Method for preparing green zirconia ceramic

Abstract

The application relates to a preparation method of green zirconia ceramics and relates to the field of ceramic materials. The application adopts a liquid phase infiltration method and is based on a three-primary-color principle, a green zirconia ceramic with uniform chroma, few defects, good luster and high strength is prepared through two-step dyeing and two-step sintering, and the problem of single color of the current zirconia ceramic is solved. Moreover, the colorant adopted in the application can stabilize the colored zirconia ceramic, has little influence on the mechanical properties of the zirconia ceramic, and is suitable for industrial production.

Description

Technical Field

[0001] This application relates to the field of ceramic materials technology, and in particular to a method for preparing green zirconia ceramic. Background Technology

[0002] Zirconia ceramics possess advantages such as good chemical stability, low thermal conductivity, low high-temperature creep, and good wear resistance. They are also free of metal and electroplating pollution, making them an ideal environmentally friendly material. They are mainly used in dental materials, grinding media, mobile phone back panels, luxury watches, and ceramic cutting tools. Oxygen ion conductivity is a unique property of zirconia, enabling its widespread application in solid oxide fuel cells, oxygen and nitrogen oxide sensors, and other fields.

[0003] In recent years, with the rapid development of the high-end decorative goods market, people's demand for high-end decorative materials such as watch cases, watch chains, bracelets, and gemstones has been increasing. Zirconia ceramics have received widespread attention due to their excellent properties such as high strength, high hardness, good toughness, and high refractive index, as well as their beautiful gemstone luster and safety and environmental friendliness. Zirconia ceramics, possessing both excellent mechanical properties and a captivating aesthetic luster, have broken through into new fields by combining mechanics and natural beauty, shining brightly in the field of personal wearable electronic devices such as mobile phone back panels and watch cases, and are highly favored by consumers. With the improvement of human production and living standards, the appearance and performance of products closely related to people's daily lives are receiving increasing attention. Therefore, possessing a beautiful appearance and excellent performance has become an important indicator of product quality.

[0004] However, ceramics sintered from pure zirconia are white, and the current zirconia ceramics are relatively limited in color, mainly black and white, making it difficult to meet people's demand for zirconia ceramics as decorative items. Summary of the Invention

[0005] Given the current state of technology and the growing trend of zirconia applications, the development of colored zirconia ceramics is imperative. The purpose of this application is to provide a method for preparing green zirconia ceramics, obtaining green zirconia ceramics with uniform color, few defects, good gloss, and high strength, thereby solving the problems existing in the prior art.

[0006] To achieve the above objectives, the technical solution adopted in this application is as follows:

[0007] In a first aspect, this application provides a method for preparing green zirconia ceramics, comprising:

[0008] S1. Weigh a certain amount of blue colorant raw material and prepare a blue colorant aqueous solution in a glass beaker using deionized water according to the concentration.

[0009] S2. Immerse the zirconia blank in the blue colorant aqueous solution, and remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0010] S3. Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain a zirconia ceramic blank.

[0011] S4. Weigh a certain amount of yellow colorant raw material, prepare a yellow colorant aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat and keep it warm in an oil bath.

[0012] S5. Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution, and remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain a dried zirconia ceramic green body.

[0013] S6. Place the dried zirconia ceramic blank into a muffle furnace and perform a second sintering under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain the green zirconia ceramic.

[0014] The blue colorant raw material includes aluminum-containing salt and nickel-containing salt, with the ratio of aluminum ions to nickel ions being 1:10 to 1:2; the yellow colorant raw material includes vanadium-containing salt, with the mass fraction of vanadium ions in the yellow colorant aqueous solution being 1 to 5%.

[0015] In one possible implementation, the aluminum-containing salt is one of aluminum chloride, aluminum sulfate, or aluminum nitrate, and the nickel-containing salt is one of nickel chloride, nickel sulfate, nickel nitrate, nickel bromide, or nickel sulfamate.

[0016] The vanadium-containing salt is one of ammonium metavanadate, sodium metavanadate, potassium metavanadate, sodium orthovanadate, vanadium oxysulfate, vanadium oxalate, vanadium tetrachloride, or vanadium oxytrichloride.

[0017] In one possible implementation, the aluminum-containing salt is aluminum nitrate, the nickel-containing salt is nickel chloride, and the ratio of aluminum ions to nickel ions is 1.0–1.4:0.1–0.5.

