CN115093225A - Y 4 Al 2 O 9 /Y 2 O 3 Preparation method of eutectic ceramic powder and spherical feed - Google Patents
Y 4 Al 2 O 9 /Y 2 O 3 Preparation method of eutectic ceramic powder and spherical feed Download PDFInfo
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- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention belongs to the field of protective coatings, and particularly relates to Y 4 Al 2 O 9 /Y 2 O 3 A preparation method of eutectic ceramic powder and a spherical feed. The powder is Y 4 Al 2 O 9 And Y 2 O 3 The eutectic ceramic powder raw material (2) is prepared by mixing the two materials in a eutectic composition ratio (molar ratio Y) 2 O 3 :Al 2 O 3 70.5: 29.5). At nano-or submicron-scale Al 2 O 3 Powder and Y 2 O 3 The powder is used as raw material, and Y is prepared by mechanical mixing and solid phase reaction 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic powder raw material is subjected to spray drying granulation and high-temperature sintering to prepare Y with smooth surface, tight internal combination, uniform particle size distribution, high sphericity and good fluidity 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding. The feed is suitable for a wear-resistant ceramic coating or a thermal barrier/environmental barrier integrated protective coating for high-temperature alloy and ceramic matrix composite materials, and meets the feeding requirement of preparing related coatings by plasma spraying, laser cladding or supersonic flame spraying.
Description
Technical Field
The invention belongs to the field of protective coatings, and particularly relates to a wear-resistant ceramic coating or thermal barrier/environmental barrier integrated protective coating suitable for high-temperature alloys and ceramic matrix composites, which meets the requirement of preparing Y-shaped coatings of related coatings by plasma spraying, laser cladding or supersonic flame spraying 4 Al 2 O 9 /Y 2 O 3 A preparation method of eutectic ceramic powder raw material and spherical feed.
Background
The development of aeronautical technology has placed higher demands on the efficiency and thrust of aircraft engines. In order to improve the thrust-weight ratio of the aircraft engine, the temperature of the forward air in front of the turbine is required to be continuously improved. The requirements put forward a series of performance requirements such as high temperature resistance, wear resistance, corrosion resistance and the like on the high-temperature structural material for the aeroengine. Typical high-temperature structural materials currently used for aeroengines are single crystal high-temperature alloy and SiC f SiC ceramic matrix composite material, and Al 2 O 3f /Al 2 O 3 And the like. Compared with high-temperature alloy, the ceramic matrix composite material has the characteristics of low density, high temperature resistance and low thermal conductivity. But when in service as an aircraft engine structural component, SiC f /SiC and Al 2 O 3f /Al 2 O 3 The ceramic matrix composite is washed by high-speed particles in the engine gas environment, and CMAS (CaO-MgO-Al) 2 O 3 -SiO 2 Low-melting-point environment sediment), high-temperature steam, molten salt and other corrosive media, has high performance degradation and failure speed, and must be coated with a protective coating with excellent high-temperature resistance, wear resistance, high-temperature mechanical properties and excellent steam and CMAS corrosion resistance.
Eutectic of alumina and aluminateThe ceramic has the characteristics of high melting point, strong wear resistance, good high-temperature mechanical property and excellent high-temperature steam and CMAS corrosion resistance, and is a novel structural material with great application prospect. For example, Y prepared by directional solidification 3 Al 5 O 12 /Al 2 O 3 After the eutectic ceramic is subjected to heat preservation for 100-200 hours in a water vapor environment at 1700 ℃, the bending strength is not obviously reduced, and excellent high-temperature mechanical properties and water vapor corrosion resistance are shown. As coating material, Y 3 Al 5 O 12 /Al 2 O 3 The coating has no obvious cracks on the service surface under the high load condition of load of 2000N and running speed of 500rpm, and shows excellent high-speed bearing capacity and wear resistance. It has been shown that the above Y 3 Al 5 O 12 /Al 2 O 3 The excellent properties of the eutectic material mainly come from strong chemical bond bonding between atoms of the eutectic aluminate material and a unique eutectic microstructure: eutectic phase is distributed continuously along the solidification direction and is intertwined with each other, Y 3 Al 5 O 12 And Al 2 O 3 The phases are mutually constrained and assisted in a three-dimensional space, so that the mechanical property of the phase is obviously improved. Y is 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic has a ratio of Y 3 Al 5 O 12 /Al 2 O 3 Higher eutectic temperature, possibly better high temperature resistance; while being compared with Al 2 O 3 Matrix phase, Y 2 O 3 The matrix phase has better high-temperature mechanical property, steam resistance and CMAS corrosion resistance. It can be expected that Y 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic is expected to become a protective coating material for the aeroengine, which can meet the requirements of higher service temperature, stronger abrasion resistance and corrosion resistance.
