CN112299855B - MgAlON ceramic powder preparation method based on 3D printing forming - Google Patents

MgAlON ceramic powder preparation method based on 3D printing forming Download PDF

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CN112299855B
CN112299855B CN202011280219.3A CN202011280219A CN112299855B CN 112299855 B CN112299855 B CN 112299855B CN 202011280219 A CN202011280219 A CN 202011280219A CN 112299855 B CN112299855 B CN 112299855B
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mgalon
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CN112299855A (en
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岳映雷
徐婷婷
任俊业
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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    • 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
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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
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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Abstract

The invention discloses a preparation method of MgAlON ceramic powder based on 3D printing and forming, which comprises the following steps: (1) firstly, mixing raw material powder, a solvent and an additive to prepare raw material ink with high solid content; (2) then printing the raw ink into a raw material blank body with a regular three-dimensional through hole structure by adopting a 3D printing and forming process, and drying the raw material blank body; (3) then placing the raw material blank into a reaction device with the functions of air flow control and pollution prevention in a high-temperature graphite sintering furnace, and carrying out high-temperature synthesis in a controlled reaction environment; (4) finally, the MgAlON ceramic powder with high purity can be obtained after ball milling process treatment. According to the method, the raw material powder can be printed into the blank with the regular three-dimensional through hole structure, so that the full implementation of gas-solid synthesis reaction during high-temperature synthesis is facilitated, and the high-purity MgAlON ceramic powder can be obtained by combining the airflow control and anti-pollution functions of a ceramic powder synthesis reaction device.

