CN115028449B - AlHfTaO6 ceramic powder and preparation method and application thereof - Google Patents

AlHfTaO6 ceramic powder and preparation method and application thereof Download PDF

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CN115028449B
CN115028449B CN202210957161.4A CN202210957161A CN115028449B CN 115028449 B CN115028449 B CN 115028449B CN 202210957161 A CN202210957161 A CN 202210957161A CN 115028449 B CN115028449 B CN 115028449B
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alhftao
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temperature
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CN115028449A (en
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余艺平
李�浩
王松
李伟
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National University of Defense Technology
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Abstract

The invention discloses an AlHfTaO 6 The preparation method comprises the following steps of weighing Al according to a molar ratio of 1 2 O 3 Powder, hfO 2 Powder and Ta 2 O 5 The powder is used as a raw material, the molar ratio can promote different raw materials to react according to a certain reaction path to generate a target product without generating byproducts, unreacted reactant phases in the product are effectively prevented from remaining, and the AlHfTaO is prepared by ball milling, uniformly mixing, dry pressing and roasting 6 Ceramic powder. The preparation method has simple process, low equipment requirement and short preparation period, and can prepare the AlHfTaO with single phase, high dispersion, fine and uniform particle size by controlling the high-temperature roasting process conditions 6 The ceramic powder can be used for preparing high-temperature-resistant thermal protection environmental barrier coatings for hot end parts of aero-engines and rocket engines. In addition, the method has wide source of raw materials and low cost, and can be popularized to industrial production.

