CN109467438A - A kind of silicon carbide ceramics Stereolithography method - Google Patents
A kind of silicon carbide ceramics Stereolithography method Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 55
- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 6
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- ZDHCZVWCTKTBRY-UHFFFAOYSA-N omega-Hydroxydodecanoic acid Natural products OCCCCCCCCCCCC(O)=O ZDHCZVWCTKTBRY-UHFFFAOYSA-N 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 2
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 2
- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000000197 pyrolysis Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 238000000465 moulding Methods 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000000016 photochemical curing Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Abstract
The present invention relates to a kind of silicon carbide ceramics Stereolithography methods, belong to silicon carbide ceramics forming field.Forming method of the invention obtains finely dispersed SiC slurry first by SiC ceramic powder, photosensitive resin, photoinitiator mixing and ball milling；Then SiC ceramic green compact are printed as using Stereolithography equipment；Using making SiC ceramic green compact be transformed into C/SiC green body after pyrolysis；Again by high temperature siliconising, so that the C in Si and C/SiC green body is carried out reaction in-situ and generate SiC.Forming method of the invention realizes the Stereolithography preparation of silicon carbide ceramics.
Description
Technical field
The present invention relates to a kind of silicon carbide ceramics Stereolithography methods, belong to silicon carbide ceramics forming field.
Background technique
Silicon carbide due to stable chemical performance, thermal coefficient is high, thermal expansion coefficient is small, wear-resisting property is good, intensity is high,
The advantages that hardness is big, therefore application is very extensive.Silicon carbide mainly has four big application fields, it may be assumed that function ceramics, advanced fire proofed wood
Material, abrasive material and metallurgical raw material.However, therefore, it is difficult to machine-shapings due to the performances such as silicon carbide ceramics quality is crisp, hardness is big.It passes
System silicon carbide ceramics forming method mainly has compression moulding and two kinds of colloidal formation.Conventional method prepares silicon carbide and lacks there are following
Point: precision is low, is difficult to prepare complex-shaped product, is essential and wants mold and corresponding process tool, leads to preparation cost height.Tradition
The deficiency of molding silicon carbide ceramics method causes its use to be restricted.Therefore need to develop a kind of novel silicon carbide molding side
Method, to make up the deficiency of traditional molding methods.
Summary of the invention
The purpose of the invention is to realize that silicon carbide ceramics quickly prepares the requirement of high-precision, finished pieces with complex shapes, and
One-pass molding is not necessarily to following process, and the invention proposes a kind of silicon carbide ceramics Stereolithography methods.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of silicon carbide ceramics Stereolithography method of the invention, specific forming step are as follows:
1) by SiC ceramic powder (25vol~40vol%), photosensitive resin (55vol~70vol%), photoinitiator
(2wt%~5wt%) mixing is added in ball grinder, 2~10h of ball milling under 300~400r/min of revolving speed on planetary ball mill,
Then dispersing agent (1wt%~5wt%) 1~2h of ball milling again is added, obtains finely dispersed SiC slurry；
2) SiC slurry that step 1) obtains is printed as SiC ceramic green compact using Stereolithography equipment；
3) the SiC ceramic green compact for obtaining step 2) are heated to 200 DEG C from room temperature with the heating rate of 3~5 DEG C/min,
Again with the heating rate of 5 DEG C/min, 500 DEG C are heated to from 200 DEG C, then with the heating rate of 10 DEG C/min, is heated from 500 DEG C
To 1200~1300 DEG C, cools to room temperature with the furnace, C/SiC green body is obtained after taking-up；
4) the C/SiC green body that step 3) obtains is put into graphite crucible, and is embedded with Si powder, be subsequently placed in vacuum sintering furnace
Middle carry out reaction-sintered, heating rate: 10 DEG C/min, sintering temperature: 1500~1600 DEG C, soaking time: 1~2h；It is cold with furnace
But to room temperature, the SiC ceramic product taken out；
The photosensitive resin is 1,6- hexylene glycol double methacrylate (HDDA)；
The photoinitiator is 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO)；
The dispersing agent is solsperse 17000.
Beneficial effect
The present invention realizes the Stereolithography preparation of silicon carbide ceramics, provides centainly for the photocuring preparation of coloured ceramics
It uses for reference.It is handled by infiltration pyrolysis, finally obtained silicon carbide product relative density can achieve 80% or more, bending strength
It can achieve 100MPa or more.
