CN111116211A - Preparation method of ternary nano lamellar MAX phase powder and product thereof - Google Patents
Preparation method of ternary nano lamellar MAX phase powder and product thereof Download PDFInfo
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- CN111116211A CN111116211A CN201911372605.2A CN201911372605A CN111116211A CN 111116211 A CN111116211 A CN 111116211A CN 201911372605 A CN201911372605 A CN 201911372605A CN 111116211 A CN111116211 A CN 111116211A
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
- C04B35/5615—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium silicon carbides
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
- C04B35/5618—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium aluminium carbides
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
Abstract
The invention discloses a preparation method of ternary nano lamellar MAX phase powder and a product thereof, wherein the preparation method comprises the following steps: s1, mixing the MAX phase powder and ethanol uniformly according to a certain proportion to obtain MAX phase powder-ethanol first slurry; s2, performing ball milling on the first slurry to obtain a solid content of 40-50 wt.% and a particle size d50A second slurry between 200 and 300 nm; s3, adding 3-5wt.% of PVA binder into the second slurry, and uniformly stirring to obtain a third slurry; and S4, placing the third slurry into a spray granulation dryer for granulation to obtain spherical MAX phase powder with the average particle size of 20-30 microns, and storing. The scheme utilizes spray granulation to prepare MAX phase powder spherical particles, the average particle size is 20-30 microns, the particles are consistent in shape and size, and good in liquidity, and the MAX phase powder spherical particles can be used in the fields of thermal spraying powder materials, functional ceramics, structural ceramics and the like. The method has the advantages of simple process, low cost and high granulation efficiencyHigh quality and suitability for industrial mass production.
Description
Technical Field
The invention relates to the field of MAX phase materials, in particular to a preparation method of ternary nano laminar MAX phase spraying powder and a product thereof.
Background
The MAX phase material integrates the excellent properties of ceramics and metals due to its unique atomic unit cell structure. It has good electrical conductivity, thermal conductivity, higher thermal expansion coefficient and machinability like metal; it has low density, high elastic modulus, high temperature resistance, high wear resistance, excellent antioxidant performance and high temperature crack self-healing performance similar to that of ceramic. Therefore, the MAX phase ceramic is an ideal thermal spraying protective material.
The MAX phase granulated powder with excellent quality is a precondition for the MAX phase to be used as a thermal spraying protective material. Typically, the shape, size distribution, purity, flowability, etc. of the MAX phase powder particles directly affect the performance and bond strength of the thermal spray coating.
The conventional MAX phase granulation is to prepare MAX phase materials, and then to obtain MAX phase materials through crushing and ball milling, wherein the MAX powder particles obtained by the method have the defects of non-uniform shape and particle size, non-uniform particle size distribution and poor liquidity.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method for obtaining spherical ternary nano lamellar MAX phase powder with uniform particle size distribution by utilizing a spray granulation process and a product thereof.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the ternary nano lamellar MAX phase powder comprises the following steps:
s1, mixing the MAX phase powder and ethanol uniformly according to a certain proportion to obtain MAX phase powder-ethanol first slurry;
s2, performing ball milling on the first slurry to obtain a solid content of 40-50 wt.% and a particle size d50A second slurry between 200 and 300 nm;
s3, adding 3-5wt.% of PVA binder into the second slurry, and uniformly stirring to obtain a third slurry;
and S4, placing the third slurry into a spray granulation dryer for granulation to obtain spherical MAX phase powder with the average particle size of 20-30 microns, and storing.
Preferably, in the preparation method of the ternary nano-lamellar MAX phase powder, in the step S1, the MAX phase powder is 211 type, 312 type, or 413 type.
Preferably, in the preparation method of the ternary nano laminar MAX phase powder, in the step S1, the mass percentage of the MAX phase powder is 40-50 wt.%, and the mass percentage of the ethanol is 50-60 wt.%.
Preferably, in the preparation method of the ternary nano-lamellar MAX phase powder, in the step S1, the mass ratio of the MAX phase powder to the ethanol is between 0.6 and 1.
Preferably, in the preparation method of the ternary nano-lamellar MAX phase powder, in the step S1, the MAX phase powder and ethanol are uniformly mixed by a pneumatic stirrer or an electric stirrer, wherein the rotation speed of the pneumatic stirrer or the electric stirrer is between 200 and 500 revolutions per minute.