Description

AlHfTaO6 ceramic powder and preparation method and application thereof
Technical Field
The invention relates to the technical field of high-temperature functional ceramic powder, in particular to AlHfTaO 6 Ceramic powder and a preparation method and application thereof.
Background
The silicon carbide ceramic matrix composite has the excellent characteristics of low density, high temperature resistance, high strength, creep resistance and the like, and is an excellent candidate material for hot end parts of turbine blades, combustion chambers and the like of high thrust-weight ratio aeroengines. However, in the high water oxygen and molten salt gas environment of the aeroengine, the silicon carbide ceramic matrix composite material also faces the challenges of water oxygen corrosion, molten salt corrosion and the like. The adoption of the environmental barrier coating is an effective way for improving the water oxygen resistance and molten salt corrosion resistance of the silicon carbide ceramic matrix composite. The currently common environmental barrier coatings are primarily rare earth silicates (e.g., Y) 2 SiO 5 、Y 2 Si 2 O 7 And the like) which has good high-temperature water-oxygen corrosion resistance, high-temperature stability and the like, but has poor thermal matching with the silicon carbide ceramic-based composite material, and is easy to peel off and fail due to thermal mismatch in the circulating service process. Therefore, a novel material with good temperature resistance, good corrosion resistance and proper thermal expansion coefficient is developedEnvironmental barrier coating material systems have become a research hotspot in countries around the world.
AlHfTaO 6 The melting point of the ceramic is up to 2160 deg.C, no phase change from room temperature to melting point, and its thermal expansion coefficient is about 4.43 × 10 -6 and/K is an environmental barrier coating material with great development potential. However, up to now, alHfTaO has been required as a coating for the production of coatings 6 The preparation method of the ceramic powder is not reported. How to prepare AlHfTaO with single phase and controllable grain diameter 6 Ceramic powder is a difficult problem to be solved.
Disclosure of Invention
The invention provides AlHfTaO 6 Ceramic powder, preparation method and application thereof, solving the problem of AlHfTaO 6 The ceramic powder is difficult to prepare and the like, and the AlHfTaO is realized 6 Controllable preparation of ceramic powder, and obtaining of AlHfTaO with single phase, high dispersion and uniform grain diameter 6 Ceramic powder.
In order to achieve the above object, the present invention provides an AlHfTaO 6 The preparation method of the ceramic powder comprises the following steps:
s1: weighing Al according to a molar ratio of 1 2 O 3 Powder and HfO 2 Powder and Ta 2 O 5 Ball-milling and uniformly mixing the powder, and dry-pressing and molding in a mold to obtain a green body;
s2: roasting the green body at the temperature of 1500-1700 ℃ for 2-5 h in air, cooling, mechanically crushing, and sieving to obtain AlHfTaO 6 Ceramic powder.
In order to achieve the purpose, the invention also provides AlHfTaO 6 The ceramic powder is prepared by the preparation method.
In order to achieve the purpose, the invention also provides AlHfTaO 6 The ceramic powder prepared by the preparation method or the ceramic powder is applied to the preparation of high-temperature-resistant thermal protection environmental barrier coatings for hot end parts of aero-engines and rocket engines.
Compared with the prior art, the invention has the following beneficial effects:
AlH provided by the inventionfTaO 6 The preparation method of the ceramic powder comprises the following steps of weighing Al 2 O 3 Powder, hfO 2 Powder and Ta 2 O 5 The powder is used as a raw material, the molar ratio can promote different raw materials to react according to a certain reaction path to generate a target product without generating byproducts, unreacted reactant phases in the product are effectively prevented from remaining, and the AlHfTaO is prepared by ball milling, uniformly mixing, dry pressing and roasting 6 Ceramic powder.
The first step of physical change: monodisperse Al by ball milling 2 O 3 Powder and HfO 2 Powder and Ta 2 O 5 Powder mixing becomes the mixed powder that mix with evenly distributed, makes the mutual contact between different looks inseparabler between the mixed powder through dry pressing shaping, is favorable to the atom interdiffusion among the later stage reaction process.
The second step of chemical change: by high temperature calcination, al is made 2 O 3 、HfO 2 And Ta 2 O 5 Generates AlHfTaO by solid phase reaction 6 . When the roasting temperature is lower than 1500 ℃, the activation energy of the chemical reaction between different raw materials is insufficient, so that the reaction is incomplete, and the product contains unreacted raw materials. When the roasting temperature exceeds 1700 ℃, ta with lower melting point in the raw material 2 O 5 The phase will volatilize and lose due to large saturated vapor pressure, thereby affecting the composition of the target product, and the higher temperature will bring higher requirements to the equipment, increasing the production cost. When the roasting temperature is between 1500-1700 ℃, on one hand, the complete reaction of different raw materials can be promoted, on the other hand, the product composition can be ensured, and the method has no special equipment requirement and low cost.
The preparation method provided by the invention has the advantages of simple process, low equipment requirement and short preparation period, and can prepare the AlHfTaO with single phase, high dispersion, fine and uniform particle size by controlling the high-temperature roasting process conditions 6 The ceramic powder can be used for preparing high-temperature-resistant thermal protection environmental barrier coatings for hot end parts of aero-engines and rocket engines. In addition, the method has wide source of raw materials and low cost, and can be popularized to industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is AlHfTaO prepared in example 1 6 SEM photograph of ceramic powder;
FIG. 2 is AlHfTaO prepared in example 1 6 XRD spectrogram of ceramic powder.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides an AlHfTaO 6 The preparation method of the ceramic powder comprises the following steps:
s1: weighing Al according to a molar ratio of 1 2 O 3 Powder, hfO 2 Powder and Ta 2 O 5 And (3) uniformly mixing the powder by ball milling, and performing dry pressing in a mould to obtain a green body.
The purpose of adopting ball milling and mixing is to mix the raw material powder of the three components more evenly, thereby being beneficial to the mutual reaction among the following different raw materials and simultaneously avoiding residual unreacted materials in the product.
The purpose of dry pressing is to further reduce the diffusion distance of solid-phase reaction between different raw materials, thereby accelerating the formation of the product and shortening the production time.
S2: roasting the green body at the temperature of 1500-1700 ℃ for 2-5h in air, cooling, mechanically crushing, and sieving to obtain AlHfTaO 6 Ceramic powder.
