CN115650735B - Preparation method of coloring composite ceramic powder and coloring composite ceramic - Google Patents
Preparation method of coloring composite ceramic powder and coloring composite ceramic Download PDFInfo
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Abstract
The invention provides a coloring composite ceramic and a preparation method thereof, wherein a coloring agent is mixed with alumina powder and zirconia powder, and the coloring composite ceramic is obtained through ball milling, calcining, forming and sintering; the colorant is mixed with the alumina powder and the zirconia powder and then calcined and sintered, so that the problem of high-temperature volatilization of the colorant during direct mixing, molding and sintering of the colorant, the alumina powder and the zirconia powder is avoided; the doping of zirconia powder in the matrix material improves the toughness and the breaking strength of the colored composite ceramic; the obtained colored composite ceramic has pure color, matt and hydrolysis resistance, and has excellent mechanical properties.
Description
Technical Field
The invention belongs to the technical field of advanced ceramics, and particularly relates to a preparation method of coloring composite ceramic powder and coloring composite ceramic.
Background
Alumina ceramic is a ceramic material with Al2O3 as main raw material and corundum (alpha-Al 2O 3) as main crystal phase. Because of the advantages of high mechanical strength, high hardness, small high-frequency dielectric loss, high-temperature insulation resistance, good chemical corrosion resistance, good thermal conductivity and the like, and the advantages of wide raw material sources, relatively low price, mature processing and manufacturing technology and the like, the alumina ceramic is widely applied to industries such as electronics, electrical appliances, machinery, chemical industry, spinning, automobiles, metallurgy, aerospace and the like, and becomes the oxide ceramic material with the largest use amount in the world at present.
The ceramic sintered by common zirconia has white appearance and single color, and is difficult to meet the increasing material culture demands of people, so zirconia ceramic products with different colors are produced.
CN102674894B discloses a method for coloring the surface of a ceramic body and a ceramic colorant, the method is as follows: (1) Spraying a colorant on the surface of a ceramic blank, wherein the colorant is prepared from water, a chemical material, a ceramic pigment and a suspension stabilizer, and the chemical material is one or a combination of a plurality of low-temperature luminous flux, a high Wen Moguang raw material and an opacifier; (2) drying the ceramic body sprayed with the colorant; (3) And firing the dried ceramic blank at high temperature to obtain a finished product. The raw materials of the colorant comprise water, chemical materials, ceramic pigment and suspension stabilizer. The method uses the colorant which is mainly water, has less chemical materials and ceramic pigment, is sprayed on the surface of the ceramic blank body in a spraying mode, has small spraying quantity, and has very low cost and simple process compared with the existing glazing method. However, in the method of spraying and glazing, the glaze is easy to collide and fade.
CN114560685a discloses an alumina ceramic, a preparation method and application thereof, the alumina ceramic comprises the following raw materials in parts by mass: 96-104 parts of aluminum oxide, 0.3-0.4 part of magnesium oxide, 0.9-1.2 parts of calcium oxide, 6.4-6.7 parts of silicon oxide, 0.9-1.2 parts of titanium dioxide, 0.5-0.9 part of ferric oxide, 0.5-0.9 part of cobalt oxide and 1.8-2.7 parts of chromium oxide; through reasonable proportion of the components, iron oxide, cobalt oxide and chromium oxide with specific content proportion are selected as colorants, and are matched with other raw materials, and the obtained alumina ceramic has brown red color.
White zirconia has been used as a medical ceramic for many years, after which black zirconia overcomes the lack of white zirconia to reflect light, but the essential difficulty that zirconia may hydrolyze at low temperatures in a water environment has not yet been solved.
However, in the existing method, the brittleness of the colored alumina ceramic is large, and the colorant is volatile, resulting in color unevenness. Therefore, there is still a need to provide a new colored ceramic that has high toughness, is not easily broken, and is not hydrolyzed at low temperatures for use in a water environment. The colored ceramic is a ceramic having a different color from the natural color ceramic, such as black ceramic, gray ceramic, blue ceramic, pink ceramic, etc., in which a colorant is added to the natural color ceramic.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of coloring composite ceramic powder, wherein the coloring agent is mixed with alumina powder and zirconia powder and then calcined and sintered, so that the problem of high-temperature volatilization of the coloring agent during direct mixing, molding and sintering of the coloring agent, the alumina powder and the zirconia powder is avoided; the doping of zirconia powder in the matrix material improves the toughness and the breaking strength of the colored composite ceramic; the obtained colored composite ceramic has pure color, matt and hydrolysis resistance, and has excellent mechanical properties.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a colored composite ceramic powder, the method comprising the steps of:
(1) Mixing 80-95wt% of alumina powder and 5-20wt% of zirconia powder to obtain a mixture;
(2) Mixing the colorant and the mixture obtained in the step (1), and then performing ball milling to obtain a ball grinding material;
(3) Calcining the ball abrasive material in the step (2) to obtain the coloring composite ceramic powder.
