CN115894041B - Preparation method of powder extrusion 3D printing forming reaction sintering silicon carbide ceramic - Google Patents
Preparation method of powder extrusion 3D printing forming reaction sintering silicon carbide ceramic Download PDFInfo
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Abstract
The invention relates to a preparation method of powder extrusion 3D printing forming reaction sintering silicon carbide ceramic. The preparation method comprises the following steps: mixing inorganic powder composed of silicon carbide powder, carbon black and a surfactant to obtain modified powder; uniformly mixing the modified powder with an organic binder, crushing and granulating to obtain a silicon carbide mixture; the mass of the silicon carbide powder is 50-90wt% of the mass of the inorganic powder, and the mass of the carbon black is 10-50wt% of the mass of the inorganic powder; extruding the silicon carbide mixture powder, and performing 3D printing to form a silicon carbide ceramic green body; thermal degreasing to obtain a silicon carbide ceramic degreased blank; the silicon carbide ceramic degreasing blank and Si grains are mixed according to the following ratio of 1: and mixing the materials according to the mass ratio of 1-2, and performing reactive sintering to obtain the powder extrusion 3D printing forming reactive sintering silicon carbide ceramic.
Description
Technical Field
The invention belongs to the technical field of preparation of silicon carbide ceramics with complex structures, and particularly relates to a preparation method of reactive sintering silicon carbide ceramics by powder extrusion 3D printing molding.
Background
Silicon carbide (SiC) ceramic materials have unique properties such as high hardness (over 24 GPa), low density (3.215 g/cm) -3 ) High heat conductivity (more than 100W/(m.K)), low thermal expansion coefficient, wear resistance, corrosion resistance and the like, and is widely applied to chemical industry, machinery, electronics, aerospace and biological medicineThe ceramic is one of the most widely used non-oxide ceramics in the fields of engineering and the like. Generally, national defense and industrial applications require the use of complex shaped SiC ceramic material articles, which presents significant challenges and challenges to ceramic manufacture. Conventional molding methods, including injection molding, compression molding, casting, gel casting, and the like, have difficulty in achieving highly complex geometries and interconnected pore structures. At the same time, the design and manufacture of the mold also brings about an increase in processing time and cost.
The additive manufacturing technology (Additive Manufacturing) is based on a computer model, and materials are piled up into parts and components with certain shapes point by point, line by line or surface by surface, so that the method is not limited by a mould manufacturing or processing technology, and meanwhile, the defect brought to ceramic materials in the process of reducing the materials is avoided. The silicon carbide ceramic additive manufacturing technology has unique advantages in the aspect of ceramic complex shape forming.
The powder extrusion printing (Power Extrusion Printing) technology inherits the characteristic of line-by-line printing of the traditional fused deposition modeling (Fused Deposition Modeling). In contrast, powder extrusion printing technology uses mixed particles of inorganic powder and organic binder instead of conventional plastic wires. Most 3D printing processes with binder or organic monomer addition have difficulty bypassing the degreasing step, which tends to reduce the density of the ceramic body, since most of the binder or organic monomer is expelled, leaving only loose ceramic powder. Therefore, insufficient density is one of the main problems of the 3D printing ceramic, and the density of the ceramic after printing has decisive influence on the performance of the ceramic besides influencing the mechanical property of the ceramic.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a preparation method of powder extrusion 3D printing forming reaction sintering silicon carbide ceramic. The method has high density of the formed blank, solves the problem of cracking after degreasing or sintering due to insufficient density of the blank in the prior 3D printing of the silicon carbide ceramic, improves the mechanical property of the 3D printing ceramic material, and can realize near-net forming of the complex shape of the ceramic material by combining with reaction sintering.
In a first aspect, the invention provides a preparation method of powder extrusion 3D printing forming reaction sintering silicon carbide ceramic, comprising the following steps:
mixing inorganic powder composed of silicon carbide powder, carbon black and a surfactant to obtain modified powder; uniformly mixing the modified powder with an organic binder, crushing and granulating to obtain a silicon carbide mixture; the mass of the silicon carbide powder is 50-90wt% of the mass of the inorganic powder, and the mass of the carbon black is 10-50wt% of the mass of the inorganic powder;
extruding the silicon carbide mixture powder, and performing 3D printing to form a silicon carbide ceramic green body;
thermal degreasing to obtain a silicon carbide ceramic degreased blank;
the silicon carbide ceramic degreasing blank and Si grains are mixed according to the following ratio of 1: and mixing the materials according to the mass ratio of 1-2, and performing reactive sintering to obtain the powder extrusion 3D printing forming reactive sintering silicon carbide ceramic.