The preparation technology of the ceramic protective coating for the common aeroengine mainly comprises the following steps: plasma spraying, laser cladding, supersonic flame spraying and the like. The atmospheric plasma spraying has the advantages of moderate porosity of prepared coating, low thermal conductivity, wide range of prepared powder (both high melting point and low melting point can be applied), and the like; the coating prepared by the laser cladding technology has a small heat affected zone, a good microstructure and excellent bonding performance; compared with the atmospheric plasma spraying, the supersonic flame spraying has wider and longer flame and higher spraying efficiency. These typical preparation methods must be based on the development of high quality powder raw material preparation techniques, and in order to ensure that a uniform, dense protective coating is obtained, conventional powders need to be light in weight and good in flow.
To sum up, establish Y 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic powder and the preparation method of the spherical feed for plasma spraying, laser cladding or supersonic flame spraying provide basic material support and technical reserve for a novel protective coating with excellent high temperature resistance, wear resistance, steam resistance and CMAS corrosion resistance for a new generation of aircraft engines.
Disclosure of Invention
Aiming at the requirements of a new generation of aero-engine on a protective ceramic coating with high temperature resistance, wear resistance and corrosion resistance, the invention aims to provide a Y 4 Al 2 O 9 /Y 2 O 3 The raw material of the powder is suitable for a wear-resistant ceramic coating or a thermal barrier/environmental barrier integrated protective coating for a high-temperature alloy or a ceramic matrix composite material, so that the powder meets the requirements of preparation processes such as plasma spraying, laser cladding, supersonic flame spraying and the like.
The technical scheme of the invention is as follows:
y 4 Al 2 O 9 /Y 2 O 3 Preparation method of eutectic ceramic powder and spherical feed, wherein the powder is Y 4 Al 2 O 9 And Y 2 O 3 The eutectic ceramic powder raw material (2) is prepared by mixing the two materials in a eutectic composition ratio (molar ratio Y) 2 O 3 :Al 2 O 3 70.5: 29.5); with Al 2 O 3 Powder and Y 2 O 3 The powder is used as raw material, and Y is prepared by mechanical mixing and solid phase reaction 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials; then spray drying granulation and high temperature sintering are carried out to prepareThe obtained Y has smooth surface, tight internal combination, uniform particle size distribution, high sphericity and good fluidity 4 Al 2 O 9 /Y 2 O 3 And (4) feeding eutectic ceramic in a spherical shape. Wherein, the meaning of eutectic composition ratio is: y in the powder component 4 Al 2 O 9 And Y 2 O 3 The relative proportions of the two phases are such that the two phases can undergo a eutectic reaction under specific temperature conditions (eutectic temperature), in particular in the present invention, Y 2 O 3 With Al 2 O 3 In a molar ratio of 70.5: 29.5.
Said Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed comprises the following specific steps:
(1) using nano-grade or submicron-grade alumina powder and yttrium oxide powder as raw materials, Al 2 O 3 The mass fraction of the powder is 5-25 wt%, and Y 2 O 3 The mass fraction range of the powder is 75 wt% -95 wt%, and the sum of the mass percentages of the powder and the powder is 100 wt%;
(2) mixing alumina powder and yttrium oxide powder, mixing raw material powder with a ball milling solvent, and then sequentially performing ball milling and drying to obtain uniformly mixed Al 2 O 3 -Y 2 O 3 Powder of the mixture;
(3) will obtain Al 2 O 3 -Y 2 O 3 Mixing the powder at T 1 Carrying out a solid phase reaction at a temperature to obtain Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials;
(4) will Y 4 Al 2 O 9 /Y 2 O 3 Mixing the eutectic ceramic powder raw material with deionized water, a binder, a dispersant and a pH regulator by using a ball mill to obtain uniform and stable slurry;
(5) carrying out powder agglomeration treatment on the obtained slurry by adopting spray drying equipment to obtain agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feeding;
(6) agglomerating the agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feed is at T 2 Post-sintering at temperature, cooling, and sieving to obtain Y 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding.