In the preparation method of the colored composite ceramic powder, the colorant, the alumina powder and the zirconia powder are mixed and then calcined and sintered, so that the problem of high-temperature volatilization of the colorant during direct mixing, molding and sintering of the colorant, the alumina powder and the zirconia powder is avoided; the doping of zirconia powder in the matrix material improves the toughness and the breaking strength of the colored composite ceramic.
The alumina powder content is illustratively 80-95wt%, and may be, for example, 80wt%, 81wt%, 82wt%, 83wt%, 84wt%, 85wt%, 86wt%, 87wt%, 88wt%, 89wt%, 90wt%, 91wt%, 92wt%, 93wt%, 94wt% or 95wt%; the zirconia powder may be contained in an amount of 5 to 20wt%, for example, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 17wt%, 19wt% or 20wt%, but is not limited to the recited values, and other non-recited values within the above-mentioned range are equally applicable.
As a preferred embodiment of the present invention, the alumina powder in step (1) includes gamma-phase alumina powder.
Preferably, the alumina powder of step (1) has a purity of 99.0% or more, for example 99%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8% or 99.9%; the particle size is 0.02 to 2.0. Mu.m, for example, 0.02 μm, 0.1 μm, 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm, 1.0 μm, 1.1 μm, 1.3 μm, 1.5 μm, 1.7 μm, 1.9 μm or 2.0. Mu.m, but not limited to the values listed, and other values not listed in the above-mentioned numerical ranges are equally applicable.
Preferably, the zirconia powder in step (1) comprises 2-4mol% yttria stabilized zirconia powder, for example, 2mol%, 2.2mol%, 2.4mol%, 2.6mol%, 2.8mol%, 3mol%, 3.2mol%, 3.4mol%, 3.6mol%, 3.8mol% or 4mol%, but not limited to the recited values, and other non-recited values within the above range are equally applicable.
Preferably, the zirconia powder in step (1) has a purity of 99.0% or more, for example, 99%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8% or 99.9%; the particle size is 20 to 100nm, and may be, for example, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm or 100nm, but is not limited to the values recited, and other values not recited in the above-mentioned ranges are equally applicable.
As a preferred embodiment of the present invention, the colorant in the step (2) includes any one of a nitrate colorant, an oxide colorant, and a ceramic colorant.
Preferably, the nitrate colorant comprises cobalt nitrate, copper nitrate, manganese nitrate, and vanadium nitrate.
Preferably, the mass ratio of cobalt nitrate, copper nitrate and manganese nitrate is 1 (2-4): (2-4): (0.02-4), for example, may be 1:2:2:0.02, 1:3:3:0.5, 1:4:4:1, 1:4:2:1.5, 1:3:4:2, 1:3:3:2.7, 1:2:2:3, 1:2:4:3.4 or 1:4:2:4, but not limited to the recited values, and other non-recited values within the above range of values are equally applicable.
Preferably, the oxide colorant comprises a combination of chromium oxide or cobalt oxide, copper oxide, manganese oxide, and vanadium pentoxide.
Preferably, the copper oxide comprises copper oxide and/or cuprous oxide.
Preferably, the mass ratio of cobalt oxide, copper oxide, manganese oxide and vanadium pentoxide is 1 (2-4): 0.02-4, for example, it may be 1:2:2:0.02, 1:3:3:0.5, 1:4:4:1, 1:4:2:1.5, 1:3:4:2, 1:3:2.7, 1:2:2:3, 1:2:4:3.4 or 1:4:2:4, but not limited to the recited values, and other non-recited values within the above range are equally applicable.
As a preferable technical scheme of the invention, the addition amount of the colorant in the step (2) is 0.05-25wt% of the mixture, and can be, for example, 0.05wt%, 0.1wt%, 0.2wt%, 0.3wt%, 0.8wt%, 1wt%, 5wt%, 10wt%, 15wt%, 20wt%, 22wt% or 25wt%; further preferably 0.1 to 15wt%, for example, 0.1wt%, 0.2wt%, 0.5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt% or 15wt%, but not limited to the values recited, and other values not recited in the above ranges are equally applicable.