[0018] The concentration of aluminum ions in the aqueous solution of the blue colorant is 1.0–1.5 mol / L, and the concentration of nickel ions is 0.1–0.5 mol / L.

[0019] The vanadium-containing salt is ammonium metavanadate, and the concentration of the ammonium metavanadate solution is 1-3 g / 100 ml.

[0020] In one possible implementation, in step S2:

[0021] The soaking time for immersing the zirconia blank in the blue colorant aqueous solution is 5 to 10 minutes.

[0022] The step of removing the soaked zirconia blank from the blue colorant aqueous solution and drying it specifically involves drying it under an infrared therapy device for 30 minutes.

[0023] In one possible implementation, in step S3:

[0024] The temperature conditions for the first sintering are 300–500℃, the holding time is 1–2 h, and the heating rate is 3–5℃ / min.

[0025] In one possible implementation, in step S4:

[0026] The heating temperature of the oil bath is maintained at 60-80℃.

[0027] In one possible implementation, in step S5:

[0028] The soaking time for immersing the zirconia ceramic blank obtained in step S3 into the prepared yellow colorant aqueous solution is 5 to 10 minutes.

[0029] In one possible implementation, in step S6:

[0030] The temperature conditions for the second sintering are 1350–1550℃, and the holding time is 2–3 hours.

[0031] In one possible implementation, the second sintering process involves sequentially sintering through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period to form a mature embryo, specifically including:

[0032] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0033] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0034] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0035] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0036] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0037] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0038] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0039] Secondly, this application provides a green zirconia ceramic, prepared by any of the above-described methods for preparing green zirconia ceramic, wherein the green zirconia ceramic comprises zirconia, yttrium oxide, a blue colorant and a yellow colorant, and the content of yttrium oxide is 1-3%.

[0040] The beneficial effects of the technical solution provided in this application include at least the following:

[0041] This application employs a liquid-phase infiltration method based on the principle of three primary colors, and prepares a green zirconia ceramic with uniform color, few defects, good gloss, and high strength through two-step dyeing and two-step sintering, solving the problem of the current zirconia ceramics having a single color. Furthermore, the colorant used in this application can stably color the zirconia ceramic with minimal impact on its mechanical properties, making it suitable for industrial production. Attached Figure Description

[0042] The accompanying drawings are provided to further illustrate the present application and form part of the specification. They are used together with the embodiments of the present application to explain the application and do not constitute a limitation thereof. In the drawings:

[0043] Figure 1 A flowchart illustrating a method for preparing green zirconia ceramics according to an exemplary embodiment of this application is shown. Detailed Implementation

[0044] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0045] In this specification, identical components are represented by the same reference numerals. It should be noted that the terms "front," "rear," "left," "right," "upper," and "lower" used in the following description refer to directions in the accompanying drawings, while the terms "bottom surface," "top surface," "inner," and "outer" refer to directions towards or away from a specific component, respectively. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Therefore, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this specification, "multiple" means two or more.

[0046] The present application will be further described below with reference to the accompanying drawings and embodiments.

[0047] Figure 1 A flowchart illustrating a method for preparing green zirconia ceramic according to an exemplary embodiment of this application is shown. The method for preparing green zirconia ceramic includes the following steps:

[0048] Step S1: Weigh a certain amount of blue colorant raw material and prepare a blue colorant aqueous solution in a glass beaker using deionized water according to the concentration.

[0049] In the embodiments of this application, the blue colorant raw material includes an aluminum-containing salt and a nickel-containing salt, wherein the ratio of aluminum ions to nickel ions is 1:10 to 1:2. Optionally, the aluminum-containing salt is one of aluminum chloride, aluminum sulfate, or aluminum nitrate, and the nickel-containing salt is one of nickel chloride, nickel sulfate, nickel nitrate, nickel bromide, or nickel sulfamate.

[0050] In one example, the aluminum-containing salt is aluminum nitrate, the nickel-containing salt is nickel chloride, and the ratio of aluminum ions to nickel ions is 1.0–1.4:0.1–0.5; the concentration of aluminum ions in the blue colorant aqueous solution is 1.0–1.5 mol / L, and the concentration of nickel ions is 0.1–0.5 mol / L.

[0051] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0052] In this embodiment, the zirconia blank is immersed in the blue colorant aqueous solution for 5 to 10 minutes; the immersed zirconia blank is then removed from the blue colorant aqueous solution and dried, specifically under an infrared therapy device for 30 minutes.