Said Y 4 Al 2 O 9 /Y 2 O 3 A preparation method of eutectic ceramic powder and spherical feed comprises the following steps of (1) preparing Al 2 O 3 The particle size of the powder is nano-scale or submicron scale, the particle size range is 50-500 nm, and Y is 2 O 3 The particle size of the powder is nano-scale or submicron-scale, and the particle size range is 50-500 nm.
Said Y 4 Al 2 O 9 /Y 2 O 3 Preparation method of eutectic ceramic powder and spherical feed, in step (2), Al 2 O 3 -Y 2 O 3 The mixture powder is mixed with Al 2 O 3 Powder and Y 2 O 3 The powder is finished by a planet ball mill, the medium is absolute ethyl alcohol, the mass ratio of the mixture powder to the absolute ethyl alcohol is (1:2) - (2:1), the ball material mass ratio is (1:2) - (4:1), the rotating speed of the ball mill is 120-350 rpm, and the mixing and ball milling time is 2-24 hours.
Said Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of eutectic ceramic powder and spherical feed comprises (3) obtaining Y by solid phase reaction 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw material and solid phase reaction temperature T 1 The temperature is 1200-1600 ℃, and the heat preservation time is 2-24 h.
Said Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of eutectic ceramic powder and spherical feed comprises the following steps of (4), wherein the solid content of slurry is 30-70 wt%; the binder is selected from at least one of polyvinyl alcohol, paraffin, sodium lignosulfonate or glycerol, and the addition amount of the binder is 0.1-2.0 wt%; the dispersant is at least one selected from polyacrylamide, polymethacrylic acid, polyethyleneimine, sodium silicate and polyethylene glycol, and the addition amount of the dispersant is 0.1 wt% >, E2.0 wt%; the pH regulator is selected from at least one of glacial acetic acid, hydrochloric acid and tetramethylammonium water, and the addition amount is 0.3 wt% -1.5 wt%; the ball material mass ratio is (1:2) - (2:1), the rotating speed of the ball mill is 160-350 rpm, and the mixing and ball milling time is 6-24 h.
Said Y 4 Al 2 O 9 /Y 2 O 3 In the step (5), the agglomeration treatment adopts spray drying equipment, and the parameters are as follows: the air inlet temperature is 100-300 ℃, the air outlet temperature is 100-200 ℃, the rotating speed of the peristaltic pump is 10-30 rpm, the rotating speed of the atomizer is 11000-14000 rpm, the pressure of the nozzle is 0.05-0.30 MPa, and the air inlet amount is 1.5-3.0 m 3 /min。
Said Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of eutectic ceramic powder and spherical feed comprises the step (6) of sintering at a temperature T 2 The temperature is 1000-1500 ℃, the heat preservation time is 2-5 h, and the granularity range of the screened spherical feed is 5-85 μm.
The design idea of the invention is as follows:
the invention aims at the ceramic protective coating for the high-temperature structural component of the new generation of aeroengine, in particular to a wear-resistant ceramic coating or a thermal barrier/environmental barrier integrated protective coating, and selects the high-melting-point Y to meet the performance requirements of sand/high-speed airflow scouring wear resistance and high-temperature steam/CMAS/molten salt corrosion resistance at higher temperature 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramics were used as the target material. In one aspect, Y 4 Al 2 O 9 And Y 2 O 3 All have stronger interatomic chemical bond bonding, belong to high-melting-point, high corrosion-resistant oxide ceramic, have better high-temperature performance; on the other hand, using Y 4 Al 2 O 9 And Y 2 O 3 The eutectic reaction characteristic of the eutectic structure can form a unique microstructure with continuous distribution and interweaving winding of the eutectic phase and a eutectic morphology with mutual restriction and auxiliary enhancement of a matrix phase and a reinforcing phase in a three-dimensional space in the preparation process, so that the mechanical property of the eutectic structure is further obviously improved. Considering that the protective coating is formed by plasma spraying or laserThe powder is further agglomerated by using spray drying equipment in order to meet the requirements of powder granularity control, fluidity and apparent density in the spraying process, and the agglomerated powder with specific granularity distribution is screened out, so that Y can be ensured 4 Al 2 O 9 /Y 2 O 3 The powder is easier to melt and deposit in the coating preparation process, the eutectic reaction between the powder and the coating is promoted, and the uniformity and the compactness of the protective coating are ensured.
