CN106673662A - Silicon carbide ceramic part and preparation method thereof - Google Patents
Silicon carbide ceramic part and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of inorganic nonmetal materials and relates to a silicon carbide ceramic part and a preparation method thereof, in particular to a preparation method of hollow silicon carbide ceramic spheres. The preparation method comprises steps as follows: phenol-formaldehyde resin powder, silicon carbide powder and polyvinyl alcohol are subjected to spray granulation, and powder is subjected to printing forming with a 3D printing method; a green body is nested in a high-temperature-resistant mold in a corresponding shape for heating curing, put in a graphite boat and covered with hexagonal silicon nitride and silica powder for reaction sintering, and the sintered silicon carbide green body is obtained after the cooling process ends; residues on the surface of the sintered silicon carbide green body are removed with a NaOH solution, and the silicon carbide ceramic part is obtained. The provided preparation process is simple and easy to implement, and compact silicon carbide ceramic in any shape, particularly, in the hollow sphere shape , can be prepared. The prepared silicon carbide ceramic has higher size accuracy.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, is related to silicon carbide ceramic part and preparation method thereof, especially one
Plant the preparation method of silicon carbide ceramics hollow ball.
Background technology
Silicon carbide ceramics has the excellent properties such as high intensity, high rigidity, high temperature resistant, wear-resistant, corrosion-resistant, is widely used in
The fields such as machinery, electronics, ocean engineering, space flight and aviation.Reaction sintering technology has low cost, base substrate change in size little, easy
The advantages of industry is amplified, is the selection process for preparing high accuracy silicon carbide ceramic product.
Because thyrite itself is hard and crisp, the processing of powder forming and sintered article is all extremely difficult.Therefore,
It is difficult to prepare the spherical silicon carbide products of open circles using conventional technique.Selective laser sintering technology (Selective Laser
Sintering, SLS) it is the rapid shaping technique for developing comparative maturity in 3D printing, with not being limited by shape, need not support
The advantages of, but, ceramic is printed using SLS techniques, often there are problems that density and intensity.
The content of the invention
The present invention overcomes above-mentioned technique to limit to, and SLS techniques and reaction sintering technology are combined, and by combined sintering etc.
Method, can prepare the high-performance silicon carbide part of arbitrary shape, can be widely applied to numerous industrial circles.Further
, using same technical scheme, the higher carborundum hollow ball of consistency height, dimensional accuracy can be prepared.
In order to realize above technique effect, the preparation method of the silicon carbide ceramic part of the present invention is real as follows
It is existing：
S1. after Phenolic resin powder is mixed with silicon carbide powder, the polyvinyl alcohol of gross mass 10~20%, ball milling are added
After mix homogeneously, mist projection granulating obtains the powder that phenolic resin coats carborundum；
S2. laser selective sintering process is adopted, by the method for 3D printing by the phenolic resin carbon coated in step S1
The powder of SiClx prints the silicon carbide green body of the part shape for needing；
S3. the silicon carbide green body in step S2 is enclosed within the high-temperature resistance die of respective shapes, in nitrogen protection atmosphere or
In vacuum environment, after being warming up to 450 DEG C with the speed of 5 DEG C/min, after 1~3h of insulation, cooling carries out the carbon that degumming obtains solidifying
SiClx base substrate；
S4. the silicon carbide green body of the solidification in step S3 is put in graphite boat, and is piled with graphite boat by six side's nitrogen
SiClx is fully embedded wherein with the infiltrant powder of silica flour composition up to the silicon carbide green body of solidification, carries out reaction-sintered, and Jing
Temperature-fall period is crossed, the silicon carbide green body after being sintered；Described reaction-sintered condition is not less than 5 × 10 for vacuum-1Pa, delays
Slowly after being warming up to 1550~1700 DEG C, 2h is incubated, after temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min；The drop
Warm process under nitrogen or argon, keeps gas pressure to be not less than 0.5MPa to turn off vacuum system, and slow cooling is extremely
Less than 200 DEG C, cooling rate is not higher than 5 DEG C/min；This step is one of important sport technique segment of the present invention, is also the present invention's
Innovation.Using the reaction-sintered effect produced during silica flour infiltration, coordinate reaction-sintered proposed by the present invention and cooling
Condition, enables technical scheme proposed by the present invention to make whole spheres of ceramic obtain uniform siliconising, and obtains fully dense ceramics
Spheroid (porosity is less than 0.1%).On the other hand, the silicon infiltrant that the present invention is adopted is made up of hexagonal boron nitride and silica flour, can
To prevent ceramic body surface to be adhered excessive residual silicon, follow-up difficulty of processing and processing capacity is reduced；
S5. the silicon carbide green body after sintering in step S4 is immersed in into 0.5~1h in 60~90 DEG C of NaOH solution, is removed
The residue on surface, then through clean water, drying, obtain silicon carbide ceramic part.