The high-temperature roasting is used for promoting the solid-phase reaction of different raw materials to generate a target product.
The crushing and sieving are performed to obtain a ceramic powder having a high dispersion and a uniform particle size.
Preferably, in step S1, the Al 2 O 3 Powder, hfO 2 Powder and Ta 2 O 5 The particle size of the powder is 50 to 1000nm. The particle size is controlled to better promote the reaction, and when the particle size is too small, the raw material powder is extremely difficult to obtain, and when the particle size is too large, the raw material powder is difficult to completely react.
Preferably, in the step S1, the ball-milling ball-material mass ratio is 3 to 6, the ball-milling speed is 300 to 500r/min, and the ball-milling time is 3 to 10h. By controlling the ball milling process parameters, the AlHfTaO6 ceramic powder with single phase, high dispersion, fine and uniform grain diameter is further obtained by control. The ball milling process mainly realizes more uniform mixing of powder, and incomplete reaction is easily caused when the powder is not uniformly mixed.
Preferably, in step S1, the pressure of the dry pressing is 10 to 20mpa, and the pressing time is 10 to 30min.
Preferably, in step S2, the mechanical crushing is grinding.
Preferably, in step S2, the sieving is to sieve the powder through 200 meshes and then through 600 meshes, and collect the intermediate powder.
The invention also provides AlHfTaO 6 The ceramic powder is prepared by the preparation method.
The invention also provides AlHfTaO 6 The ceramic powder prepared by the preparation method or the ceramic powder is applied to the preparation of high-temperature-resistant thermal protection environmental barrier coatings for hot end parts of aero-engines and rocket engines.
Example 1
This example provides an AlHfTaO 6 The preparation method of the ceramic powder comprises the following steps:
(1) Weighing Al having an average particle diameter of 50nm 2 O 3 5.10g of HfO powder having an average particle size of 100nm 2 Powder of 10.53g in total, ta having an average particle diameter of 1000nm 2 O 5 22.10g of powder and 114g of agate ball milling particles, placing the powder in an agate ball milling tank for ball milling and mixing, wherein the ball milling speed is 300r/min, stopping ball milling for half an hour every half an hour, then continuing ball milling for half an hour in the opposite direction, and continuing the ball milling for half an hour in sequence until the ball milling time reaches 3 hours to obtain mixed powder; and then, putting the mixed powder into a steel mould with the diameter of 20mm for dry pressing and forming, controlling the pressure to be 10MPa, keeping the pressure for 10min, and then taking out to obtain a green body.
(2) And placing the green body in a muffle furnace for high-temperature roasting at 1500 ℃ for 5h, cooling with the furnace to obtain a porous green body, grinding the porous green body, sieving with a 200-mesh sieve, sieving with a 600-mesh sieve, and collecting intermediate powder. FIG. 1 shows AlHfTaO prepared in this example 6 The ceramic powder has good dispersibility and uniform particle size, and the average particle size is about 10 μm. FIG. 2 shows AlHfTaO prepared in this example 6 The ceramic powder has a single phase in XRD spectrogram and only contains AlHfTaO 6 And (4) phase(s).
Example 2
This example provides an AlHfTaO 6 The preparation method of the ceramic powder comprises the following steps:
(1) Weighing Al having an average particle diameter of 100nm 2 O 3 5.10g of HfO powder with an average particle size of 500nm 2 Powder of 10.53g in total, ta having an average particle diameter of 500nm 2 O 5 22.10g of powder and 226g of agate ball mill, placing the powder in an agate ball mill tank for ball milling and mixing, wherein the ball milling process conditions areMixed powder was obtained as in example 1; and then, putting the mixed powder into a steel mould with the diameter of 20mm for dry pressing and forming, controlling the pressure to be 20MPa, keeping the pressure for 10min, and then taking out to obtain a green body.
(2) Placing the green body in a muffle furnace for high-temperature roasting under the roasting process conditions as in example 1, cooling the green body along with the furnace to obtain a porous green body, grinding and sieving the porous green body, and performing a sieving process as in example 1 to finally obtain the AlHfTaO with single phase, good dispersibility and uniform particle size 6 Ceramic powder.
Example 3
This example provides an AlHfTaO 6 The preparation method of the ceramic powder comprises the following steps:
(1) Weighing Al having an average particle diameter of 500nm 2 O 3 Powder 5.10g in total, hfO having an average particle diameter of 1000nm 2 Powder of 10.53g in total, ta having an average particle diameter of 1000nm 2 O 5 22.10g of powder and 226g of agate ball milling particles, placing the powder in an agate ball milling tank for ball milling and mixing, wherein the ball milling speed is 500r/min, the ball milling is stopped for 10 minutes every 10 minutes, then the ball milling is stopped for 10 minutes along the reverse direction, and continuing sequentially until the ball milling time reaches 10 hours to obtain mixed powder; and then, putting the mixed powder into a steel mould with the diameter of 20mm for dry pressing and forming, controlling the pressure to be 20MPa, keeping the pressure for 30min, and then taking out to obtain a green body.
(2) Placing the green body in a muffle furnace for high-temperature roasting at 1700 ℃, wherein the roasting time is 2h, cooling along with the furnace to obtain a porous green body, grinding the porous green body, sieving with a 200-mesh sieve, sieving with a 600-mesh sieve, collecting intermediate powder, and obtaining the AlHfTaO with single phase, good dispersibility and uniform particle size 6 Ceramic powder.
Comparative example 1
The present comparative example provides an AlHfTaO 6 Method for preparing ceramic powder, in comparison with example 1, in this comparative example, al having an average particle diameter of 50nm was weighed 2 O 3 Powder 10.20g in total, hfO having an average particle diameter of 100nm 2 Powder of 10.53g in total, ta having an average particle diameter of 1000nm 2 O 5 The total amount of the powder was 22.10g. The rest is the same as example 1. Obtained byThe product powder contains not only AlHfTaO6, but also unreacted Al 2 O 3 And (4) phase(s).
Comparative example 2
The present comparative example provides an AlHfTaO 6 Compared with the preparation method of the ceramic powder in the example 1, the roasting temperature in the comparative example is 1400 ℃, and the roasting time is 5 hours. The rest was the same as in example 1. The obtained product powder only contains a trace amount of AlHfTaO 6 Phase, mostly by-product Hf 6 Ta 2 O 17 、AlTaO 4 And unreacted HfO 2 、Al 2 O 3 And Ta 2 O 5 And are equal.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or any other related technical fields, which are directly or indirectly applied to the present invention, are included in the scope of the present invention.