Description

MgAlON ceramic powder preparation method based on 3D printing forming
Technical Field
The invention belongs to the field of powder preparation, and particularly relates to a preparation method of MgAlON ceramic powder based on 3D printing and forming.
Background
MgAlON can be regarded as a stable spinel-structure ceramic material formed after MgO is dissolved in gamma-AlON in a solid solution mode, and the addition of Mg enables the ceramic material to have better thermodynamic stability than gamma-AlON ceramic. The MgAlON ceramic has the properties of small thermal expansion coefficient, good thermal shock resistance, strong slag corrosion resistance, small infiltration on molten metal and the like, and can be used as a refractory material in the ferrous metallurgy industry; the sapphire glass fiber reinforced plastic composite material has the characteristics of excellent mechanical property and good optical transmittance (the light transmittance is greater than 82 percent within the range of 0.5-4.5 mu m), and can be used for replacing sapphire to prepare a wave-transmitting window and a transparent armor. The wide application of high-performance MgAlON transparent ceramics depends on the macro supply of high-purity and low-cost MgAlON powder. At present, commercial MgAlON ceramic products are not seen in the domestic market, and the biggest restriction factor is that the macro synthesis technology of MgAlON powder with high purity and low cost is not broken through.
Among the synthesis methods of MgAlON ceramic powder, the carbothermal reduction nitridation method is one of the most studied methods, and the method relates to high-temperature gas-solid reaction (the temperature is as high as 1600-1700 ℃). At present, a few colleges and scientific research institutions realize the preparation of MgAlON ceramic powder in laboratory level, for example, Ma Benyuan and the like (DOI: doi.org/10.1016/j.jallcom.2018.02.254) provide a traditional process and a method for synthesizing MgAlON ceramic powder. The difficulty of synthesizing high-purity MgAlON powder in a macroscopic quantity is two: firstly, the phenomenon of phase impurity is easy to appear after the synthetic amount of the powder is amplified, and the reason is that the powder on the surface has shielding and blocking effects on the inward diffusion of gas, so that the gas-solid reaction of the powder inside is incomplete; and secondly, equipment suitable for powder mass synthesis is lacked, and the existing equipment has the problems of small hearth size, very limited single powder loading amount, uncontrollable airflow in the furnace and pollution of ceramic powder.
Disclosure of Invention
The invention aims to provide a preparation method of MgAlON ceramic powder based on 3D printing and forming, which aims to solve the problem of macroscopic preparation of the MgAlON ceramic powder needing high-temperature gas-solid reaction.
The invention provides a preparation method of MgAlON ceramic powder based on 3D printing and forming, which comprises the following steps:
(1) firstly, mixing raw material powder, a solvent and an additive to prepare raw material ink with high solid content; the raw material powder consists of 87-87.5 wt% of alumina, 8.0-9.5 wt% of magnesium oxide and 3.5-4.5 wt% of carbon black, wherein the phase of the alumina is an alpha phase or a gamma phase, and the particle size is nano;
(2) then printing the raw material ink into a raw material blank body with a regular three-dimensional through hole structure by adopting a 3D printing and forming process, and drying the raw material blank body;
(3) then the raw material blank is placed in a reaction device with the functions of air flow control and pollution prevention in a high-temperature graphite sintering furnace (see patent CN210718675U), and high-temperature synthesis is carried out in a controlled reaction environment;
(4) finally, the MgAlON ceramic powder with high purity can be obtained after ball milling process treatment.
Preferably, in the step (1), the solvent is a mixed solution of water and tert-butyl alcohol; the additive comprises a binder and a dispersant, the additive amount of the additive is 2-6% of the weight of the powder, wherein the binder is one or more of polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and carboxymethyl cellulose, and the dispersant is one or more of urea, ammonium citrate, tetramethylammonium hydroxide and ammonium polyacrylate; the solid content of the raw material powder in the prepared raw material ink is 40-50 wt%, and the preparation method is one of ball milling, homogenizing and three-roll grinding.
Preferably, in the step (2), the diameter of a printing nozzle of the 3D printing machine is 1-4 mm, the printing pressure is 150-350 kPa, and the printing speed is 5-20 mm/s; the drying mode of the blank is freeze drying.
Preferably, in the step (3), the raw material blank is placed on a MgAlON ceramic cushion block of the reaction device, and the distance between the raw material blank and the wall plates at the periphery in the reaction device is not less than 10 mm; the temperature range of high-temperature synthesis is 1600-1650 ℃, and the heat preservation time is 2-6 h; the reaction atmosphere is one of nitrogen and ammonia, and the gas flow is 1-5L/min.
Preferably, the rotation speed of the ball milling process in the process step (4) is 200-1000 rpm, and the ball milling time is 2-24 h.
Preferably, the ball milling process is followed by a carbon removal process, wherein the carbon removal process is carried out at a temperature of 500-700 ℃ for 4-12 h. Usually, the carbon removal process is added when the carbon content in the powder exceeds a certain range, and the carbon content in the powder is reduced by adjusting the amount of carbon black added to the raw material, whereby the purity of the powder can be ensured even if the carbon removal step is omitted.
The design idea of the invention is as follows:
the 3D printing forming is a new ceramic body forming technology developed in recent years, has the advantages of no mould forming, high forming efficiency, controllable size, near net forming and the like, and is a research hotspot in recent years. Compared with other 3D printing forming methods, the ink (slurry) used for slurry extrusion 3D printing has the advantages of small binder dosage, high solid phase content, capability of forming at normal temperature, no need of ultraviolet light and laser radiation, and the printed blank has the characteristics of controllable framework structure and extremely high through hole rate, and is very suitable for forming the raw material blank in the invention.
