CN117263656A - 95 high alumina ceramic and preparation method thereof - Google Patents

95 high alumina ceramic and preparation method thereof Download PDF

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CN117263656A
CN117263656A CN202310978661.0A CN202310978661A CN117263656A CN 117263656 A CN117263656 A CN 117263656A CN 202310978661 A CN202310978661 A CN 202310978661A CN 117263656 A CN117263656 A CN 117263656A
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alumina ceramic
temperature
silicon carbide
high alumina
ball milling
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戚志宇
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Zhengzhou Yana Powder Co ltd
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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Abstract

The invention discloses a 95 high alumina ceramic, which comprises, by mass, 93% -95% of alumina, 3-5% of modified silicon carbide whiskers, 1-2% of magnesia and 1-2% of silicon dioxide. The dispersibility of the silicon carbide whisker is improved by modifying the silicon carbide whisker by using a silane coupling agent, and then nickel-based modification is performed on the silicon carbide whisker, so that the mechanical strength, toughness and wear resistance of the 95 high alumina ceramic are improved as a whole by modifying the silicon carbide whisker twice.

Description

95 high alumina ceramic and preparation method thereof
Technical Field
The invention relates to the technical field of ceramics, in particular to a 95 high alumina ceramic and a preparation method thereof.
Background
Alumina ceramic is a material taking alumina as a main body, has good conductivity, mechanical strength and high temperature resistance, is a base material for manufacturing high-performance ceramic components with high strength, wear resistance, high temperature resistance and the like, and has been widely applied to the fields of machinery, communication, semiconductors, medicines, foods, petroleum, chemical industry, aerospace and the like.
According to the alumina ceramic, the content of alumina can be divided into varieties of 99 porcelain, 96 porcelain, 95 porcelain, 90 porcelain, 85 porcelain and the like, the comprehensive performance of the alumina ceramic is improved along with the improvement of the content of alumina, but the excessively high content of alumina leads to the rise of the cost of raw materials and the technical cost, the alumina ceramic with the content of 95 percent is mostly burned in the market and is matched with other auxiliary agents, wherein the problems of mechanical strength, toughness, sintering melting point and the like of the alumina ceramic are improved by adding silicon carbide, boron oxide, magnesium oxide, calcium oxide and calcium dioxide components, the chemical property of the silicon carbide is stable, the heat conductivity coefficient is high, the thermal expansion coefficient is small, the wear resistance is good, the shape of the silicon carbide micropowder after mechanical crushing in the industrial production process is irregular, agglomeration is easy to occur through the action of hydrogen bonds, the dispersion degree is low in the mixing process with other components, and the corresponding mechanical strength and toughness cannot be exerted stably, so the mechanical strength, toughness and wear resistance of the existing 95 ceramics need to be further improved.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a 95 high alumina ceramic with high mechanical strength, good toughness and good wear resistance and a preparation method thereof.
One of the purposes of the invention is to provide a 95 high alumina ceramic, which is realized by the following technical scheme: comprises the following components, by mass, 90% -95% of aluminum oxide, 3-5% of modified silicon carbide whisker, 1-2% of magnesium oxide and 1-2% of silicon dioxide.
The second purpose of the invention is to provide a preparation method of the 95 high alumina ceramic, which is realized by the following technical scheme: comprises the following steps of the method,
(1) Preparing materials: weighing the components according to the proportion and proportioning;
(2) Mixing: adding a solvent, a dispersing agent, a defoaming agent, an adhesive and a plasticizer into the weighed components for ball milling;
(3) Defoaming: placing the slurry subjected to ball milling into a vacuum deaeration machine for deaeration;
(4) And (3) forming: placing the defoamed slurry on a casting machine for casting and forming, and then stamping by using a stamping machine;
(5) And (3) low-temperature glue discharging: placing the obtained green sheet on a vacuum glue discharging machine to discharge glue for 3-5h at 500-550 ℃;
