CN111087241A - Preparation process of colorful ceramic product with imitated natural texture and colorful ceramic product - Google Patents
Preparation process of colorful ceramic product with imitated natural texture and colorful ceramic product Download PDFInfo
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Abstract
A preparation process of a colorful ceramic product with imitated natural textures comprises pretreatment, material selection, grading treatment, proportioning preparation, iron removal, drying, press forming, metallographic detection, isostatic pressing, degreasing and sintering; wherein the material selection refers to selecting the re-granulation granular zirconium oxide ceramic powder with the grain diameter of 0.4-0.6 mu m, the B.E.T specific surface area of 8-10 square meters per gram and the granularity of 50-100 meshes, wherein the re-granulation grains with 50-60 meshes account for 75-80 percent and the re-granulation grains with 70-100 meshes account for 20-25 percent; the grading treatment is to grade the re-granulated granular zirconia ceramic powder of 50-100 meshes and separate the re-granulated granular zirconia ceramic powder of 50-60 meshes in low mesh number and 70-100 meshes in high mesh number; the mixture ratio is prepared according to the ratio of 100 of the low mesh number to the high mesh number: 5-13, and preparing the synthetic powder. The preparation process can make the ceramic product present various colors, realize the color consistency of the inside and outside of the colorful ceramic product, and does not influence the luster, texture and performance of the ceramic.
Description
Technical Field
The invention relates to the technical field of colorful ceramics, in particular to a preparation process of a colorful ceramic product with imitated natural textures and the colorful ceramic product.
Background
At present, along with excellent performance and rapid research and development progress of ceramics, the application of the ceramics in various fields is more and more prominent, various structural ceramics and functional ceramics represented by smart phones, watch wearing and living goods are closely related to the life of human beings, a plurality of representative enterprises generate strong interest in the ceramics, and the ceramics are widely applied and developed in products of the structural ceramics and the functional ceramics, wherein the appearance and the surface treatment of the products are always the key points of the ceramic development, the existing ceramics are biased to be monochromatic, the color number is single, the distribution is narrow and less, and the color distribution of the existing ceramics cannot be compared with the color distribution of plastics and hardware, if the color appearance needs to be realized, the surface treatment needs to be carried out after the traditional processing technology, such as glazing, sand blasting, color printing, NMT non-damage micrometering technology and the like, but the luster, the texture and partial performance of the ceramics are greatly discounted, and the multiple colors are limited to the surface of the product only.
Because of the special property of the ceramic material, the ceramic material is directly made to have multiple colors, and is greatly limited, the sintering shrinkage rates of the ceramics with different colors are inconsistent, the ceramics are molded and sintered after being directly mixed, the ceramics can deform and even crack after being sintered, the particles with different colors are difficult to combine together, the sintering temperatures of the ceramics with different colors, which are stable in crystalline phase, are inconsistent, the performance of the ceramic blank with multiple colors is difficult to meet and guarantee simultaneously, the ceramics with different colors have color migration and permeation phenomena in the sintering process, and the color boundary is not obvious. In addition, the existing colorful ceramic preparation process has the following defects:
the prior art has the defects that: the preparation process of the powder has strict requirements, and the research and development are continuously required to improve the consistency of the prepared powder particles and the purity of the powder, so that the cost is increased;
the prior art has the following defects: because the affinity of different auxiliary material powder and main powder of the colorful ceramic is difficult to control, the requirements on the selection of the powder and the degreasing sintering conditions are very high;
the prior art has three defects: the ceramic product has a single color, and is excessively dependent on other surface treatment processes to obtain colorful ceramic, so that the process is elongated, the cost is high, and the luster, texture and performance of the ceramic are affected.
Disclosure of Invention
The invention aims to provide a preparation process of a colorful ceramic product with imitated natural textures and the colorful ceramic product, which can enable the ceramic product to present multiple colors, realize the color consistency of the inside and the outside of the colorful ceramic product, and do not influence the luster, the texture and partial performance of the ceramic product.
