CN108101520B - Aluminum oxide-silicon carbide composite material and preparation method thereof - Google Patents
Aluminum oxide-silicon carbide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of an aluminum oxide-silicon carbide composite material, which is characterized by comprising the following steps: the preparation method comprises the following steps: providing Al2O3Powder, SiC powder and Si3N4Pulverizing; mixing Al2O3Powder, SiC powder and Si3N4Performing first ball milling on the powder to obtain first mixed powder; providing Ti powder, Ni powder and Co powder; carrying out second ball milling on the Ti powder, the Ni powder and the Co powder to obtain second mixed powder; carrying out first reduction heat treatment on the second mixed powder to obtain third mixed powder; mixing the first mixed powder and the third mixed powder, and performing third ball milling to obtain fourth mixed powder, wherein the mass percentage of the first mixed powder in the fourth mixed powder is 85-95%; carrying out second reduction heat treatment on the second mixed powder to obtain fifth mixed powder; performing cold isostatic pressing on the fifth mixed powder so as to form a plate; and performing microwave sintering on the plate. The aluminum oxide-silicon carbide composite material has good fracture toughness, hardness and bending strength, and the product has excellent comprehensive performance.
Description
Technical Field
The invention relates to the field of composite materials, in particular to an aluminum oxide-silicon carbide composite material and a preparation method thereof.
Background
The alumina ceramic is a ceramic material which is developed earlier and applied widely, and has the advantages of high temperature resistance, high hardness, corrosion resistance, wear resistance, low density, low price and the like. However, the disadvantage of lower fracture toughness of alumina limits its widespread use. In order to overcome the defect of low fracture toughness of alumina, the prior art proposes a plurality of toughening methods and principles of alumina ceramics, wherein the more representative methods comprise: the composite material has the advantages of particle dispersion toughening, fiber and whisker toughening, zirconia phase change toughening, composite toughening, self toughening and the like. Among them, the alumina-silicon carbide composite is a more typical alumina ceramic with toughening property, and in order to further toughen, some prior arts propose a technology for toughening alumina ceramic by using mullite whisker, and the defects of the technology are: 1. the mullite whisker and the aluminum oxide-silicon carbide powder are difficult to mix, and the mullite whisker and the aluminum oxide-silicon carbide powder are difficult to mix uniformly, so that the product quality is unstable; 2. just because the mullite whisker and the alumina-silicon carbide powder are difficult to mix, when the mass of the powder and the whisker is larger, the powder and the whisker can not be uniformly mixed basically, which limits the industrialized application of the material; 3. the mullite whisker has higher price, which causes higher production cost.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide an aluminum oxide-silicon carbide composite material and a preparation method thereof, so that the defects of the prior art are overcome.
In order to achieve the above object, the present invention provides a method for preparing an aluminum oxide-silicon carbide composite material, which is characterized by comprising: the preparation method comprises the following steps: providing Al2O3Powder, SiC powder and Si3N4Pulverizing; mixing Al2O3Powder, SiC powder and Si3N4Performing first ball milling on the powder to obtain first mixed powder; providing Ti powder, Ni powder and Co powder; carrying out second ball milling on the Ti powder, the Ni powder and the Co powder to obtain second mixed powder; carrying out first reduction heat treatment on the second mixed powder to obtain third mixed powder; mixing the first mixed powder and the third mixed powder, and performing third ball milling to obtain fourth mixed powder, wherein the mass percentage of the first mixed powder in the fourth mixed powder is 85-95%; carrying out second reduction heat treatment on the second mixed powder to obtain fifth mixed powder; performing cold isostatic pressing on the fifth mixed powder so as to form a plate; and performing microwave sintering on the plate.
Preferably, in the above technical scheme, in percentage by weight, Al2O3The mass of the powder accounts for 40-50% of the mass of the first mixed powder, the mass of the SiC powder accounts for 40-45% of the mass of the first mixed powder, and the balance is Si3N4And (3) pulverizing.
Preferably, in the above technical scheme, the first ball milling process specifically comprises: the rotating speed of the ball mill is 500-700rpm, and the ball milling time is 2-3 h.
Preferably, in the above technical scheme, the mass of the Ti powder accounts for 30-40% of the mass of the second mixed powder, the mass of the Ni powder accounts for 30-40% of the mass of the second mixed powder, and the balance is Co powder.