The preparation process of silicon carbide is different from conventional molding process in the present invention, it is advantageous that shaping speed is fast, very little essence
Degree is high, can prepare extremely complex shape product.A kind of new thinking is provided for silicon carbide ceramics rapid prototyping and small lot production,
Mould development step can be saved.
This technique can prepare high-precision, complex-shaped, without following process silicon carbide ceramics product.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the SiC green compact SEM figure that example 1 obtains；
Fig. 3 is the SEM figure for the final product that example 1 obtains.
Specific embodiment
The contents of the present invention are further described with reference to the accompanying drawings and examples.
Embodiment 1
A kind of silicon carbide ceramics Stereolithography method of the invention, process flow chart is as shown in Figure 1, specific forming step
It is as follows:
1) firstly, 30ml slurry is prepared, by SiC ceramic powder 28.9g, photosensitive resin (HDDA, 21.2g), photoinitiator
(TPO, 0.58g) mixing is added in ball grinder, then dispersion is added in the ball milling 2h under revolving speed 400r/min on planetary ball mill
Agent (17000,0.29g) ball milling 2h again.Finally obtain finely dispersed SiC slurry.Slurry viscosity is lower than 3pa.s.
2) SiC slurry that step 1) obtains is printed as SiC ceramic green compact, SEM figure such as Fig. 2 using Stereolithography equipment
It is shown；
3) the silicon carbide ceramics green compact that photocuring obtains are placed in graphite crucible, put into vacuum sintering furnace and is pyrolyzed
Carbonization.Heating rate: room temperature~200 DEG C: 3 DEG C/min；200~500:5 DEG C/min；500~1200:10 DEG C/min；1200℃
Heat preservation 2 hours；Then it cools to room temperature with the furnace, obtains C/SiC green body；
4) C/SiC green body is placed in graphite crucible, and is embedded with Si powder, graphite crucible is then placed in vacuum sintering furnace
Middle progress reaction in-situ sintering.Heating rate: room temperature~200 DEG C: 3 DEG C/min；200~1600:10 DEG C/min；Holding temperature:
1600℃；Soaking time: 1h；Then it cools to room temperature with the furnace, takes out product, SEM figure is as shown in Figure 3；
Clear up product after, handled by infiltration pyrolysis, the relative density of obtained SiC product can achieve 80% with
On, bending strength is 100MPa or more.
Embodiment 2
Except following step difference, other preparation steps are same as Example 1: in step 1, SiC ceramic powder (33.7g),
Photosensitive resin (HDDA, 19.7g), photoinitiator (TPO, 0.39g) mixing are added in ball grinder, the revolving speed on planetary ball mill
Then 400r/min, ball milling 2h are added dispersing agent (17000,0.34g), are further continued for ball milling 2h.It finally obtains finely dispersed
SiC slurry.Viscosity is lower than 3pa.s.Compared with Example 1, obtained SiC product relative density and bending strength be
It improves.
Embodiment 3
Except following step difference, other preparation steps are same as Example 1: in step 1, SiC ceramic powder (38.4g),
Photosensitive resin (HDDA, 18.2g), photoinitiator (TPO, 0.36g) mixing are added in ball grinder, the revolving speed on planetary ball mill
Then 400r/min, ball milling 2h are added dispersing agent (17000,0.38g), are further continued for ball milling 2h.It finally obtains finely dispersed
SiC slurry.Viscosity is lower than 3pa.s.Compared with Examples 1 and 2, the SiC relative density and bending strength that embodiment 3 obtains are equal
It increases.
Embodiment 4
Except following step difference, other preparation steps are same as Example 1: step 4, when keeping the temperature at 1600 DEG C of reaction-sintered
Between be 2h.Compared with Example 1, increase soaking time, siliconising reaction is more complete, and obtained SiC sample relative density has
Increased.