In order to achieve the above object, in one aspect, the invention provides a process for preparing a natural-grain-imitated multicolor ceramic product, which comprises the following steps:
s1, preprocessing, namely putting a plurality of single-color zirconia ceramic powder materials with single color into a drying oven for drying treatment so as to enable the water content of the powder materials to be lower than 0.5%, and respectively carrying out repeated granulation process on the powder materials to prepare re-granulated particles;
s2, selecting materials, namely selecting re-granulated zirconia ceramic powder with the grain diameter of 0.4-0.6 mu m, the specific surface area of B.E.T. of 8-10 square meters per gram and the granularity of 50-100 meshes, wherein the re-granulated grains with 50-60 meshes account for 75-80 percent, and the re-granulated grains with 70-100 meshes account for 20-25 percent;
s3, grading treatment, namely grading the re-granulated granular zirconia ceramic powder of 50-100 meshes to separate a low-mesh granular zirconia ceramic powder of 50-60 meshes and a high-mesh granular zirconia ceramic powder of 70-100 meshes;
s4, preparing a mixture, namely preparing the graded re-granulated particle zirconia ceramic powder according to the ratio of the low mesh number to the high mesh number of 100: 5-13, preparing synthetic powder by using synthetic equipment;
s5, removing iron, namely removing iron from the synthetic powder prepared according to the proportion through an iron remover;
s6, drying, namely putting the synthesized powder into an oven for drying treatment, wherein the temperature of the oven is 40-60 ℃, and the drying time is 0.5-2 h;
s7, pressing and forming, namely pressing and forming the dried synthetic powder into a primary blank by using dry pressing equipment, wherein the unit pressure of the dry pressing equipment is not lower than 10 Mpa;
s8, performing metallographic detection, namely judging whether the synthetic powder particles are thoroughly crushed or not by performing metallographic detection on the primary blank subjected to compression molding;
s9, isostatic pressing, namely carrying out isostatic pressing treatment on the primary blank subjected to metallographic detection, wherein the pressure is 200-220 Mpa, and the pressure maintaining time is 5-10 min;
and S10, degreasing and sintering, namely firstly, carrying out green body processing on the primary blank body subjected to isostatic pressing treatment to obtain the specification and shape required by the colorful ceramic product, and then carrying out glue removal and sintering molding through degreasing and sintering equipment.
As a further improvement, the step S10 is followed by the following steps:
s11, index detection is carried out, the index detection is carried out on the degreased and sintered and formed colorful ceramic product, and whether each performance index of the degreased and sintered and formed colorful ceramic product is qualified or not is determined;
s12, machining, namely machining the colorful ceramic product qualified in index detection to obtain the size and shape of the colorful ceramic product with the required precision;
s13, surface treatment, namely performing surface treatment on the machined colorful ceramic product to improve the glossiness of the surface of the colorful ceramic product;
s14, performance detection, namely detecting the performance indexes of strength, fracture toughness, falling balls and ROR of the surface-treated colorful ceramic product to judge whether the product is qualified or not so as to obtain a colorful ceramic product with qualified performance indexes.
As a further improvement, the step S12 specifically includes the following steps:
s12-1, coarse grinding, namely, performing coarse grinding processing on the colorful ceramic product with qualified index detection through a coarse grinding machine;
s12-2, performing fine grinding, and performing fine grinding processing on the coarse-ground colorful ceramic product through a fine grinder;
and S12-3, grinding, and finally grinding the finely ground colorful ceramic product.
As a further improvement, the step S13 specifically includes the following steps:
s13-1, performing sweeping surface treatment on the machined colorful ceramic product through a sweeping machine;
s13-2, polishing, and then performing polishing surface treatment on the colorful ceramic product after the surface treatment by a polishing machine;
s13-3, ultrasonic cleaning, and finally ultrasonic cleaning the colorful ceramic product after the polishing surface treatment.
