CN112624789B - Black zirconia ceramic material and preparation method thereof - Google Patents
Black zirconia ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of zirconia ceramic injection molding, and particularly relates to a black zirconia ceramic material and a preparation method thereof. The black zirconia ceramic material is prepared by zirconia ceramic feed injection molding and black pigment suspension infiltration; the zirconia ceramic feed comprises zirconia powder, a pore-forming agent and a binder, wherein the mass ratio of the zirconia powder to the pore-forming agent to the binder is 75-85. The black zirconia ceramic material has uniform color and good physical properties; the invention also provides a preparation method thereof, wherein the black zirconia ceramic material is prepared by adopting zirconia ceramic feeding injection molding and black pigment suspension infiltration, and the preparation method has the advantages of simple process, low cost, convenient operation and easy industrialization.
Description
Technical Field
The invention belongs to the field of zirconia ceramic injection molding, and particularly relates to a black zirconia ceramic material and a preparation method thereof.
Background
Zirconia ceramics have received much attention because of their excellent properties and are applied to various aspects of industrial production. In the field of structural ceramics, zirconia ceramics have been widely used in the field of structural ceramics because of their advantages such as high toughness, high bending strength, high wear resistance, excellent heat insulating properties, and thermal expansion coefficients close to those of steel. Mainly comprises the following steps: Y-TZP grinding ball, dispersing and grinding medium, nozzle, ball valve ball seat, zirconia mould, miniature fan axle center, optical fiber inserting needle, watchcase and watchband. In the aspect of functional ceramics, the excellent high-temperature resistance performance of the functional ceramics is used as an induction heating pipe, a refractory material and a heating element. The zirconia ceramic has sensitive electrical performance parameters and is mainly applied to oxygenSensors, solid Oxide Fuel Cells (SOFC), and high-temperature heating elements. ZrO (ZrO) 2 Has high refractive index, and certain coloring element (V) is added into superfine zirconia powder 2 O 5 ,MoO 3 ,Fe 2 O 3 Etc.), it can be made into a multi-colored translucent polycrystalline ZrO 2 The material twinkles with colorful light like natural jewel, and can be made into various ornaments.
The black zirconia ceramic product is widely applied to more than ten industry fields such as electronic component jigs, chemical and mechanical industry accessories, medical industry accessories, ornaments, daily necessities and the like. The current preparation process of the black zirconia ceramics comprises the following steps: (1) The solid phase mixing method is characterized in that oxide particles such as a coloring agent, a mineralizer and the like are mixed with the stable zirconia nano powder according to a certain chemical ratio and are subjected to ball milling, and the obtained powder is molded and sintered to obtain the zirconium oxide nano powder. (2) The chemical coprecipitation method is characterized in that zirconium salt, stabilizer salt and coloring ion salt solution are mixed, and then react with alkali or carbonate to jointly generate hydroxide or carbonate precipitate, and then the precipitate is heated and decomposed to obtain the zirconium oxide composite powder. (3) Liquid phase impregnation method, adopting liquid phase precursor impregnation method doping technology, in ZrO 2 Colored ions are introduced into the blank body and dissolved into the matrix through diffusion, and the black, blue, powder and green zirconia ceramics with pure color and uniform doping are prepared.
Compared with the method, the solid phase mixing method has the advantages of simple process, low cost, convenient operation and easy industrialization, but can not overcome the agglomeration of nano particles, the coloring phase and the matrix nano particles are not uniformly mixed, the ball milling time is long, and the ball milling medium or atmosphere can cause serious pollution to the powder; the chemical coprecipitation method has more complex process, but the obtained powder has high purity and excellent performance; the liquid phase infiltration method is simpler and more convenient in process, and the prepared colored zirconia ceramic has obvious advantages in color uniformity and physical properties, and is a novel doping technology.
