitable for direct-write 3D printing according to claim 8, wherein the blank in step S3 is a ceramic bisque-fired blank.
10. The method for preparing a high solid content glaze suitable for direct-write 3D printing according to claim 9, wherein the firing conditions in the step S4 are as follows:
the first stage is as follows: the temperature interval is normal temperature to 300 ℃, and the glaze firing time is 60 to 90 minutes;
and a second stage: the temperature interval is 300-920 ℃, and the glaze firing time is 120-150 minutes;
and a third stage: the temperature interval is 920-1050 ℃, and the glaze firing time is 60-80 minutes;
a fourth stage: the temperature interval is 1050-1280 ℃, and the glaze firing time is 180-210 minutes;
the fifth stage: the temperature range is 1280 ℃ to normal temperature, and the natural cooling is carried out.
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