CN113121210B - Nano-grade alumina ceramic powder, composite ceramic material and preparation method thereof - Google Patents
Nano-grade alumina ceramic powder, composite ceramic material and preparation method thereof Download PDFInfo
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- CN113121210B CN113121210B CN202110605439.7A CN202110605439A CN113121210B CN 113121210 B CN113121210 B CN 113121210B CN 202110605439 A CN202110605439 A CN 202110605439A CN 113121210 B CN113121210 B CN 113121210B
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Abstract
The invention provides a preparation method of nano-alumina ceramic powder, which comprises the following steps: and mixing the alumina powder with deionized water to prepare alumina slurry. Adding the alumina slurry into a sand mill, sequentially adding two groups of dispersing agents for sand milling, and firstly adding a first group of small molecular weight dispersing agents; the second group of dispersants is then added and the sand is milled, followed by the addition of the second group of high molecular weight dispersants. And (4) performing spray granulation on the sanded slurry to obtain the nano-scale alumina ceramic powder. Also provides a preparation method of the composite ceramic material, and the nano-scale alumina ceramic powder and the composite ceramic material prepared by the method. The preparation method of the nano-scale alumina ceramic powder, the composite ceramic material and the preparation method thereof provided by the invention have the advantages of simple steps and low production cost, and can be used for preparing spherical and spheroidal nano-scale alumina ceramic powder, and the prepared composite ceramic material has more excellent performance.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a nano-scale alumina ceramic powder, a composite ceramic material and a preparation method thereof.
Background
The alumina ceramic material is becoming an excellent structural material and functional material due to its excellent properties such as higher strength and high temperature resistance, especially the nano-scale alumina ceramic, which has more excellent strength and toughness, thus having wider development and application prospects. However, the preparation of nano-scale alumina powder is difficult, and the preparation of spherical and spheroidal nano-scale alumina powder is more difficult.
The spherical and sphere-like nano alumina powder prepared by the prior art has the defects of difficult operation, high cost and difficult industrial popularization due to the complex process, and the poor overall performance of the alumina powder due to the uneven particle size distribution of the powder.
At present, most of nano-alumina powder is prepared by preparing micron-level alumina powder and a dispersant into slurry, then controlling the particle size range of the slurry through sanding, and finally obtaining the nano-alumina ceramic powder through spray granulation. The preparation method is simple to operate, low in cost and beneficial to large-scale industrial production. However, the prepared powder has uneven particle size distribution and wider distribution interval, and is very easy to have double peaks, namely two extreme peak phenomena, and the sphericity of the powder cannot be controlled, so that the prepared powder particles are all special-shaped and cannot meet the requirement of materials with higher performance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the nanoscale alumina ceramic powder, the composite ceramic material and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of nano alumina ceramic powder comprises the following steps:
preparing alumina slurry: mixing alumina powder with deionized water to prepare alumina slurry;
sanding: adding the alumina slurry into a sand mill, firstly adding a first group of dispersing agents, and performing sand milling, wherein the first group of dispersing agents are small molecular weight dispersing agents; adding a second group of dispersing agents and sanding, wherein the second group of dispersing agents are high molecular weight dispersing agents;
spray granulation: and carrying out spray granulation on the sanded alumina slurry to obtain the nano-scale alumina ceramic powder.
The further improvement of the technical scheme is as follows:
the small molecular weight dispersant comprises at least one of sodium benzoate, ammonium benzoate, sodium hexametaphosphate and citric acid.
The high molecular weight dispersant comprises at least one of polyethylene glycol, acrylic acid ammonium salt copolymer, higher fatty acid and lipid.
The aluminum oxide slurry comprises, by mass, 30-50 parts of aluminum oxide powder and 50-70 parts of deionized water.
The mass ratio of the dispersing agent to the alumina powder is (0.5-2.5): 100, respectively; wherein the mass ratio of the small molecular weight dispersant to the large molecular weight dispersant to the alumina powder is (0.3-1.5): (0.5-2) 100.
The grain diameter of the alumina powder in the alumina slurry preparation step is 2-25 μm.
In the sanding step, the rotational speed of the sanding main machine is 500-2500 rpm, the flow is 100-5500L/h, the rotational speed of a stirring paddle of the sanding tank is 50-1500 rpm, and the sanding cycle is 10-500 times.
The invention also provides a preparation method of the composite ceramic material, which comprises the following steps:
mixing nano-alumina ceramic powder with PPS plastic powder, carrying out banburying, injection molding, heat treatment and machining to prepare the composite ceramic material with the solid content of 70-80%, wherein the nano-alumina ceramic powder is prepared according to the preparation method of the nano-alumina ceramic powder.
The invention also provides nano-scale alumina ceramic powder and a composite ceramic material, which are respectively prepared by the preparation method.