[0053] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program stops and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0054] In the embodiments of this application, the temperature conditions for the first sintering are 300-500°C, the holding time is 1-2 hours, and the heating rate is 3-5°C / min.

[0055] Step S4: Weigh a certain amount of yellow colorant raw material, prepare a yellow colorant aqueous solution in a glass beaker using deionized water according to the mass fraction / concentration, and heat and keep warm in an oil bath.

[0056] In the embodiments of this application, the yellow colorant raw material includes a vanadium-containing salt, and the mass fraction of vanadium ions in the yellow colorant aqueous solution is 1-5%. Optionally, the vanadium-containing salt is one of ammonium metavanadate, sodium metavanadate, potassium metavanadate, sodium orthovanadate, vanadium oxysulfate, vanadium oxalate, vanadium tetrachloride, or vanadium oxychloride.

[0057] In one example, the vanadium-containing salt is ammonium metavanadate, and the concentration of the ammonium metavanadate solution is 1–3 g / 100 ml.

[0058] In the embodiments of this application, the heating temperature of the oil bath is maintained at 60-80°C.

[0059] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution, and remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0060] In this embodiment of the application, the zirconia ceramic blank obtained in step S3 is immersed in the prepared yellow colorant aqueous solution for 5 to 10 minutes.

[0061] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0062] In the embodiments of this application, the temperature conditions for the second sintering are 1350-1550°C, and the holding time is 2-3 hours.

[0063] Specifically, in the second sintering process, a mature embryo is formed by sintering sequentially through the first heating period, the first holding period, the second heating period, the second holding period, the third heating period, the third holding period, and the first cooling period, which includes:

[0064] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0065] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0066] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0067] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0068] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0069] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0070] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0071] It should be noted that the green zirconia ceramic prepared by the above-mentioned method includes zirconia, yttrium oxide, blue colorant and yellow colorant, and the content of yttrium oxide is 1-3%.

[0072] To better understand this application, several specific embodiments are described below for further explanation. It should be noted that the embodiments described in these specific embodiments are merely some embodiments of this application and do not limit the scope of protection of this application.

[0073] Example 1:

[0074] This embodiment provides a method for preparing green zirconia ceramics, including the following steps:

[0075] Step S1: Weigh 0.3 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0076] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0077] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. The heating rate is 3°C per minute, and the temperature is held at 300°C for 1 hour. After sintering is completed, the program is stopped and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0078] Step S4: Weigh 1g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat it in an oil bath at 80℃.

[0079] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0080] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0081] In the aforementioned second sintering process, a mature embryo is formed by sintering sequentially through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period, specifically including:

[0082] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0083] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0084] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0085] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0086] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0087] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0088] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0089] Example 2:

[0090] This embodiment provides a method for preparing green zirconia ceramics, including the following steps:

[0091] Step S1: Weigh 0.3 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0092] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0093] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. The heating rate is 3°C per minute, and the temperature is held at 300°C for 1 hour. After sintering is completed, the program is stopped and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0094] Step S4: Weigh 2g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat and keep warm in an oil bath at 80℃.

[0095] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0096] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0097] In the aforementioned second sintering process, a mature embryo is formed by sintering sequentially through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period, specifically including:

[0098] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0099] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0100] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0101] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0102] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0103] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0104] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0105] Example 3:

[0106] This embodiment provides a method for preparing green zirconia ceramics, including the following steps:

[0107] Step S1: Weigh 0.3 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0108] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0109] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. The heating rate is 3°C per minute, and the temperature is held at 300°C for 1 hour. After sintering is completed, the program is stopped and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0110] Step S4: Weigh 3g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat it in an oil bath at 80℃.

[0111] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0112] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0113] In the aforementioned second sintering process, a mature embryo is formed by sintering sequentially through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period, specifically including:

[0114] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0115] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0116] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0117] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0118] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0119] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0120] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0121] Example 4:

[0122] This embodiment provides a method for preparing green zirconia ceramics, including the following steps:

[0123] Step S1: Weigh 0.5 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0124] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0125] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. The heating rate is 3°C per minute, and the temperature is held at 300°C for 1 hour. After sintering is completed, the program is stopped and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0126] Step S4: Weigh 1g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat it in an oil bath at 80℃.