As a preferable technical scheme of the invention, the ball milling mode in the step (2) is dry ball milling.
Preferably, the ball milling medium of the ball milling in step (2) comprises zirconia balls.
Preferably, the ball-to-material ratio of the ball mill in step (2) is (2-4): 1, which may be, for example, 2:1, 2.1:1, 2.2:1, 2.4:1, 2.5:1, 2.7:1, 2.9:1, 3:1, 3.3:1, 3.7:1 or 4:1, but is not limited to the recited values, and other non-recited values within the above ranges are equally applicable.
Preferably, the rotational speed of the ball mill in the step (2) is 100-300rpm, for example, 100rpm, 120rpm, 150rpm, 170rpm, 200rpm, 230rpm, 250rpm, 280rpm or 300rpm, but not limited to the recited values, and other non-recited values within the above range are equally applicable.
Preferably, the ball milling time in the step (2) is 20-24h, for example, 20h, 20.5h, 21h, 21.5h, 22h, 22.5h, 23h, 23.5h or 24h, but not limited to the recited values, and other non-recited values in the above range are equally applicable.
In a preferred embodiment of the present invention, the calcination temperature in the step (3) is 1150 to 1250 ℃, for example 1150 ℃, 1160 ℃, 1170 ℃, 1180 ℃, 1190 ℃, 1200 ℃, 1210 ℃, 1220 ℃, 1230 ℃, 1240 ℃, or 1250 ℃, but the present invention is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned numerical ranges are equally applicable.
Preferably, the temperature rising rate of the calcination in the step (3) is 5-10 ℃/min, for example, 5 ℃/min, 5.5 ℃/min, 6 ℃/min, 6.5 ℃/min, 7 ℃/min, 7.5 ℃/min, 8 ℃/min, 8.5 ℃/min, 9 ℃/min, 9.5 ℃/min or 10 ℃/min, but not limited to the listed values, and other non-listed values in the above range are equally applicable.
Preferably, the calcination in step (3) is carried out for a period of time ranging from 1 to 3 hours, for example, 1h, 1.2h, 1.4h, 1.6h, 1.8h, 2h, 2.2h, 2.4h, 2.6h, 2.8h or 3h, but not limited to the values recited, and other values not recited in the above ranges are equally applicable.
Preferably, the calcination of step (3) is carried out in an oxidizing atmosphere.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Mixing 80-95wt% of alumina powder and 5-20wt% of zirconia powder to obtain a mixture;
wherein the alumina powder comprises gamma-phase alumina powder with the purity more than or equal to 99.0 percent and the particle diameter of 0.02-2.0 mu m; the zirconia powder comprises 2-4mol% of yttria-stabilized zirconia powder with the purity of more than or equal to 99.0% and the grain diameter of 20-100 nm;
(2) Mixing the colorant and the mixture obtained in the step (1), and performing ball milling for 20-24 hours at the rotating speed of 100-300rpm, wherein the ball material ratio is controlled to be (2-4): 1, so as to obtain a ball abrasive;
wherein the addition amount of the colorant is 0.05-25wt% of the mixture; the colorant comprises any one of nitrate colorant, oxide colorant or ceramic colorant; the nitrate colorant comprises cobalt nitrate, copper nitrate, manganese nitrate and vanadium nitrate with the mass ratio of 1 (2-4) to 2-4 to 0.02-4; the oxide colorant comprises chromium oxide or cobalt oxide, copper oxide, manganese oxide and vanadium pentoxide with the mass ratio of (2-4) to (0.02-4), wherein the copper oxide comprises copper oxide and/or cuprous oxide;
(3) And (3) calcining the ball-milling material in an oxidizing atmosphere at 1150-1250 ℃ for heat preservation for 1-3h, and controlling the temperature rising rate of the calcination to be 5-10 ℃/min to obtain the colored composite ceramic powder.
In a second aspect, the invention provides a colored composite ceramic, which is prepared from the colored composite ceramic powder prepared by the preparation method.
Preferably, the colored composite ceramic is prepared by granulating, molding and sintering the colored ceramic powder.
Preferably, the sintering temperature is 1350-1650 ℃ and the sintering time is 48-72h.
The sintering temperature may be 1350 ℃, 1400 ℃, 1450 ℃, 1500 ℃, 1520 ℃, 1550 ℃, 1580 ℃, 1600 ℃, 1630 ℃, 1640 ℃ or 1650 ℃ and the time may be 48h, 50h, 52h, 55h, 58h, 60h, 63h, 64h, 66h, 68h, 70h or 72h, but the sintering temperature is not limited to the above-mentioned values, and other non-mentioned values in the above-mentioned respective ranges are equally applicable.