Therefore, the raw material powder is printed into the raw material blank body with the regular three-dimensional through hole structure by adopting 3D printing and forming, so that gas can be favorably diffused into the blank body through the three-dimensional through hole structure, and the gas-solid reaction in the blank body can be completely carried out; and then, a ceramic powder synthesis reaction device (patent CN210718675U) suitable for a high-temperature graphite sintering furnace is adopted, so that the functions of air flow control and pollution prevention can be realized, and the high-purity ceramic powder can be obtained.
Compared with the prior art, the invention has the following technical effects:
1. according to the scheme adopted by the invention, after the raw material powder is subjected to 3D printing to form the raw material green bodies, a plurality of raw material green bodies can be placed in the cavity of the reaction device, and the single synthesis amount of the powder can be increased by tens of times by increasing the number of the cavities, so that the macroscopic synthesis preparation of the ceramic powder is realized.
2. The ceramic raw material powder is printed and formed by 3D, and the blank has certain shape and strength, so that the ceramic raw material powder can be conveniently carried and the charging amount can be increased.
3. The raw material blank obtained by 3D printing and forming has a regular three-dimensional through hole structure, so that gas can be diffused and permeated into the blank, and the gas-solid synthesis reaction in the blank can be completely carried out.
4. The special reaction device (patent CN210718675U) capable of realizing the functions of air flow control and pollution prevention is adopted, so that the participation of gas in synthesis reaction and the prevention of external pollution can be further facilitated, and high-purity ceramic powder can be obtained.
5. The preparation method of the MgAlON ceramic powder provided by the invention has the advantages of high preparation efficiency, high phase purity, simple process steps, easy realization of industrialization, good application prospect and popularization value.
Drawings
FIG. 1 is a diagram showing an example of a MgAlON green body after a high-temperature synthesis reaction in example 1;
FIG. 2 is an enlarged view of the crushed powder in example 1;
FIG. 3 is an XRD spectrum of MgAlON powder synthesized at high temperature in examples 1 and 2.
Detailed Description
The present invention is further illustrated by the following figures and examples, which include, but are not limited to, the following examples.
Example 1
The preparation method of the MgAlON powder based on 3D printing forming comprises the following steps:
(1) weighing nanoscale gamma-A12O387.4g of powder, 8.8g of nanoscale MgO powder, 3.8g of high-purity carbon black powder, 5g of polyethylene glycol, 0.5g of urea, 0.5g of ammonia water, 125g of composite solvent (mixed liquid consisting of water and tert-butyl alcohol, the weight ratio is 75 percent and 25 percent respectively) and alumina grinding balls are put into a polyurethane ball milling tank and ball milled for 2 minutes on a homogenizer with the rotating speed of 2000r/min to obtain the raw material ink with the solid phase content of about 44 percent;
(2) injecting the raw material ink into a charging barrel of a 3D printer for printing and molding, wherein the diameter of a printing nozzle is 2mm, the printing pressure is 180kPa, the printing speed is 15mm/s, and after printing, putting the raw material blank into a blast oven at 100 ℃ for drying for 12h to obtain a raw material blank with an internal regular three-dimensional through hole structure;
(3) placing the raw material blank in a ceramic powder reaction device in a high-temperature graphite sintering furnace for high-temperature synthesis, wherein the synthesis reaction condition is that the temperature is kept for 3h at 1625 ℃ under the flowing nitrogen atmosphere, and the gas flow is 2.5L/min, so as to obtain a blank consisting of MgAlON particles (see figure 1);
(4) crushing the raw material blank synthesized at high temperature, putting the crushed raw material blank into an alumina ball milling tank, ball milling for 12 hours at the rotating speed of 300r/min by using alcohol as a ball milling medium and alumina as a milling ball, drying to obtain white powder (an enlarged view is shown in figure 2), and analyzing the powder to be a pure MgAlON phase by XRD (shown in figure 3).
Example 2
The preparation method of the MgAlON powder based on 3D printing forming comprises the following steps:
(1) weighing nanoscale alpha-A12O387.5g of powder, 8.5g of nano-scale MgO powder, 4.0g of high-purity carbon black powder, 4g of polyvinyl alcohol, 0.4g of tetramethylammonium hydroxide, 0.4g of ammonia water, 112g of a composite solvent (a mixed liquid consisting of water and tert-butyl alcohol, the weight ratio is 80% and 20% respectively) and alumina grinding balls, putting the mixture into a plastic container, stirring the mixture, and fully grinding the mixture on a three-roll grinder to obtain the raw material ink with the solid phase content of about 47%;
(2) injecting the raw material ink into a charging barrel of a 3D printer for printing and forming, wherein the diameter of a printing nozzle is 3mm, the printing pressure is 120kPa, the printing speed is 15mm/s, and after printing, putting the raw material blank into a freeze dryer at the temperature of-30 ℃ for drying for 24h to obtain the raw material blank with an internal regular three-dimensional through hole structure;
(3) placing the raw material blank in a ceramic powder reaction device in a high-temperature graphite sintering furnace for high-temperature synthesis, wherein the synthesis reaction condition is to keep the temperature at 1650 ℃ for 3h under the flowing ammonia atmosphere, and the gas flow is 3L/min, so as to obtain a blank consisting of MgAlON particles (see figure 1);
(4) crushing the raw material blank synthesized at high temperature, putting the crushed raw material blank into an alumina ball milling tank, ball milling the crushed raw material blank for 12 hours at the rotating speed of a rod mill of 300r/min by using alcohol as a ball milling medium and alumina as a milling ball, putting the dried powder into an oxidation furnace to remove carbon for 6 hours at 675 ℃, finally obtaining white powder, and analyzing the white powder to be a pure MgAlON phase by XRD (see figure 3).
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but all changes that can be made by applying the principles of the present invention and performing non-inventive work on the basis of the principles shall fall within the scope of the present invention.