Wherein, Phenolic resin powder described in step S1 and silicon carbide powder mass ratio are 5~12:88~95.
Wherein, the laser selective sintering process parameter of 3D printing silicon carbide green body described in step S2 is：Laser power
Powdering thickness for 50~200W, 200~800mm/s of laser scanning speed, every layer of powder is 0.05~0.2mm.
Wherein, the material of high temperature resistant grinding tool described in step S3 is steel.
Wherein, reaction-sintered described in step S4 and temperature-fall period are carried out in a vacuum furnace.
Wherein, the hexagonal boron nitride in infiltrant powder described in step S4 and the mass ratio of silica flour are 1:2~3.
Wherein, silicon carbide green body described in step S2 be two can mutually in button hemispherical shell；Described in step S4
The silicon carbide green body of solidification be to buckle well two can mutually in button hemispherical shell solidification silicon carbide green body, this preparation
Method is prepared into silicon carbide ceramics hollow ball.Relative to one georama of direct 3D printing, printed using 3D printing technique
Two hemisphere for cooperating, can be prepared using SLS technologies, and technical difficulty is greatly lowered；Two hemisphere are added in addition
The connection between them is already allowed in size design, in step s 4 by the carborundum base of the solidification of two hemispherical shells
Body make-up reaction-sintered can finally be closely attached two hemisphere together.
Silicon carbide ceramic part prepared by above-mentioned preparation method.
The density of above-mentioned silicon carbide ceramics hollow ball carborundum hollow ball is not less than 3.05g/cm3, porosity is less than
0.1%.
The invention has the beneficial effects as follows：
1st, preparation is simple for present invention offer, can prepare densification, hollow ball-shape silicon carbide ceramics；Enter one
Step, can be the fine and close silicon carbide ceramics of arbitrary shape；
2nd, silicon carbide ceramics prepared by the present invention does not need more following process, and dimensional accuracy is higher.
Description of the drawings
Fig. 1 can the interior hemispherical shell schematic diagram detained mutually for the present invention provides two.
The interior two silicon carbide green body schematic diagrams buckled well that Fig. 2 is provided for the present invention.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
A kind of preparation method of silicon carbide ceramic part, preparation technology is comprised the following steps：
Step one, is 8 by mass ratio:After 92 Phenolic resin powder mixes with silicon carbide powder, gross mass 15% is added
Polyvinyl alcohol, after ball milling mixing is uniform, mist projection granulating, obtain phenolic resin coat carborundum powder；
Step 2, using laser selective sintering process, part shape is printed as by the method for 3D printing by powder.Tool
The technological parameter of body is：Laser power is 80W, laser scanning speed 500mm/s, the powdering thickness of every layer of powder are 0.1mm；
Step 3, part is placed in the steel ball of respective shapes, in nitrogen protection atmosphere or vacuum environment, is warming up to
450 DEG C carry out degumming process, and programming rate is 5 DEG C/min, is incubated furnace cooling after 1h；
Step 4, by the part after degumming process, in being put into graphite boat, it is 1 to pile with graphite boat by mass ratio:The six of 2
The infiltrant powder that square silicon nitride is constituted with silica flour, and carborundum ball is fully embedded in above-mentioned mixed-powder, it is positioned over
In vacuum drying oven, reaction-sintered is carried out：Vacuum is kept to be not less than 5 × 10-1Pa, then 1650 DEG C are to slowly warm up to, and 2h is incubated,
After furnace temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min；
Step 5, after sintered heat insulating terminates, turns off vacuum system, and nitrogen or argon are filled with stove, keeps gas pressure
0.5MPa is not less than, and slowly furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min；
Step 6, is immersed in 80 DEG C, in the NaOH solution that mass fraction is 30% by the carbonization silicon ball after reaction-sintered
0.5h, removes the residue on surface, then through clean water, drying, obtains silicon carbide ceramic part.