The invention has the advantages and beneficial effects that:
1. the invention selects Y from the selection of materials compared with the traditional Y 3 Al 5 O 12 /Al 2 O 3 New system Y with higher eutectic point temperature of eutectic ceramics 4 Al 2 O 9 /Y 2 O 3 The material has better high temperature resistance; while being compared with Al 2 O 3 ,Y 2 O 3 The composite material has better steam and CMAS corrosion resistance, and can provide better wear resistance and corrosion resistance for eutectic materials.
2. Different from the conventional method of directly mixing yttrium oxide and alumina powder and then spray-drying and granulating, the invention firstly obtains Y by a solid-phase reaction method 4 Al 2 O 9 /Y 2 O 3 The raw material of the eutectic ceramic powder ensures the distribution uniformity of yttrium aluminate phase and yttrium oxide phase (or the two Chinese characters are directly written into chemical formulas), and is favorable for obtaining the eutectic ceramic spherical feed with good sphericity, uniform size, tight internal combination and stability when being subjected to spray drying granulation treatment.
3. The eutectic ceramic spherical feed designed by the invention can be used for preparing high-quality protective coatings, and the application range of matrix materials is wide, including high-temperature alloys and SiC f a/SiC ceramic matrix composite material and an oxide ceramic matrix composite material.
4. Y for spraying prepared by the invention 4 Al 2 O 9 /Y 2 O 3 The grain size distribution of the eutectic ceramic spherical feed is 10-60 mu m, and the apparent density is 0.8-1.5 g/cm 3 Has a fluidity of 70 to 150 s-50g, smooth surface, compact interior and good fluidity, and meets the requirements of the preparation technologies such as plasma spraying, laser cladding or supersonic flame spraying and the like on the spherical feed.
Drawings
FIG. 1 shows Y in example 1 4 Al 2 O 9 /Y 2 O 3 XRD pattern of eutectic ceramic powder raw material. In the figure, the abscissa 2 θ represents the diffraction angle (degrees), and the ordinate Intensity represents the relative Intensity (arb. units).
FIGS. 2(a) to 2(b) show Y in example 1 4 Al 2 O 9 /Y 2 O 3 Scanning electron microscope picture (a) and particle size distribution diagram (b) of eutectic ceramic powder raw material. In FIG. 2(b), Particle size on the abscissa represents Particle size (. mu.m), and Volume (%) on the ordinate represents Volume%.
FIGS. 3(a) to 3(c) show Y prepared in example 2 4 Al 2 O 9 /Y 2 O 3 The surface topography picture of the scanning electron microscope (a) and the section topography picture of the scanning electron microscope (b) of the eutectic ceramic spherical feed material (c) are the particle size distribution map. In FIG. 3(c), Particle size on the abscissa represents Particle size (. mu.m), and Volume (%) on the ordinate represents Volume%.
FIG. 4 shows Y prepared in example 3 4 Al 2 O 9 /Y 2 O 3 Scanning distribution diagram of the element (Al, Y and O) surface of the eutectic ceramic spherical feed.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be illustrative of the invention only and are not intended to be limiting.
In the practice of the invention, Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed comprises the following specific steps:
(1) using alumina powder and yttrium oxide powder as raw material, Al 2 O 3 The mass fraction of the powder is 5-25 wt% (preferably 15 wt%), Y 2 O 3 The mass fraction range of the powder is 75 wt% -95 wt% (preferably 85 wt%), the sum of the two mass percents being 100 wt%;
(2) mixing alumina powder and yttrium oxide powder, mixing raw material powder and a ball milling solvent, and then sequentially performing ball milling and drying to obtain uniformly mixed Al 2 O 3 -Y 2 O 3 Powder of the mixture;
(3) will obtain Al 2 O 3 -Y 2 O 3 Mixing the powder at T 1 Carrying out a solid phase reaction at a temperature to obtain Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials;
(4) will Y 4 Al 2 O 9 /Y 2 O 3 Mixing the eutectic ceramic powder raw material with deionized water, a binder, a dispersant and a pH regulator by using a ball mill to obtain uniform and stable slurry;
(5) carrying out powder agglomeration treatment on the obtained slurry by adopting spray drying equipment to obtain agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feeding;
(6) agglomerating the agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feed is at T 2 Post-sintering at temperature, cooling, and sieving to obtain Y with smooth surface, tight internal combination, uniform particle size distribution, high sphericity and good fluidity 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feeding;
in step (1), Al 2 O 3 The particle size of the powder is nano-scale or submicron scale, the particle size range is 50-500 nm (preferably 200nm), and Y is 2 O 3 The particle size of the powder is nano-scale or submicron-scale, and the particle size range is 50-500 nm (preferably 200 nm).