As a further improvement, the step S2 specifically includes the following steps:
s2-01, carrying out particle size analysis on the re-granulated particle zirconia ceramic powder by a laser particle size analyzer to select the re-granulated particle zirconia ceramic powder with the particle size of 0.4-0.6 mu m and the B.E.T specific surface area of 8-10 square meters per gram;
s2-02, screening the granularity, and screening the re-granulated zirconia ceramic powder with the granularity of 50-100 meshes by using a vibration screening machine.
As a further improvement, the content of yttrium in the re-granulated zirconia ceramic powder selected in the step S2-01 is 2.5-3%.
As a further improvement, the degreasing sintering process in the step S10 has four sintering temperature sections of a low temperature region, a medium temperature region, a high temperature region and a cooling temperature region, wherein the temperature of the low temperature region is less than 800 ℃, the temperature of the medium temperature region is 800-950 ℃, and the temperature of the high temperature region is 1300-1600 ℃.
As a further improvement, the steps S1-S10 are all completed in a dust-free workshop.
On the other hand, the technical scheme of the invention also provides a colorful ceramic product, and the colorful ceramic product is prepared by the preparation process in any one of the technical schemes.
As a further improvement, the colorful ceramic product is a mobile phone product or a watch product.
In summary, the technical scheme of the invention has the following beneficial effects: the preparation process of the natural texture imitating colorful ceramic product enables the ceramic product to present various colors in order to meet the requirements of different customers, perfectly solves the technical problem that the colorful ceramic is applied to appearance structural parts and functional parts under the condition of not influencing the luster, the texture and partial physical properties of the ceramic, and can realize mass production on the existing ceramic production process. In the actual production process, the preparation process of the colorful ceramic product prepares the synthetic powder through grading treatment and specific proportion, overcomes the phenomenon of extremely easy color migration and diffusion existing in the co-firing of various powders, directly completes the manufacturing procedure of the appearance effect at the initial stage of molding, reduces the subsequent procedure flow and saves the cost.
In addition, the appearance effect of the colorful ceramic product manufactured by the preparation process is different from the appearance effect of the colorful ceramic product manufactured by the traditional methods such as sand blasting, glazing, color printing and the like, the colorful ceramic product manufactured by the preparation process is more natural and vivid in texture, the luster, the texture and partial performances of the ceramic product are not influenced, and the partial performances comprise strength, hardness, density, fracture toughness, elastic modulus, thermal expansion coefficient and the like.
Drawings
FIG. 1 is a flow chart of a process for preparing a colorful ceramic product with natural texture.
Detailed Description
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, but the technical solutions in the embodiments of the present invention are not limited to the scope of the present invention.
The embodiment provides a preparation process of a colorful ceramic product with imitated natural textures, which is a brand-new preparation method for the appearance effect of the colorful ceramic product, enriches the appearance effect and the completion mode of the colorful ceramic product, is different from other existing popular ceramic appearance treatment methods, has more direct and vivid appearance effect, ensures the luster and texture of the ceramic product, and simultaneously ensures the performance index of the whole ceramic product to meet the standard requirement. On the basis of not depending on other materials and processes, the preparation of the multicolor ceramic powder is completed directly from the powder, the process breakthrough of the ceramic from white and black to various single colors to multicolor is realized, the technical problems of poor affinity and difficult degreasing sintering of different color series ceramics are overcome, breakthrough openings are searched at two ends of the material and the degreasing sintering process curve together, the preparation requirements and the process requirements which meet various color series ceramics are found, and the phenomenon that the serious color migration is generated when the different color series ceramics are co-fired in the prior art is avoided. More importantly, the preparation process is different from other traditional surface coloring processes and is only limited on the surface of the ceramic product, so that the consistency of the internal color and the external color of the ceramic product is realized, and more possibilities are provided for the structural design and diversification of the product; in addition, starting from the powder, the colorful appearance effect of the imitated natural texture is realized, the prior post-process is reduced, and the manufacturing process cost of the product is greatly reduced.
