CN113233878A - Alumina ceramic composite material and preparation method thereof - Google Patents
Alumina ceramic composite material and preparation method thereof Download PDFInfo
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- CN113233878A CN113233878A CN202110667404.6A CN202110667404A CN113233878A CN 113233878 A CN113233878 A CN 113233878A CN 202110667404 A CN202110667404 A CN 202110667404A CN 113233878 A CN113233878 A CN 113233878A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 239000002131 composite material Substances 0.000 title claims abstract description 111
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 68
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 61
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 61
- 238000000034 method Methods 0.000 claims abstract description 27
- 230000008595 infiltration Effects 0.000 claims abstract description 19
- 238000001764 infiltration Methods 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 230000009466 transformation Effects 0.000 claims abstract description 5
- 238000005269 aluminizing Methods 0.000 claims abstract description 4
- 239000011159 matrix material Substances 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 230000007704 transition Effects 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 239000000835 fiber Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 230000036961 partial effect Effects 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000007733 ion plating Methods 0.000 claims description 3
- 238000007750 plasma spraying Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 25
- 238000007789 sealing Methods 0.000 abstract description 4
- 239000012071 phase Substances 0.000 description 30
- 238000005452 bending Methods 0.000 description 11
- 230000007797 corrosion Effects 0.000 description 11
- 238000005260 corrosion Methods 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 229910052574 oxide ceramic Inorganic materials 0.000 description 7
- 239000011224 oxide ceramic Substances 0.000 description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- SAUMVKNLVQDHMJ-UHFFFAOYSA-N dichlorine trioxide Inorganic materials ClOCl(=O)=O SAUMVKNLVQDHMJ-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/40—Metallic constituents or additives not added as binding phase
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Abstract
The invention relates to the technical field of material surface engineering, in particular to an alumina ceramic composite material and a preparation method thereof. The preparation method of the alumina ceramic composite material comprises the following steps: aluminizing the surface of the alumina ceramic substrate to form an aluminum film layer, then carrying out infiltration treatment, and then carrying out Al2O3The phase transformation treatment makes the aluminum film layer become Al2O3And (4) a stable phase layer. The method can effectively inhibit the crack propagation of the composite material, can perform hole sealing treatment, is convenient and low in cost, and prolongs the service life of the composite material.
Description
Technical Field
The invention relates to the technical field of material surface engineering, in particular to an alumina ceramic composite material and a preparation method thereof.
Background
The alumina ceramic matrix composite material has low density and high strength, becomes a hot door material which replaces nickel-based high-temperature alloy and is applied to important aerospace devices at present, wherein the alumina fiber toughens the alumina ceramic matrix composite material (Al)2O3f/Al2O3) The composite material is a composite material which takes alumina ceramic as a matrix, introduces alumina fibers as a reinforcing material into the matrix, and takes the alumina fibers as a reinforcing phase and a ceramic matrix as a continuous phase. The material has high specific strength, corrosion resistance and fracture toughness which are superior to those of single-phase alumina ceramic materials, has higher oxidation resistance and lower cost compared with silicon carbide non-oxide ceramic base materials, is an ideal high-temperature oxidation resistant and fracture resistant material, and has great application value in aerospace hot end parts such as a returning cabin, an engine combustion chamber, a tail nozzle and the like.
Conventional preparation of Al2O3f/Al2O3The basic principle of the composite material is that matrix slurry or liquid-phase precursor is filled into fiber cloth or a prefabricated member, and then drying and sintering are carried out, so as to finally obtain the composite material. Among them, the alumina ceramic matrix filling method can be classified into a slurry method and a sol-gel method. And preparing Al by sol-gel method2O3f/Al2O3When the composite material is used, after the molten gel is dried and gelled, the high-temperature heat treatment process is carried out, and the gel loses water to cause volume shrinkage, so that the defects of microcracks, pores and the like are formed in the surface of the composite material. The microcrack defect can become a crack propagation source to directly influence the service life of the material, and the pore defect can influence the overall physical and chemical properties of the material by reducing the internal oxidation resistance of the material and softening the toughness of the material, so that the overall degradation of the material is caused. For Al2O3f/Al2O3Preparation of composite materialThe process is insufficient for forming microcracks and pore defects on the surface of the material, and if the surface defects are removed by using the traditional machining method, on one hand, the material processing allowance needs to be reserved, which may cause raw material waste and surge cost, and on the other hand, the alumina fiber structure may be damaged, which affects the toughness of the material.