According to the technical scheme, the method for preparing the nano alumina ceramic powder adopts a mode of grouping the dispersing agents, the dispersing agents with different molecular weights are added into the sand mill in batches, the dispersing agent with the small molecular weight is added firstly for sand milling, at the moment, the dispersing agent with the small molecular weight can play a role in efficient grinding, and the dispersing agent with the large molecular weight is added for sand milling, at the moment, the dispersing agent with the large molecular weight can increase steric hindrance among particles, so that the cutting force is improved, the purpose of controlling the morphology of the powder is achieved, the prepared nano alumina ceramic powder is spherical and spheroidal, and the performance of the alumina ceramic powder is improved. The composite ceramic material prepared by the method also has excellent performance.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing nano-alumina ceramic powder according to an embodiment of the present invention.
FIG. 2 is an SEM image of nano-alumina ceramic powder prepared in example 1 of the present invention.
FIG. 3 is a distribution diagram of the particle size of the nano-alumina ceramic powder prepared in example 1 of the present invention.
FIG. 4 is an SEM image of the nano-alumina ceramic powder prepared in example 2 of the present invention.
FIG. 5 is a distribution diagram of the particle size of the nano-alumina ceramic powder prepared in example 2 of the present invention.
FIG. 6 is an SEM image of an alumina ceramic powder prepared by the prior art.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
As shown in fig. 1, the method for preparing nano alumina ceramic powder of the embodiment includes the following steps:
s1, preparing alumina slurry: mixing the alumina powder with deionized water to prepare alumina slurry with the mass fraction of 35-45%. The grain diameter of the alumina powder is 2-25 μm. The aluminum oxide slurry comprises, by mass, 30-50 parts of aluminum oxide powder and 50-70 parts of deionized water.
S2, sanding: adding the alumina slurry into a sanding tank of a sand mill, sequentially adding two groups of dispersing agents, firstly adding a first group of dispersing agents, and sanding, wherein the first group of dispersing agents are small molecular weight dispersing agents; the small molecular weight dispersant comprises at least one of sodium benzoate, ammonium benzoate, sodium hexametaphosphate and citric acid; the rotational speed of the sanding main machine is 500-2500 rpm, the flow is 100-5500L/h, the rotational speed of a stirring paddle of the sanding tank is 50-1500 rpm, and the sanding cycle is 10-500 times.
Then adding a second group of dispersing agents and sanding, wherein the second group of dispersing agents are high molecular weight dispersing agents; the high molecular weight dispersant comprises at least one of polyethylene glycol, acrylic acid ammonium salt copolymer, higher fatty acid and lipid; the rotational speed of the sanding main machine is 500-2500 rpm, the flow rate is 100-5500L/h, the rotational speed of a stirring paddle of the sanding tank is 50-1500 rpm, and the sanding cycle time is 10-500 times.
The mass ratio of the dispersing agent to the alumina powder is (0.5-2.5): 100; wherein the mass ratio of the small molecular weight dispersant to the large molecular weight dispersant to the alumina powder is (0.3-1.5): (0.5-2) 100.
S3, spray granulation: and (3) carrying out spray granulation on the sanded alumina slurry through a spray drying tower, wherein the heating speed is 3-6 ℃/min, the heat preservation temperature is 450-550 ℃, and the heat preservation time is 2-4 h, so as to obtain the nano-grade alumina ceramic powder.
Wherein the rotating speed of the spray head is 4500-5500 rpm, the air pressure difference is 200-250 Pa, the air outlet temperature is 100-150 ℃, and the flow rate of the alumina slurry is 1.5-2L/h.
The final grain diameter of the nano-grade alumina ceramic powder prepared by the method is 50-3500 nm.
A preparation method of a composite ceramic material comprises the following steps:
mixing nano-alumina ceramic powder with PPS (polyether plastic) plastic powder, carrying out banburying, injection molding, heat treatment and machining to prepare the composite ceramic material with the solid content of 70-80%, wherein the nano-alumina ceramic powder is prepared according to the preparation method of the nano-alumina ceramic powder.
Example 1: the preparation method of the nano alumina ceramic powder of the embodiment is basically consistent with the preparation method, and is not described herein again, and the specific preparation parameters are as follows:
s1, preparing alumina slurry: 20kg of alumina powder is mixed with deionized water to prepare alumina slurry with the mass fraction of 40%.
S2, sanding: adding the alumina slurry into a sanding tank of a sand mill, adding 0.6 percent of the mass of alumina powder, namely 120g of sodium benzoate, and sanding; the rotational speed of sanding host computer is 900rpm, and the flow is 1500L/h, and sanding jar stirring rake rotational speed is 600rpm, and the sanding cycle number is 100 times.
Then adding 80g of acrylic acid ammonium salt copolymer which accounts for 0.4 percent of the mass of the alumina powder and sanding; the rotational speed of sanding host computer is 900rpm, and the flow is 1500L/h, and sanding jar stirring rake rotational speed is 600rpm, and the sanding cycle number is 20 times.
