CN109796208A - Si3N4Ceramic structural member and method for manufacturing same - Google Patents
Si3N4Ceramic structural member and method for manufacturing same Download PDFInfo
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Abstract
The invention discloses a Si3N4 ceramic structural member and a preparation method thereof. According to the method, Si powder is used as a raw material and the grain composition of a sintering aid and the Si powder is adjusted when Si3N4 ceramic is subjected to 3D printing for the first time, so that the problems that silicon nitride is easy to agglomerate due to moisture absorption, micron-sized silicon nitride is extremely difficult to sinter and the like are solved, the cost and time for manufacturing a traditional process mold are saved, the powder grain size of the mixed raw material is limited, and preparation is made for subsequent cold isostatic pressing and reaction sintering; sintering aid powder is added into the raw material, so that preparation is made for subsequent liquid-phase re-sintering; the density of the ceramic structural member prepared by the method is (2.14-2.6) g/cm3, the bending strength is (151-300) MPa, and the total shrinkage rate of the ceramic structural member is less than 1% after reaction sintering and liquid-phase re-sintering.
Description
[technical field]
The invention belongs to 3D printing fields, and in particular to a kind of Si3N4Ceramic structures and preparation method thereof.
[background technique]
Ceramics have excellent mechanical property, high bending strength, excellent inoxidizability, good corrosion resistance, height
Abrasion resistance and low coefficient of friction, and nitride ceramics are that one kind can be realized the integrated material of structure-function
Material, mechanics, chemistry, electricity, in terms of have excellent performance, in heat resisting structural material field have oxygen
Compound ceramics and the irreplaceable status advantage of cermet, in metallurgy, aviation, chemical industry, ceramics, electronics, machinery and semiconductor
Etc. industries have a wide range of applications.Silicon nitride (Si3N4) is a kind of compound of strong covalent bond, is capable of forming dioxy in air
SiClx protective film has good stability.Silicon nitride material hardness big (HRA is 91~93), decomposition temperature are high, thermal expansion is
Small (2.7 × the 10- of number6/ DEG C (20~1000 DEG C)), thermal conductivity low (9.46W/mK), intensity is high, it is compacted to hardly happen high temperature
Change, antioxygenic property are good, are widely used in high temperature resistant component, the erosion-resistant component in chemical industry, semiconductor of gas engine
The support of crucible material, high-temperature bearing material, dental material, high-speed cutting tool, radome, nuclear reactor in industry
Material, separator and carrier of fissile material etc., and thin silicon nitride film and coating is in high speed memory device and optics wave
The field of leading has been extensively studied.
With the development of industry, these traditional techniques are no longer satisfied the demand of high-tech product.3D printing is quick
Forming technique is a kind of novel forming technology fast-developing in recent years, and the technique can be applicable to main in ceramics molding at present
There are technique Fused Deposition Modeling (FDM), Selective Laser Sintering (SLS) and stereolithography apparatus (SLA) technology, these
The application of technology combines follow-up sintering technique that the molding cycle of ceramic component is greatly shortened, and solving traditional handicraft can not overcome
Design size change or adjustment, by need redesign and manufacture mold；And manufacture that die cost is higher, the period is longer,
A series of problems, such as article shape of preparation is simple.
The molding Si of SLS at present3N4Ceramics are mostly by Si3N4Powder directly carries out printing sintering, raw material preparation cost
Height, because its raw material powder partial size is larger to be unfavorable for following liquid-phase sintering, intensity is lower after printing sintering；There is research to report
Road can realize that the SLS compared with small particle silicon nitride ceramic powder is printed by mist projection granulating or method with plastic film, but it is due to resin content
Higher, contraction distortion is larger, is unfavorable for subsequent members dimension control, because densified sintering product is low, leads to the structural member power of preparation
Performance is poor, and bending strength is lower, and it is even more impossible to apply under high temperature environment.The main reason for consistency is low after it is sintered is Si3N4
For powder after SLS forms degreasing, more carbon residue, Si are contained in inside3N4Powder contraction distortion is big, leads to interior porosity
It is higher, and Si3N4Powder diameter is larger, is unfavorable for liquid-phase sintering, leads to its mechanical properties decrease；Although method with plastic film can reduce examination
Part prints the porosity after degreasing, realizes compared with small particle Si3N4The SLS of powder is printed, but its period is longer, and expense is higher than dry
Mixed method.Therefore a kind of preparation method is needed to prepare high mechanical properties, the high Si of consistency3N4Ceramic structures.