In the present invention, the molding method includes isostatic molding, dry-press molding, injection molding, gel casting or slip casting, and further preferably isostatic molding.
Preferably, the application of the colored composite ceramic comprises the preparation of ceramic sheath heads for manufacturing medical devices, painless syringe ceramic needle heads, ceramic cleavers for integrated circuit packaging, integrated circuit ceramic shells and LED packaging substrates.
The colored composite ceramic obtained by the invention has pure color, matte property, hydrolysis resistance and excellent mechanical property.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
(1) In the preparation method of the colored composite ceramic powder, the colorant, the alumina powder and the zirconia powder are mixed and then calcined and sintered, so that the problem of high-temperature volatilization of the colorant during direct mixing, molding and sintering of the colorant, the alumina powder and the zirconia powder is avoided; the doping of zirconia powder in the matrix material improves the toughness and hardness of the colored composite ceramic;
(2) The colored composite ceramic has pure color, matte property, hydrolysis resistance and excellent mechanical property.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
In the specific embodiment of the invention, the purity of the gamma-phase alumina powder is more than or equal to 99.0 percent, and the particle size is in the range of 0.02-2.0 mu m; the purity of the yttria-stabilized zirconia powder is more than or equal to 99.0 percent, and the grain diameter is in the range of 20-100 nm.
Example 1
The embodiment provides black composite ceramic powder and ceramic and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) 90g of gamma-phase alumina powder and 10g of 3mol% yttria-stabilized zirconia powder are mixed to obtain a mixture;
(2) Mixing the colorant and the mixture obtained in the step (1), and performing dry ball milling for 20 hours at a rotating speed of 100rpm, wherein the ball-material ratio is controlled to be 4:1 to obtain a ball abrasive;
wherein the addition amount of the colorant is 21g, and the colorant comprises 3g of cobalt nitrate, 9g of copper nitrate, 6g of manganese nitrate and 3g of vanadium nitrate;
(3) Calcining the ball-milling material in an oxidizing atmosphere at 1200 ℃ for 2 hours, and controlling the temperature rising rate of the calcination to be 7 ℃/min to obtain composite ceramic powder;
(4) And (3) granulating, forming and sintering the calcined material at 1600 ℃ for 60 hours to obtain the black composite ceramic.
Example 2
The embodiment provides black composite ceramic powder and ceramic and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing 80g of gamma-phase alumina powder and 20g of 4mol% yttria-stabilized zirconia powder to obtain a mixture;
(2) Mixing the colorant and the mixture obtained in the step (1), and performing dry ball milling for 24 hours at a rotating speed of 200rpm, wherein the ball-material ratio is controlled to be 2:1 to obtain a ball abrasive;
wherein the colorant is cobalt black ceramic pigment, and the addition amount is 25g;
(3) Calcining the ball-milling material in an oxidizing atmosphere at 1250 ℃ for 1h, and controlling the temperature rising rate of the calcination to be 10 ℃/min to obtain composite ceramic powder;
(4) And (3) granulating, forming and sintering the calcined material at 1650 ℃ for 48 hours to obtain the black composite ceramic.
Example 3
The embodiment provides green composite ceramic powder and ceramic and a preparation method thereof, wherein the preparation method comprises the following steps:
(1) Mixing 95g of gamma-phase alumina powder and 5g of 2mol% yttria-stabilized zirconia powder to obtain a mixture;
(2) Mixing the colorant and the mixture obtained in the step (1), and performing dry ball milling for 22 hours at a rotating speed of 300rpm, wherein the ball-to-material ratio is controlled to be 3:1 to obtain a ball abrasive;
wherein, the colorant is green ceramic pigment, and the addition amount is 0.2g;
(3) Calcining the ball-milling material in an oxidizing atmosphere at 1150 ℃ for 3 hours, and controlling the temperature rising rate of the calcination to be 5 ℃/min to obtain composite ceramic powder;
(4) And (3) granulating, forming and sintering the calcined material at 1350 ℃ for 72 hours to obtain the green composite ceramic.
Example 4
The present embodiment provides a black composite ceramic powder and ceramic and a preparation method thereof, and the preparation method of reference embodiment 1 is different only in that: the colorant was added in an amount of 24g, including 2g cobalt oxide, 8g cuprous oxide, 6g manganese oxide, and 8g vanadium pentoxide.