Preferably, the silicon carbide powder is a mixture of silicon carbide particles with two particle size distributions of d50=1-5 μm and d50=20-60 μm, and the mass ratio of the silicon carbide particles with two particle size distributions of d50=1-5 μm and d50=20-60 μm is controlled to be 1:1-3.
Preferably, the surfactant is selected from one of polyvinylpyrrolidone, a silane coupling agent, tetramethylammonium hydroxide, stearic acid or polyethyleneimine; the addition amount of the surfactant is 0.5-3% of the mass of the inorganic powder.
Preferably, the mass fraction of the binder can be controlled to be 10-25wt% of the total mass of the modified powder and the binder; the adhesive is high-density polyethylene HDPE, ethylene-vinyl acetate copolymer EVA and solid paraffin PW according to the following ratio of 1:1:1-7 by mass ratio.
Preferably, the mixing temperature is 140-170 ℃, the mixing rotating speed is 10-40rpm, and the mixing time is 0.5-2h.
Preferably, the temperature of the powder extrusion 3D printing nozzle is 140-180 ℃, the temperature of the printing platform is 100-120 ℃, and the aperture of the nozzle is 0.4-1 mm.
Preferably, the conditions for thermal degreasing are: and heating the silicon carbide ceramic green body to 400-600 ℃ according to the heating rate of 0.2-2 ℃/min under argon or vacuum atmosphere, and preserving heat for 0.5-4h.
Preferably, the carbon density of the silicon carbide ceramic degreasing blank is controlled to be 0.55-0.90.
Preferably, the reaction sintering atmosphere is vacuum, the sintering temperature is 1500-1800 ℃, and the sintering time is 0.5-2h.
In a second aspect, the invention provides a powder extrusion 3D printing forming reaction sintering silicon carbide ceramic obtained by the preparation method.
Advantageous effects
According to the preparation method of the powder extrusion 3D printing forming reaction sintered silicon carbide, the formed green body has high density, the size of the sintered silicon carbide ceramic material almost has no shrinkage, the complex shape can be maintained, the strength is high, and the structure is uniform and compact.
Drawings
FIG. 1 is a diagram of a green body of powder extruded 3D printed gear silicon carbide ceramic prepared in step (2) of example 1 of the present invention;
FIG. 2 is a diagram of a silicon carbide ceramic material for a reaction-sintered gear formed by powder extrusion 3D printing, which is prepared in example 1 of the present invention;
FIG. 3 is a diagram showing the microscopic morphology of the reactive sintered silicon carbide ceramic obtained by the powder extrusion 3D printing molding method according to the embodiment 1 of the present invention;
fig. 4 is an XRD phase analysis chart of the powder extrusion 3D printing-molded reaction-sintered silicon carbide ceramic prepared in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
The invention provides a preparation method of powder extrusion 3D printing forming reaction sintering silicon carbide ceramic, which mainly comprises the following steps of.
(1) And preparing the powder extrusion 3D printing silicon carbide mixture. Performing ball milling mixing on inorganic powder consisting of silicon carbide powder and carbon black and a surfactant in absolute ethyl alcohol by taking silicon carbide balls as a medium, drying the ball-milled slurry in a 60 ℃ oven for 12 hours, and sieving the slurry with a 100-mesh sieve to obtain modified powder; and mixing the modified powder and the organic binder on a double-roller mixer until the modified powder and the organic binder are uniform, and crushing the mixture in a jaw crusher until the particle size is 2-5mm to obtain the powder extrusion 3D printing silicon carbide mixture.