Preferably, in the above technical scheme, the second ball milling process specifically comprises: the rotating speed of the ball mill is 1000-1500rpm, and the ball milling time is 15-25 h.
Preferably, in the above technical solution, the process of the first reduction heat treatment specifically includes: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 600-700 ℃, and the heat treatment time is 40-70 min.
Preferably, in the above technical solution, the third ball milling process specifically comprises: the rotating speed of the ball mill is 1000-1500rpm, and the ball milling time is 4-5 h.
Preferably, in the above technical solution, the second reduction heat treatment process specifically includes: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 800-900 ℃, and the heat treatment time is 40-70 min.
Preferably, in the above technical scheme, the specific process of microwave sintering is as follows: the microwave sintering atmosphere is argon, the microwave sintering temperature is 1200-1350 ℃, and the sintering time is 20-25 min.
The invention also provides an alumina-silicon carbide composite material prepared by the preparation method as claimed in the claim.
Compared with the prior art, the invention has the following beneficial effects: 1. the metal powder is used for replacing mullite whiskers, and experiments show that the metal powder and the aluminum oxide-silicon carbide powder are easier to mix, so that the ball milling time can be shortened, and a product with larger total mass can be manufactured; 2. the invention designs a new technical powder component, and experiments show that the metal mixed powder can greatly improve the fracture toughness of the aluminum oxide-silicon carbide composite material; 3. the ball milling can be carried out for a long time through the reduction heat treatment, the accurate chemical components of the product are ensured, and the product performance is improved; 4. the components of the aluminum oxide-silicon carbide composite material are optimized, and the mechanical property is improved.
Detailed Description
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component. The device is conventional in the field, the raw materials used in the device can be purchased from chemical product stores, and the fracture toughness, the bending strength and the hardness are tested according to the relevant national standards.
Example 1
The aluminum oxide-silicon carbide composite material is prepared by the following method: providing Al2O3Powder, SiC powder and Si3N4Pulverizing; mixing Al2O3Powder, SiC powder and Si3N4Performing first ball milling on the powder to obtain first mixed powder; providing Ti powder, Ni powder and Co powder; carrying out second ball milling on the Ti powder, the Ni powder and the Co powder to obtain second mixed powder; carrying out first reduction heat treatment on the second mixed powder to obtain third mixed powder; mixing the first mixed powder and the third mixed powder, and performing third ball milling to obtain fourth mixed powder, wherein the mass percentage of the first mixed powder in the fourth mixed powder is 85%; carrying out second reduction heat treatment on the second mixed powder to obtain fifth mixed powder; performing cold isostatic pressing on the fifth mixed powder so as to form a plate; and performing microwave sintering on the plate. By weight percent, Al2O3The mass of the powder is 40% of the mass of the first mixed powder, the mass of the SiC powder is 40% of the mass of the first mixed powder, and the balance is Si3N4And (3) pulverizing. The first ball milling process comprises the following specific steps: the rotating speed of the ball mill is 500rpm, and the ball milling time is 3 h. The mass of the Ti powder accounts for 30% of the mass of the second mixed powder, the mass of the Ni powder accounts for 30% of the mass of the second mixed powder, and the balance is Co powder. The second ball milling process comprises the following specific steps: the rotating speed of the ball mill is 1000rpm, and the ball milling time is 25 h. The first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 600 ℃, and the heat treatment time is 70 min. The third ball milling process comprises the following specific steps: the rotating speed of the ball mill is 1000, and the ball milling time is 5 h. The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 800 ℃, and the heat treatment time is 70 min. Details of microwave sinteringThe process comprises the following steps: the microwave sintering atmosphere is argon, the microwave sintering temperature is 1200 ℃, and the sintering time is 25 min.
