CN112194484A - Preparation method of gradient-color ceramic material - Google Patents
Preparation method of gradient-color ceramic material Download PDFInfo
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Abstract
The invention discloses a preparation method of a gradient-color ceramic material, which comprises the steps of mixing an azeotropic mixture solvent, a dispersant and ceramic powder to obtain a first mixture, adding a plasticizer and a binder into the first mixture to mix to obtain a second mixture, respectively adding pigments with continuously changing mass gradients into the second mixture to respectively obtain mixed slurry with continuously changing pigment concentration gradients, respectively carrying out tape casting on the mixed slurry with continuously changing pigment concentration gradients to obtain tape casting sheets with continuously changing pigment concentration gradients, sequentially superposing the tape casting sheets from high to low according to the content of the pigments, carrying out isostatic pressing to obtain green bodies, and sequentially carrying out glue removal treatment and sintering treatment on the green bodies to obtain the gradient-color ceramic material. The preparation method disclosed by the invention is simple, the ceramic material is uniform in color transition, rich and attractive in color, environment-friendly and safe, and the appearance of the ceramic material is improved on the basis of excellent corrosion resistance and wear resistance of the ceramic material.
Description
Technical Field
The invention belongs to the technical field of gradient ceramic, and particularly relates to a preparation method of a gradient ceramic material.
Background
The ceramic has excellent corrosion resistance and wear resistance, and is widely applied to the fields of industrial and commercial products and daily necessities. However, because the color of the ceramic is single, the appearance of the ceramic material is poor, the existing gradient ceramic is subjected to glazing treatment by a spraying mode on pure-color ceramic, the mode is not environment-friendly and is easy to fade, and the inferior colored glaze is not healthy after being contacted with a human body for a long time.
In view of this, a method for preparing a gradient-color ceramic material is provided.
Disclosure of Invention
The application aims to provide a preparation method of a gradient ceramic material aiming at the defects in the prior art, which comprises the steps of respectively adding pigments with continuously changed mass gradients into ceramic mixtures in one-to-one correspondence to be uniformly mixed, carrying out independent casting to obtain casting sheets with continuously changed pigment content gradients, sequentially superposing the casting sheets in sequence from high to low in pigment content, and carrying out isostatic pressing, glue discharging and sintering treatment to obtain the gradient ceramic material. The preparation method is simple, environment-friendly and safe, the ceramic material has uniform color transition and rich and beautiful color, and the appearance of the ceramic material is improved on the basis of the excellent corrosion resistance and wear resistance of the ceramic material.
The object of the application can be achieved by the following technical measures:
in order to achieve the above object, the present application provides a method for preparing a gradient-color ceramic material, the method comprising:
step S1: mixing an azeotropic mixture solvent, a dispersant and ceramic powder to obtain a first mixture;
step S2: adding a plasticizer and a binder into the first mixture and mixing to obtain a second mixture;
step S3: respectively adding the pigments with continuously changed mass gradients into the second mixture to respectively obtain mixed slurry with continuously changed pigment concentration gradients;
step S4: respectively carrying out tape casting on the mixed slurry containing the continuous change of the pigment concentration gradient to obtain tape casting sheets containing the continuous change of the pigment concentration gradient;
step S5: sequentially superposing the casting sheets according to the pigment content from high to low, and carrying out isostatic pressing to obtain a green body;
step S6: and sequentially carrying out glue removal treatment and sintering treatment on the green body to obtain the gradient-color ceramic material.
Preferably, the casting sheet in which the gradient of the coloring material concentration continuously changes is a casting sheet in which the coloring material concentration is graded in an arithmetic progression.
Preferably, the step S3 specifically includes:
respectively adding the pigment with continuously changed mass gradient into the second mixture for graded ball milling to respectively obtain mixed slurry with continuously changed pigment concentration gradient;
or preparing the pigment into a pigment solution, and respectively spraying the pigment solution into the second mixture in a pulse mode according to the pulse times of continuous gradient change to respectively obtain mixed slurry containing the continuous gradient change of the pigment concentration.