In some embodiments, the silicon carbide powder may be a mixture of silicon carbide particles having two particle size distributions d50=1 to 5 μm and d50=20 to 60 μm, and the mass ratio of the silicon carbide particles having two particle size distributions d50=1 to 5 μm and d50=20 to 60 μm is controlled to be 1:1-3. By adopting the silicon carbide particles in bimodal distribution, the bulk density of the powder can be improved, so that the silicon carbide ceramic biscuit with high solid content is obtained after molding. The particle size of the carbon black powder is d50=0.2-2 μm. The surfactant may be selected from one of polyvinylpyrrolidone, a silane coupling agent, tetramethylammonium hydroxide, stearic acid, or polyethyleneimine.
Preferably, the mass of the silicon carbide powder can account for 50-90wt% of the mass of the inorganic powder, and the mass of the carbon black can account for 10-50wt% of the mass of the inorganic powder; the addition amount of the surfactant can be 0.5-3% of the mass of the inorganic powder. The adjustment of the carbon density can be realized by controlling the mass fraction of the silicon carbide powder and the carbon black powder, so that the theoretical density of the sintered ceramic is adjusted. Too low a carbon density can lead to too high a free silicon content, resulting in reduced mechanical properties of the material, and too high a carbon density can lead to incomplete reaction sintering.
At the same time, the addition of the surfactant prevents direct contact between the powder particles. Too low a surfactant content can lead to insufficient coating of the powder surface by the surfactant, and a particle network can be formed, so that the high-temperature viscosity of the mixture is increased, and the extrusion is not facilitated; the content of the surfactant is too high, which is not beneficial to molding, and the blank body can bring defects such as cracks and the like in the thermal degreasing process.
The ball milling medium can be silicon carbide pellets, and the mass ratio of the ball milling balls can be 1:1-3. The rotating speed of the ball mill can be 80rpm-150rpm, and the ball milling time can be 10-30h.
In the process of mixing the modified powder and the organic binder, the mass fraction of the binder can be controlled to be 10-25wt% of the total mass of the modified powder and the binder. Too low a binder content may result in the modified powder not being sufficiently mixed with the binder, resulting in too high a viscosity, which is detrimental to extrusion; too high a binder content results in a lower overall solids content, resulting in defects after degreasing and lower mechanical properties after sintering.
In some embodiments, the binder may be a high density polyethylene HDPE, an ethylene-vinyl acetate copolymer EVA, a paraffin wax PW according to 1:1:1-7 by mass ratio. The melting point of the high-density polyethylene is 130 ℃, the boiling point of the stearic acid is 183 ℃, and the mixing temperature can be controlled to 140-170 ℃, so that the binder can be fully melted without decomposition. The mixing speed can be 10-40rpm, and the mixing time can be 0.5-2h.
(2) Powder extrusion 3D printing of the silicon carbide ceramic green body. And (3) taking the silicon carbide mixture prepared in the step (1) as a raw material, and adopting powder extrusion printing equipment to print and mold the silicon carbide mixture into a silicon carbide ceramic green body.
Wherein, the temperature of the printing nozzle can be set to 140-180 ℃, and the mixture can be ensured to be melted and extruded without decomposition in the temperature range. The temperature of the printing platform can be set to be 100-120 ℃, and the aperture of the nozzle can be selected to be 0.4-1 mm.
The powder extrusion printing technology has the advantages of high solid content (about 60 vol%) and high strength of the printed blank (8 MPa-10 MPa) and high forming density (1.6-1.8 g/cm) 3 ) The method comprises the steps of carrying out a first treatment on the surface of the Moreover, defects are not easy to occur after degreasing, and the sintered ceramic microstructure is compact and uniform, so that the manufacturing of the ceramic material with high strength and complex shape can be realized.
(3) And (5) thermal degreasing. And (3) placing the silicon carbide ceramic green body prepared in the step (2) into a degreasing furnace, heating the silicon carbide ceramic green body to 400-600 ℃ at a heating rate of 0.2-2 ℃/min under argon or vacuum atmosphere, preserving heat for 0.5-4h, and performing thermal degreasing to obtain a silicon carbide ceramic degreased body sample. The over-fast heating rate can easily cause the defects of cracking, bubbling and the like of the adhesive due to inconsistent shrinkage in the degreasing process.
