CN112250444A - Gradient ceramic and preparation method and application thereof - Google Patents
Gradient ceramic and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides gradient color ceramic and a preparation method and application thereof, wherein the preparation method comprises the following steps: stacking a plurality of layers of white transparent second film sheets and colored first film sheets to form a stacked body, wherein the first film sheets are clamped between the second film sheets, or stacking a plurality of layers of white opaque third film sheets, colored first film sheets and white transparent second film sheets to form a stacked body, wherein the first film sheets are clamped between the second film sheets and the third film sheets; carrying out isostatic pressing treatment, glue discharging and sintering on the stacked body in sequence to obtain composite ceramic; and processing the composite ceramic to obtain the gradient color ceramic, wherein in the processing process, the included angle formed by the feed route of the cutter on the composite ceramic and the stacking direction is 0-90 degrees. The preparation method is simple, and the prepared ceramic material presents gradual change colors, changes the condition that the existing ceramic material has single color, and presents better visual effect.
Description
Technical Field
The invention belongs to the technical field of ceramic material preparation, and particularly relates to gradient color ceramic and a preparation method and application thereof.
Background
The ceramic has excellent mechanical property and electrical property, but the ceramic is single in color and is not attractive when used for preparing products (such as shells of mobile equipment), the existing ceramic materials mostly adopt black and white, so that the visual impression of the prepared products is poor, the colored ceramic materials are sprayed with colored ink or paint on the back of the white ceramic, the mode is not environment-friendly and can fade for a long time, and in addition, the poor-quality ink or paint is not safe when contacting with a human body.
In view of the above, a gradient color ceramic, a preparation method and applications thereof are provided.
Disclosure of Invention
The invention aims to provide a gradient color ceramic and a preparation method and application thereof aiming at the defects in the prior art.
The object of the invention can be achieved by the following technical measures:
the invention provides a preparation method of gradient color ceramic, which comprises the following steps:
respectively carrying out tape casting on first ceramic slurry, second ceramic slurry and third ceramic slurry to form a film, and drying to obtain a corresponding first membrane, a corresponding second membrane and a corresponding third membrane, wherein the first membrane is a colored membrane, the second membrane is a white transparent membrane, and the third membrane is a white opaque membrane;
stacking a number of layers of the second membrane sheet and a first membrane sheet to form a stack in which the number of layers of the first membrane sheet is sandwiched between the number of layers of the second membrane sheet,
or, stacking a plurality of layers of the third membrane sheet, the first membrane sheet and the second membrane sheet to form a stacked body, wherein the plurality of layers of the first membrane sheet are clamped between the plurality of layers of the second membrane sheet and the plurality of layers of the third membrane sheet;
carrying out isostatic pressing treatment, glue discharging and sintering on the stacked body in sequence to obtain composite ceramic;
and processing the composite ceramic to obtain the gradient-color ceramic, wherein in the processing process, the included angle formed by the feed path of the cutter on the composite ceramic and the stacking direction is theta, and the theta is more than 0 degree and less than 90 degrees.
Preferably, the method further comprises preparing a ceramic slurry, specifically:
preparing first ceramic powder, second ceramic powder and third ceramic powder, wherein the first ceramic powder comprises zirconia powder, a stabilizer and pigment powder, the second ceramic powder comprises zirconia powder and a stabilizer, the third ceramic powder comprises zirconia powder, alumina powder and a stabilizer, the stabilizer powder comprises at least one of yttria, magnesia, calcium oxide and scandium oxide, and the pigment powder comprises metal oxide;
and respectively adding additives into the first ceramic powder, the second ceramic powder and the third ceramic powder, mixing and grinding to obtain grinding fluid, and filtering the grinding fluid through a micron-sized filter membrane to obtain first ceramic slurry, second ceramic slurry and third ceramic slurry.
Preferably, the step of adding additives to the first ceramic powder, the second ceramic powder and the third ceramic powder respectively, mixing and grinding to obtain the grinding fluid comprises:
and respectively adding a solvent, a defoaming agent and a dispersing agent into the first ceramic powder, the second ceramic powder and the third ceramic powder for ball milling, and adding a binder and a plasticizer for sand milling after ball milling.
Preferably, the conditions of the isostatic pressing treatment include that the isostatic pressing treatment is carried out under the conditions of the pressure of 100-300MPa and the temperature of 40-90 ℃.