(6) Firing: and (3) placing the green body sheet after glue discharge in a sintering furnace, heating and sintering for three times, and naturally cooling to room temperature to obtain the 95 high alumina ceramic.
Further, the preparation steps of the modified silicon carbide whisker are as follows,
(1) Dispersing silicon carbide whiskers in hydrochloric acid to prepare suspension, and centrifugally washing and drying;
(2) Adding the dried silicon carbide whisker into a silane coupling agent to obtain slurry;
(3) Dissolving nickel carbonate and polyacrylamide in ammonia water;
(4) Adding ammonia water dissolved with nickel carbonate and polyacrylamide into the slurry to adjust to alkalescence;
(5) And standing the slurry for layering, filtering and drying to obtain the modified silicon carbide whisker.
Further, the silane coupling agent is one or more of methyltriethoxysilane, vinyltriethoxysilane and 3-aminopropyl triethoxysilane.
In the step (2), the weighed components are firstly added with a solvent, a dispersing agent and a defoaming agent for primary ball milling, wherein the primary ball milling time is 8 hours, and then added with an adhesive and a plasticizer for secondary ball milling, and the secondary ball milling time is 15 hours.
Further, in the step (6), firstly, the temperature is raised to 1200 ℃ at the speed of 5-8 ℃/min, the heat is preserved for 1h, then the temperature is raised to 1450 ℃ at the speed of 2-4 ℃/min, the heat is preserved for 1h, finally, the temperature is raised to 1650 ℃ at the speed of 1-2 ℃/min, the heat is preserved for 4h, the sintering furnace is closed, the temperature is naturally lowered to 800 ℃, and the sintering furnace is taken out and placed in a dryer, and is naturally cooled to the room temperature, thus obtaining the 95 high alumina ceramic.
Further, the drying temperature in step (5) is 50 to 60 ℃.
The invention has the following advantages: the silicon carbide whisker is cubic whisker and diamond belongs to a crystal form, the silicon carbide whisker has the highest hardness, the highest modulus and the highest tensile strength in the whisker synthesized at present, and is added into 95 high-alumina ceramic, so that the mechanical strength and toughness of the ceramic can be greatly enhanced, but the silicon carbide whisker has the problems of uneven mixing and agglomeration in the mixing process with other components.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below.
The invention provides a preparation method of 95 high alumina ceramic, which comprises the following steps,
(1) Preparing modified silicon carbide whiskers: dispersing purchased silicon carbide whiskers in 5-10% hydrochloric acid, stirring to prepare a suspension, centrifuging, washing and drying by using deionized water, dissolving one or more of methyltriethoxysilane, vinyltriethoxysilane and 3-aminopropyl triethoxysilane in ethanol to prepare a silane coupling agent with the concentration of about 2-6%, adding the dried silicon carbide whiskers into the silane coupling agent to obtain a stirring slurry, stirring and dissolving nickel carbonate and polyacrylamide in ammonia water, adding the ammonia water dissolved with the nickel carbonate and the polyacrylamide into the slurry, adjusting pH to 8-9, standing and layering the slurry, filtering, and drying at 50-60 ℃ to obtain modified silicon carbide whiskers;
(2) Preparing materials: weighing and batching the components according to the proportion of 90-95% of aluminum oxide, 3-5% of modified silicon carbide whisker, 1-2% of magnesium oxide and 1-2% of silicon dioxide;
(3) Mixing: firstly, adding a solvent, a dispersing agent and a defoaming agent into the weighed components for primary ball milling, wherein the primary ball milling time is 8 hours, and then adding an adhesive and a plasticizer for secondary ball milling, and the secondary ball milling time is 15 hours;
(4) Defoaming: placing the slurry subjected to ball milling into a vacuum deaeration machine for deaeration;
(5) And (3) forming: placing the defoamed slurry on a casting machine for casting and forming, and then stamping by using a stamping machine;
(6) And (3) low-temperature glue discharging: placing the obtained green sheet on a vacuum glue discharging machine to discharge glue for 3-5h at 500-550 ℃;
(7) Firing: and (3) placing the green sheet after glue discharging in a sintering furnace, firstly heating to 1200 ℃ at the speed of 5-8 ℃/min, preserving heat for 1h, then heating to 1450 ℃ at the speed of 2-4 ℃/min, preserving heat for 1h, finally heating to 1650 ℃ at the speed of 1-2 ℃/min, preserving heat for 4h, closing the sintering furnace, naturally cooling to 800 ℃, taking out, and naturally cooling to room temperature in a dryer to obtain the 95 high alumina ceramic.