In patent CN201810649627.8, a black zirconia ceramic material, a preparation method of the black zirconia ceramic and a product thereof are disclosed, wherein the black zirconia ceramic material comprises the following components in percentage by weight: 80% -95% of zirconium oxide; 2.5 to 5 percent of yttrium oxide; the balance of black pigment; the black pigment comprises the following components in percentage by weight: 0-40% of ferric oxide, 0-30% of chromic oxide, 10-30% of cobalt oxide, 0-10% of manganese oxide, 0-10% of nickel oxide, 5-30% of aluminum oxide, 0-6% of zinc oxide, 0-5% of silicon oxide, and the weight percentages of ferric oxide, chromic oxide, cobalt oxide, manganese oxide, nickel oxide, aluminum oxide, zinc oxide and silicon oxide are the percentage of the total weight of the black pigment. The preparation method of the black zirconia ceramics adopts tape casting and warm isostatic pressing processes for treatment according to the material characteristics, and adopts proper binder removal and sintering processes. The process is complicated, the whole operation time is long, and the industrial production is not facilitated.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a black zirconia ceramic material which has uniform color and good physical properties; the invention also provides a preparation method thereof, wherein the black zirconia ceramic material is prepared by adopting zirconia ceramic feeding injection molding and black pigment suspension infiltration, and the preparation method has the advantages of simple process, low cost, convenient operation and easy industrialization.
The black zirconia ceramic material is prepared by adopting zirconia ceramic feed injection molding and black pigment suspension liquid infiltration; the zirconia ceramic feed comprises zirconia powder, a pore-forming agent and a binder, wherein the mass ratio of the zirconia powder to the pore-forming agent to the binder is 75-85.
Wherein, the granularity of the zirconia powder is 0.35-0.50 μm, the yttria partially stabilized zirconia powder prepared by a hydrothermal method is preferred, and the zirconia powder with the characteristics has better permeability. The zirconia powder is a common material in the market.
The pore-forming agent is one or more of silicon dioxide, bismuth oxide and calcium oxide.
The adhesive is a general adhesive in the field of injection molding, and comprises a high molecular substance and a low molecular substance; the high molecular substance is one or more of high-density polyethylene, low-density polyethylene and polymethacrylic resin; the low molecular substance is one or more of palm wax, semi-refined paraffin and oleic acid.
The black pigment is obtained by mixing iron oxide, manganese oxide and molybdenum oxide according to the mass ratio of 30-60.
The preparation method of the black zirconia ceramic material comprises the following steps:
(1) Pretreating a pore-forming agent: calcining the pore-forming agent at 700-900 ℃, and then ball-milling until the granularity is 400-600 mu m to obtain the pretreated pore-forming agent;
(2) Banburying and granulating: adding zirconia powder, the pretreated pore-forming agent and the binder into an internal mixer, uniformly mixing to form a feed, taking out, cooling and granulating to obtain a zirconia ceramic feed;
(3) Feeding, molding, degreasing and presintering: feeding zirconia ceramics into an injection molding machine to be molded into a ceramic green body, and then degreasing and presintering to obtain a ceramic presintering blank;
(4) Preparing and pretreating a black pigment: mixing iron oxide, manganese oxide and molybdenum oxide, calcining at high temperature, and ball-milling to obtain black pigment powder with the granularity of 30-80 mu m, and then mixing the black pigment powder with olive oil and kerosene to obtain black pigment suspension;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, treating the ceramic pre-sintered blank in an ultrasonic oscillator for 12 to 24 hours, taking out and drying the ceramic pre-sintered blank to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: and sintering the black ceramic pre-sintered blank to obtain the black zirconia ceramic material.
In the step (2), the temperature of the internal mixer is set to be 180-200 ℃.
In the step (3), the pre-sintering temperature is 950-1100 ℃, and the pre-sintering time is 1-2 h.
In the step (4), the calcining temperature is 1100-1200 ℃, and the mass ratio of the black pigment powder, the olive oil and the kerosene is 1.
In the step (6), the sintering temperature is 1450-1500 ℃, and the sintering time is 2-4 h.
Compared with the prior art, the invention has the following beneficial effects:
the black zirconia ceramic material is prepared by zirconia ceramic feeding injection molding and black pigment suspension infiltration, the process is simple, the cost is low, the operation is convenient, the industrialization is easy, and the prepared black zirconia ceramic material has uniform color and good physical properties.
Detailed Description
The present invention will be described in further detail with reference to examples. The binder used in the examples is a binder commonly used in the field of injection molding, and comprises the following raw materials: 15wt% high density polyethylene, 20wt% low density polyethylene, 40wt% carnauba wax, 25wt% semi-refined paraffin wax.