(4) And (5) performing reaction sintering. And (3) placing the silicon carbide ceramic degreasing blank obtained in the step (3) and Si particles into a high-temperature sintering furnace for reaction sintering to obtain the powder extrusion 3D printing forming reaction sintering silicon carbide ceramic.
The carbon density refers to the mass of carbon element in unit volume in the ceramic degreased blank; the carbon density of the silicon carbide ceramic degreasing blank can be controlled to be 0.55-0.90. Too high a carbon density can result in incomplete carbon reactions and cracking of the sample; too low a carbon density may result in too high a silicon content of the material. In some embodiments, the silicon carbide ceramic degreased green body to Si grain mass ratio may be 1:1-2; the atmosphere of the reaction sintering is vacuum, the sintering temperature is 1500-1800 ℃, and the sintering time is 0.5-2h.
The reactive sintering means that liquid Si reactive at a high temperature penetrates into a body having a certain porosity by capillary force, reacts with C in the body, and generates SiC. Compared with other sintering processes of SiC ceramics, the reaction sintering process has the following characteristics: the sintering time is short, and the sintering temperature is low; the reaction sintering process is a net-size sintering process, and the size of a green body hardly changes in the sintering process; an almost fully dense sintered body can be obtained without external pressure during sintering; no special and expensive equipment is needed, and the cost of the reaction sintering process is far lower than that of hot pressing and pressureless sintering of silicon carbide.
The carbon density can be adjusted by adjusting the mass fractions of the silicon carbide powder and the carbon black powder, so that the theoretical density of the sintered ceramic is adjusted, the content of free silicon is too high due to the too low carbon density, the mechanical properties of the sample are reduced, and the incomplete reaction sintering is caused due to the too high carbon density. In the reaction sintering process, if the mass of the added Si particles is small, insufficient reaction sintering can be caused; if the Si particles are added in a large amount, the subsequent processing becomes difficult. At the same time, too low or too high sintering temperatures and inadequate holding times lead to incomplete reaction sintering and thus poor mechanical properties of the test specimens.
The powder extrusion 3D printing forming and the reaction sintering are combined, and the prepared silicon carbide ceramic green body has the advantages of high solid content and high strength; the degreased part has complete appearance, and can well maintain the complex shape of 3D printing molding. The silicon carbide ceramic after reaction sintering has uniform and compact internal structure and high strength, and the size of the silicon carbide ceramic material after sintering is almost free from shrinkage, can maintain a complex shape, and can realize near net shape forming of the complex shape.
The density of the silicon carbide ceramic obtained by the preparation method provided by the invention can reach 2.85-3.12g/cm 3 The three-point bending strength can reach 229-400MPa, the elastic modulus is 329-367GPa, and the free Si content is 10.0-41.0vol%.
The present invention will be further illustrated by the following examples. It should also be understood that the following examples are given by way of illustration only and are not to be construed as limiting the scope of the invention, since numerous insubstantial modifications and adaptations of the invention to those skilled in the art will now be apparent to those in light of the foregoing disclosure, and that the specific process parameters and the like set forth below are merely one example of a suitable scope.
Example 1
(1) Preparation of powder extrusion 3D printed silicon carbide mixture. Silicon carbide powder, carbon black and stearic acid are mixed according to a proportion of 60:40:1.7, wherein silicon carbide powder is mixed with silicon carbide particles of two particle size distributions d50=5 μm and d50=50 μm in a weight ratio of 1:1.7 mass ratio of the mixture formed. Adding a proper amount of absolute ethyl alcohol, and performing ball milling by taking silicon carbide balls as ball milling media, wherein the mass ratio of the balls is 1:2, the rotating speed of the ball mill is 100rpm, and the ball milling time is 24 hours. Drying the ball-milled slurry in a 60 ℃ oven for 12 hours, and sieving the slurry with a 100-mesh sieve after the drying is finished to obtain modified powder. The modified powder was combined with an organic binder at 82:18, uniformly mixing the materials on a double-roll mixer, and crushing the materials in a jaw crusher until the particle size is 3mm to obtain the powder extrusion 3D printing silicon carbide mixture. Wherein the organic binder is high-density polyethylene, ethylene-vinyl acetate copolymer and paraffin wax according to the following weight ratio of 1:1:2.8 weight ratio of the mixture formed. The mixing temperature was 170℃and the mixing speed was 32rpm, and the mixing time period was 1 hour.