Example 2: the preparation method of the nano-alumina ceramic powder of the present embodiment is basically the same as the preparation method of embodiment 1, and is not repeated here, except that:
s2, sanding: adding the alumina slurry into a sanding tank of a sand mill, adding two small molecular weight dispersing agents, namely 100g of sodium benzoate and 80g of sodium hexametaphosphate, which are respectively 0.5% of the mass of the alumina powder, and sanding; the rotational speed of sanding host computer is 900rpm, and the flow is 2000L/h, and sanding jar stirring rake rotational speed is 600rpm, and the sanding cycle number is 160.
Then adding 60g of polyethylene glycol which accounts for 0.3 percent of the mass of the alumina powder and sanding; the rotational speed of sanding host computer is 900rpm, and the flow is 2000L/h, and sanding jar stirring rake rotational speed is 600rpm, and the sanding cycle number is 40 times.
The composite materials prepared by the preparation methods of example 1 and example 2 were examined, and the examination results are shown in table 1.
As can be seen from the above table, the particle size of the alumina powder prepared in the two embodiments reaches the nanometer level, and the density and strength indexes of the composite ceramic material are both high.
FIG. 2 is a SEM photograph of the nano-sized alumina ceramic powder prepared in example 1, and FIG. 3 is a particle size distribution diagram of the nano-sized alumina ceramic powder under a laser particle sizer. As can be seen from FIG. 2, the alumina ceramic powder has a uniform particle size and a high sphericity, which is mostly similar to a sphere. As can be seen from FIG. 3, the particle size distribution of the alumina ceramic powder is normal distribution, the particle size is mainly distributed between 300 to 2000nm, the median diameter D50 is 769nm, no double peak appears, and the peak width is narrow.
FIG. 4 is a SEM photograph of the nano-sized alumina ceramic powder prepared in example 2, and FIG. 5 is a particle size distribution diagram under a laser particle sizer. As can be seen from FIG. 4, the alumina ceramic powder has a uniform particle size and a high sphericity, and is substantially spherical or spheroidal. As can be seen from FIG. 5, the particle size distribution of the alumina ceramic powder was normal, the particle size distribution was mainly 70 to 800nm, the median diameter D50 was 177nm, no double peak was observed, and the peak width was narrow.
Fig. 6 is an SEM image of alumina powder prepared by the prior art, which has non-uniform particle size distribution, wide interval, and is very likely to have double peaks, i.e., two extreme peaks. The sphericity of the powder is not good, and the particles are all special.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only express the preferred embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as the limitation of the invention patent scope. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (6)
1. A preparation method of nano alumina ceramic powder is characterized by comprising the following steps: the method comprises the following steps:
preparing alumina slurry: mixing alumina powder with deionized water to prepare alumina slurry; the grain diameter of the alumina powder is 2-25 μm;
sanding: adding the alumina slurry into a sand mill, firstly adding a first group of dispersing agents, and performing sand milling, wherein the first group of dispersing agents are small molecular weight dispersing agents; then adding a second group of dispersing agents and sanding, wherein the second group of dispersing agents are high molecular weight dispersing agents; the mass ratio of the dispersing agent to the alumina powder is (0.5-2.5): 100, respectively; wherein the mass ratio of the small molecular weight dispersant to the large molecular weight dispersant to the alumina powder is (0.3-1.5): (0.5-2) 100;
spray granulation: carrying out spray granulation on the sanded alumina slurry to obtain nano-scale alumina ceramic powder;
the small molecular weight dispersant comprises at least one of sodium benzoate, ammonium benzoate, sodium hexametaphosphate and citric acid;
the high molecular weight dispersant comprises at least one of polyethylene glycol, acrylic acid ammonium salt copolymer, higher fatty acid and lipid.
2. The method for preparing the nanoscale alumina ceramic powder according to claim 1, wherein the method comprises the following steps: the aluminum oxide slurry comprises, by mass, 30-50 parts of aluminum oxide powder and 50-70 parts of deionized water.
3. The method for preparing the nanoscale alumina ceramic powder according to claim 1, wherein the method comprises the following steps: in the sanding step, the rotational speed of the sanding main machine is 500-2500 rpm, the flow is 100-5500L/h, the rotational speed of a stirring paddle of the sanding tank is 50-1500 rpm, and the sanding cycle is 10-500 times.
4. The preparation method of the composite ceramic material is characterized by comprising the following steps: the method comprises the following steps:
mixing nano-scale alumina ceramic powder with PPS plastic powder, and carrying out banburying, injection molding, heat treatment and machining to prepare the composite ceramic material with the solid content of 70-80%, wherein the nano-scale alumina ceramic powder is prepared according to the preparation method of the nano-scale alumina ceramic powder disclosed by any one of claims 1-3.
5. A nanometer alumina ceramic powder is characterized in that: the nano-alumina ceramic powder is prepared by the preparation method of the nano-alumina ceramic powder as claimed in any one of claims 1 to 3.
6. A composite ceramic material characterized by: the composite ceramic material is prepared by the preparation method of the composite ceramic material of claim 4.
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