Preferably, after the ball milling in the step S3, the average particle size D50 of the ceramic powder in the mixed slurry is 0.1 to 1.0 micron, wherein the maximum particle size D100 is not greater than twice the average particle size D50.
Preferably, the solid content of the second mixture is 40-70 wt%.
Preferably, the second mixture comprises 0.5-2.0 wt% of a dispersant, 0.5-2.0 wt% of a binder and 0.1-2.0 wt% of a plasticizer.
Preferably, the mass ratio of the pigment to the ceramic powder in the tape-casting sheet is not more than 0.1, and the pigment is nano powder or micro-nano powder.
Preferably, the step S4 specifically includes: respectively carrying out vacuum defoaming on the mixed slurry containing different pigment concentrations, wherein the vacuum degree of the vacuum defoaming is-0.9-0.96 KPa; and respectively carrying out tape casting on the mixed slurry containing different pigment concentrations to obtain tape casting sheets containing different pigment concentrations.
Preferably, in the step S4, the casting temperature is 45-80 ℃, and the thickness of the obtained casting sheet is less than 0.2 mm.
Preferably, in the sintering process, the heating rate is not higher than 10.0 ℃/min, and the sintering temperature is 1300-1600 ℃.
The beneficial effects of this application are that a preparation method of gradual change look ceramic material is provided, mix azeotropic mixture solvent, dispersant and ceramic powder and obtain first mixture, add plasticizer and binder and mix in first mixture and obtain the second mixture, add the pigment of quality gradient continuous change respectively in the second mixture, obtain the mixed slurry of pigment concentration gradient continuous change respectively, carry out the curtain coating respectively with the mixed slurry of pigment concentration gradient continuous change, obtain the curtain coating piece that contains pigment concentration gradient continuous change, carry out isostatic compaction after overlapping the curtain coating piece in proper order by high to low according to pigment content, obtain the unburned bricks, carry out binder removal processing and sintering treatment in proper order with the unburned bricks, obtain gradual change look ceramic material. The preparation method disclosed by the invention is simple, the ceramic material is uniform in color transition, rich and attractive in color, environment-friendly and safe, and the appearance of the ceramic material is improved on the basis of excellent corrosion resistance and wear resistance of the ceramic material.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a gradient-color ceramic material according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the description of the present disclosure more complete and complete, the following description is given for illustrative purposes with respect to the embodiments and examples of the present invention; it is not intended to be the only form in which the embodiments of the invention may be practiced or utilized. The embodiments are intended to cover the features of the various embodiments as well as the method steps and sequences for constructing and operating the embodiments. However, other embodiments may be utilized to achieve the same or equivalent functions and step sequences.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1 shows a process flow diagram of a method for preparing a gradient-color ceramic material according to an embodiment of the present invention.
Referring to fig. 1, a method for preparing a gradient-color ceramic material includes:
step S1: and mixing the azeotropic mixture solvent, the dispersant and the ceramic powder to obtain a first mixture.
Specifically, the azeotropic mixture solvent comprises at least two of water, ethanol, methyl ethyl ketone, trichloroethylene, toluene, xylene and ethyl acetate, and the dispersant comprises at least one of an ethoxy compound, triethanolamine, a fatty amine salt and fish oil.
Step S2: and adding a plasticizer and a binder into the first mixture and mixing to obtain a second mixture.
Specifically, step S2 includes:
simultaneously adding a plasticizer and a binder into the first mixture and mixing to obtain a second mixture;
or, covering a plasticizer on the surface of the first mixture so that the plasticizer forms a plasticizer film on the surface of the first mixture, adding the adhesive into the plasticizer film so as to mix the adhesive and the plasticizer, and uniformly mixing the plasticizer film dissolved with the adhesive with the first mixed solution to obtain the second mixture.
It should be noted that, in order to ensure the stability and the dispersion uniformity of the ceramic slurry suspension, it is preferable to add the plasticizer or the binder to the first mixture in sequence, so that the plasticizer and the binder are mixed and dissolved to prepare the second mixture, thereby further improving the stability and the dispersion uniformity of the ceramic slurry suspension.