Preferably, in the preparation method of the ternary nano-lamellar MAX phase powder, in the step S2, the first slurry is ball-milled by a nano-sand mill or a planetary ball mill for 2-6 hours.
Preferably, in the preparation method of the ternary nano-lamellar MAX phase powder, in the step S3, a stirrer or an electric stirrer is started for stirring, the rotating speed is between 300-600 revolutions per minute, and the stirring time is between 0.5 and 1 hour.
Preferably, in the preparation method of the ternary nano lamellar MAX phase powder, the step S4 includes the following steps:
s41, conveying the third slurry to a spray drying granulator through a peristaltic pump;
s42, atomizing the third slurry by a spray head to form spherical MAX phase powder according to the conditions that the rotating speed of an atomizing disc is 5000-;
s43, filling the MAX phase powder obtained in the S42 into a bag, and sealing and storing.
The ternary nano lamellar MAX phase powder is prepared by any preparation method of the ternary nano lamellar MAX phase powder.
Preferably, in the ternary nano lamellar MAX phase powder, the particles of the ternary nano lamellar MAX phase powder are spherical and have an average particle size of 20-30 micrometers.
The technical scheme of the invention has the advantages that:
the scheme has the advantages of ingenious design and simple process, utilizes spray granulation to prepare the spherical particles of the MAX phase powder particles, has the particle size of 20-30 microns, consistent shape and size and good fluidity, and can be used in the fields of thermal spraying powder materials, functional ceramics, structural ceramics and the like. The method has the characteristics of simple process, low cost and high granulation efficiency, and is suitable for industrialized mass production.
The design of the process parameters can effectively ensure the uniformity of each component in the slurry, thereby improving the quality of the final material.
Drawings
FIG. 1 shows high purity Ti for spray granulation in example 1 of the present invention3AlC2Diffraction pattern of the primary powder;
FIG. 2 shows high purity Ti for spray granulation in example 1 of the present invention3AlC2Scanning electron microscope pictures of the primary powder;
FIG. 3 shows Ti prepared in example 1 of the present invention3AlC2A map of spherical spray particles of (a);
FIG. 4 shows high purity Ti for spray granulation in example 2 of the present invention2Diffraction patterns of AlC primary powder;
FIG. 5 shows the morphology of the particles after 3 hours of ball milling in the sand mill in example 2 of the present invention;
FIG. 6 shows Ti obtained in example 2 of the present invention2Spherical spray grain pattern of AlC;
FIG. 7 shows high purity Ti for spray granulation in example 2 of the present invention3SiC2Diffraction pattern of the primary powder;
FIG. 8 isTi obtained in example 3 of the present invention3SiC2Figure of spherical spray particles.
Detailed Description
Objects, advantages and features of the present invention will be illustrated and explained by the following non-limiting description of preferred embodiments. The embodiments are merely exemplary for applying the technical solutions of the present invention, and any technical solution formed by replacing or converting the equivalent thereof falls within the scope of the present invention claimed.
In the description of the schemes, it should be noted that the terms "center", "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In the description of the embodiment, the operator is used as a reference, and the direction close to the operator is a proximal end, and the direction away from the operator is a distal end.
The preparation method of the ternary nano-layered MAX phase powder disclosed by the invention is explained by combining the attached drawings, and comprises the following steps:
s1, mixing the MAX phase powder and ethanol uniformly according to a certain proportion to obtain MAX phase powder-ethanol first slurry; wherein the MAX phase powder comprises MAX phase powder of all types, such as 211 type Ti2AlC,Cr2AlC,Ti2SnC et al, type 312 Ti3AlC2,Ti3SiC2Etc., 413 type Ti4AlN3,Ta4AlC3，V4AlC3And the like. Putting MAX phase powder and ethanol into a barrel with a stirrer according to the mass ratio of 0.6-1, and stirring and mixing, preferably, the mass percentage of the MAX phase powder is 40-50 wt.%, and the mass percentage of the ethanol isAnd in the range of 50-60wt.%, the stirrer can be a pneumatic stirrer or an electric stirrer, the rotation speed during stirring is 200-.