Example 1
(1) Pretreating a pore-forming agent: calcining silicon dioxide at 700 ℃, and then ball-milling until the granularity is 400 mu m to obtain a pretreated pore-forming agent;
(2) Banburying and granulating: the temperature of an internal mixer is set to be 180 ℃, zirconia powder, the pretreated pore-forming agent and the binder are weighed according to the mass ratio of 75;
(3) Feeding, molding, degreasing and presintering: forming a zirconia ceramic feed into a ceramic green body in an injection molding machine, degreasing, and presintering at 950 ℃ for 1h to obtain a ceramic presintering blank;
(4) Pretreatment of black pigment: weighing iron oxide, manganese oxide and molybdenum oxide according to a mass ratio of 30;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, treating the ceramic pre-sintered blank in an ultrasonic oscillator for 12 hours, taking out and drying the ceramic pre-sintered blank to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: and sintering the black ceramic pre-sintered blank at 1450 ℃ for 2h to obtain the black zirconia ceramic material.
Example 2
(1) Pretreating a pore-forming agent: calcining bismuth oxide at 750 ℃, and then performing ball milling until the particle size is 450 mu m to obtain a pretreated pore-forming agent;
(2) Banburying and granulating: the temperature of the internal mixer is set to be 180 ℃, the zirconia powder, the pretreated pore-forming agent and the binder are weighed according to the mass ratio of 85 to 10, then are added into the internal mixer to be uniformly mixed to form a feed, and the feed is taken out and cooled to be granulated to obtain the zirconia ceramic feed;
(3) Feeding, molding, degreasing and presintering: forming a zirconia ceramic feed into a ceramic green body in an injection molding machine, degreasing, and pre-sintering at 1000 ℃ for 1.5 hours to obtain a ceramic pre-sintered blank;
(4) Pretreatment of black pigment: weighing and mixing iron oxide, manganese oxide and molybdenum oxide according to a mass ratio of 40;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, treating the ceramic pre-sintered blank in an ultrasonic oscillator for 15 hours, taking out and drying the ceramic pre-sintered blank to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: and sintering the black ceramic pre-sintered blank at 1460 ℃ for 2.5 hours to obtain the black zirconia ceramic material.
Example 3
(1) Pretreating a pore-forming agent: calcining calcium oxide and bismuth oxide at 800 ℃, and then ball-milling until the granularity is 500 mu m to obtain a pretreated pore-forming agent;
(2) Banburying and granulating: setting the temperature of the internal mixer to 190 ℃, weighing the zirconia powder, the pretreated pore-forming agent and the binder according to a mass ratio of 76 to 14, adding the materials into the internal mixer, uniformly mixing to form a feed, taking out, cooling and granulating to obtain a zirconia ceramic feed;
(3) Feeding, molding, degreasing and presintering: forming a zirconia ceramic feed into a ceramic green body in an injection molding machine, degreasing, and presintering at 1050 ℃ for 2 hours to obtain a ceramic presintering blank;
(4) Pretreatment of black pigment: weighing iron oxide, manganese oxide and molybdenum oxide according to a mass ratio of 50;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, treating the ceramic pre-sintered blank in an ultrasonic oscillator for 18 hours, taking out and drying the ceramic pre-sintered blank to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: and sintering the black ceramic pre-sintered blank at the temperature of 1480 ℃ for 3 hours to obtain the black zirconia ceramic material.
Example 4
(1) Pretreating a pore-forming agent: calcining silicon dioxide and calcium oxide at 850 ℃, and then performing ball milling until the particle size is 550 mu m to obtain a pretreated pore-forming agent;
(2) Banburying and granulating: the temperature of the internal mixer is set to 190 ℃, the zirconia powder, the pretreated pore-forming agent and the binder are weighed according to the mass ratio of 80;
(3) Feeding, molding, degreasing and presintering: forming a zirconia ceramic feed into a ceramic green body in an injection molding machine, degreasing, and pre-sintering at 1050 ℃ for 1.5 hours to obtain a ceramic pre-sintered blank;
(4) Pretreatment of black pigment: weighing, mixing and high-temperature calcining iron oxide, manganese oxide and molybdenum oxide at 1180 ℃ and ball milling according to a mass ratio of 60;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, treating the ceramic pre-sintered blank in an ultrasonic oscillator for 20 hours, taking out and drying the ceramic pre-sintered blank to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: and sintering the black ceramic pre-sintered blank at 1490 ℃ for 3.5h to obtain the black zirconia ceramic material.