Example 2
The aluminum oxide-silicon carbide composite material is prepared by the following method: providing Al2O3Powder, SiC powder and Si3N4Pulverizing; mixing Al2O3Powder, SiC powder and Si3N4Performing first ball milling on the powder to obtain first mixed powder; providing Ti powder, Ni powder and Co powder; carrying out second ball milling on the Ti powder, the Ni powder and the Co powder to obtain second mixed powder; carrying out first reduction heat treatment on the second mixed powder to obtain third mixed powder; mixing the first mixed powder and the third mixed powder, and performing third ball milling to obtain fourth mixed powder, wherein the mass percentage of the first mixed powder in the fourth mixed powder is 95%; carrying out second reduction heat treatment on the second mixed powder to obtain fifth mixed powder; performing cold isostatic pressing on the fifth mixed powder so as to form a plate; and performing microwave sintering on the plate. By weight percent, Al2O3The mass of the powder is 50% of the mass of the first mixed powder, the mass of the SiC powder is 45% of the mass of the first mixed powder, and the balance is Si3N4And (3) pulverizing. The first ball milling process comprises the following specific steps: the rotating speed of the ball mill is 700rpm, and the ball milling time is 2 h. The mass of the Ti powder accounts for 40% of the mass of the second mixed powder, the mass of the Ni powder accounts for 40% of the mass of the second mixed powder, and the balance is Co powder. The second ball milling process comprises the following specific steps: the rotating speed of the ball mill is 1500rpm, and the ball milling time is 15 h. The first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 700 ℃, and the heat treatment time is 40 min. The third ball milling process comprises the following specific steps: the rotating speed of the ball mill is 1500rpm, and the ball milling time is 4 h. The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 900 ℃, and the heat treatment time is 40 min. The specific process of microwave sintering comprises the following steps: the microwave sintering atmosphere is argon, the microwave sintering temperature is 1350 ℃, and the sintering time is 20 min.
Example 3
Aluminum oxide-silicon carbideThe composite material is prepared by the following method: providing Al2O3Powder, SiC powder and Si3N4Pulverizing; mixing Al2O3Powder, SiC powder and Si3N4Performing first ball milling on the powder to obtain first mixed powder; providing Ti powder, Ni powder and Co powder; carrying out second ball milling on the Ti powder, the Ni powder and the Co powder to obtain second mixed powder; carrying out first reduction heat treatment on the second mixed powder to obtain third mixed powder; mixing the first mixed powder and the third mixed powder, and performing third ball milling to obtain fourth mixed powder, wherein the fourth mixed powder comprises 90% of the first mixed powder by mass; carrying out second reduction heat treatment on the second mixed powder to obtain fifth mixed powder; performing cold isostatic pressing on the fifth mixed powder so as to form a plate; and performing microwave sintering on the plate. By weight percent, Al2O3The mass of the powder is 45% of the mass of the first mixed powder, the mass of the SiC powder is 45% of the mass of the first mixed powder, and the balance is Si3N4And (3) pulverizing. The first ball milling process comprises the following specific steps: the rotating speed of the ball mill is 600rpm, and the ball milling time is 2.5 h. The mass of the Ti powder accounts for 30-40% of the mass of the second mixed powder, the mass of the Ni powder accounts for 35% of the mass of the second mixed powder, and the balance is Co powder. The second ball milling process comprises the following specific steps: the rotating speed of the ball mill is 1200rpm, and the ball milling time is 20 h. The first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 650 ℃, and the heat treatment time is 60 min. The third ball milling process comprises the following specific steps: the rotating speed of the ball mill is 1200rpm, and the ball milling time is 4.5 h. The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 850 ℃, and the heat treatment time is 60 min. The specific process of microwave sintering comprises the following steps: the microwave sintering atmosphere is argon, the microwave sintering temperature is 1300 ℃, and the sintering time is 20 min.
Example 4
The first mixed powder is only Al2O3Powder and SiC powder, Al2O3The mass of the powder is 50% of the mass of the first mixed powder, the mass of the SiC powder is 50% of the mass of the first mixed powder, and the other conditions, parameters, and,The procedure and composition were the same as in example 3.
Example 5
The second mixed powder was composed of only Ti powder and Ni powder, the mass of the Ti powder accounted for 50% by mass of the second mixed powder, and the mass of the Ni powder accounted for 50% by mass of the second mixed powder, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 6
The third ball milling was carried out without the first reduction heat treatment, and the other conditions, parameters, steps and components were the same as in example 3.
Example 7
The cold isostatic pressing was carried out without the second reduction heat treatment, and the conditions, parameters, steps and components were the same as those in example 3.
Example 8
The first mixed powder was 80% by mass, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 9
Carrying out hot-pressing sintering on the plate, wherein the specific hot-pressing sintering process comprises the following steps: the sintering temperature is 1300 ℃ and 1400 ℃, the pressure is 50-100MPa, the sintering time is 5-6h, and the rest conditions, parameters, steps and components are the same as those in the embodiment 3.