Referring to fig. 1, the process for preparing the natural-grain-imitated multicolor ceramic product of the embodiment specifically comprises the following steps:
s1, preprocessing, namely putting a plurality of single-color zirconia ceramic powder materials with single color into a drying oven for drying treatment so as to enable the water content of the powder materials to be lower than 0.5%, and respectively carrying out repeated granulation process on the powder materials to prepare re-granulated particles;
s2, selecting materials, namely selecting re-granulated zirconia ceramic powder with the grain diameter of 0.4-0.6 mu m, the specific surface area of B.E.T. of 8-10 square meters per gram and the granularity of 50-100 meshes, wherein the re-granulated grains with 50-60 meshes account for 75-80 percent, and the re-granulated grains with 70-100 meshes account for 20-25 percent;
s3, grading treatment, namely grading the re-granulated granular zirconia ceramic powder of 50-100 meshes to separate a low-mesh granular zirconia ceramic powder of 50-60 meshes and a high-mesh granular zirconia ceramic powder of 70-100 meshes;
s4, preparing a mixture, namely preparing the graded re-granulated particle zirconia ceramic powder according to the ratio of the low mesh number to the high mesh number of 100: 5-13, preparing synthetic powder by using synthetic equipment;
s5, removing iron, namely removing iron from the synthetic powder prepared according to the proportion through an iron remover;
s6, drying, namely putting the synthesized powder into an oven for drying treatment, wherein the temperature of the oven is 40-60 ℃, the drying time is 0.5-2 h, and the preferable drying time is 1 h;
s7, pressing and forming, namely pressing and forming the dried synthetic powder into a primary blank by a bidirectional pressing or floating pressing mode of dry pressing forming equipment, wherein the unit pressure of the dry pressing forming equipment is not lower than 10 Mpa;
s8, performing metallographic detection, namely judging whether the synthetic powder particles are thoroughly crushed or not by performing metallographic detection on the primary blank subjected to compression molding; specifically, metallographic detection is carried out on the section of the primary blank, whether powder particles are completely crushed or not is confirmed, when the powder particles are spherical or hemispherical, uneven in the whole surface and hollow, the powder particles are not completely crushed, NO is judged, when the whole surface of the powder particles is relatively flat, the powder particles are completely crushed, and OK is judged.
S9, isostatic pressing, namely carrying out isostatic pressing treatment on the primary blank subjected to metallographic detection, wherein the pressure is 200-220 Mpa, and the pressure maintaining time is 5-10 min;
and S10, degreasing and sintering, namely firstly, carrying out green body processing on the primary blank body subjected to isostatic pressing treatment to obtain the specification and shape required by the colorful ceramic product, and then carrying out glue removal and sintering molding through degreasing and sintering equipment. Specifically, during firing, a large amount of organic matters in the green body are melted, decomposed and volatilized, so that the green body is deformed and cracked, and meanwhile, the carbon content of the organic matters is high, and when oxygen is insufficient to form a reducing atmosphere, the sintering quality is affected. Therefore, organic matters in the green body need to be removed completely before the green body is fired so as to ensure that the shape, size and quality of the fired product meet the standard requirements, and the process is glue removal.
As a preferred embodiment, step S10 is followed by the following steps:
s11, index detection, namely performing index detection on the degreased and sintered and molded colorful ceramic product to determine relevant parameters such as size and density of the fired colorful ceramic product and determine whether each performance index of the degreased and sintered and molded colorful ceramic product is qualified;
s12, machining, namely machining the colorful ceramic product qualified in index detection to obtain the size and shape of the colorful ceramic product with the required precision;
s13, surface treatment, namely performing surface treatment on the machined colorful ceramic product to improve the glossiness of the surface of the colorful ceramic product;
s14, performance detection, namely detecting the performance indexes of strength, fracture toughness, falling balls and ROR of the surface-treated colorful ceramic product to judge whether the product is qualified or not so as to obtain a colorful ceramic product with qualified appearance luster, size and shape and part of physical performance indexes.