Claims (6)

1. A preparation method of MgAlON ceramic powder based on 3D printing forming is characterized by comprising the following steps:
(1) firstly, mixing raw material powder, a solvent and an additive to prepare raw material ink with high solid content; the raw material powder consists of 87-87.5 wt% of alumina, 8.0-9.5 wt% of magnesium oxide and 3.5-4.5 wt% of carbon black, wherein the phase of the alumina is an alpha phase or a gamma phase, and the particle size is nano;
(2) then printing the raw ink into a raw material blank body with a regular three-dimensional through hole structure by adopting a 3D printing and forming process, and drying the raw material blank body;
(3) then placing the raw material blank into a reaction device with the functions of air flow control and pollution prevention in a high-temperature graphite sintering furnace, and carrying out high-temperature synthesis in a controlled reaction environment;
(4) finally, the MgAlON ceramic powder with high purity can be obtained after ball milling process treatment.
2. The MgAlON ceramic powder preparation method of claim 1, wherein in the step (1), the solvent is a mixed solution of water and tert-butyl alcohol; the additive comprises a binder and a dispersant, the additive amount of the additive is 2-6% of the weight of the powder, wherein the binder is one or more of polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and carboxymethyl cellulose, and the dispersant is one or more of urea, ammonium citrate, tetramethylammonium hydroxide and ammonium polyacrylate; the solid content of the raw material powder in the prepared raw material ink is 40-50 wt%, and the preparation method is one of ball milling, homogenizing and three-roll grinding.
3. The MgAlON ceramic powder preparation method according to claim 1, wherein in the step (2), the diameter of a printing nozzle of a 3D printer is 1-4 mm, the printing pressure is 150-350 kPa, and the printing speed is 5-20 mm/s; the drying mode of the blank is freeze drying.
4. The MgAlON ceramic powder preparation method according to claim 1, characterized in that in the step (3), the raw material blank is placed on the MgAlON ceramic cushion block of the reaction device, and the distance between the MgAlON ceramic cushion block and the wall plates at the periphery inside the reaction device is not less than 10 mm; the temperature range of high-temperature synthesis is 1600-1650 ℃, and the heat preservation time is 2-6 h; the reaction atmosphere is one of nitrogen and ammonia, and the gas flow is 1-5L/min.
5. The preparation method of MgAlON ceramic powder according to claim 1, wherein the ball milling process in the process step (4) has a rotation speed of 200-1000 rpm and a ball milling time of 2-24 h.
6. The preparation method of MgAlON ceramic powder according to claim 1 or 5, characterized in that the ball milling process is followed by a carbon removal process, the temperature of the carbon removal process is 500-700 ℃, and the heat preservation time is 4-12 h.
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