Preferably, in the glue discharging process, when the glue discharging temperature is increased from room temperature to 500 ℃, the heating rate is 0.5 ℃/min, the heat preservation is carried out for 0.5-2h, when the glue discharging temperature is increased from 500 ℃ to 900 ℃, the heating rate is 1 ℃/min, the heat preservation is carried out for 1-3h under the condition of 900 ℃, and the ceramic biscuit is obtained.
Preferably, in the sintering process, the sintering atmosphere is argon, the sintering is carried out for 1-3h under the condition that the pressure is 20-180 MPa, the temperature is raised to the highest sintering temperature, and the hot isostatic pressing sintering is carried out under the condition that the highest sintering temperature is 1250-1550 ℃.
Preferably, in the sintering process, when the sintering temperature is increased from room temperature to 1300 ℃, the temperature rising speed is 5-10 ℃/min, the pressure in the furnace is increased from 30MPa to 150MPa, and the temperature is kept for 40-180 min; reducing the temperature from 1300 deg.C to 800 deg.C at 3-5 deg.C/min, and reducing the pressure from 150Mpa to 100 Mpa; cooling to room temperature at 800 deg.C at 5-10 deg.C, reducing pressure from 100Mpa to 10Mpa, maintaining pressure until pressure is released, opening the furnace, and taking out the product.
The invention also provides a gradient color ceramic prepared by the preparation method.
The invention also provides a shell which is made of the above gradient ceramic.
The invention also provides a mobile terminal which is characterized by comprising the shell.
The invention has the beneficial effects of providing the gradient color ceramic and the preparation method and the application thereof, wherein the preparation method comprises the following steps: stacking a plurality of layers of white transparent second membrane sheets and colored first membrane sheets to form a stacked body, wherein the plurality of layers of the first membrane sheets are clamped among the plurality of layers of the second membrane sheets, or stacking a plurality of layers of white opaque third membrane sheets, colored first membrane sheets and white transparent second membrane sheets to form a stacked body, and the plurality of layers of the first membrane sheets are clamped among the plurality of layers of the second membrane sheets and the plurality of layers of the third membrane sheets; carrying out isostatic pressing treatment, glue discharging and sintering on the stacked body in sequence to obtain composite ceramic; and processing the composite ceramic to obtain the gradient color ceramic, wherein in the processing process, the included angle formed by the feed route of the cutter on the composite ceramic and the stacking direction is 0-90 degrees. The preparation method is simple, and the prepared ceramic material presents gradual change colors, changes the condition that the existing ceramic material has single color, and presents better visual effect.
Drawings
FIG. 1 is a flow chart of a method for preparing a gradient color ceramic 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.
Referring to fig. 1, the present invention provides a method for preparing a gradient color ceramic, the method comprising the following steps:
in the step S100, the first ceramic slurry, the second ceramic slurry and the third ceramic slurry are respectively cast into films and then dried to obtain a corresponding first membrane, a corresponding second membrane and a corresponding third membrane, where the first membrane is a colored membrane, the second membrane is a white transparent membrane, and the third membrane is a white opaque membrane.
Optionally, in step S100, preparing a ceramic slurry, specifically: preparing first ceramic powder, second ceramic powder and third ceramic powder, wherein the first ceramic powder comprises zirconium oxide powder, a stabilizer and pigment powder; the second ceramic powder comprises zirconium oxide powder and a stabilizer; the third ceramic powder comprises zirconium oxide powder, aluminum oxide powder and a stabilizer; the stabilizer powder comprises at least one of yttrium oxide, magnesium oxide, calcium oxide and scandium oxide; the colorant powder includes a metal oxide.
And respectively adding additives into the first ceramic powder, the second ceramic powder and the third ceramic powder, mixing, grinding to obtain grinding fluid, and filtering the grinding fluid through micron-sized filter membranes to obtain first ceramic slurry, second ceramic slurry and third ceramic slurry.
Optionally, in the process of obtaining the grinding fluid, the first ceramic powder, the second ceramic powder and the third ceramic powder are respectively added with a solvent, a defoaming agent and a dispersing agent for ball milling, and then a binder and a plasticizer are added for sand milling after ball milling.