S2, placing the first slurry into a nano sand mill for ball milling for 2-6h to obtain a product with a solid content of 40-50 wt.% and a particle size d50A second slurry between 200 and 300 nm.
S3, adding 3-5wt.% of PVA binder into the second slurry, and stirring for 0.5-1h by an electric stirrer or a pneumatic stirrer at the rotation speed of 300-600 rpm, so as to uniformly stir the PVA binder, thereby obtaining third slurry.
And S4, placing the third slurry into a spray granulation dryer for granulation to obtain spherical MAX phase powder with the average particle size of 20-30 microns, and storing.
The method specifically comprises the following steps:
s41, conveying the third slurry to a spray drying granulator through a peristaltic pump;
s42, atomizing the third slurry by a spray head to form spherical MAX phase powder according to the conditions that the rotating speed of an atomizing disc is 5000-;
s43, filling the MAX phase powder obtained in the S42 into a bag, and sealing and storing.
Example 1 was carried out:
5kg of high purity Ti sheet-like material of type 312 shown in FIGS. 1 and 2 in the form of layer3AlC2Putting the MAX phase powder and 5kg of ethanol into a barrel provided with a pneumatic stirrer, connecting the MAX phase powder and the 5kg of ethanol with a nano sand mill, then opening the pneumatic stirrer, and uniformly mixing materials in the barrel to ensure that the MAX phase powder is in a stable suspension state.
And then starting the nano sand mill, wherein the rotating speed of the pneumatic stirrer is 300 rpm, and the ball milling time is 6 h.
Then adding 5 wt% of PVA binder into the slurry after ball milling, and then adding Ti of the binder3AlC2MAX phase powderThe slurry was stirred for 0.5h to homogeneity using a pneumatic stirrer with a rotational speed of 300 rpm.
And then putting the uniformly mixed slurry into a spray granulation dryer for granulation. The method specifically comprises the following steps: the slurry obtained by preparation is sent to a spray head of a spray drying agent through a peristaltic pump to be atomized into small liquid drops, the rotating speed of an atomizing disc is 10000 rpm, and the inlet temperature of a spray granulator is as follows: 200 ℃ and an outlet temperature of 90 ℃. And finally, filling the prepared MAX phase powder particles into a bag, and sealing and storing. Ti having good fluidity as shown in FIG. 3 was obtained3AlC2MAX phase powder spherical particles with an average particle size of 20-30 microns.
EXAMPLES example 2
3kg of type 211 high purity lamellar Ti as shown in FIG. 42And putting the AlC MAX phase powder and 4kg of ethanol into a barrel provided with a pneumatic stirrer, connecting the barrel with a nano sand mill, and then opening the pneumatic stirrer to uniformly mix materials in the barrel.
And (3) starting the nano sand mill, wherein the rotating speed of the pneumatic stirrer is 500 rpm, and the ball milling time is 3h to obtain lamellar particles with the particle size of less than 1 micron as shown in the attached figure 5.
Then adding 3 wt% of PVA binder into the ball-milled slurry, and adding Ti of the binder2And stirring the AlC MAX phase powder slurry for 1 hour by using a pneumatic stirrer until the slurry is uniform, wherein the rotating speed of the pneumatic stirrer is 200 revolutions per minute.
And then putting the uniformly mixed slurry into a spray granulation dryer for granulation. The method specifically comprises the following steps: the prepared slurry is sent to a spray head of a spray drying agent to be atomized into small droplets, the rotating speed of an atomizing disc is 12000 r/min, and the inlet temperature of a spray granulator is as follows: 180 ℃ and an outlet temperature of 80 ℃. And finally, filling the prepared MAX phase powder particles into a bag, and sealing and storing. Ti having good fluidity as shown in FIG. 6 was obtained2AlC MAX phase powder spherical particles.
EXAMPLE 3
3kg of 312 type high purity lamellar Ti as shown in FIG. 73SiC2MAX phase powder and 3kg ethanol are put into a barrel with a pneumatic stirrer, and the barrel is connected with a nano sand millAnd then, opening the pneumatic stirrer, and uniformly mixing the materials in the barrel to ensure that the MAX phase powder is in a stable suspension state.