In the step (2), the mixture powder Al 2 O 3 Powder and Y 2 O 3 The powder is mixed in a planetary ball mill, the medium is absolute ethyl alcohol, the mass ratio of the powder of the mixture to the absolute ethyl alcohol is (1:2) - (2:1) (preferably 1:1), the ball material mass ratio is (1:2) - (4:1) (preferably 2:1), and the ball mill is characterized in thatThe rotating speed is 120-350 rpm (preferably 260rpm), and the mixing and ball milling time is 2-24 h (preferably 6 h).
In the step (3), Y is obtained by a solid-phase reaction method 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw material and solid phase reaction temperature T 1 The temperature is 1200-1600 ℃ (preferably 1400 ℃), and the heat preservation time is 2-24 h (preferably 6 h).
In the step (4), the solid content of the slurry is 30-70 wt% (preferably 50 wt%); the binder is selected from at least one of polyvinyl alcohol, paraffin, sodium lignosulfonate or glycerol (preferably polyvinyl alcohol), and the addition amount of the binder is 0.1-2.0 wt% (preferably 1.0 wt%); the dispersant is at least one (preferably polyethylene glycol) selected from polyacrylamide, polymethacrylic acid, polyethyleneimine, sodium silicate and polyethylene glycol, and the addition amount of the dispersant is 0.1-2.0 wt% (preferably 1.0 wt%); the pH regulator is at least one selected from glacial acetic acid, hydrochloric acid and tetramethylammonium water (preferably glacial acetic acid), and the addition amount of the pH regulator is 0.3-1.5 wt% (preferably 1.0 wt%); the ball-material mass ratio is (1:2) - (2:1) (preferably 1:1), the rotation speed of the ball mill is 160-350 rpm (preferably 260rpm), and the mixing and ball-milling time is 6-24 h (preferably 6 h).
In the step (5), the agglomeration treatment adopts spray drying equipment, and the parameters are as follows: the air inlet temperature is 100-300 ℃ (preferably 200 ℃), the air outlet temperature is 100-200 ℃ (preferably 150 ℃), the rotating speed of the peristaltic pump is 10-30 rpm (preferably 20rpm), the rotating speed of the atomizer is 11000-14000 rpm (preferably 12000rpm), the pressure of the nozzle is 0.05-0.30 MPa (preferably 0.20MPa), and the air inlet amount is 1.5-3.0 m 3 Min (preferably 2.0 m) 3 /min)。
In the step (6), the sintering temperature T 2 The temperature is 1000-1500 ℃ (preferably 1200 ℃), the heat preservation time is 2-5 h (preferably 3h), and the particle size range of the screened spherical feed is 5-85 μm (preferably 40 μm).
The present invention will be described in further detail by way of examples.
The performance test information in the following examples is as follows:
1. and (3) appearance observation:
observing the appearance of the aggregate powder by adopting a Zeiss Supra 35 field emission scanning electron microscope;
2. x-ray diffraction analysis:
phase analysis was performed using an X-ray diffractometer (Rigaku D/max-2400, Tokyo, Japan);
3. and (3) testing the fluidity:
performing fluidity detection on the aggregate powder by using a BT-200 metal powder fluidity tester (Hall flow meter) produced by Dandongbeit instruments and Co;
4. and (3) detecting apparent density:
carrying out loose packing density detection on the aggregate powder by using a BT-100 loose packing density instrument produced by Dandongbeit instruments ltd; the laser particle size test adopts a Mastersizer 2000 laser particle size analyzer produced by Malvern Panalytical company to detect the particle size distribution of the aggregate powder.