In view of the above problems, there is a need to develop a method for improving Al by effectively inhibiting the crack propagation of a material and performing a hole sealing treatment2O3f/Al2O3A preparation method of the service life of the composite material.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide an alumina ceramic composite material and a preparation method thereof. The method can effectively inhibit the crack propagation of the composite material, can perform hole sealing treatment, is convenient and low in cost, and prolongs the service life of the composite material.
The invention is realized by the following steps:
in a first aspect, an embodiment of the present invention provides a method for preparing an alumina ceramic composite material, including: aluminizing the surface of the alumina ceramic substrate to form an aluminum film layer, then carrying out infiltration treatment, and then carrying out Al2O3The phase transformation treatment makes the aluminum film layer become Al2O3And (4) a stable phase layer.
In a preferred embodiment, the aluminum film layer has a thickness of 10-15 microns.
In a preferred embodiment, the method of forming the aluminum film layer comprises: any one of magnetron sputtering, evaporation coating, ion plating and plasma spraying;
preferably, the method for forming the aluminum film layer is magnetron sputtering.
In a preferred embodiment, the conditions of magnetron sputtering include: the magnetron target current is 2-5A, the bias voltage is 100-200V, and the air pressure is less than 5 multiplied by 10-3Pa, raw material is a cylindrical aluminum target with 99.9% purity.
In a preferred embodiment, the infiltration process comprises: carrying out vacuum heat treatment on the alumina ceramic matrix with the aluminum film layer on the surface;
preferably, the conditions of the vacuum heat treatment include: 500-800 ℃ heat preservation for 3-5h, and the vacuum oxygen partial pressure is less than 2 multiplied by 10-4Pa; the heating rate is 15-20 ℃/min.
In a preferred embodiment, Al2O3The phase transition process includes: subjecting the infiltrated alumina ceramic matrix to Al in the presence of oxygen2O3Phase transition heat treatment;
preferably, Al2O3The phase transition process includes: in the atmospheric environment, the temperature of the infiltrated alumina ceramic matrix is kept for 1 to 3 hours at the temperature of 1300 ℃ and 1400 ℃, and the heating rate is 6 to 10 ℃/min.
In a preferred embodiment, the alumina ceramic matrix is pretreated before the aluminum film layer is formed;
preferably, the pre-treatment comprises: and ultrasonic cleaning and impurity removal are carried out on the alumina ceramic matrix by sequentially utilizing acetone, alcohol and water.
In a preferred embodiment, the alumina ceramic matrix is an alumina ceramic composite matrix that has been toughened with alumina fibers.
In a second aspect, the embodiment of the present invention provides an alumina ceramic composite material, which is prepared by the above preparation method of the alumina ceramic composite material.
In a preferred embodiment, the aluminum oxide ceramic matrix comprises an aluminum oxide ceramic matrix and Al attached to the surface of the aluminum oxide ceramic matrix2O3A stable phase layer;
preferably, the alumina ceramic composite is an alumina ceramic composite matrix that has been toughened by alumina fibers.
The invention has the following beneficial effects: according to the embodiment of the invention, the aluminum material is melted by carrying out infiltration treatment on the alumina ceramic matrix with the aluminum film layer on the surface, the molten aluminum liquid flows and is filled into microcracks and pores in the alumina ceramic matrix under the action of capillary force and is fused with the alumina ceramic matrix, the stretchability of the alumina ceramic matrix is enhanced, and then Al is carried out2O3The single metal aluminum film on the surface is changed into compact Al by phase transition treatment2O3The method not only achieves the aim of inhibiting crack propagation, but also carries out hole sealing treatment on the material, reduces the internal oxidation rate of the material and improves the oxidation resistance and corrosion resistance of the alumina ceramic composite material.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 shows Al of example 22O3f/Al2O3A cross-sectional profile of the composite;
FIG. 2 shows Al of example 22O3f/Al2O3Surface crack topography of the composite;
FIG. 3 is a cross-sectional profile of the alumina ceramic composite of example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the invention provides a preparation method of an alumina ceramic composite material, which comprises the following steps:
pretreating the alumina ceramic matrix, wherein the alumina ceramic matrix can be an alumina ceramic composite matrix base toughened by alumina fibers, namely the alumina ceramic matrix can be Al2O3f/Al2O3Composite material of the Al2O3f/Al2O3The composite material is prepared by a sol-gel method in the prior art, and the productInventive embodiments will not be described in detail.