As a preferred embodiment, step S12 specifically includes the following steps:
s12-1, coarse grinding, namely, performing coarse grinding processing on the colorful ceramic product with qualified index detection through a coarse grinding machine;
s12-2, performing fine grinding, and performing fine grinding processing on the coarse-ground colorful ceramic product through a fine grinder;
and S12-3, grinding, and finally grinding the finely ground colorful ceramic product.
As a preferred embodiment, step S13 specifically includes the following steps:
s13-1, performing sweeping surface treatment on the machined colorful ceramic product through a sweeping machine;
s13-2, polishing, and then performing polishing surface treatment on the colorful ceramic product after the surface treatment by a polishing machine;
s13-3, ultrasonic cleaning, and finally ultrasonic cleaning the colorful ceramic product after the polishing surface treatment.
As a preferred embodiment, step S2 specifically includes the following steps:
s2-01, carrying out particle size analysis on the re-granulated particle zirconia ceramic powder by a laser particle size analyzer to select the re-granulated particle zirconia ceramic powder with the particle size of 0.4-0.6 mu m and the B.E.T specific surface area of 8-10 square meters per gram;
s2-02, screening the granularity, and screening the re-granulated zirconia ceramic powder with the granularity of 50-100 meshes by using a vibration screening machine.
As a preferred embodiment, the content of yttrium in the re-granulated zirconia ceramic powder selected in the step S2-01 is 2.5-3%.
As a preferred embodiment, the degreasing sintering process in step S10 includes four sintering temperature zones, namely a low temperature zone, a medium temperature zone, a high temperature zone and a cooling temperature zone, wherein the temperature of the low temperature zone is less than 800 ℃, the temperature of the medium temperature zone is 800-950 ℃, and the temperature of the high temperature zone is 1300-1600 ℃. Specifically, it is required to ensure that the temperature rise in the low temperature region is relatively gentle, the temperature rise in the medium temperature region is rapid, the heat preservation in the high temperature region is short, and the cooling temperature region is relatively slow.
As a preferred embodiment, steps S1-S10 are all performed in a clean room facility.
On the other hand, the technical scheme of the invention also provides a colorful ceramic product, and the colorful ceramic product is prepared by the preparation process in any one of the technical schemes.
As a preferred embodiment, the multi-colored ceramic article is a mobile phone article or a watch article. The preparation process of the colorful ceramic product is mainly used for manufacturing colorful ceramic products such as smart phones, watches, daily necessities and the like.
In summary, the technical scheme of the invention has the following beneficial effects: the preparation process of the natural texture imitating colorful ceramic product enables the ceramic product to present various colors in order to meet the requirements of different customers, perfectly solves the technical problem that the colorful ceramic is applied to appearance structural parts and functional parts under the condition of not influencing the luster, the texture and partial physical properties of the ceramic, and can realize mass production on the existing ceramic production process. In the actual production process, the preparation process of the colorful ceramic product prepares the synthetic powder through grading treatment and specific proportion, overcomes the phenomenon of extremely easy color migration and diffusion existing in the co-firing of various powders, directly completes the manufacturing procedure of the appearance effect at the initial stage of molding, reduces the subsequent procedure flow and saves the cost.
In addition, the appearance effect of the colorful ceramic product manufactured by the preparation process is different from the appearance effect of the colorful ceramic product manufactured by the traditional methods such as sand blasting, glazing, color printing and the like, the colorful ceramic product manufactured by the preparation process is more natural and vivid in texture, the luster, the texture and partial performances of the ceramic product are not influenced, and the partial performances comprise strength, hardness, density, fracture toughness, elastic modulus, thermal expansion coefficient and the like.
Five experiments are given below to test some properties of the multi-color ceramics prepared by the preparation process of the present invention.
Experimental test one:
test items (one): falling ball
(II) test method
1. The sample requirements are as follows: selecting a good sample product with a structure and a size meeting the requirements of a finished product;
2. recording the serial numbers of all samples;
3. determining sample surface test points, uniformly distributing nine points according to the nine-square grid, and hitting each point for three times;
4. starting from 5cm, the heights are in sequence: the length of the groove is increased gradually by 7, 10, 12 and 15cm until the groove fails;
5. the test fixture is required to simulate the assembly of the whole machine.