Example 1
In this example, Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed comprises the following specific steps:
(1) with nanoscale Al 2 O 3 Powder and Y 2 O 3 The powder is used as raw material and has an original particle size of Al 2 O 3 Powder 50-100 nm, Y 2 O 3 50-100 nm powder of Al 2 O 3 The mass fraction of the powder is 15 wt%, Y 2 O 3 The mass fraction of the powder is 85 wt%, and the sum of the mass fractions of the powder and the powder is 100 wt%;
(2) using absolute ethyl alcohol as medium, adding raw material (Al) 2 O 3 Powder and Y 2 O 3 Powder) and absolute ethyl alcohol are put into a ball milling tank according to the mass ratio of 1:1 for ball milling for 6h, and then the mixture is dried and screened to obtain Al which is uniformly mixed 2 O 3 -Y 2 O 3 Powder of the mixture; the ball milling parameters were as follows: the ball material mass ratio is 2:1, the rotating speed of the ball mill is 260 rpm;
(3) the obtained Al 2 O 3 -Y 2 O 3 Keeping the mixture powder at 1400 ℃ in a muffle furnace for 6h to obtain Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials;
(4) adding deionized water, adhesive polyvinyl alcohol (PVA), dispersant polyethylene glycol (PEG) and pH regulator glacial acetic acid (CH) into eutectic ceramic powder raw material 3 COOH) and mixing for 6 hours by using a ball mill to obtain uniform and stable slurry; the solid content of the slurry is 50 wt%, the addition amount of the binder is 1.0 wt%, the addition amount of the dispersant is 1.0 wt%, and the addition amount of the pH regulator is 1.0 wt%; the ball milling parameters are as follows: the ball material mass ratio is 2:1, and the rotating speed of the ball mill is 260 rpm;
(5) carrying out powder agglomeration treatment on the obtained slurry by adopting spray drying equipment to obtain agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feeding; the parameters of spray drying granulation are as follows: the air inlet temperature is 200 ℃, the air outlet temperature is 150 ℃, the rotation speed of the peristaltic pump is 20rpm, the rotation speed of the atomizer is 12000rpm, the nozzle pressure is 0.20MPa, and the air inlet volume is 2.0m 3 /min;
(6) Agglomerating the agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Carrying out post-sintering treatment on the eutectic ceramic spherical feed in a muffle furnace at 1200 ℃, preserving heat for 3h, then cooling, and screening by a screen of 300-700 meshes to obtain Y for spraying, wherein the Y is smooth in surface, tight in internal combination, good in fluidity and good in high-temperature stability 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding.
The obtained eutectic ceramic powder and the eutectic ceramic spherical feed are detected, and the results are as follows:
as shown in FIG. 1, the eutectic ceramic powder obtained after heat preservation at 1400 ℃ for 6h in a muffle furnace has high component purity of only Y 4 Al 2 O 9 /Y 2 O 3 Two, no other substance.
As shown in FIG. 2(a), a scanning electron microscope photograph of the eutectic ceramic powder raw material was taken, and Y was obtained after solid-phase reaction sintering 4 Al 2 O 9 /Y 2 O 3 The grain size of the eutectic ceramic powder raw material is distributed uniformly and has smaller grain size.
As shown in FIG. 2(b)) Shown by (Y) 4 Al 2 O 9 /Y 2 O 3 The laser particle size distribution of the eutectic ceramic powder can be obtained from the figure, the particle size distribution is 0.1-1.3 mu m, D 50 About 0.4 μm.
By detecting the fluidity, Y for spraying 4 Al 2 O 9 /Y 2 O 3 The fluidity of the eutectic ceramic spherical feed was 135s/50 g.
The Y for spraying can be known through loose density detection 4 Al 2 O 9 /Y 2 O 3 The apparent density of the eutectic ceramic spherical feed is 1.40g/cm 3 。
Example 2
In this example, Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed comprises the following specific steps:
(1) in submicron order of Al 2 O 3 Powder and Y 2 O 3 The powder is used as raw material and has an original particle size of Al 2 O 3 Powder 100-500 nm, Y 2 O 3 100 to 500nm powder of Al 2 O 3 The mass fraction of the powder is 20 wt%, Y 2 O 3 The mass fraction of the powder is 80 wt%, and the sum of the mass percentages of the powder and the powder is 100 wt%;
(2) using absolute ethyl alcohol as medium, adding raw material (Al) 2 O 3 Powder and Y 2 O 3 Powder) and absolute ethyl alcohol according to a mass ratio of 1:1 ball-milling in a ball-milling tank for 6h, drying and screening to obtain uniformly mixed Al 2 O 3 -Y 2 O 3 Powder of the mixture; the ball milling parameters are as follows: the ball material mass ratio is 2:1, the rotating speed of the ball mill is 260 rpm;
(3) the obtained Al 2 O 3 -Y 2 O 3 Keeping the mixture powder at 1500 ℃ in a muffle furnace for 6h to obtain Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials;
(4) adding deionized water, a binder polyvinyl alcohol (PVA), a dispersant polyethylene glycol (PEG) and a pH regulator ice into a eutectic ceramic powder raw materialAcetic acid (CH) 3 COOH) and mixing by using a ball mill to obtain uniform and stable slurry; the solid content of the slurry is 50 wt%, the addition amount of the binder is 1.0 wt%, the addition amount of the dispersant is 1.0 wt%, and the addition amount of the pH regulator is 1.0 wt%; the ball milling parameters were as follows: the mass ratio of the ball materials is 2:1, and the rotating speed of the ball mill is 260 rpm;
(5) carrying out powder agglomeration treatment on the obtained slurry by adopting spray drying equipment to obtain agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feeding; the parameters of spray drying granulation are as follows: the air inlet temperature is 200 ℃, the air outlet temperature is 150 ℃, the rotating speed of the peristaltic pump is 20rpm, the rotating speed of the atomizer is 12000rpm, the nozzle pressure is 0.20MPa, and the air inlet volume is 2.0m 3 /min;
(6) Agglomerating the Y 4 Al 2 O 9 /Y 2 O 3 Carrying out post-sintering treatment on eutectic ceramic spherical feed in a muffle furnace at 1200 ℃, preserving heat for 3 hours, then cooling, and screening by a screen of 300-700 meshes to obtain Y for spraying, wherein the Y is smooth in surface, tight in internal combination, good in fluidity and high in high-temperature stability 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding.