Example 5
The present embodiment provides a black composite ceramic powder and ceramic and a preparation method thereof, and the preparation method of reference embodiment 1 is different only in that: the colorant was added in an amount of 21.06g, including 3g cobalt oxide, 6g cuprous oxide, 12g manganese oxide, and 0.06g vanadium pentoxide.
Example 6
The present embodiment provides a blue composite ceramic powder and ceramic and a preparation method thereof, and the preparation method of reference embodiment 1 is different only in that: the colorant is blue ceramic pigment, and the addition amount is 8g.
Example 7
The present embodiment provides a black composite ceramic powder and ceramic and a preparation method thereof, and the preparation method of reference embodiment 1 is different only in that: the calcination temperature in step (3) was 1100 ℃.
Example 8
This example provides a pink composite ceramic powder and ceramic and its preparation method, and the difference is only that with reference to the preparation method of example 1: the colorant is chromium oxide, and the addition amount is 2g.
The colored composite ceramics in the above examples and comparative examples were tested as follows:
before detection, polishing a sample by using diamond until the roughness Ra0.1 is lower, and testing the Vickers hardness of the material by using a microhardness tester; the bending strength of the material was measured using a three-point bending tester.
Hydrolysis test: the colored composite ceramics (10 samples) prepared in examples 1 to 8 were placed in a sealed environment having a humidity of 98% and a temperature of 120℃for 48 hours, after which stress was applied to the ceramic surface, and whether the ceramic surface had flaking was observed, and if there was flaking, no flaking was noted, and a commercially available black zirconia ceramic (10 samples) was placed in the above environment as a control. The results of the above tests are shown in Table 1.
TABLE 1
From table 1, the following points can be found:
(1) The examples 1-6 show that the invention avoids the problem of high-temperature volatilization of the colorant when the colorant, the alumina powder and the zirconia powder are directly mixed, molded and sintered, and has higher toughness and hardness;
(2) Comparing example 1 with example 7, it can be seen that the sintering effect is deteriorated and the mechanical properties are lowered due to the calcination temperature of example 7 being 1100 ℃ which is lower than the preferred 1150-1250 ℃ according to the present invention.
The colored ceramic of the invention is used for manufacturing a ceramic sheath head for medical equipment, a ceramic needle head for a painless injector and a ceramic chopper for integrated circuit encapsulation. The invention is used for manufacturing the ceramic shell of the integrated circuit and increasing the light resistance of the integrated circuit. The LED packaging substrate is used as an LED packaging substrate, and the brightness of an LED is improved.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (2)
1. A method for preparing colored composite ceramic powder, which is characterized by comprising the following steps:
(1) Mixing 80-95wt% of alumina powder and 5-20wt% of zirconia powder to obtain a mixture;
wherein the alumina powder is gamma-phase alumina powder with the purity more than or equal to 99.0 percent and the particle diameter of 0.02-2.0 mu m; the zirconia powder is 2-4mol% yttria stabilized zirconia powder with the purity more than or equal to 99.0% and the grain diameter of 20-100 nm;
(2) Mixing the colorant and the mixture obtained in the step (1), and then ball-milling for 20-24 hours at the rotating speed of 100-300rpm, wherein the ball-material ratio is controlled to be (2-4): 1, so as to obtain a ball abrasive;
wherein the addition amount of the colorant is 0.05-25wt% of the mixture; the colorant comprises any one of nitrate colorant, oxide colorant or ceramic colorant; the nitrate colorant comprises cobalt nitrate, copper nitrate, manganese nitrate and vanadium nitrate with the mass ratio of 1 (2-4) to 2-4 to 0.02-4; the oxide colorant comprises chromium oxide or cobalt oxide, copper oxide, manganese oxide and vanadium pentoxide with the mass ratio of (2-4) to (0.02-4), wherein the copper oxide comprises copper oxide and/or cuprous oxide;
(3) And (3) calcining the ball-milling material in an oxidizing atmosphere at 1150-1250 ℃ for heat preservation for 1-3h, and controlling the temperature rising rate of the calcination to be 5-10 ℃/min to obtain the colored composite ceramic powder.
2. A colored composite ceramic, characterized in that the colored composite ceramic is prepared by the colored composite ceramic powder prepared by the preparation method of claim 1;
the colored composite ceramic is prepared by granulating, forming and sintering the colored composite ceramic powder;
the sintering temperature is 1350-1650 ℃ and the sintering time is 48-72h;
the application of the colored composite ceramic comprises the preparation of a ceramic sheath head for medical equipment, a painless syringe ceramic needle, a ceramic chopper for integrated circuit packaging, an integrated circuit ceramic shell and an LED packaging substrate.
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