The following describes the detailed technical scheme in connection with specific embodiments.
Example 1, (1) preparation of modified silicon carbide whiskers: dispersing purchased silicon carbide whiskers in 5% hydrochloric acid, stirring to prepare a suspension, centrifuging, washing with deionized water, drying, adding methyltriethoxysilane into ethanol to prepare about 2% of silane coupling agent, adding the dried silicon carbide whiskers into the silane coupling agent to obtain stirring slurry, stirring and dissolving nickel carbonate and polyacrylamide in ammonia water, adding ammonia water dissolved with nickel carbonate and polyacrylamide into the slurry, adjusting pH to 8, standing and layering the slurry, filtering, and drying at 50 ℃ to obtain modified silicon carbide whiskers;
(2) Preparing materials: weighing and mixing the components according to the proportion of 93% of aluminum oxide, 5% of modified silicon carbide whisker, 1% of magnesium oxide and 1% of silicon dioxide;
(3) Mixing: firstly, adding absolute ethyl alcohol solvent, polyethyleneimine dispersant and n-octanol deaerator into the weighed components for primary ball milling for 8 hours, and then adding polyvinyl butyral adhesive and dibutyl phthalate plasticizer for secondary ball milling for 15 hours;
(4) Defoaming: placing the slurry subjected to ball milling into a vacuum deaeration machine for deaeration;
(5) And (3) forming: placing the defoamed slurry on a casting machine for casting and forming, and then stamping by using a stamping machine;
(6) And (3) low-temperature glue discharging: placing the obtained green sheet on a vacuum glue discharging machine to discharge glue for 5 hours at 500 ℃;
(7) Firing: and (3) placing the green sheet after glue discharging in a sintering furnace, firstly heating to 1200 ℃ at a speed of 5 ℃/min, preserving heat for 1h, then heating to 1450 ℃ at a speed of 2 ℃/min, preserving heat for 1h, finally heating to 1650 ℃ at a speed of 1 ℃/min, preserving heat for 4h, closing the sintering furnace, naturally cooling to 800 ℃, taking out, placing in a dryer, and naturally cooling to room temperature to obtain the 95 high alumina ceramic.
The alumina ceramic substrate prepared in this example was tested and the performance was as follows: the bending strength is 830.5MPa, and the Rockwell hardness is 97.
Example 2, (1) preparation of modified silicon carbide whiskers: dispersing purchased silicon carbide whiskers in 5% hydrochloric acid, stirring to prepare a suspension, centrifuging, washing with deionized water, drying, dissolving two of vinyl triethoxysilane and 3-aminopropyl triethoxysilane in ethanol to prepare about 6% into a silane coupling agent, adding the dried silicon carbide whiskers into the silane coupling agent to obtain a stirring slurry, stirring and dissolving nickel carbonate and polyacrylamide in ammonia water, adding the ammonia water dissolved with the nickel carbonate and the polyacrylamide into the slurry, adjusting pH to 9, standing and layering the slurry, filtering, and drying at 60 ℃ to obtain modified silicon carbide whiskers;
(2) Preparing materials: weighing and mixing the components according to the proportion of 95% of aluminum oxide, 3% of modified silicon carbide whisker, 1% of magnesium oxide and 1% of silicon dioxide;
(3) Mixing: firstly, adding absolute ethyl alcohol solvent, polyethyleneimine dispersant and n-octanol deaerator into the weighed components for primary ball milling for 8 hours, and then adding polyvinyl butyral adhesive and dibutyl phthalate plasticizer for secondary ball milling for 15 hours;
(4) Defoaming: placing the slurry subjected to ball milling into a vacuum deaeration machine for deaeration;
(5) And (3) forming: placing the defoamed slurry on a casting machine for casting and forming, and then stamping by using a stamping machine;
(6) And (3) low-temperature glue discharging: placing the obtained green sheet on a vacuum glue discharging machine to discharge glue for 3 hours at 550 ℃;
(7) Firing: and (3) placing the green sheet after glue discharging in a sintering furnace, firstly heating to 1200 ℃ at the speed of 8 ℃/min, preserving heat for 1h, then heating to 1450 ℃ at the speed of 4 ℃/min, preserving heat for 1h, finally heating to 1650 ℃ at the speed of 1 ℃/min, preserving heat for 4h, closing the sintering furnace, naturally cooling to 800 ℃, taking out, placing in a dryer, and naturally cooling to room temperature to obtain the 95 high alumina ceramic.
The alumina ceramic substrate prepared in this example was tested and the performance was as follows: the bending strength is 813.2MPa, and the Rockwell hardness is 98.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.