[summary of the invention]
It is an object of the invention to overcome the above-mentioned prior art, a kind of Si is provided3N4Ceramic structures and its preparation
Method；Degreasing reaction-sintered generates silicon nitride after the present invention is printed by Si powder SLS, while introducing in the technique of preparation ceramics
Isostatic cool pressing (CIP) technology improves the consistency of printing rear part, while sintering aid is added in raw material and is reacting
Liquid-phase sintering has been carried out after sintering, is reduced final structure part interior porosity, is improved its mechanical property.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of Si3N4The preparation method of ceramic structures, comprising the following steps:
Step 1, mixing Si powder, sintering aid powder and adhesive powder, obtain uniformly mixed ceramic powders；
Step 2 prints consistent ceramic powder made from step 1 by SLS Method of printing, and ceramic idiosome is made；
Step 3 is set with jacket after cooling down the ceramic body that step 2 obtains or adds protective film in billet surface；It is cold etc.
Static pressure processing is cased with the ceramic body of jacket or protective film, cooling test specimen after isostatic cool pressing, the test specimen after obtaining isostatic cool pressing；
Test specimen degreasing in a nitrogen environment after step 4, the isostatic cool pressing for obtaining step 3, reaction-sintered after degreasing obtain
To sintered Si3N4Ceramic test piece；
Step 5, by sintered Si obtained in step 43N4Ceramic test piece pressurizes liquid-phase sintering in a nitrogen environment, obtains
To the Si of high-compactness3N4Ceramic structures.
A further improvement of the present invention is that:
Preferably, in step 2, in SLS print procedure, slicing delamination is with a thickness of 0.1mm~0.3mm.
Preferably, in step 2, the mass percent of Si powder in mixed-powder are as follows: 65%~80%, the matter of sintering aid powder
Measure percentage are as follows: 8%~20%, the mass percent of adhesive powder is 5%~17%.
Preferably, in step 2, Si powder diameter size is 10~200 μm.
Preferably, in step 2, binder is epoxy resin or phenolic resin, and binder powder partial size is 1~10 μm.
Preferably, in step 2, sintering aid is the mixed of any one or more of aluminium oxide, yttrium oxide or silica
Close object；Sintering aid powder diameter is 1~25 μm.
Preferably, in step 4, isostatic cool pressing pressure is 200~300Mpa, cooling 10~30min of test specimen after isostatic cool pressing.
Preferably, in step 5, skimming temp is 600~900 DEG C, and degreasing time is 60~120min；The reaction-sintered time
For 30~90min, reaction-sintered temperature is 1300~1400 DEG C.
Preferably, in step 6, the temperature for liquid-phase sintering of pressurizeing is 1700~1800 DEG C, and pressure is 0.1~0.2MPa.
Si made from preparation method described in a kind of above-mentioned any one3N4Ceramic structures, the Si3N4Ceramic structures
Density be 2.14~2.6g/cm3, bending strength is 151~300MPa.
One kind Si as made from above-mentioned any one preparation method3N4Ceramic structures, the Si3N4Ceramic structures
Density be 2.14~2.6g/cm3, bending strength is 151~300MPa.