Claims (6)

1. AlHfTaO 6 The preparation method of the ceramic powder is characterized by comprising the following steps:
s1: weighing Al according to a molar ratio of 1 2 O 3 Powder and HfO 2 Powder and Ta 2 O 5 Ball-milling and uniformly mixing the powder, and performing dry pressing molding in a mold to obtain a green body;
s2: roasting the green body at the temperature of 1500-1700 ℃ for 2-5h in air, cooling, mechanically crushing, and sieving to obtain AlHfTaO 6 Ceramic powder.
2. The method according to claim 1, wherein in step S1, the Al is 2 O 3 Powder, hfO 2 Powder and Ta 2 O 5 The particle size of the powder is 50 to 1000nm.
3. The preparation method according to claim 1, wherein in step S1, the ball-milling ball-material mass ratio is 3 to 6, the ball-milling speed is 300 to 500r/min, and the ball-milling time is 3 to 10h.
4. The method according to claim 1, wherein in step S1, the pressure of the dry pressing is 10 to 20MPa, and the pressing time is 10 to 30min.
5. The method of claim 1, wherein in step S2, the mechanical disruption is milling.
6. The method of claim 1, wherein in step S2, the sieving is performed by sieving with a 200-mesh sieve and then with a 600-mesh sieve to obtain the intermediate powder.
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