Test result, porosity is 0.09%, and Rockwell hardness HRA is 94.5.
Embodiment 2
A kind of preparation method of silicon carbide ceramics hollow ball, preparation technology is comprised the following steps：
Step one, is 8 by mass ratio:After 92 Phenolic resin powder mixes with silicon carbide powder, gross mass 15% is added
Polyvinyl alcohol, after ball milling mixing is uniform, mist projection granulating, obtain phenolic resin coat carborundum powder；
Step 2, using laser selective sintering process, by the method for 3D printing by powder be printed as two it is hemispherical
Silicon carbide green body (such as Fig. 1).Specifically technological parameter is：Laser power is 80W, laser scanning speed 500mm/s, every layer of powder
The powdering thickness at end is 0.1mm；
Step 3, two hemispherical base substrates is enclosed within the steel ball of respective shapes, in nitrogen protection atmosphere or vacuum environment
In, being warming up to 450 DEG C carries out degumming process, and programming rate is 5 DEG C/min, is incubated furnace cooling after 1h；
Step 4, by degumming process after two silicon carbide green bodies to buckling well (such as Fig. 2), in being put into graphite boat, graphite boat
In pile with by mass ratio be 1:The infiltrant powder that 2 six side's silicon nitrides are constituted with silica flour, and it is fully embedded carborundum ball
In above-mentioned mixed-powder, in being positioned over vacuum drying oven, reaction-sintered is carried out：Vacuum is kept to be not less than 5 × 10-1Pa, then slowly
1650 DEG C are warming up to, and are incubated 2h, after furnace temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min；
Step 5, after sintered heat insulating terminates, turns off vacuum system, and nitrogen or argon are filled with stove, keeps gas pressure
0.5MPa is not less than, and slowly furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min；
Step 6, is immersed in 80 DEG C, in the NaOH solution that mass fraction is 30% by the carbonization silicon ball after reaction-sintered
0.5h, removes the residue on surface, then through clean water, drying, obtains density for 3.06g/cm3, porosity is less than
0.1% carborundum hollow ball.
Test result, porosity is 0.08%, and Rockwell hardness HRA is 95.
Embodiment 3
A kind of preparation method of silicon carbide ceramics hollow ball, preparation technology is comprised the following steps：
Step one, is 10 by mass ratio:After 90 Phenolic resin powder mixes with silicon carbide powder, gross mass 20% is added
Polyvinyl alcohol, after ball milling mixing is uniform, mist projection granulating, obtain phenolic resin coat carborundum powder；
Step 2, using laser selective sintering process, by the method for 3D printing by powder be printed as two it is hemispherical
Silicon carbide green body (such as Fig. 1)；Laser power is 150W, laser scanning speed 400mm/s, the powdering thickness of every layer of powder are
0.15mm。
Step 3, two hemispherical base substrates is enclosed within the steel ball of respective shapes, in nitrogen protection atmosphere or vacuum environment
In, being warming up to 450 DEG C carries out degumming process, and programming rate is 5 DEG C/min, is incubated furnace cooling after 3h；
Step 4, by degumming process after two silicon carbide green bodies to buckling well (such as Fig. 2), in being put into graphite boat, graphite boat
In pile with by mass ratio be 1:The infiltrant powder that 2 six side's silicon nitrides are constituted with silica flour, and it is fully embedded carborundum ball
In above-mentioned mixed-powder, in being positioned over vacuum drying oven, reaction-sintered is carried out：Vacuum is kept to be not less than 5 × 10-1Pa, then slowly
1700 DEG C are warming up to, and are incubated 2h, after furnace temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min；
Step 5, after sintered heat insulating terminates, turns off vacuum system, and nitrogen or argon are filled with stove, keeps gas pressure
0.5MPa is not less than, and slowly furnace temperature is reduced to into less than 200 DEG C, cooling rate is not higher than 5 DEG C/min；
Step 6, is immersed in 90 DEG C, in the NaOH solution that mass fraction is 35% by the carbonization silicon ball after reaction-sintered
0.5h, removes the residue on surface, then through clean water, drying, obtains density for 3.07g/cm3, porosity is less than
0.1% carborundum hollow ball.