Compared with prior art, the invention has the following advantages:
The invention discloses a kind of Si3N4The indirect SLS preparation method of ceramic structures.This method is indirect SLS preparation
Si3N4Ceramic structures overcome alpha-silicon nitride powders since itself distinctive moisture absorption, the sintering of easy to reunite and micron order are extremely difficult
The problems such as, it is put forward for the first time after mixing Si powder powder, sintering aid and adhesive powder through the SLS technology preparation in 3D printing
Ceramic body out first passes through isostatic cool pressing technical treatment ceramic body, reduces the porosity in ceramic body, improves ceramic body
Consistency；Before isostatic cool pressing, ceramic body is put on into rubber sleeve or adds protective film on surface, rubber sleeve or protective film can
Water or oil during isostatic cool pressing is avoided to enter billet surface；After isostatic cool pressing, the arrangement between ceramic body particle is more
Closely, consistency improves for the first time；The resin in ceramic body can be removed by degreasing, but the porosity of product itself at this time
It is larger, and its aggregate is Si powder；Again by reaction-sintered under nitrogen atmosphere, so that silicon and nitrogen react during the sintering process
Form Si3N4, so that the silicon powder in test specimen is converted into silicon nitride, to realize the generation of silicon nitride, improve test specimen mechanical property；
Si is made by liquid-phase sintering again3N4The consistency of test specimen further increases, and reduces the porosity of test specimen, promotes test specimen mechanics
Performance；This method is for the first time in 3D printing Si3N4When ceramic, using Si powder as adjusting sintering aid and Si powder together of raw material
Grade is matched, and the powder diameter of mixed raw material is limited, and is prepared for subsequent isostatic cool pressing and reaction-sintered, by increasing in the feed
If sintering aid powder, prepare for subsequent liquid phase reheating knot, eliminates cost and the time of mold manufacture；This method is not
It is directly printed alpha-silicon nitride powders as raw material, therefore existing method with plastic film SLS printing silicon nitride can be overcome to be occurred
Degreasing contraction distortion is big and the problem of micron silicon nitride liquid-phase sintering difficulty after printing；By SLS printer directly at
Reaction-sintered generates silicon nitride member after type silicon powder, and step is simple, easily operated, and the personalization for realizing silicon nitride ceramics is fixed
System, shortens its R&D cycle.
The invention also discloses a kind of Si3N4Ceramic structures, the density of the ceramic structures are (2.14-2.6) g/cm3,
Bending strength is (151-300) MPa, and reaction-sintered and the total shrinkage in liquid phase reheating two stages of knot be less than 1%, consistency
Height, mechanical property are good.
[Detailed description of the invention]
Fig. 1 is the structure chart in the present invention after silicon powder printing；
Fig. 2 is the schematic diagram of structural member after being sintered in the present invention；
Fig. 3 is the Si of final high-compactness in the present invention3N4The inside SEM of ceramic structures schemes；
[specific embodiment]
Below with reference to specific steps, the invention will be described in further detail；The invention discloses a kind of Si3N4Ceramic structure
Part and preparation method thereof；The structural member is a kind of Si3N4Ceramic structures, the Si3N4Ceramic structures density be 2.14~
2.6g/cm3, bending strength be 51~300MPa, preparation method specifically includes the following steps:
S1, the threedimensional model for constructing structural member, are converted to STL formatted file for threedimensional model；Pass through magics software point
Layer slicing treatment STL formatted file, obtains lift height and the number of plies, and lift height is 0.1mm~0.3mm, the layering number of plies according to
Actual ceramic structures size determines；It exports as SLC file and imports 3D printer；
S2, Si powder, sintering aid powder and adhesive powder are uniformly mixed by mixing machine, obtain uniformly mixed ceramics
Powder；The mass percent of Si powder in mixed-powder are as follows: 65%~80%, the mass percent of sintering aid powder are as follows: 8%~
20%, the mass percent of adhesive powder is 5%~17%.Binder is epoxy resin or phenolic resin；Si powder diameter
Size is 10~200 μm, and sintering aid powder diameter is 1~25 μm, and binder powder partial size is 1~10 μm, wherein sintering aid
For the mixture of any one or more of aluminium oxide, yttrium oxide and silica, when several mixing, mixed with arbitrary proportion；
In the step, using Si powder as the grain composition for adjusting sintering aid and Si powder together of raw material, the powder of mixed raw material is limited
Partial size and mass fraction are prepared for subsequent isostatic cool pressing and reaction-sintered；
S3, consistent ceramic powder made from step S2 is put into the work box of 3D printer, is printed and is made by laser head
Obtain ceramic body；The operating temperature of work box is 30~70 DEG C, and work gas is nitrogen atmosphere；Laser power is 16~25W, scanning
Speed is 2000~4000mm/s, and the individual-layer data that laser head is obtained according to step 1 in print procedure prints layer by layer from the bottom to top,
Ceramic body is made；
S4, jacket is set with after cooling down the ceramic body that step S3 is obtained or adds protective film in billet surface；It is cold etc. quiet
Pressure processing is cased with the ceramic body of jacket or protective film, and isostatic cool pressing pressure is 200~300Mpa, the examination after obtaining isostatic cool pressing
Part, the ceramic body after isostatic cool pressing cool down 10~30min at room temperature, obtain cooling ceramic body.