Specifically, the binder comprises at least one of polyvinyl butyral, polyacrylate, ethyl cellulose, polyvinyl alcohol, acrylic emulsion and polyacrylic amine salt, and the plasticizer comprises at least one of polyethylene glycol, ethylene glycol and dibutyl phthalate.
Further, the solid content of the second mixture is 40-70 wt%.
Further, the second mixture comprises 0.5-2.0 wt% of a dispersant, 0.5-2.0 wt% of a binder and 0.1-2.0 wt% of a plasticizer.
Step S3: and respectively adding the pigments with continuously changed mass gradients into the second mixture to respectively obtain mixed slurry with continuously changed pigment concentration gradients.
Further, step S3 specifically includes:
respectively adding the pigment with continuously changed mass gradient into the second mixture for graded ball milling to respectively obtain mixed slurry with continuously changed pigment concentration gradient;
or preparing the pigment into a pigment solution, and respectively spraying the pigment solution into the second mixture in a pulse mode according to the pulse times of continuous gradient change to respectively obtain mixed slurry containing the continuous gradient change of the pigment concentration.
Further, after the ball milling in the step S3, the average particle size D50 of the ceramic powder in the mixed slurry is 0.1 to 1.0 micron, wherein the maximum particle size D100 is not more than twice of the average particle size D50, so as to ensure that the particle size of the ceramic powder is uniform and fine, and further improve the dispersion uniformity of the plasticizer and the binder in the mixed slurry.
Step S4: and respectively carrying out tape casting on the mixed slurry containing the continuous change of the pigment concentration gradient to obtain a tape casting sheet containing the continuous change of the pigment concentration gradient.
Furthermore, the casting sheet with the continuously changed gradient of the pigment concentration is a casting sheet with the pigment concentration being in an arithmetic progression, the pigment concentration difference between adjacent casting sheets is uniform and small, the color transition is uniform, and the color presenting effect of the gradient ceramic material is further improved.
Furthermore, the mass ratio of the pigment to the ceramic powder in the tape-casting sheet is not more than 0.1, and the pigment is nano powder or micro-nano powder, so that the particle size of the pigment is smaller than that of the ceramic powder, and the dispersion uniformity of the pigment in the mixed slurry is further improved.
Further, step S4 specifically includes: respectively carrying out vacuum defoaming on the mixed slurry containing different pigment concentrations, wherein the vacuum degree of the vacuum defoaming is-0.9-0.96 KPa; and respectively carrying out tape casting on the mixed slurry containing different pigment concentrations to obtain tape casting sheets containing different pigment concentrations.
Further, in step S4, the casting temperature is 45-80 ℃, and the thickness of the obtained casting sheet is less than 0.2 mm.
Step S5: and (3) sequentially superposing the casting sheets according to the pigment content from high to low, and carrying out isostatic pressing to obtain a green body.
Step S6: and sequentially carrying out glue removal treatment and sintering treatment on the green body to obtain the gradient-color ceramic material.
Furthermore, in the sintering process, the heating rate is not higher than 10.0 ℃/min, abnormal growth of crystal grains is avoided, the compactness of the ceramic is ensured, and the color presenting effect is further improved; the sintering temperature is 1300-1600 ℃, in order to ensure the color development effect, the highest sintering temperature is preferably 1350-1450 ℃, so that the color development temperature of the pigment is matched with the highest sintering temperature, the highest sintering temperature is not higher than the optimal color development temperature of the pigment, the lowest calcining temperature is the same as the using temperature of the pigment, the color development effect is further improved, and the appearance of the ceramic material is improved.
Specifically, when the gradient-color ceramic material with the same color is prepared, the same colored oxide is selected as a pigment to be graded according to the addition proportion, so that the preparation of the gradient-color ceramic material with the same color is realized; when the gradual change between the two colors is prepared, two coloring oxides with different colors are selected for mixing and gradual change of the addition content of the toner, the color transition is easily generated between the middle color and the two colors, and the transition color is overlapped between the two different colors, so that the gradual change ceramic material between the two colors is prepared.