Test result, porosity is 0.09%, and Rockwell hardness HRA is 94.3.
The above is presently preferred embodiments of the present invention, but the present invention should not be limited to disclosed in the embodiment
Content.So it is every without departing from the equivalent or modification completed under spirit disclosed in this invention, both fall within the model of present invention protection
Enclose.
Claims (9)
1. a kind of preparation method of silicon carbide ceramic part, it is characterised in that comprise the steps：
S1. after Phenolic resin powder is mixed with silicon carbide powder, the polyvinyl alcohol of gross mass 10~20%, ball milling mixing are added
After uniform, mist projection granulating obtains the powder that phenolic resin coats carborundum；
S2. laser selective sintering process is adopted, the phenolic resin in step S1 is coated by carborundum by the method for 3D printing
Powder print need part shape silicon carbide green body；
S3. the silicon carbide green body in step S2 is enclosed within the high-temperature resistance die of respective shapes, in nitrogen protection atmosphere or vacuum
In environment, after being warming up to 450 DEG C with the speed of 5 DEG C/min, after 1~3h of insulation, cooling carries out the carborundum that degumming obtains solidifying
Base substrate；
S4. the silicon carbide green body of the solidification in step S3 is put in graphite boat, and is piled with graphite boat by six side's silicon nitrides
It is fully embedded wherein up to the silicon carbide green body of solidification with the infiltrant powder of silica flour composition, carries out reaction-sintered, and through drop
Warm process, the silicon carbide green body after being sintered；Described reaction-sintered condition is not less than 5 × 10 for vacuum-1Pa, it is slow to rise
Temperature is incubated 2h to after 1550~1700 DEG C, and after temperature is more than 800 DEG C, programming rate is less than 2 DEG C/min；It is described to lower the temperature
Journey under nitrogen or argon, keeps gas pressure to be not less than 0.5MPa to turn off vacuum system, and slow cooling is to 200
Below DEG C, cooling rate is not higher than 5 DEG C/min；
S5. the silicon carbide green body after sintering in step S4 is immersed in into 0.5~1h in 60~90 DEG C of NaOH solution, removes surface
Residue, then through clean water, drying, obtain silicon carbide ceramic part.
2. the preparation method of the silicon carbide ceramic part according to right 1, it is characterised in that：Phenolic resin described in step S1
Powder is 5~12 with silicon carbide powder mass ratio:88~95.
3. the preparation method of the silicon carbide ceramic part according to right 1, it is characterised in that：3D printing carbon described in step S2
The laser selective sintering process parameter of SiClx base substrate is：Laser power is 50~200W, 200~800mm/ of laser scanning speed
S, the powdering thickness of every layer of powder are 0.05~0.2mm.
4. the preparation method of the silicon carbide ceramic part according to right 1, it is characterised in that：High temperature resistant described in step S3 is ground
Tool material is steel.
5. the preparation method of the silicon carbide ceramic part according to right 1, it is characterised in that：Reaction-sintered described in step S4
Carry out in a vacuum furnace with temperature-fall period.
6. the preparation method of the silicon carbide ceramic part according to right 1, it is characterised in that：Infiltrant powder described in step S4
Hexagonal boron nitride in end is 1 with the mass ratio of silica flour:2~3.
7. the preparation method of the silicon carbide ceramic part according to right 1, it is characterised in that：Carborundum base described in step S2
Body be two can mutually in button hemispherical shell；The silicon carbide green body solidified described in step S4 is can be with to buckle well two
The silicon carbide green body of the solidification of the hemispherical shell of button in mutually.
8. any preparation method according to right 1-7 prepares silicon carbide ceramic part.
9. the preparation method according to right 7 prepares silicon carbide ceramic part and is silicon carbide ceramics hollow ball, and its feature exists
In：The density of the carborundum hollow ball is not less than 3.05g/cm3, porosity is less than 0.1%.
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| CN113788703A (en) * | 2021-10-26 | 2021-12-14 | 西安交通大学 | Method for preparing silicified graphite through carbon source modification and reaction infiltration and silicified graphite |
| US11285242B1 (en) * | 2019-12-20 | 2022-03-29 | The University Of North Carolina At Charlotte | Processing and bioactivation of a novel SiC medical device |
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