(III) test equipment and auxiliary materials
A65 g steel ball, a steel ball drop test machine and a complete machine simulation test jig are adopted.
(IV) test results
The steel ball has no crack or damage (allowing white spots or pits) after impacting the sample at a specified height.
Experiment test two:
test items (one): 4PB bending Strength (test piece)
(II) test method
1. The sample requirements are as follows: selecting a good sample product with a structure and a size meeting the requirements of a finished product;
2. the upper wheel base is 18mm, the lower wheel base is 36mm, the diameter of the loading rod is 6mm, and the speed is 10 mm/min;
3. the upper roller and the lower roller are clean, the surfaces of the upper roller and the lower roller are not seriously scratched, and the lower roller needs to be subjected to profiling processing according to the outline of a finished product;
each set was made in XY direction, 5pcs for each set.
(III) test equipment and auxiliary materials
Universal material testing machine with model number INSTRON5965
(IV) test results
The strength of the solid black ceramic sample is more than or equal to 900 MPa.
And (3) experimental test III:
test items (one): density (based on apparent density)
(II) test method
1. The quality of the ceramic sample block is not lower than 6g, the surface is free from pollution, and the test process is free from collapse;
2. drying the sample in an oven, cooling to room temperature, weighing again, and repeating the steps until the weight is constant;
3. boiling the sample in water for at least 3 hr and cooling to room temperature;
4. measuring the floating weight of a sample, putting the sample into a hanging basket, immersing the sample into liquid, weighing the mass of the sample by using a balance, taking out the sample, weighing the mass of the hanging basket at the same depth by using the balance, wherein the difference between the two is the floating weight;
5. measuring the temperature of the immersed liquid, corresponding to the liquid density of the comparison table, and calculating the density of the sample;
6. each sample is measured at least twice, ensuring reproducibility of the measurement results.
(III) test equipment and auxiliary materials
A balance, thermometer, distilled water preparation device, heating device, spreader and oven (controlled temperature range 110+/-5 ℃) were used.
(IV) test results
Carrying out bulk density of the solid black ceramic sample on more than or equal to 6.0 g/cm;
carrying out high-yield high;
carrying out volume density of the blackened ceramic sample on more than or equal to 6.08 g/cm;
carrying out high-yield high;
and others: the relative density is more than or equal to 98.5 percent.
And (4) experimental test four:
test items (one): fracture toughness
(II) test method
1. The sample requirements are as follows: 36mmX4mmX3mm, wherein the roughness Ra of four surfaces of the sample in the length direction is not more than 0.2 um;
2. a crack initiation source, which may be surface indentation pre-crack marks and cut methods (single-sided through cuts or miter cuts) pre-crack marks;
3. pre-cracking, namely placing a sample with a crack source on a loading platform of a pre-crack initiation device, introducing a burst crack, vertically applying a load until a tiny cracking sound is heard, immediately stopping loading to avoid damaging a test device to cause crack expansion, pre-cracking by an indentation method at a loading speed of 300N/s-1000N/s and pre-cracking by an oblique notch method at a loading speed of 10N/s-300N/s;
4. taking down the sample, confirming that a crack is initiated on the surface of the sample, dripping dyed acetone into the crack, determining the position of the pre-crack tip, and performing a bending test after the dye is completely dried;
(III) test equipment and auxiliary materials
The method comprises the steps of adopting a crack prefabricating device, a pre-crack initiating loading device, a material testing machine, a bending testing device, a flexibility changing device and a vernier caliper.
(IV) test results
The sample KIC is more than or equal to 5Mpa m1/2
And (5) testing five:
test items (one): vickers hardness
(II) test method
1. The sample requirements are as follows: the surface of the sample needs to be polished, the test needs to be carried out on a smooth and flat pollution-free surface, the thickness of the sample is not less than 0.5mm, at least 1.5 times of the diagonal length d of the indentation and at least 2 times of the length c of the crack, and the back of the sample has no visible indentation damage during the test.