S5, the test specimen for obtaining step S4 60~120min of degreasing at 600~900 DEG C, then in a nitrogen environment into
Reaction-sintered after row degreasing, reaction-sintered time are 30~90min, and reaction-sintered temperature is 1300~1400 DEG C, after sintering
To Si3N4Ceramic test piece.
S6, test specimen obtained in step S5 is put into gas pressure sintering furnace pressurization progress liquid-phase sintering in a nitrogen environment,
Liquid phase sintering conditions are 1700-1800 DEG C, and pressure 0.1-0.2MPa obtains the Si of high-compactness3N4Ceramic structures.
The ceramic structures obtained through the above steps, density 2.14-2.6g/cm3, bending strength is (151-300)
MPa, and reaction-sintered and the sintered shrinking percentage of liquid phase weight be less than 1%, during the preparation process, ceramic structures when reaction-sintered
Expansion, when liquid-phase sintering, shrink, and the total recovery after cancelling out each other is less than 1%.
Embodiment 1
S1, the threedimensional model for constructing structural member, are converted to STL formatted file for threedimensional model；Pass through magics software point
Layer slicing treatment STL formatted file, obtains lift height and the number of plies, lift height 0.15mm；It exports as SLC file and imports
3D printer；
S2, Si powder, alumina powder and epoxy powder are uniformly mixed by mixing machine, obtain uniformly mixed ceramics
Powder；The mass percent of Si powder in mixed-powder are as follows: 70%, the quality hundred of aluminium oxide, yttrium oxide, silica hybrid powder
Divide accounting are as follows: 15% (wherein, aluminium oxide: yttrium oxide: silica=5%:3.5%:6.5%), the matter of epoxy powder
Measuring percentage is 15%.
S3, consistent ceramic powder made from step S2 is put into the work box of 3D printer, is printed and is made by laser head
Obtain ceramic body；The operating temperature of work box is 50 DEG C, and work gas is nitrogen atmosphere；Laser power is 20W, and scanning speed is
3000mm/s, the individual-layer data that laser head is obtained according to step 1 in print procedure print layer by layer from the bottom to top, and ceramic blank is made
Body；
S4, jacket is set with after cooling down the ceramic body that step S3 is obtained or adds protective film in billet surface；It is cold etc. quiet
Pressure processing is cased with the ceramic body of jacket or protective film, and isostatic cool pressing pressure is 250Mpa, and the test specimen after obtaining isostatic cool pressing is cold
Ceramic body after equal static pressure cools down 20min at room temperature, obtains cooling ceramic body.
S5, the test specimen for obtaining step S4 degreasing 80min at 800 DEG C are then anti-after progress degreasing in a nitrogen environment
It should be sintered, the reaction-sintered time is 70min, and reaction-sintered temperature is 1400 DEG C, and Si is obtained after sintering3N4Ceramic test piece.
S6, test specimen obtained in step S5 is put into gas pressure sintering furnace pressurization progress liquid-phase sintering in a nitrogen environment,
Liquid phase sintering conditions are 1800 DEG C, and pressure 0.0.2MPa obtains the Si of high-compactness3N4Ceramic structures.
The ceramic structures obtained through the above steps, density 2.6g/cm3, bending strength 300MPa.
Fig. 1 is the photo after the ceramic body that step S3 is obtained in this implementation after silicon powder printing；Fig. 2 is in the present embodiment
Final step S6 obtains the photo figure of structural member, and the main aggregate that comparison diagram 1 and Fig. 2 can be seen that silicon powder after printing is silicon powder,
So that entire ceramic body is in black, the reaction of later period internal chemical is sintered to it and generates silicon nitride and a small amount of silicon oxynitride, is made
It is partially white to obtain entire green body color, it is partially grey.