Example 10
Al2O3The mass of the powder was 35% of the mass of the first mixed powder, and the remaining conditions, parameters, steps, and ingredients were the same as in example 3.
Example 11
The mass of the SiC powder accounted for 35% of the mass of the first mixed powder, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 12
The first ball milling process comprises the following specific steps: the rotation speed of the ball mill is 400rpm, the ball milling time is 5h, and the rest conditions, parameters, steps and components are the same as those in example 3.
Example 13
The mass of the Ti powder was 25% of the mass of the second mixed powder, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 14
The mass of the Ti powder was 45% of the mass of the second mixed powder, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 15
The mass of the Ni powder was 25% of the mass of the second mixed powder, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 16
The mass of the Ni powder was 45% of the mass of the second mixed powder, and the remaining conditions, parameters, steps, and components were the same as in example 3.
Example 17
The second ball milling process comprises the following specific steps: the rotation speed of the ball mill is 800rpm, the ball milling time is 35h, and the rest conditions, parameters, steps and components are the same as those in example 3.
Example 18
The first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 550 ℃, and the heat treatment time is 60 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 19
The first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 750 ℃, and the heat treatment time is 60 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 20
The first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 650 ℃, and the heat treatment time is 30 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 21
The third ball milling process comprises the following specific steps: the rotation speed of the ball mill is 1700rpm, the ball milling time is 3h, and the rest conditions, parameters, steps and components are the same as those in the embodiment 3.
Example 22
The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 700 ℃, and the heat treatment time is 60 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 23
The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 1000 ℃, and the heat treatment time is 60 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 24
The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 850 ℃, and the heat treatment time is 30 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 25
The second reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 850 ℃, and the heat treatment time is 100 min. The other conditions, parameters, steps and components were the same as in example 3.
Example 26
The specific process of microwave sintering comprises the following steps: the microwave sintering atmosphere is argon, the microwave sintering temperature is 1100 ℃, and the sintering time is 100 min. The other conditions, parameters, steps and components were the same as in example 3.
The composite materials manufactured in examples 1 to 26 were tested for fracture toughness, flexural strength, and hardness, and the test results are shown in Table 1. For comparison, the above test result values were normalized with respect to the value of example 1.
TABLE 1
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (1)
1. A preparation method of an aluminum oxide-silicon carbide composite material is characterized by comprising the following steps: providing Al2O3Powder, SiC powder and Si3N4Pulverizing; mixing Al2O3 powder, SiC powder and Si3N4Performing first ball milling on the powder to obtain first mixed powder; providing Ti powder, Ni powder and Co powder; carrying out second ball milling on the Ti powder, the Ni powder and the Co powder to obtain second mixed powder; carrying out first reduction heat treatment on the second mixed powder to obtain third mixed powder; mixing the first mixed powder and the third mixed powder, and performing third ball milling to obtain fourth mixed powder, wherein the mass percentage of the first mixed powder in the fourth mixed powder is 95%; performing second reduction heat treatment on the fourth mixed powder to obtain fifth mixed powder; performing cold isostatic pressing on the fifth mixed powder so as to form a plate; and microwave sintering the plate, wherein the weight percentage of Al is2O3The mass of the powder is 50% of the mass of the first mixed powder, the mass of the SiC powder is 45% of the mass of the first mixed powder, and the balance is Si3N4The powder is prepared by a first ball milling process which specifically comprises the following steps: the rotating speed of the ball mill is 700rpm, the ball milling time is 2 hours, the mass of Ti powder accounts for 40% of the mass of the second mixed powder, the mass of Ni powder accounts for 40% of the mass of the second mixed powder, and the balance is Co powder, wherein the second ball milling process specifically comprises the following steps: the rotating speed of the ball mill is 1500rpm, the ball milling time is 15h, and the first reduction heat treatment process specifically comprises the following steps: the heat treatment atmosphere is hydrogen, the heat treatment temperature is 700 ℃, the heat treatment time is 40min, and the third ball milling process specifically comprises the following steps: the rotating speed of the ball mill is 1500rpm, the ball milling time is 4h, and the process of the second reduction heat treatment specifically comprises the following steps: the heat treatment atmosphere is hydrogen, and the heat treatment is carried outThe temperature is 900 ℃, the heat treatment time is 40min, and the specific process of microwave sintering is as follows: the microwave sintering atmosphere is argon, the microwave sintering temperature is 1350 ℃, and the sintering time is 20 min.
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