[0127] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0128] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0129] In the aforementioned second sintering process, a mature embryo is formed by sintering sequentially through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period, specifically including:

[0130] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0131] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0132] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0133] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0134] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0135] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0136] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0137] Example 5:

[0138] This embodiment provides a method for preparing green zirconia ceramics, including the following steps:

[0139] Step S1: Weigh 0.5 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0140] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0141] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. The heating rate is 3°C per minute, and the temperature is held at 300°C for 1 hour. After sintering is completed, the program is stopped and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0142] Step S4: Weigh 2g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat and keep warm in an oil bath at 80℃.

[0143] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0144] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0145] In the aforementioned second sintering process, a mature embryo is formed by sintering sequentially through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period, specifically including:

[0146] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0147] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0148] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0149] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0150] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0151] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0152] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0153] Example 6:

[0154] This embodiment provides a method for preparing green zirconia ceramics, including the following steps:

[0155] Step S1: Weigh 0.5 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0156] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0157] Step S3: Place the dried zirconia blank into a muffle furnace and perform the first sintering under air atmosphere conditions. The heating rate is 3°C per minute, and the temperature is held at 300°C for 1 hour. After sintering is completed, the program is stopped and the blank is cooled naturally to obtain the zirconia ceramic blank.

[0158] Step S4: Weigh 3g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat it in an oil bath at 80℃.

[0159] Step S5: Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain the dried zirconia ceramic green body.

[0160] Step S6: Place the dried zirconia ceramic blank into a muffle furnace and sinter it for the second time under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain green zirconia ceramic.

[0161] In the aforementioned second sintering process, a mature embryo is formed by sintering sequentially through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period, specifically including:

[0162] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0163] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0164] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0165] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0166] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0167] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0168] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0169] As a supplementary explanation, sky-blue zirconia ceramics and yellow zirconia ceramics can also be obtained by using a single colorant, as illustrated below with two examples.

[0170] Example 7:

[0171] This embodiment provides a method for preparing sky-blue zirconia ceramic, including the following steps:

[0172] Step S1: Weigh 0.5 mol / L nickel chloride and 1.4 mol / L aluminum nitrate as raw materials for blue coloring agent, and prepare an aqueous solution of blue coloring agent in a glass beaker with deionized water according to the concentration.

[0173] Step S2: Immerse the zirconia blank in a blue colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank.

[0174] Step S3: Place the dried zirconia blank into a muffle furnace and sinter it under air atmosphere. During the sintering process, the blank is formed by sequentially passing through the first heating period, the first holding period, the second heating period, the second holding period, the third heating period, the third holding period, and the first cooling period. Specifically, this includes:

[0175] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0176] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0177] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0178] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0179] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0180] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0181] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0182] Step S4: After natural cooling, sky-blue zirconia ceramic is obtained.

[0183] Example 8:

[0184] This embodiment provides a method for preparing yellow zirconia ceramic, including the following steps:

[0185] Step S1: Weigh 3g / 100ml of ammonium metavanadate as the raw material for yellow coloring agent, prepare a yellow coloring agent aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat it in an oil bath at 80℃.

[0186] Step S2: Immerse the zirconia blank in the prepared yellow colorant aqueous solution for 10 minutes, and then remove the immersed zirconia blank from the yellow colorant aqueous solution and dry it to obtain the dried zirconia blank.

[0187] Step S3: Place the dried zirconia blank into a muffle furnace and sinter it under air atmosphere. During the sintering process, the blank is formed by sequentially passing through the first heating period, the first holding period, the second heating period, the second holding period, the third heating period, the third holding period, and the first cooling period. Specifically, this includes:

[0188] During the first heating phase, the temperature inside the muffle furnace is raised from room temperature to 200°C over a period of 30 minutes.

[0189] During the first heat preservation period, the temperature inside the muffle furnace is kept constant at 200℃ for 30 minutes.

[0190] During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min.

[0191] During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes.

[0192] In the third heating period, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a heating rate of 5℃ / min and a heating time of 90min.

[0193] During the third heat preservation period, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes.

[0194] After the first cooling period and the end of the process, the temperature inside the muffle furnace will naturally cool down from 1450℃ to room temperature.

[0195] Step S4: After natural cooling, yellow zirconia ceramic is obtained.

[0196] The above description is only a preferred embodiment of this application. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of this application, and these improvements and modifications should also be considered within the scope of protection of this application.