Example 5
(1) Pretreating a pore-forming agent: calcining silicon dioxide, bismuth oxide and calcium oxide at 900 ℃, and then ball-milling until the particle size is 600 mu m to obtain a pretreated pore-forming agent;
(2) Banburying and granulating: the temperature of the internal mixer is set to 200 ℃, the zirconia powder, the pretreated pore-forming agent and the binder are weighed according to the mass ratio of 78;
(3) Feeding, molding, degreasing and presintering: forming a zirconia ceramic feed into a ceramic green body in an injection molding machine, degreasing, and presintering at 1100 ℃ for 2 hours to obtain a ceramic presintering blank;
(4) Pretreatment of black pigment: weighing iron oxide, manganese oxide and molybdenum oxide according to a mass ratio of 40;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, treating the ceramic pre-sintered blank in an ultrasonic oscillator for 24 hours, taking out and drying the ceramic pre-sintered blank to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: and sintering the black ceramic pre-sintered blank at 1500 ℃ for 4 hours to obtain the black zirconia ceramic material.
The ceramic articles prepared in examples 1-5 were tested for performance, where strength was measured using "three point bending", density was measured using an archimedean densitometer, hardness was measured using the "indentation method", toughness was measured using the "single edge notched beam method", and chroma was measured using a colorimeter, the test data being shown in table 1.
Table 1 results of performance testing of ceramic articles prepared in examples 1-5
Claims (4)
1. A black zirconia ceramic material is characterized in that: the material is prepared by adopting zirconia ceramic feeding injection molding and black pigment suspension infiltration; the zirconia ceramic feed is composed of zirconia powder, a pore-forming agent and a binder, wherein the mass ratio of the zirconia powder to the pore-forming agent to the binder is 75 to 85;
the pore-forming agent is one or more of silicon dioxide, bismuth oxide and calcium oxide;
the black pigment is obtained by mixing iron oxide, manganese oxide and molybdenum oxide according to the mass ratio of 30-60;
the preparation method of the black zirconia ceramic material comprises the following steps:
(1) Pretreating a pore-forming agent: calcining the pore-forming agent at 700 to 900 ℃, and then performing ball milling until the particle size is 400 to 600 mu m to obtain a pretreated pore-forming agent;
(2) Banburying and granulating: adding zirconia powder, the pretreated pore-forming agent and the binder into an internal mixer, uniformly mixing to form a feed, taking out, cooling and granulating to obtain a zirconia ceramic feed;
(3) Feeding, molding, degreasing and presintering: feeding zirconia ceramics to an injection molding machine to form a ceramic green body, and then degreasing and presintering to obtain a ceramic presintering blank;
(4) Preparing and pretreating a black pigment: mixing iron oxide, manganese oxide and molybdenum oxide, calcining at high temperature, and ball-milling to obtain black pigment powder with the granularity of 30-80 mu m, and then mixing the black pigment powder with olive oil and kerosene to obtain black pigment suspension;
(5) Liquid-phase impregnation: soaking the ceramic pre-sintered blank in the black pigment suspension, placing the ceramic pre-sintered blank in an ultrasonic oscillator for processing for 12 to 24h, taking out the ceramic pre-sintered blank and drying to obtain a black ceramic pre-sintered blank;
(6) And (3) sintering: sintering the black ceramic pre-sintered blank to obtain a black zirconia ceramic material;
in the step (3), the pre-sintering temperature is 950 to 1100 ℃, and the pre-sintering time is 1 to 2h;
in the step (4), the calcining temperature is 1100 to 1200 ℃, the mass ratio of the black pigment powder to the olive oil to the kerosene is 1 to 2 to 6;
in the step (6), the sintering temperature is 1450 to 1500 ℃, and the sintering time is 2 to 4 hours.
2. The black zirconia ceramic material of claim 1, wherein: the granularity of the zirconia powder is 0.35 to 0.50 mu m.
3. The black zirconia ceramic material of claim 1, wherein: the binder comprises a high molecular substance and a low molecular substance;
the high molecular substance is one or more of high-density polyethylene, low-density polyethylene and polymethacrylic resin;
the low molecular substance is one or more of palm wax, semi-refined paraffin and oleic acid.
4. The black zirconia ceramic material of claim 1, wherein: in the step (2), the temperature of the internal mixer is set to be 180 to 200 ℃.
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