The ceramic powder comprises at least one of zirconium oxide powder, aluminum oxide powder, silicon carbide powder, silicon nitride powder and boron nitride powder, and in order to ensure that the gradient-color ceramic material is healthy and nontoxic when in long-term contact with a human body, the coloring material adopts coloring oxide, green color can be selected from 2CoO.TiO2, blue color can be selected from CoO.Al2O3, grey color can be selected from CuO.Al2O3, black color can be selected from FeO.Fe2O3, dark color can be selected from MnO.Al2O3, brown color can be selected from one of ZnO-Al2O3-Fe2O3-Cr2O3, ZnO-Al2O3-Fe2O3-MnO2 and ZnO-Al2O3-Fe2O3-Cr2O3-MnO 2.
The following detailed description of specific implementations of the present invention is provided in conjunction with specific embodiments:
example 1
Step S1: 100 g of zirconia ceramic powder and 1 g of ethoxy compound are added into 50 g of azeotropic mixture solvent consisting of water and ethanol for ball milling and uniform dispersion, and a first mixture is obtained.
Step S2: adding 1 g of plasticizer and 2 g of adhesive into the first mixture in sequence, specifically, adding the plasticizer from the surface of the first mixture to form a plasticizer film on the surface of the first mixture, adding the adhesive into the plasticizer film, and uniformly mixing after the adhesive is dissolved in the plasticizer to obtain a second mixture.
Step S3: uniformly dividing the second mixture into 5 parts, sequentially adding a coloring oxide CoO.Al2O3 serving as a coloring material into each second mixture according to the weight percentages of 0.10 wt%, 0.15 wt%, 0.20 wt%, 0.25 wt% and 0.30 wt% of the zirconia ceramic powder, carrying out grading ball milling and uniform dispersion to ensure that the average particle size D50 of the zirconia ceramic powder is 0.1-1.0 micron, wherein the maximum particle size D100 is not more than twice of the average particle size D50, uniformly mixing to obtain 5 parts of mixed slurry with different pigment concentrations, and sequentially numbering the mixed slurry according to the pigment concentration from low to high by 1-1, 1-2, 1-3, 1-4 and 1-5.
Step S4: and (3) respectively carrying out vacuum defoaming on 5 parts of mixed slurry under the vacuum degree of 0.2KPa for 30min, carrying out independent casting after defoaming to obtain casting sheets with different pigment concentrations, wherein the specific casting process parameters are as follows: the casting temperature was 70 ℃ and the casting speed was 1.5m/min, and the thickness of the obtained cast sheet was 0.1 mm.
Step S5: and (3) superposing the tape casting sheet once from high to low according to the pigment concentration, and carrying out isostatic compaction for 3min under the conditions of the temperature of 75 ℃ and the pressure of 50Mpa to obtain green bodies with different pigment concentrations.
Step S6: and (3) placing the green body into a glue discharging furnace for discharging glue, heating at the temperature lower than 350 ℃ at the heating rate of 0.5 ℃/min, heating at the temperature between 350 ℃ and 650 ℃ at the heating rate of 1 ℃/min, and keeping the temperature at 650 ℃ for 60 min. And (3) after removing the glue, placing the mixture in a sintering furnace to be heated and sintered in the air atmosphere, heating at the temperature lower than 1000 ℃ by adopting the heating rate of 5 ℃/min, preserving the heat at 1000 ℃ for 60min, heating at the temperature of 1000-1450 ℃ by adopting the heating rate of 2.0 ℃/min, preserving the heat at 1450 ℃ for 120min, and then cooling along with the furnace to obtain the blue gradient-color ceramic material.
Example 2
Step S1: 100 g of zirconia ceramic powder and 1 g of ethoxy compound are added into 50 g of azeotropic mixture solvent consisting of water and ethanol for ball milling and uniform dispersion, and a first mixture is obtained.
Step S2: 1 g of plasticizer and 2 g of binder were simultaneously added to the first mixture and ball-milled and uniformly dispersed to obtain a second mixture.