The pretreatment comprises the following steps: the alumina ceramic matrix is subjected to ultrasonic cleaning by sequentially utilizing acetone, alcohol and water, and then impurities such as oil stains on the surface of the alumina ceramic matrix are removed, so that the subsequent formed Al is promoted2O3The binding force between the stable phase layer and the alumina ceramic group improves the performance of the formed alumina ceramic composite material.
Then aluminizing the surface of the alumina ceramic substrate to form an aluminum film layer, wherein the thickness of the aluminum film layer is 10-15 microns. The aluminum film layer can be favorable for improving the performance of the formed alumina ceramic composite material within the thickness range, if the thickness of the aluminum film layer is too high, the aluminum film layer is easy to fall off from the alumina ceramic matrix, and if the thickness of the aluminum film layer is too low, the mechanical properties such as strength, toughness and the like of the subsequently formed alumina ceramic composite material are reduced.
Further, the method for forming the aluminum film layer comprises the following steps: any one of magnetron sputtering, evaporation coating, ion plating and plasma spraying. The above mode can be used for forming the aluminum film layer, magnetron sputtering is adopted only more preferably, the thickness of the formed aluminum film layer can be controlled more easily by adopting the mode, the formed aluminum film layer is ensured to be in a required thickness range, the aluminum film layer can also be formed by other modes, only the thickness of the formed aluminum film layer is not easy to control, and the fluctuation is large.
Further, the magnetron sputtering conditions include: the magnetron target current is 2-5A, the bias voltage is 100-200V, and the air pressure is less than 5 multiplied by 10-3Pa, raw material is a cylindrical aluminum target with 99.9% purity. The adoption of the conditions is more beneficial to controlling the thickness of the formed aluminum film layer.
And then, carrying out infiltration treatment to melt the aluminum of the aluminum film layer, and then enabling the molten aluminum liquid to flow and fill the microcracks and the pores under the action of capillary force to be fused with the alumina ceramic matrix so as to enhance the stretchability of the material.
Specifically, the alumina ceramic matrix with the aluminum film layer on the surface is subjected to vacuum heat treatment; after vacuumizing, the crystal lattice of the metal expands in a low-pressure environment, the melting point is reduced, then the aluminum material can be efficiently liquefied at the temperature lower than the melting point of the aluminum, and the molten aluminum flows and is filled into the microcracks and the pores under the action of capillary force and is fused with the aluminum oxide ceramic matrix, so that the stretchability of the material is enhanced.
Specifically, the conditions of the vacuum heat treatment include: 500-800 ℃ heat preservation for 3-5h, and the vacuum oxygen partial pressure is less than 2 multiplied by 10-4Pa; the heating rate is 15-20 ℃/min. Adopt above-mentioned condition can guarantee the effect of infiltration, if vacuum heat treatment's temperature is too high, probably lead to the aluminium material to evaporate, lead to the infiltration effect to reduce then, if the temperature is too low, probably lead to not can the infiltration, also can lead to the infiltration effect to reduce.
Then, Al is further performed2O3The phase transformation treatment makes the aluminum film layer become Al2O3Stationary phase layers, i.e. formation of Al2O3A stable phase layer, the infiltration does not form large area of Al2O3Since the phase is basically aluminum material, Al is carried out2O3Phase transformation treatment to form Al2O3And the stable phase layer can further improve mechanical properties such as oxidation resistance, corrosion resistance and the like of the alumina ceramic composite material.