(2) Powder extrusion 3D printing of the silicon carbide ceramic green body. And (3) taking the silicon carbide mixture prepared in the step (1) as a raw material, and adopting powder extrusion printing equipment to print and mold the silicon carbide mixture into a silicon carbide ceramic green body. Wherein the temperature of the printing nozzle is set to 170 ℃, the temperature of the printing platform is set to 100 ℃, and the aperture of the nozzle is selected to be 0.8mm.
(3) And (5) thermal degreasing. And (3) placing the silicon carbide ceramic green body prepared in the step (2) into a degreasing furnace, heating the silicon carbide ceramic green body to 480 ℃ at a heating rate of 0.5 ℃/min under an argon atmosphere, and preserving heat for 2 hours, and performing thermal degreasing to obtain the silicon carbide ceramic degreasing blank.
(4) And (5) performing reaction sintering. And (3) placing the silicon carbide ceramic degreasing blank and Si particles obtained in the step (3) into a high-temperature sintering furnace for reaction sintering. The carbon density of the silicon carbide ceramic degreasing blank is controlled to be 0.80, and the mass ratio of the silicon carbide ceramic degreasing blank to Si particles is controlled to be 1: and 1.2, reacting for 0.5h at a sintering temperature of 1600 ℃ in a vacuum atmosphere to obtain the powder extrusion 3D printing forming reaction sintering silicon carbide ceramic.
The silicon carbide ceramic obtained by the reaction sintering in this example has a density of 3.05g/cm 3 The three-point bending strength was 310MPa, the elastic modulus was 346GPa, and the free Si content was 18.2vol%.
Fig. 1 is a physical diagram of a powder extrusion 3D printing gear silicon carbide ceramic green body prepared in step (2) of example 1 of the present invention. From the figure, the blank has higher precision after 3D printing and forming, clear edge profile and no sagging phenomenon.
Fig. 2 is a diagram of a silicon carbide ceramic material for a reaction-sintered gear obtained by extrusion 3D printing of the powder prepared in example 1 of the present invention. As can be seen from the figure, the size of the reaction-sintered silicon carbide blank has little shrinkage compared with the green body, and near net shape formation of the reaction-sintered silicon carbide ceramic component with a complex shape is realized.
Fig. 3 is a microscopic morphology diagram of the powder extrusion 3D printing reaction sintered silicon carbide ceramic prepared in example 1 of the present invention. As can be seen from the graph, the microstructure of the silicon carbide ceramic after reaction sintering is uniform and compact, and no silicon lake formed by aggregation of free silicon and unreacted complete carbon black area appear.
Fig. 4 is an XRD phase analysis chart of the powder extrusion 3D printing-molded reaction-sintered silicon carbide ceramic prepared in example 1 of the present invention. As can be seen from the figure, the reaction sintered sample mainly consists of three phases of 6H-SiC, 3C-SiC and Si.
Example 2
The preparation procedure of this example is described in example 1. The main differences are that: in the step (1), the mass ratio of the silicon carbide powder to the carbon black to the stearic acid is 50:50:1.7; the mass ratio of the modified powder to the organic binder is 78:22, wherein the organic binder is formed from high density polyethylene, ethylene vinyl acetate copolymer, paraffin wax at a ratio of 1:1:4.3 weight ratio. In the step (4), the mass ratio of the silicon carbide ceramic degreasing blank to the Si particles is controlled to be 1:1.24.
the silicon carbide ceramic obtained by the reaction sintering in this example has a density of 3.01g/cm 3 The three-point bending strength was 229MPa, the elastic modulus was 329GPa, and the free Si content was 22.7vol%.
Example 3
The preparation procedure of this example is described in example 1. The main differences are that: in the step (1), the mass ratio of the silicon carbide powder to the carbon black to the stearic acid is 50:50:1.7; the ratio of the modified powder to the organic binder is 80:20, wherein the organic binder is prepared from high density polyethylene, ethylene-vinyl acetate copolymer, paraffin wax at a ratio of 1:1:3.5 weight ratio. In the step (4), the carbon density of the silicon carbide ceramic degreasing blank is controlled to be 0.86, and the mass ratio of the silicon carbide ceramic degreasing blank to Si particles is controlled to be 1:1.25.
the silicon carbide ceramic obtained by the reaction sintering in this example has a density of 3.06g/cm 3 The three-point bending strength was 253MPa, the elastic modulus was 367GPa, and the free Si content was 17.0vol%.