2. The sample is placed on a clean rigid support, so that the stability of the sample is ensured, and the test process is ensured not to move.
3. When focusing is clear, the indenter is brought into contact with the sample surface, test forces (recommended 1kgf and 5 kgf) are applied perpendicularly to the test surface, no impact or vibration should occur during the loading until the test force is applied to a prescribed value, the time from the loading until the entire test force is applied should be between 1 and 5s, and the maximum constant test force holding time should be 15 s.
4. At least 5 effective indentations were used to calculate the average hardness value.
(III) test equipment and auxiliary materials
A hardness tester (capable of applying a test force of 0.5kgf to 20 kgf), a diamond indenter, a microscope 4, and a measurement device for measuring the diagonal of indentation (accuracy not less than +/-0.2 μm) were used.
(IV) test results
The Vickers hardness of the solid black ceramic sample is more than or equal to 1200;
the Vickers hardness of the solid and white ceramic sample is more than or equal to 1300;
the Vickers hardness of the blackened ceramic sample is more than or equal to 1200;
the Vickers hardness of the white ceramic sample is more than or equal to 1200.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation process of a colorful ceramic product with imitated natural textures is characterized by comprising the following steps:
s1, preprocessing, namely putting a plurality of single-color zirconia ceramic powder materials with single color into a drying oven for drying treatment so as to enable the water content of the powder materials to be lower than 0.5%, and respectively carrying out repeated granulation process on the powder materials to prepare re-granulated particles;
s2, selecting materials, namely selecting re-granulated zirconia ceramic powder with the grain diameter of 0.4-0.6 mu m, the specific surface area of B.E.T. of 8-10 square meters per gram and the granularity of 50-100 meshes, wherein the re-granulated grains with 50-60 meshes account for 75-80 percent, and the re-granulated grains with 70-100 meshes account for 20-25 percent;
s3, grading treatment, namely grading the re-granulated granular zirconia ceramic powder of 50-100 meshes to separate a low-mesh granular zirconia ceramic powder of 50-60 meshes and a high-mesh granular zirconia ceramic powder of 70-100 meshes;
s4, preparing a mixture, namely preparing the graded re-granulated particle zirconia ceramic powder according to the ratio of the low mesh number to the high mesh number of 100: 5-13, preparing synthetic powder by using synthetic equipment;
s5, removing iron, namely removing iron from the synthetic powder prepared according to the proportion through an iron remover;
s6, drying, namely putting the synthesized powder into an oven for drying treatment, wherein the temperature of the oven is 40-60 ℃, and the drying time is 0.5-2 h;
s7, pressing and forming, namely pressing and forming the dried synthetic powder into a primary blank by using dry pressing equipment, wherein the unit pressure of the dry pressing equipment is not lower than 10 Mpa;
s8, performing metallographic detection, namely judging whether the synthetic powder particles are thoroughly crushed or not by performing metallographic detection on the primary blank subjected to compression molding;
s9, isostatic pressing, namely carrying out isostatic pressing treatment on the primary blank subjected to metallographic detection, wherein the pressure is 200-220 Mpa, and the pressure maintaining time is 5-10 min;
and S10, degreasing and sintering, namely firstly, carrying out green body processing on the primary blank body subjected to isostatic pressing treatment to obtain the specification and shape required by the colorful ceramic product, and then carrying out glue removal and sintering molding through degreasing and sintering equipment.