And then starting the nano sand mill, wherein the rotating speed of the pneumatic stirrer is 400 rpm, and the ball milling time is 5 hours.
Then adding 5 wt% of PVA binder into the slurry after ball milling, and then adding Ti of the binder3AlC2And stirring the MAX phase powder slurry for 1 hour by using a pneumatic stirrer until the MAX phase powder slurry is uniform, wherein the rotating speed of the pneumatic stirrer is 300 revolutions per minute.
And then putting the uniformly mixed slurry into a spray granulation dryer for granulation. The method specifically comprises the following steps: the prepared slurry is sent to a spray head of a spray drying agent to be atomized into small droplets, the rotating speed of an atomizing disc is 8000 rpm, and the inlet temperature of a spray granulator is as follows: 200 ℃ and an outlet temperature of 80 ℃. And finally, filling the prepared MAX phase powder particles into a bag, and sealing and storing. Ti having good fluidity as shown in FIG. 8 was obtained3SiC2MAX phase powder spherical particles.
The invention has various embodiments, and all technical solutions formed by adopting equivalent transformation or equivalent transformation are within the protection scope of the invention.
Claims (10)
1. The preparation method of the ternary nano lamellar MAX phase powder is characterized by comprising the following steps: the method comprises the following steps:
s1, mixing the MAX phase powder and ethanol uniformly according to a certain proportion to obtain MAX phase powder-ethanol first slurry;
s2, performing ball milling on the first slurry to obtain a solid content of 40-50 wt.% and a particle size d50A second slurry between 200 and 300 nm;
s3, adding 3-5wt.% of PVA binder into the second slurry, and uniformly stirring to obtain a third slurry;
and S4, placing the third slurry into a spray granulation dryer for granulation to obtain spherical MAX phase powder with the average particle size of 20-30 microns, and storing.
2. The method for preparing the ternary nano laminar MAX phase powder according to claim 1, wherein the method comprises the following steps: in step S1, the MAX phase powder is 211 type, 312 type, or 413 type.
3. The method for preparing the ternary nano laminar MAX phase powder according to claim 1, wherein the method comprises the following steps: in the step of S1, the mass percent of the MAX phase powder is 40-50 wt.%, and the mass percent of the ethanol is 50-60 wt.%.
4. The method for preparing the ternary nano laminar MAX phase powder according to claim 1, wherein the method comprises the following steps: in the step S1, the mass ratio of the MAX phase powder to the ethanol is between 0.6 and 1.
5. The method for preparing the ternary nano laminar MAX phase powder according to claim 1, wherein the method comprises the following steps: the method comprises the following steps: in step S1, the MAX phase powder is mixed with ethanol uniformly by a pneumatic stirrer or an electric stirrer, wherein the rotation speed of the pneumatic stirrer or the electric stirrer is between 200 and 500 rpm.
6. The method for preparing the ternary nano laminar MAX phase powder according to claim 1, wherein the method comprises the following steps: in the step S2, the first slurry is ball-milled by a nanometer sand mill for 2-6 h.
7. The method for preparing the ternary nano laminar MAX phase powder according to claim 1, wherein the method comprises the following steps: in the step S3, stirring is carried out by starting a stirrer or an electric stirrer, the rotating speed is between 300 and 600 revolutions per minute, and the stirring time is between 0.5 and 1 hour.
8. The method for preparing ternary nano laminar MAX phase powder according to any one of claims 1 to 7, wherein the method comprises the following steps: the step S4 includes the following processes:
s41, conveying the third slurry to a spray drying granulator through a peristaltic pump;
s42, spray drying granulator according to atomizing diskThe rotating speed is 5000-oC, the outlet temperature is 70-100 DEG CoC, atomizing the third slurry through a spray head to form spherical MAX phase powder;
s43, filling the MAX phase powder obtained in the S42 into a bag, and sealing and storing.
9. The ternary nano lamellar MAX phase powder is characterized in that: the ternary nano-layered MAX phase powder prepared by the method of any one of claims 1 to 8.
10. The ternary nano-lamellar MAX phase powder of claim 9, characterized in that: the particles of the ternary nano lamellar MAX phase powder are spherical and the average particle size is between 20 and 30 micrometers.
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