Fig. 3 is the SEM figure inside final sample, as can be seen from the figure sample internal comparatively dense, powder after sintering
By being combined together for sintered compact, but inside, still with the presence of a small amount of hole, these holes can increase silicon nitride ceramics
Wave, so that it is had better application prospect.
See Table 2 for details for the detailed process parameter of embodiment 2- embodiment 5.
The procedure parameter of 2 embodiment 2- embodiment 5 of table
See Table 3 for details for the procedure parameter of embodiment 6- embodiment 9.
The procedure parameter of 3 embodiment 6-9 of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of Si3N4The preparation method of ceramic structures, which comprises the following steps:
Step 1, mixing Si powder, sintering aid powder and adhesive powder, obtain uniformly mixed ceramic powders；
Step 2 prints consistent ceramic powder made from step 1 by SLS Method of printing, and ceramic idiosome is made；
Step 3 is set with jacket after cooling down the ceramic body that step 2 obtains or adds protective film in billet surface；Isostatic cool pressing
Processing is cased with the ceramic body of jacket or protective film, cooling test specimen after isostatic cool pressing, the test specimen after obtaining isostatic cool pressing；
Test specimen degreasing in a nitrogen environment after step 4, the isostatic cool pressing for obtaining step 3, reaction-sintered after degreasing are burnt
Si after knot3N4Ceramic test piece；
Step 5, by sintered Si obtained in step 43N4Ceramic test piece pressurizes liquid-phase sintering in a nitrogen environment, obtains height
The Si of consistency3N4Ceramic structures.
2. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 2, SLS
In print procedure, slicing delamination is with a thickness of 0.1mm~0.3mm.
3. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 2, mixing
The mass percent of Si powder in powder are as follows: 65%~80%, the mass percent of sintering aid powder are as follows: 8%~20%, binder
The mass percent of powder is 5%~17%.
4. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 2, Si powder
Last particle size is 10~200 μm.
5. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 2, bonding
Agent is epoxy resin or phenolic resin, and binder powder partial size is 1~10 μm.
6. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 2, sintering
Auxiliary agent is the mixture of any one or more of aluminium oxide, yttrium oxide or silica；Sintering aid powder diameter is 1~25 μ
m。
7. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that cold etc. in step 4
Static pressure pressure is 200~300Mpa, cooling 10~30min of test specimen after isostatic cool pressing.
8. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 5, degreasing
Temperature is 600~900 DEG C, and degreasing time is 60~120min；The reaction-sintered time is 30~90min, and reaction-sintered temperature is
1300~1400 DEG C.
9. a kind of Si according to claim 13N4The preparation method of ceramic structures, which is characterized in that in step 6, pressurization
The temperature of liquid-phase sintering is 1700~1800 DEG C, and pressure is 0.1~0.2MPa.
10. Si made from a kind of preparation method as described in claim 1-9 any one3N4Ceramic structures, feature exist
In the Si3N4The density of ceramic structures is 2.14~2.6g/cm3, bending strength is 151~300MPa.
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| CN111203535A (en) * | 2020-01-13 | 2020-05-29 | 无锡英特派金属制品有限公司 | Method for preparing iridium crucible by adopting 3D printing technology |
| CN113105247A (en) * | 2021-03-25 | 2021-07-13 | 威海圆环先进陶瓷股份有限公司 | Preparation method of silicon nitride ceramic tooth |
| CN113182514A (en) * | 2021-03-31 | 2021-07-30 | 北京科技大学 | TiAl alloy ceramic welding part and integral forming preparation method thereof |
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| CN111203535A (en) * | 2020-01-13 | 2020-05-29 | 无锡英特派金属制品有限公司 | Method for preparing iridium crucible by adopting 3D printing technology |
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| CN116041051A (en) * | 2023-01-16 | 2023-05-02 | 广东工业大学 | Granulating powder applied to 3DP printing and printing forming method thereof |
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| CN116606149A (en) * | 2023-05-22 | 2023-08-18 | 西北工业大学 | High-strength high-purity silicon nitride crucible, and preparation method and application thereof |
| CN116813354A (en) * | 2023-06-06 | 2023-09-29 | 东莞理工学院 | Method for preparing silicon nitride ceramic in situ, prepared silicon nitride ceramic and application thereof |
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