Claims

1. A method for preparing green zirconia ceramic, characterized in that, The solution is prepared using a liquid-phase impregnation method based on the principle of three primary colors, through a two-step dyeing and two-step sintering process; specifically, the steps include: S1. Weigh a certain amount of blue colorant raw material and prepare a blue colorant aqueous solution in a glass beaker using deionized water according to the concentration. S2. Immerse the zirconia blank in the blue colorant aqueous solution, and remove the immersed zirconia blank from the blue colorant aqueous solution and dry it to obtain a dried zirconia blank. S3. Place the dried zirconia blank into a muffle furnace and sinter it at 300-500°C under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain a zirconia ceramic blank. The holding time for the first sintering is 1-2 hours and the heating rate is 3-5°C / min. S4. Weigh a certain amount of yellow colorant raw material, prepare a yellow colorant aqueous solution in a glass beaker with deionized water according to the mass fraction / concentration, and heat and keep it warm in an oil bath. S5. Immerse the zirconia ceramic green body obtained in step S3 in the prepared yellow colorant aqueous solution for 5-10 minutes, and remove the immersed zirconia ceramic green body from the yellow colorant aqueous solution and dry it to obtain a dried zirconia ceramic green body. S6. Place the dried zirconia ceramic blank into a muffle furnace and sinter it a second time at 1350-1550°C under air atmosphere. After sintering is completed according to the preset heating rate and holding time, the program is stopped and the blank is cooled naturally to obtain the green zirconia ceramic. The holding time for the second sintering is 2-3 hours. The blue colorant raw material includes aluminum-containing salt and nickel-containing salt, with the ratio of aluminum ions to nickel ions being 1:10 to 1:2; the yellow colorant raw material includes vanadium-containing salt, with the mass fraction of vanadium ions in the yellow colorant aqueous solution being 1 to 5%.

2. The method for preparing green zirconia ceramic according to claim 1, characterized in that, The aluminum-containing salt is one of aluminum chloride, aluminum sulfate, or aluminum nitrate; the nickel-containing salt is one of nickel chloride, nickel sulfate, nickel nitrate, nickel bromide, or nickel sulfamate; and the vanadium-containing salt is one of ammonium metavanadate, sodium metavanadate, potassium metavanadate, sodium orthovanadate, vanadium oxysulfate, vanadium oxalate, vanadium tetrachloride, or vanadium oxychloride.

3. The method for preparing green zirconia ceramic according to claim 2, characterized in that, The aluminum-containing salt is aluminum nitrate, and the nickel-containing salt is nickel chloride, with an aluminum ion to nickel ion ratio of 1.0–1.4:0.1–0.5; The concentration of aluminum ions in the aqueous solution of the blue colorant is 1.0–1.5 mol / L, and the concentration of nickel ions is 0.1–0.5 mol / L. The vanadium-containing salt is ammonium metavanadate, and the concentration of the ammonium metavanadate solution is 1-3 g / 100 ml.

4. The method for preparing green zirconia ceramic according to claim 1, characterized in that, In step S2: the soaking time of immersing the zirconia blank in the blue colorant aqueous solution is 5-10 minutes; the soaking time of removing the zirconia blank from the blue colorant aqueous solution and drying it is specifically to dry it under an infrared therapy device for 30 minutes.

5. The method for preparing green zirconia ceramic according to claim 1, characterized in that, In step S4, the heating temperature of the oil bath is maintained at 60-80°C.

6. The method for preparing green zirconia ceramic according to claim 1, characterized in that, The second sintering process involves sequentially sintering through a first heating period, a first holding period, a second heating period, a second holding period, a third heating period, a third holding period, and a first cooling period to form a mature embryo, specifically including: The first heating phase involves raising the temperature inside the muffle furnace from room temperature to 200℃ for 30 minutes; the first holding phase involves maintaining the temperature inside the muffle furnace at 200℃ for 30 minutes. During the second heating period, the temperature inside the muffle furnace is raised from 200℃ to 1000℃ at a heating rate of 5℃ / min for a heating time of 160min. During the second heat preservation period, the temperature inside the muffle furnace is kept constant at 1000℃ for 30 minutes. In the third heating phase, the temperature inside the muffle furnace is raised from 1000℃ to 1450℃ at a rate of 5℃ / min for 90 minutes. In the third holding phase, the temperature inside the muffle furnace is kept constant at 1450℃ for 120 minutes. In the first cooling phase, the program ends and the temperature inside the muffle furnace is allowed to cool naturally from 1450℃ to room temperature.

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