Step S3: dividing the second mixture into 5 parts, adding a coloring oxide 2CoO. TiO2 serving as a coloring material into each part of the second mixture in sequence according to the content of 0.10 wt%, 0.15 wt%, 0.20 wt%, 0.25 wt% and 0.30 wt% of the zirconia ceramic powder, configuring the coloring material into a solution, adding the coloring material into 5 parts of the second mixture in a pulse mode respectively, wherein the pulse frequency ratio is 1:2:3:4:5, uniformly mixing to obtain 5 parts of mixed slurry with different coloring material concentrations, and numbering the mixed slurry according to the coloring material concentration from low to high as 2-1, 2-2, 2-3, 2-4 and 2-5 in sequence.
Step S4: and (3) respectively carrying out vacuum defoaming on 5 parts of mixed slurry under the vacuum degree of 0.2KPa for 30min, and carrying out independent casting after defoaming to obtain casting sheets with different pigment concentrations, wherein the specific casting process parameters are as follows: the casting temperature was 70 ℃ and the casting speed was 1.5m/min, and the thickness of the obtained cast sheet was 0.1 mm.
Step S5: and (3) superposing the tape casting sheet once from high to low according to the pigment concentration, and carrying out isostatic compaction for 3min under the conditions of the temperature of 75 ℃ and the pressure of 50Mpa to obtain green bodies with different pigment concentrations.
Step S6: and (3) placing the green body into a glue discharging furnace for discharging glue, heating at the temperature lower than 350 ℃ at the heating rate of 0.5 ℃/min, heating at the temperature between 350 ℃ and 650 ℃ at the heating rate of 1 ℃/min, and keeping the temperature at 650 ℃ for 60 min. And (3) after removing the glue, placing the mixture in a sintering furnace to be heated and sintered in the air atmosphere, heating at the temperature lower than 1000 ℃ by adopting the heating rate of 5 ℃/min, preserving the heat at 1000 ℃ for 60min, heating at the temperature of 1000-1430 ℃ by adopting the heating rate of 2.0 ℃/min, preserving the heat at 1450 ℃ for 120min, and then cooling along with the furnace to obtain the green gradient-color ceramic material.
Example 3
Step S1: 100 g of zirconia ceramic powder and 1 g of ethoxy compound are added into 50 g of azeotropic mixture solvent consisting of water and ethanol for ball milling and uniform dispersion, and a first mixture is obtained.
Step S2: 1 g of plasticizer and 2 g of binder are added into the first mixture at the same time, and the mixture is continuously ball-milled and uniformly dispersed to obtain a second mixture.
Step S3: uniformly dividing the second mixture into 5 parts, sequentially adding a coloring oxide ZnO-Al2O3-Fe2O3-Cr2O3 serving as a coloring material into each second mixture according to the weight percentage of 0.10 wt%, 0.15 wt%, 0.20 wt%, 0.25 wt% and 0.30 wt% of the zirconia ceramic powder, carrying out graded ball milling and uniform dispersion to ensure that the average grain diameter D50 of the zirconia ceramic powder is 0.1-1.0 micron, wherein the maximum grain diameter D100 is not more than twice of the average grain diameter D50, uniformly mixing to obtain 5 parts of mixed slurry with different pigment concentrations, and sequentially numbering the mixed slurry according to the pigment concentration from low to high by 3-1, 3-2, 3-3, 3-4 and 3-5.
Step S4: and (3) respectively carrying out vacuum defoaming on 5 parts of mixed slurry under the vacuum degree of 0.2KPa for 30min, and carrying out independent casting after defoaming to obtain casting sheets with different pigment concentrations, wherein the specific casting process parameters are as follows: the casting temperature was 70 ℃ and the casting speed was 1.5m/min, and the thickness of the obtained cast sheet was 0.1 mm.
Step S5: and (3) superposing the tape casting sheet once from high to low according to the pigment concentration, and carrying out isostatic compaction for 3min under the conditions of the temperature of 75 ℃ and the pressure of 50Mpa to obtain green bodies with different pigment concentrations.
Step S6: and (3) placing the green body into a glue discharging furnace for discharging glue, heating at the temperature lower than 350 ℃ at the heating rate of 0.5 ℃/min, heating at the temperature between 350 ℃ and 650 ℃ at the heating rate of 1 ℃/min, and keeping the temperature at 650 ℃ for 60 min. And (3) after removing the glue, placing the mixture in a sintering furnace to be heated and sintered in the air atmosphere, heating at the temperature lower than 1000 ℃ by adopting the heating rate of 5 ℃/min, preserving the heat at 1000 ℃ for 60min, heating at the temperature between 1000 ℃ and 1400 ℃ by adopting the heating rate of 2.0 ℃/min, preserving the heat at 1400 ℃ for 120min, and then cooling along with the furnace to obtain the brown gradient-color ceramic material.