For the obtained Y 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic powder and the eutectic ceramic spherical feed are detected, and the results are as follows:
as shown in FIG. 3(a), Y 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic spherical feed has compact and smooth surface, good sphericity and uniform particle size distribution.
As shown in FIG. 3(b), Y 4 Al 2 O 9 /Y 2 O 3 The sectional view of the eutectic ceramic spherical feed shows that the spherical feed has tight internal combination and high density.
As shown in FIG. 3(c), Y 4 Al 2 O 9 /Y 2 O 3 The laser particle size distribution of the eutectic ceramic spherical feed is shown in the figure, the particle size distribution is uniform and is 20-65 mu m, D 50 About 39 μm.
By detecting the fluidity, Y for spraying 4 Al 2 O 9 /Y 2 O 3 The flowability of the eutectic ceramic ball feed is 127s/50 g.
The Y for spraying can be known through loose density detection 4 Al 2 O 9 /Y 2 O 3 The apparent density of the eutectic ceramic spherical feed is 1.44g/cm 3 。
Example 3
In this example, Y was obtained according to the procedure of example 1 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder and spherical feed. The difference from the example 1 is that the Al is in submicron order 2 O 3 Powder and Y 2 O 3 The powder is used as raw material and has an original particle size of Al 2 O 3 Powder 100-500 nm, Y 2 O 3 The powder is 100-500 nm.
As shown in FIG. 4, Y 4 Al 2 O 9 /Y 2 O 3 The scanning distribution test result of the element (Al, Y and O) surfaces of the eutectic ceramic spherical feeding materials shows that the Al, Y and O elements are uniformly distributed.
The results of the examples show that Y according to the invention 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic powder is Y 4 Al 2 O 9 And Y 2 O 3 The eutectic ceramic powder raw material; preparing Y through mechanical mixing and solid-phase reaction 4 Al 2 O 9 /Y 2 O 3 The eutectic ceramic composite powder is then spray dried and granulated to prepare high-purity Y after agglomeration 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding. The spherical feed has the characteristics of compact and smooth surface, tight internal combination, uniform particle size distribution, good sphericity, good fluidity and the like, and can meet the requirement of preparing a wear-resistant ceramic coating or a thermal barrier/environmental barrier integrated protective layer for a high-temperature alloy or a ceramic matrix composite material by plasma spraying, laser cladding or supersonic flame spraying.
Although the present invention has been described with reference to a few embodiments, it is not intended to limit the present invention, and those skilled in the art may make modifications and variations of the present invention without departing from the spirit and scope of the present invention by using the methods and technical contents disclosed above.
Claims (8)
1. Y 4 Al 2 O 9 /Y 2 O 3 The preparation method of eutectic ceramic powder and spherical feed is characterized in that the powder is Y 4 Al 2 O 9 And Y 2 O 3 The eutectic ceramic powder raw material (2) is prepared by mixing the two materials in a eutectic composition ratio (molar ratio Y) 2 O 3 :Al 2 O 3 70.5: 29.5); with Al 2 O 3 Powder and Y 2 O 3 The powder is used as raw material, and Y is prepared by mechanical mixing and solid phase reaction 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials; then spray drying granulation and high temperature sintering are carried out to prepare the Y with smooth surface, tight internal combination, even particle size distribution, high sphericity and good fluidity 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding.