2. The process of claim 1, wherein the step S10 is followed by the steps of:
s11, index detection is carried out, the index detection is carried out on the degreased and sintered and formed colorful ceramic product, and whether each performance index of the degreased and sintered and formed colorful ceramic product is qualified or not is determined;
s12, machining, namely machining the colorful ceramic product qualified in index detection to obtain the size and shape of the colorful ceramic product with the required precision;
s13, surface treatment, namely performing surface treatment on the machined colorful ceramic product to improve the glossiness of the surface of the colorful ceramic product;
s14, performance detection, namely detecting the performance indexes of strength, fracture toughness, falling balls and ROR of the surface-treated colorful ceramic product to judge whether the product is qualified or not so as to obtain a colorful ceramic product with qualified performance indexes.
3. The process for preparing the imitated natural texture colorful ceramic product according to claim 2, wherein the step S12 specifically comprises the following steps:
s12-1, coarse grinding, namely, performing coarse grinding processing on the colorful ceramic product with qualified index detection through a coarse grinding machine;
s12-2, performing fine grinding, and performing fine grinding processing on the coarse-ground colorful ceramic product through a fine grinder;
and S12-3, grinding, and finally grinding the finely ground colorful ceramic product.
4. The process for preparing the imitated natural texture colorful ceramic product according to claim 2, wherein the step S13 specifically comprises the following steps:
s13-1, performing sweeping surface treatment on the machined colorful ceramic product through a sweeping machine;
s13-2, polishing, and then performing polishing surface treatment on the colorful ceramic product after the surface treatment by a polishing machine;
s13-3, ultrasonic cleaning, and finally ultrasonic cleaning the colorful ceramic product after the polishing surface treatment.
5. The process for preparing the imitated natural texture colorful ceramic product according to claim 1, wherein the step S2 specifically comprises the following steps:
s2-01, carrying out particle size analysis on the re-granulated particle zirconia ceramic powder by a laser particle size analyzer to select the re-granulated particle zirconia ceramic powder with the particle size of 0.4-0.6 mu m and the B.E.T specific surface area of 8-10 square meters per gram;
s2-02, screening the granularity, and screening the re-granulated zirconia ceramic powder with the granularity of 50-100 meshes by using a vibration screening machine.
6. The process of claim 5, wherein the process comprises: the content of yttrium in the re-granulated particle zirconia ceramic powder selected in the step S2-01 is 2.5-3%.
7. The process of claim 1, wherein the process comprises: the degreasing sintering process of the step S10 comprises four sintering temperature sections of a low temperature region, a medium temperature region, a high temperature region and a cooling temperature region, wherein the temperature of the low temperature region is less than 800 ℃, the temperature of the medium temperature region is 800-950 ℃, and the temperature of the high temperature region is 1300-1600 ℃.
8. The process for preparing the imitated natural-textured colorful ceramic product according to any one of the claims 1 to 7, wherein the process comprises the following steps: the steps S1-S10 are all completed in a dust-free workshop.
9. A multi-colored ceramic article characterized by: the multi-colored ceramic article is produced by the process of any one of claims 1 to 8.
10. A multicolored ceramic product in accordance with claim 9, wherein: the colorful ceramic product is a mobile phone product or a watch product.
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| CN108863357A (en) * | 2018-06-15 | 2018-11-23 | 广东工业大学 | A kind of polychrome zirconia ceramics piece and its preparation method and application |
| CN109896855A (en) * | 2019-03-25 | 2019-06-18 | 广东华旺锆材料有限公司 | A kind of Coloured Anodizing zirconia material and preparation method thereof |
| CN110041070A (en) * | 2018-07-02 | 2019-07-23 | 深圳陶陶科技有限公司 | Flow liner polychrome ceramics and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107285765A (en) * | 2017-08-09 | 2017-10-24 | 湖南先导电子陶瓷科技产业园发展有限公司 | A kind of preparation method of colored cubic polycrystal zirconia ceramics |
| CN108863357A (en) * | 2018-06-15 | 2018-11-23 | 广东工业大学 | A kind of polychrome zirconia ceramics piece and its preparation method and application |
| CN110041070A (en) * | 2018-07-02 | 2019-07-23 | 深圳陶陶科技有限公司 | Flow liner polychrome ceramics and its preparation method and application |
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Application publication date: 20200501 |