TABLE 1 color value Table for examples 1-3
In the embodiment of the invention, the pigments with continuously changed mass gradients are respectively added into the ceramic mixtures which correspond one by one to be uniformly mixed, the casting sheets with continuously changed pigment content gradients are obtained through independent casting, the casting sheets are sequentially overlapped in sequence from high to low in pigment content, and then the ceramic materials with gradually changed colors are obtained through isostatic pressing, binder removal and sintering. The preparation method disclosed by the invention is simple, the ceramic material is uniform in color transition, rich and attractive in color, environment-friendly and safe, and the appearance of the ceramic material is improved on the basis of excellent corrosion resistance and wear resistance of the ceramic material.
The present invention is not limited to the above embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a gradient-color ceramic material is characterized by comprising the following steps:
step S1: mixing an azeotropic mixture solvent, a dispersant and ceramic powder to obtain a first mixture;
step S2: adding a plasticizer and a binder into the first mixture and mixing to obtain a second mixture;
step S3: respectively adding the pigments with continuously changed mass gradients into the second mixture to respectively obtain mixed slurry with continuously changed pigment concentration gradients;
step S4: respectively carrying out tape casting on the mixed slurry containing the continuous change of the pigment concentration gradient to obtain tape casting sheets containing the continuous change of the pigment concentration gradient;
step S5: sequentially superposing the casting sheets according to the pigment content from high to low, and carrying out isostatic pressing to obtain a green body;
step S6: and sequentially carrying out glue removal treatment and sintering treatment on the green body to obtain the gradient-color ceramic material.
2. The method of claim 1, wherein said cast sheet having a continuous gradient of color concentration is a cast sheet having a gradient of color concentration in an arithmetic progression.
3. The method for preparing a gradient-color ceramic material according to claim 1, wherein the step S3 specifically comprises:
respectively adding the pigment with continuously changed mass gradient into the second mixture for graded ball milling to respectively obtain mixed slurry with continuously changed pigment concentration gradient;
or preparing the pigment into a pigment solution, and respectively spraying the pigment solution into the second mixture in a pulse mode according to the pulse times of continuous gradient change to respectively obtain mixed slurry containing the continuous gradient change of the pigment concentration.
4. The method of claim 3, wherein the average particle size D50 of the ceramic powder in the mixed slurry after the ball milling in step S3 is 0.1-1.0 μm, and wherein the maximum particle size D100 is not greater than twice the average particle size D50.
5. The method of claim 1, wherein the second mixture has a solids content of 40 to 70 wt%.
6. The method of claim 1, wherein the second mixture comprises 0.5 to 2.0 wt% of a dispersant, 0.5 to 2.0 wt% of a binder, and 0.1 to 2.0 wt% of a plasticizer.
7. The method for preparing a gradient-color ceramic material according to claim 1, wherein the mass ratio of the colorant to the ceramic powder in the tape-casting sheet is not more than 0.1, and the colorant is nano powder or micro-nano powder.
8. The method for preparing a gradient-color ceramic material according to claim 1, wherein the step S4 specifically comprises: respectively carrying out vacuum defoaming on the mixed slurry containing different pigment concentrations, wherein the vacuum degree of the vacuum defoaming is-0.9-0.96 KPa; and respectively carrying out tape casting on the mixed slurry containing different pigment concentrations to obtain tape casting sheets containing different pigment concentrations.
9. The method for preparing a gradient-color ceramic material according to claim 1, wherein in step S4, the casting temperature is 45-80 ℃, and the thickness of the obtained cast sheet is less than 0.2 mm.
10. The method for preparing a gradient-color ceramic material according to claim 1, wherein in the sintering process, the temperature rise rate is not higher than 10.0 ℃/min, and the sintering temperature is 1300-1600 ℃.
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