Comparative example 1
The preparation procedure of this comparative example is described in example 1. The main differences are that: in the step (1), the mass ratio of the silicon carbide powder to the carbon black to the stearic acid is 50:50:1.7; the ratio of the modified powder to the organic binder is 82:18, wherein the organic binder is formed from high density polyethylene, ethylene vinyl acetate copolymer, paraffin wax at a ratio of 1:1:2.8 weight ratio. In the step (4), the carbon density of the silicon carbide ceramic degreasing blank is controlled to be 0.93, and the mass ratio of the silicon carbide ceramic degreasing blank to Si particles is controlled to be 1:1.27.
because of higher carbon density, the silicon carbide ceramic obtained by the reaction sintering of the comparative example has a local infiltration non-uniformity phenomenon inside, and a black core area formed by incompletely reacted carbon black exists.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Many modifications and substitutions of the present invention will become apparent to those of ordinary skill in the art upon reading the foregoing. Accordingly, the scope of the invention should be limited only by the attached claims.
Claims (4)
1. The preparation method of the powder extrusion 3D printing forming reaction sintering silicon carbide ceramic is characterized by comprising the following steps of:
mixing inorganic powder composed of silicon carbide powder, carbon black and a surfactant to obtain modified powder; uniformly mixing the modified powder with an organic binder, crushing and granulating to obtain a silicon carbide mixture; the silicon carbide powder is a mixture of silicon carbide particles with two particle size distributions of d50=1-5 μm and d50=20-60 μm, and the mass ratio of the silicon carbide particles with two particle size distributions of d50=1-5 μm and d50=20-60 μm is controlled to be 1:1-3; the mass of the silicon carbide powder is 50-90wt% of the mass of the inorganic powder, and the mass of the carbon black is 10-50wt% of the mass of the inorganic powder; the addition amount of the surfactant is 0.5-3% of the mass of the inorganic powder; the mass of the organic binder accounts for 10-25wt% of the total mass of the modified powder and the organic binder; the organic binder is high-density polyethylene HDPE, ethylene-vinyl acetate copolymer EVA and solid paraffin PW according to the following ratio of 1:1:1-7 by mass ratio; the mixing temperature is 140-170 ℃, the mixing rotating speed is 10-40rpm, and the mixing time is 0.5-2h;
extruding the silicon carbide mixture powder, and performing 3D printing to form a silicon carbide ceramic green body; wherein the temperature of a nozzle for powder extrusion 3D printing is 140-180 ℃, the temperature of a printing platform is 100-120 ℃, and the aperture of the nozzle is 0.4-1 mm;
thermal degreasing to obtain a silicon carbide ceramic degreased blank; controlling the carbon density of the silicon carbide ceramic degreasing blank to be 0.55-0.90; the carbon density is the mass of carbon element in unit volume in the ceramic degreasing blank; the conditions of thermal degreasing are: heating the silicon carbide ceramic green body to 400-600 ℃ according to the heating rate of 0.2-2 ℃/min under argon or vacuum atmosphere, and preserving heat for 0.5-4h;
the silicon carbide ceramic degreasing blank and Si grains are mixed according to the following ratio of 1: and mixing the materials according to the mass ratio of 1-2, and performing reactive sintering to obtain the powder extrusion 3D printing forming reactive sintering silicon carbide ceramic.
2. The method according to claim 1, wherein the surfactant is one selected from polyvinylpyrrolidone, a silane coupling agent, tetramethylammonium hydroxide, stearic acid, and polyethyleneimine.
3. The method according to claim 1, wherein the reaction sintering atmosphere is vacuum, the sintering temperature is 1500-1800 ℃ and the sintering time is 0.5-2h.
4. A powder extrusion 3D print molded reaction sintered silicon carbide ceramic obtained according to the preparation method of claim 1.
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