2. Y of claim 1 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed is characterized by comprising the following specific steps:
(1) using nano-grade or submicron-grade alumina powder and yttrium oxide powder as raw materials, Al 2 O 3 The mass fraction of the powder is 5-25 wt%, and Y 2 O 3 The mass fraction range of the powder is 75 wt% -95 wt%, and the sum of the mass percentages of the powder and the powder is 100 wt%;
(2) mixing alumina powder and yttrium oxide powder, and mixing the raw material powder with a ball milling solventThen ball milling and drying are carried out in sequence to obtain Al which is uniformly mixed 2 O 3 -Y 2 O 3 Powder of the mixture;
(3) will obtain Al 2 O 3 -Y 2 O 3 Mixing the powder at T 1 Carrying out a solid phase reaction at a temperature to obtain Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw materials;
(4) will Y 4 Al 2 O 9 /Y 2 O 3 Mixing the eutectic ceramic powder raw material with deionized water, a binder, a dispersant and a pH regulator by using a ball mill to obtain uniform and stable slurry;
(5) carrying out powder agglomeration treatment on the obtained slurry by adopting spray drying equipment to obtain agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feeding;
(6) agglomerating the agglomerated Y 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic spherical feed is at T 2 Post-sintering at temperature, cooling, and sieving to obtain Y 4 Al 2 O 9 /Y 2 O 3 And (3) eutectic ceramic spherical feeding.
3. Y according to claim 2 4 Al 2 O 9 /Y 2 O 3 The preparation method of eutectic ceramic powder and spherical feed is characterized in that in the step (1), Al is added 2 O 3 The particle size of the powder is nano-scale or submicron scale, the particle size range is 50-500 nm, and Y is 2 O 3 The particle size of the powder is nano-scale or submicron-scale, and the particle size range is 50-500 nm.
4. Y according to claim 2 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed is characterized in that in the step (2), Al is added 2 O 3 -Y 2 O 3 The mixture powder is mixed with Al 2 O 3 Powder and Y 2 O 3 The powder is finished by a planet ball mill, the medium is absolute ethyl alcohol, the mass ratio of the mixture powder to the absolute ethyl alcohol is (1:2) - (2:1), the ball material mass ratio is (1:2) - (4:1), the rotating speed of the ball mill is 120-350 rpm, and the mixing and ball milling time is 2-24 hours.
5. Y according to claim 2 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed is characterized in that in the step (3), Y is obtained by a solid-phase reaction method 4 Al 2 O 9 /Y 2 O 3 Eutectic ceramic powder raw material and solid phase reaction temperature T 1 The temperature is 1200-1600 ℃, and the heat preservation time is 2-24 h.
6. Y according to claim 2 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed is characterized in that in the step (4), the solid content of the slurry is 30-70 wt%; the binder is selected from at least one of polyvinyl alcohol, paraffin, sodium lignosulfonate or glycerol, and the addition amount of the binder is 0.1-2.0 wt%; the dispersant is selected from at least one of polyacrylamide, polymethacrylic acid, polyethyleneimine, sodium silicate and polyethylene glycol, and the addition amount of the dispersant is 0.1-2.0 wt%; the pH regulator is selected from at least one of glacial acetic acid, hydrochloric acid and tetramethylammonium water, and the addition amount is 0.3 wt% -1.5 wt%; the ball material mass ratio is (1:2) - (2:1), the rotating speed of the ball mill is 160-350 rpm, and the mixing and ball milling time is 6-24 h.
7. Y according to claim 2 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed is characterized in that in the step (5), spray drying equipment is adopted for agglomeration treatment, and the parameters are as follows: the air inlet temperature is 100-300 ℃, the air outlet temperature is 100-200 ℃, the rotating speed of the peristaltic pump is 10-30 rpm, the rotating speed of the atomizer is 11000-14000 rpm, the nozzle pressure is 0.05-0.30 MPa, and the air inlet quantity is 1.5-3.0 m 3 /min。
8. Y according to claim 2 4 Al 2 O 9 /Y 2 O 3 The preparation method of the eutectic ceramic powder and the spherical feed is characterized in that in the step (6), the sintering temperature T is 2 The temperature is 1000-1500 ℃, the heat preservation time is 2-5 h, and the granularity range of the screened spherical feed is 5-85 μm.
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