Specifically, 100 parts by weight of zirconia powder (the grain diameter is less than 300nm, the purity is 99.95-99.99%), 2-10 parts of stable phase (yttrium oxide, magnesium oxide, calcium oxide or scandium oxide and the like) and 1-20 parts by weight of pigment are mixed; putting zirconium oxide powder, a stabilizer and pigment powder into a ball milling tank (ball milling grinding speed is low, ball milling medium is large, homogenization treatment is performed in the early stage) for first grinding, adding a solvent, a defoaming agent and a dispersing agent into the ball milling tank in sequence, performing ball milling for 12-48h, adding a binder and a plasticizer into the ball milling tank in sequence, grinding for 1-10h by using a sand mill (the sand mill is high in speed and 0.3-1mm in ball diameter), and filtering grinding liquid by using a 0.2-0.5 micron filter membrane to obtain color membrane tape casting slurry, namely first ceramic slurry.
And (3) placing the first ceramic slurry in a vacuum device to remove bubbles, then carrying out tape casting by using a tape casting machine under the condition that the height of a tape casting knife edge is 50-1500 mu m, and drying after tape casting to obtain a color film body membrane, namely the first membrane.
Preparing 100 parts by weight of zirconia powder (the grain diameter is less than 300nm, and the purity is 99.95-99.99%) and 2-10 parts of stabilizer (yttrium oxide, magnesium oxide, calcium oxide or scandium oxide); putting zirconium oxide powder and a stabilizing agent into a ball milling tank (ball milling grinding speed is low, ball milling medium is high, homogenization treatment is performed in the early stage) for first grinding, adding a solvent, a defoaming agent and a dispersing agent into the ball milling tank in sequence, carrying out ball milling for 12-36h, then adding a binder and a plasticizer into the ball milling tank in sequence, grinding for 1-10h by using a sand mill (the speed of the sand mill is high, the grinding diameter is 0.3-1mm), and filtering grinding liquid by using a 0.2-0.5 micron filter membrane to obtain transparent membrane tape casting slurry, namely second ceramic slurry.
Preparing 100 parts by weight of zirconia powder (the grain diameter is less than 300nm, the purity is 99.95-99.99%), 2-10 parts of stable phase (yttrium oxide, magnesium oxide, calcium oxide or scandium oxide) and 5-25 parts by weight of alumina, wherein the grain diameter of the alumina is 10-150 nm; the rest is the same as the transparent one, and a white opaque film matrix membrane is prepared.
And respectively placing the second ceramic slurry and the third ceramic slurry in a vacuum device to remove bubbles, then carrying out tape casting by using a tape casting machine under the condition that the height of a tape casting knife edge is 50-1500 mu m, and respectively carrying out tape casting and drying to obtain a white transparent film matrix membrane and a white opaque film matrix membrane, namely the white transparent film matrix membrane and the white opaque film matrix membrane respectively correspond to the second membrane and the third membrane.
In step S200, a plurality of layers of the second film sheets and the first film sheet are stacked to form a stacked body, in which the plurality of layers of the first film sheets are sandwiched between the plurality of layers of the second film sheets.
Or, stacking a plurality of layers of the third membrane sheet, the first membrane sheet and the second membrane sheet to form a stacked body, wherein the plurality of layers of the first membrane sheet are clamped between the plurality of layers of the second membrane sheet and the plurality of layers of the third membrane sheet.
In step S300, the stacked body is subjected to isostatic pressing, binder removal, and sintering in sequence to obtain the composite ceramic.
Specifically, the conditions of the isostatic pressing treatment include subjecting the stacked body to the isostatic pressing treatment under the conditions of a pressure of 100-300MPa and a temperature of 40-90 ℃.
Specifically, in the glue discharging process, when the glue discharging temperature is increased from room temperature to 500 ℃, the heating rate is 0.5 ℃/min, the heat preservation is carried out for 0.5-2h, when the glue discharging temperature is increased from 500 ℃ to 900 ℃, the heating rate is 1 ℃/min, the heat preservation is carried out for 1-3h under the condition of 900 ℃, and the ceramic biscuit is obtained.
Specifically, in the sintering process, the ceramic biscuit is placed in a high-pressure container of a high-temperature furnace, the sintering atmosphere is argon, the temperature is raised to the highest sintering temperature under the pressure of 20MPa-180MPa, then isostatic pressing sintering is carried out for 1-3h, and the hot isostatic pressing sintering is carried out under the condition that the highest sintering temperature is 1250-1550 ℃. In the sintering process, when the sintering temperature is increased from room temperature to 1300 ℃, the temperature rising speed is 5-10 ℃/min, the pressure in the furnace is increased from 30MPa to 150MPa, and the temperature is kept for 40-180 min; reducing the temperature from 1300 deg.C to 800 deg.C at 3-5 deg.C/min, and reducing the pressure from 150Mpa to 100 Mpa; cooling to room temperature at 800 deg.C at 5-10 deg.C, reducing pressure from 100Mpa to 10Mpa, maintaining pressure until pressure is released, opening the furnace, and taking out the product.