Specifically, Al is carried out on the infiltrated alumina ceramic matrix under the aerobic condition2O3Phase transition heat treatment; for example, in the atmospheric environment, the temperature of the infiltrated alumina ceramic matrix is maintained at 1300-1400 ℃ for 1-3 hours, and the heating rate is 6-10 ℃/min. The adoption of the mode can be beneficial to Al2O3And forming a stable phase layer.
Specifically, the high-temperature heat treatment is carried out in an oxygen-rich atmosphere to spread on an alumina ceramic matrix such as Al2O3f/Al2O3Al is carried out on a single metal aluminum film layer on the surface of the composite material2O3Phase transition to form densification (compactness)>85%) of Al2O3And (4) a stable phase layer. The surface composition of the formed alumina ceramic composite material is basically consistent with the internal composition thereof, the chemical compatibility is good, no harmful chemical interface layer is generated, secondly, a layer of compact protective film is formed on the surface of the composite material,further increase Al content2O3f/Al2O3Oxidation and corrosion resistance of the composite material.
The embodiment of the invention also provides the alumina ceramic composite material, which is prepared by the preparation method of the alumina ceramic composite material. Specifically, the aluminum oxide ceramic substrate comprises an aluminum oxide ceramic substrate and Al attached to the surface of the aluminum oxide ceramic substrate2O3A stable phase layer; for example, the composite material comprises an alumina ceramic composite matrix toughened by alumina fibers and an Al2O3 stable phase layer attached to the surface of the matrix.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of an alumina ceramic composite material, which comprises the following steps:
for Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetic control target current of 2A, bias voltage of 150V and air pressure of 4 multiplied by 10-3Pa in Al2O3f/Al2O3Preparing an aluminum film layer with the thickness of 10 mu m on the surface of the composite material; at a vacuum oxygen partial pressure of 1X 10-4Pa, carrying out aluminum liquid infiltration treatment on the surface of the composite material in a heat treatment furnace at the temperature of 500 ℃, and keeping the temperature for 3h at the heating rate of 15 ℃/min. Then Al is carried out in the atmospheric environment in a muffle furnace with the temperature of 1300 DEG C2O3Phase transition heat treatment, keeping the temperature for 1h, and increasing the temperature at the rate of 6 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The bending strength of the modified composite material sample is 198MPa after being oxidized for 50 hours at 1400 ℃, and the bending strength is 90 percent H at 1400 DEG C2O-10O2And the service life of the product reaches 511h under the high-temperature vapor corrosion condition of 1 atm.
Example 2
Firstly to Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetic control target current of 2A, bias voltage of 150V and air pressure of 3 multiplied by 10-3Pa in Al2O3f/Al2O3Preparing an aluminum film layer with the thickness of 11 mu m on the surface of the composite material; at a vacuum oxygen partial pressure of 1X 10- 4Pa, carrying out aluminum liquid infiltration treatment on the surface of the composite material in a heat treatment furnace at the temperature of 500 ℃, and keeping the temperature for 3h at the heating rate of 16 ℃/min. Then Al is carried out in the atmospheric environment in a muffle furnace with the temperature of 1300 DEG C2O3Phase transition heat treatment, keeping the temperature for 1h, and increasing the temperature at the rate of 6 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The modified composite material sample has a bending strength of 259MPa after being oxidized for 50 hours at 1400 ℃ and 90% H at 1400 DEG C2O-10O2The service life of the catalyst reaches 592h under the high-temperature vapor corrosion condition of 1 atm.
Example 3
Firstly to Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetic control target current of 2A, bias voltage of 150V and air pressure of 4 multiplied by 10-3Pa in Al2O3f/Al2O3Preparing an aluminum film layer with the thickness of 12 mu m on the surface of the composite material; at a vacuum oxygen partial pressure of 3X 10- 5Pa, carrying out aluminum liquid infiltration treatment on the surface of the composite material in a heat treatment furnace at the temperature of 500 ℃, and keeping the temperature for 4h at the heating rate of 17 ℃/min. Then Al is carried out in the atmospheric environment in a muffle furnace with the temperature of 1300 DEG C2O3Phase transition heat treatment, keeping the temperature for 1h, and increasing the temperature at the rate of 8 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The modified composite material sample is oxidized for 50 hours at 1400 DEG CThe bending strength is 270MPa, at 1400 ℃ and 90% H2O-10O2And the service life of the product reaches 690h under the high-temperature vapor corrosion condition of 1 atm.