Claims (7)

1. The 95 high alumina ceramic is characterized by comprising, by mass, 93% -95% of alumina, 3-5% of modified silicon carbide whiskers, 1-2% of magnesium oxide and 1-2% of silicon dioxide.
2. The method for preparing the 95 high alumina ceramic according to claim 1, comprising the following steps,
(1) Preparing materials: weighing the components according to the proportion and proportioning;
(2) Mixing: adding a solvent, a dispersing agent, a defoaming agent, an adhesive and a plasticizer into the weighed components for ball milling;
(3) Defoaming: placing the slurry subjected to ball milling into a vacuum deaeration machine for deaeration;
(4) And (3) forming: placing the defoamed slurry on a casting machine for casting and forming, and then stamping by using a stamping machine;
(5) And (3) low-temperature glue discharging: placing the obtained green sheet on a vacuum glue discharging machine to discharge glue for 3-5h at 500-550 ℃;
(6) Firing: and (3) placing the green body sheet after glue discharge in a sintering furnace, heating and sintering for three times, and naturally cooling to room temperature to obtain the 95 high alumina ceramic.
3. The method for preparing the 95 high alumina ceramic according to claim 2, wherein the modified silicon carbide whisker is prepared by the following steps,
(1) Dispersing silicon carbide whiskers in hydrochloric acid to prepare suspension, and centrifugally washing and drying;
(2) Adding the dried silicon carbide whisker into a silane coupling agent to obtain slurry;
(3) Dissolving nickel carbonate and polyacrylamide in ammonia water;
(4) Adding ammonia water dissolved with nickel carbonate and polyacrylamide into the slurry to adjust to alkalescence;
(5) And standing the slurry for layering, filtering and drying to obtain the modified silicon carbide whisker.
4. The method for preparing 95 high alumina ceramic according to claim 3, wherein the silane coupling agent is one or more of methyltriethoxysilane, vinyltriethoxysilane, and 3-aminopropyl triethoxysilane.
5. The method for preparing the 95 high alumina ceramic according to claim 2, wherein in the step (2), the weighed components are firstly added with a solvent, a dispersing agent and a defoaming agent for primary ball milling, the primary ball milling time is 8 hours, then added with an adhesive and a plasticizer for secondary ball milling, and the secondary ball milling time is 15 hours.
6. The method for preparing the 95 high alumina ceramic according to claim 2, wherein in the step (6), the temperature is raised to 1200 ℃ at a speed of 5-8 ℃/min, the temperature is kept for 1h, then the temperature is raised to 1450 ℃ at a speed of 2-4 ℃/min, the temperature is kept for 1h, finally the temperature is raised to 1650 ℃ at a speed of 1-2 ℃/min, the temperature is kept for 4h, the sintering furnace is closed, the temperature is naturally lowered to 800 ℃, and the 95 high alumina ceramic is obtained after being taken out and naturally cooled to room temperature in a dryer.
7. A method for producing a 95 high alumina ceramic according to claim 3, wherein the drying temperature in step (5) is 50 to 60 ℃.
CN202310978661.0A 2023-08-04 2023-08-04 95 high alumina ceramic and preparation method thereof Withdrawn CN117263656A (en)

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