In step S400, the composite ceramic is processed to obtain a gradient color ceramic, and in the processing process, an included angle formed by a feed path of a tool on the composite ceramic and a stacking direction is θ, where θ is greater than 0 ° < θ <90 °.
Specifically, the gradual change interval is determined by the included angle between the cutter feed path and the stacking direction (the stacking direction of the plurality of first membranes and the second membranes or the stacking direction of the plurality of first membranes, the second membranes and the third membranes), and the larger the included angle is, the narrower the gradual change interval is.
If the stacked body is in a structure that a plurality of layers of first membranes are stacked among a plurality of layers of second membranes, the stacked body is processed to obtain the double-sided gradient-color ceramic. The double-sided gradual change has the scattering effect of double-sided multiple light, and the gradual change effect is more natural and real. In an embodiment of the invention, the stack has a stack structure of: 18 layers of second membrane sheets +4 layers of first membrane sheets +18 layers of second membrane sheets, the thickness of the stacked body is 0.5-1.0mm, and the thickness of each membrane sheet after the first membrane sheet, the second membrane sheet and the third membrane sheet are sintered is 25 micrometers. After processing, the thickness of the 18-layer second film sheets on both sides was continuously changed with respect to the thickness of the 4-layer first film sheet in the middle, that is, the thickness of the white transparent film sheets on both sides of the colored film sheet in the middle was changed, so that the lower the thickness, the greater the transparency, and for the transparent zirconia (second film sheet) in the embodiment of the present invention: when the thickness is 0.5-1.0mm, the transparency TP is 5-20, therefore, the double-sided gradient color ceramic can be formed.
If the stacked body is in a structure that a plurality of layers of first membrane sheets are stacked between a plurality of layers of second membrane sheets and a plurality of layers of third membrane sheets, the single-side gradually-changed ceramic is formed. In an embodiment of the invention, the stack has a stack structure of: 18 layers of second membrane sheets +4 layers of first membrane sheets +18 layers of third membrane sheets, the thickness of the stacked body is 0.5-1.0mm, and the thickness of each membrane sheet after the first membrane sheet, the second membrane sheet and the third membrane sheet are sintered is 25 micrometers. After processing, the thickness of the 18-layer second film sheet on one side was continuously changed with respect to the thickness of the 4-layer first film sheet in the middle, that is, the thickness of the white transparent film sheet on the side of the colored film sheet in the middle was changed so that the lower the thickness was, the greater the transparency was, as seen from the side of the white transparent film sheet, and for the transparent zirconia (second film sheet) in the example of the present invention: when the thickness is 0.5-1.0mm, the transparency TP is 5-20, and the zirconia ceramic added with alumina (third membrane): when the thickness is 0.5-1.0mm, the transparency TP is lower than 2, and the ceramic can be seen visually and can be regarded as opaque, so that the single-sided gradient color ceramic can be formed.
Based on the preparation method of the gradient ceramic, the invention also provides the gradient ceramic, and the gradient ceramic is prepared by the preparation method. The ceramic with the gradually changed colors has rich color levels, better visual effect than single color, and gradually changed and diversified colors.
The invention also provides a shell which is made of the gradient ceramic. In the embodiment of the invention, the shell prepared from the gradient ceramic has high-grade texture and hand feeling, and meanwhile, the color is gradually varied, so that a better visual effect can be realized, and the appearance is attractive. Meanwhile, as the colorant is a non-toxic and safe colored oxide, the colorant can also ensure safety and non-toxicity in the using and contacting processes.
The invention also provides a mobile terminal which comprises the shell. Of course, those skilled in the art will appreciate that the mobile terminal has all the features and advantages of the previous gradient color ceramic and the casing, and thus, the detailed description thereof is omitted. According to the embodiment of the invention, the specific type of the mobile terminal has no limitation requirement, and a person skilled in the art can flexibly select the mobile terminal according to actual requirements. In some embodiments of the present invention, specific types of mobile terminals include, but are not limited to, mobile phones, notebooks, game consoles, and other electronic devices. Of course, it can be understood by those skilled in the art that the electronic device includes the necessary structures or components of the conventional electronic device besides the front housing, and in addition to the front housing, the mobile phone includes the necessary structures or components such as a display panel, a glass cover plate, a CPU processor, a camera module, a voice module, a touch module, and the like. The understanding is further enhanced by the following specific examples and comparative examples.