Example 4
Firstly to Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetic control target current of 2A, bias voltage of 150V and air pressure of 3 multiplied by 10-3Pa in Al2O3f/Al2O3Preparing an aluminum film layer with the thickness of 12 mu m on the surface of the composite material; at a vacuum oxygen partial pressure of 3X 10- 5Pa, the temperature is 700 ℃, the surface of the composite material is subjected to molten aluminum infiltration treatment in a heat treatment furnace, the temperature is kept for 4h, and the heating rate is 18 ℃/min. Then Al is carried out in the atmospheric environment in a muffle furnace with the temperature of 1300 DEG C2O3Phase transition heat treatment, keeping the temperature for 1h, and increasing the temperature at the rate of 8 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The modified composite material sample has a bending strength of 259MPa after being oxidized for 50 hours at 1400 ℃ and 90% H at 1400 DEG C2O-10O2The service life of the product reaches 650h under the high-temperature vapor corrosion condition of 1 atm.
Example 5
Firstly to Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetron target current of 3A, bias voltage of 150V and air pressure of 4 multiplied by 10-3Pa in Al2O3f/Al2O3Preparing an aluminum film layer with the thickness of 15 mu m on the surface of the composite material; at vacuum oxygen partial pressure of 5X 10- 5Pa, the temperature is 700 ℃, the surface of the composite material is subjected to molten aluminum infiltration treatment in a heat treatment furnace, the temperature is kept for 4h, and the heating rate is 18 ℃/min. Then, the mixture is subjected to A in an atmospheric environment in a muffle furnace at a temperature of 1350 DEG Cl2O3Phase transition heat treatment, keeping the temperature for 3h, and increasing the temperature at a rate of 10 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The bending strength of the modified composite material sample after being oxidized for 50 hours at 1400 ℃ is 231MPa, and the bending strength is 90 percent H at 1400 DEG C2O-10O2The service life of the product reaches 630h under the high-temperature vapor corrosion condition of 1 atm.
Example 6
Firstly to Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetron target current of 3A, bias voltage of 150V and air pressure of 4 multiplied by 10-3Pa in Al2O3f/Al2O3Preparing an aluminum film layer with the thickness of 12 mu m on the surface of the composite material; at a vacuum oxygen partial pressure of 3X 10- 5Pa, carrying out aluminum liquid infiltration treatment on the surface of the composite material in a heat treatment furnace at the temperature of 800 ℃, and keeping the temperature for 5h at the heating rate of 20 ℃/min. Then Al is carried out in the atmospheric environment in a muffle furnace with the temperature of 1400 DEG C2O3Phase transition heat treatment, keeping the temperature for 2h, and increasing the temperature at a rate of 10 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The bending strength of the modified composite material sample after being oxidized for 50 hours at 1400 ℃ is 226MPa, and the bending strength is 90 percent H at 1400 DEG C2O-10O2The service life of the catalyst reaches 622h under the high-temperature vapor corrosion condition of 1 atm.
Example 7
Firstly to Al2O3f/Al2O3The composite material adopts Al in a beaker filled with acetone, alcohol and deionized water in sequence2O3f/Al2O3Ultrasonic cleaning the composite material to remove impurities on the surface, and then adopting magnetic control target current of 2A, bias voltage of 150V and air pressure of 4 multiplied by 10-3Pa in Al2O3f/Al2O3Composite materialPreparing an aluminum film layer with the thickness of 11 mu m on the surface; at a vacuum oxygen partial pressure of 1X 10- 4Pa, carrying out aluminum liquid infiltration treatment on the surface of the composite material in a heat treatment furnace at the temperature of 500 ℃, and keeping the temperature for 3h at the heating rate of 15 ℃/min. Then Al is carried out in the atmospheric environment in a muffle furnace with the temperature of 1400 DEG C2O3Phase transition heat treatment, keeping the temperature for 1h, and increasing the temperature at a rate of 10 ℃/min to finally obtain Al modified by the aluminum film2O3f/Al2O3The composite material is alumina ceramic composite material. The bending strength of the modified composite material sample is 198MPa after being oxidized for 50 hours at 1400 ℃, and the bending strength is 90 percent H at 1400 DEG C2O-10O2The service life of the catalyst reaches 592h under the high-temperature vapor corrosion condition of 1 atm.