The present invention is not limited to the above preferred 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 gradient color ceramic is characterized by comprising the following steps:
respectively carrying out tape casting on first ceramic slurry, second ceramic slurry and third ceramic slurry to form a film, and drying to obtain a corresponding first membrane, a corresponding second membrane and a corresponding third membrane, wherein the first membrane is a colored membrane, the second membrane is a white transparent membrane, and the third membrane is a white opaque membrane;
stacking a number of layers of the second membrane sheet and a first membrane sheet to form a stack in which the number of layers of the first membrane sheet is sandwiched between the number of layers of the second membrane sheet,
or, stacking a plurality of layers of the third membrane sheet, the first membrane sheet and the second membrane sheet to form a stacked body, wherein the plurality of layers of the first membrane sheet are clamped between the plurality of layers of the second membrane sheet and the plurality of layers of the third membrane sheet;
carrying out isostatic pressing treatment, glue discharging and sintering on the stacked body in sequence to obtain composite ceramic;
and processing the composite ceramic to obtain the gradient-color ceramic, wherein in the processing process, the included angle formed by the feed path of the cutter on the composite ceramic and the stacking direction is theta, and the theta is more than 0 degree and less than 90 degrees.
2. The method of preparing a gradient color ceramic according to claim 1, further comprising preparing a ceramic slurry, specifically:
preparing first ceramic powder, second ceramic powder and third ceramic powder, wherein the first ceramic powder comprises zirconia powder, a stabilizer and pigment powder, the second ceramic powder comprises zirconia powder and a stabilizer, the third ceramic powder comprises zirconia powder, alumina powder and a stabilizer, the stabilizer powder comprises at least one of yttria, magnesia, calcium oxide and scandium oxide, and the pigment powder comprises metal oxide;
and respectively adding additives into the first ceramic powder, the second ceramic powder and the third ceramic powder, mixing and grinding to obtain grinding fluid, and filtering the grinding fluid through a micron-sized filter membrane to obtain first ceramic slurry, second ceramic slurry and third ceramic slurry.
3. The method of preparing a gradient color ceramic according to claim 2,
the grinding fluid obtained by respectively adding additives into the first ceramic powder, the second ceramic powder and the third ceramic powder, mixing and grinding the mixture comprises the following components:
and respectively adding a solvent, a defoaming agent and a dispersing agent into the first ceramic powder, the second ceramic powder and the third ceramic powder for ball milling, and adding a binder and a plasticizer for sand milling after ball milling.
4. The method of preparing a gradient color ceramic according to claim 1,
the conditions of the isostatic pressing treatment comprise that the isostatic pressing treatment is carried out under the conditions of the pressure of 100-300MPa and the temperature of 40-90 ℃.
5. The method of preparing a gradient color ceramic according to claim 1,
in the glue discharging process, when the glue discharging temperature is increased from room temperature to 500 ℃, the heating rate is 0.5 ℃/min, the heat preservation is carried out for 0.5-2h, when the glue discharging temperature is increased from 500 ℃ to 900 ℃, the heating rate is 1 ℃/min, the heat preservation is carried out for 1-3h under the condition of 900 ℃, and the ceramic biscuit is obtained.
6. The method of preparing a gradient color ceramic according to claim 1,
in the sintering process, the sintering atmosphere is argon, the temperature is raised to the highest sintering temperature under the pressure of 20MPa-180MPa, then isostatic pressing sintering is carried out for 1-3h, and the hot isostatic pressing sintering is carried out under the condition that the highest sintering temperature is 1250-1550 ℃.
7. The method of preparing a gradient color ceramic according to claim 6,
in the sintering process, when the sintering temperature is increased from room temperature to 1300 ℃, the temperature rising speed is 5-10 ℃/min, the pressure in the furnace is increased from 30MPa to 150MPa, and the temperature is kept for 40-180 min; reducing the temperature from 1300 deg.C to 800 deg.C at 3-5 deg.C/min, and reducing the pressure from 150Mpa to 100 Mpa; cooling to room temperature at 800 deg.C at 5-10 deg.C, reducing pressure from 100Mpa to 10Mpa, maintaining pressure until pressure is released, opening the furnace, and taking out the product.
8. A gradient ceramic, which is prepared by the preparation method of any one of claims 1 to 7.
9. A housing made from the gradient ceramic of claim 8.
10. A mobile terminal, characterized in that it comprises a housing according to claim 9.
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