Experimental example 1
For the substrate of example 2: al (Al)2O3f/Al2O3The composite material and the alumina ceramic composite material are subjected to electron microscope scanning, and the detection result is shown in figures 1-3. Wherein FIG. 1 shows Al of example 22O3f/Al2O3A cross-sectional profile of the composite; FIG. 2 shows Al of example 22O3f/Al2O3Surface crack topography of the composite; FIG. 3 is a cross-sectional profile of the alumina ceramic composite of example 2.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the alumina ceramic composite material is characterized by comprising the following steps: aluminizing the surface of the alumina ceramic substrate to form an aluminum film layer, then carrying out infiltration treatment, and then carrying out Al2O3The phase transformation treatment makes the aluminum film layer become Al2O3And (4) a stable phase layer.
2. The method of claim 1, wherein the aluminum film layer has a thickness of 10 to 15 μm.
3. The method of preparing an alumina ceramic composite according to claim 1, wherein the method of forming the aluminum film layer comprises: any one of magnetron sputtering, evaporation coating, ion plating and plasma spraying;
preferably, the method for forming the aluminum film layer is magnetron sputtering.
4. The method for preparing an alumina ceramic composite material according to claim 3, wherein the magnetron sputtering conditions include: the magnetron target current is 2-5A, the bias voltage is 100-200V, and the air pressure is less than 5 multiplied by 10-3Pa, raw material is a cylindrical aluminum target with 99.9% purity.
5. The method of preparing an alumina ceramic composite according to claim 1, wherein the infiltration treatment comprises: carrying out vacuum heat treatment on the alumina ceramic matrix with the aluminum film layer on the surface;
preferably, the conditions of the vacuum heat treatment include: 500-800 ℃ heat preservation for 3-5h, and the vacuum oxygen partial pressure is less than 2 multiplied by 10-4Pa; the heating rate is 15-20 ℃/min.
6. The method of claim 1, wherein the Al is Al2O3The phase transition process includes: subjecting the infiltrated alumina ceramic matrix to Al in the presence of oxygen2O3Phase transition heat treatment;
preferably, Al2O3The phase transition process includes: in the atmospheric environment, the temperature of the infiltrated alumina ceramic matrix is kept for 1 to 3 hours at the temperature of 1300 ℃ and 1400 ℃, and the heating rate is 6 to 10 ℃/min.
7. The method for preparing an alumina ceramic composite material according to claim 1, wherein the alumina ceramic base is subjected to a pretreatment before the formation of the aluminum film layer;
preferably, the pre-treatment comprises: and ultrasonic cleaning and impurity removal are carried out on the alumina ceramic matrix by sequentially utilizing acetone, alcohol and water.
8. The method of preparing an alumina ceramic composite according to any one of claims 2 to 7, wherein the alumina ceramic matrix is an alumina ceramic composite matrix that has been toughened with alumina fibers.
9. An alumina ceramic composite material, characterized in that it is prepared by the method for preparing an alumina ceramic composite material according to any one of claims 1 to 8.
10. The alumina ceramic composite according to claim 9, comprising an alumina ceramic matrix and Al attached to the surface of the alumina ceramic matrix2O3A stable phase layer;
preferably, the alumina ceramic composite is an alumina ceramic composite matrix that has been toughened by alumina fibers.
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| CN115072754A (en) * | 2022-06-10 | 2022-09-20 | 广东省科学院新材料研究所 | Alumina ceramic hollow microsphere and preparation method and application thereof |
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| CN111302833A (en) * | 2020-04-06 | 2020-06-19 | 上海电机学院 | Method for improving wettability of aluminum to alumina ceramic |
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| CN111302833A (en) * | 2020-04-06 | 2020-06-19 | 上海电机学院 | Method for improving wettability of aluminum to alumina ceramic |
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