Claims (1)
1. a kind of silicon carbide ceramics Stereolithography method, it is characterised in that specific forming step is as follows:
1) by SiC ceramic powder (25vol~40vol%), photosensitive resin (55vol~70vol%), photoinitiator (2wt%~
5wt%) mixing is added in ball grinder, and 2~10h of ball milling under 300~400r/min of revolving speed, is then added on planetary ball mill
Dispersing agent (1wt%~5wt%) 1~2h of ball milling again, obtains finely dispersed SiC slurry；
2) SiC slurry that step 1) obtains is printed as SiC ceramic green compact using Stereolithography equipment；
3) the SiC ceramic green compact for obtaining step 2) are heated to 200 DEG C from room temperature with the heating rate of 3~5 DEG C/min, then with 5
DEG C/heating rate of min, 500 DEG C are heated to from 200 DEG C, then with the heating rate of 10 DEG C/min, is heated to from 500 DEG C
It 1200~1300 DEG C, cools to room temperature with the furnace, C/SiC green body is obtained after taking-up；
4) the C/SiC green body that step 3) obtains is put into graphite crucible, and is embedded with Si powder, be subsequently placed in vacuum sintering furnace into
Row reaction-sintered, heating rate: 10 DEG C/min, sintering temperature: 1500~1600 DEG C, soaking time: 1~2h；It cools to the furnace
Room temperature, the SiC ceramic product taken out；
The photosensitive resin is 1,6- hexylene glycol double methacrylate (HDDA)；
The photoinitiator is 2,4,6- trimethylbenzoy-dipheny phosphine oxide (TPO)；
The dispersing agent is solsperse 17000.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171976A (en) * | 2019-05-27 | 2019-08-27 | 华中科技大学 | The preparation method and product of SiC base ceramic part based on increasing material manufacturing |
| CN110922190A (en) * | 2019-12-12 | 2020-03-27 | 北京理工大学 | Digital light processing additive manufacturing method of silicon carbide ceramic space reflector |
| CN111116205A (en) * | 2019-12-30 | 2020-05-08 | 中国建筑材料科学研究总院有限公司 | Photosensitive resin-based carbon source/silicon carbide ceramic slurry, method for preparing porous carbon/silicon carbide blank, structural member and preparation method |
| CN112047737A (en) * | 2020-07-23 | 2020-12-08 | 西安交通大学 | Infiltration method for silicon carbide-based ceramic with microstructure characteristics |
| CN112171848A (en) * | 2020-09-29 | 2021-01-05 | 江西金石三维智能制造科技有限公司 | Photocuring silicon carbide ceramic slurry and preparation method and application thereof |
| CN113735590A (en) * | 2021-09-29 | 2021-12-03 | 北京理工大学 | Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material |
| CN114478049A (en) * | 2020-11-13 | 2022-05-13 | 西安增材制造国家研究院有限公司 | High-thickness high-strength photocuring silicon nitride ceramic and preparation method thereof |
| CN115215661A (en) * | 2021-04-15 | 2022-10-21 | 南京航空航天大学 | Photocuring 3D printing silicon carbide ceramic part and near-net-shape forming preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110171976A (en) * | 2019-05-27 | 2019-08-27 | 华中科技大学 | The preparation method and product of SiC base ceramic part based on increasing material manufacturing |
| CN110922190A (en) * | 2019-12-12 | 2020-03-27 | 北京理工大学 | Digital light processing additive manufacturing method of silicon carbide ceramic space reflector |
| CN110922190B (en) * | 2019-12-12 | 2021-10-19 | 北京理工大学 | Digital light processing additive manufacturing method of silicon carbide ceramic space reflector |
| CN111116205A (en) * | 2019-12-30 | 2020-05-08 | 中国建筑材料科学研究总院有限公司 | Photosensitive resin-based carbon source/silicon carbide ceramic slurry, method for preparing porous carbon/silicon carbide blank, structural member and preparation method |
| CN112047737A (en) * | 2020-07-23 | 2020-12-08 | 西安交通大学 | Infiltration method for silicon carbide-based ceramic with microstructure characteristics |
| CN112047737B (en) * | 2020-07-23 | 2021-07-13 | 西安交通大学 | Infiltration method for silicon carbide-based ceramic with microstructure characteristics |
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| CN114478049A (en) * | 2020-11-13 | 2022-05-13 | 西安增材制造国家研究院有限公司 | High-thickness high-strength photocuring silicon nitride ceramic and preparation method thereof |
| CN115215661A (en) * | 2021-04-15 | 2022-10-21 | 南京航空航天大学 | Photocuring 3D printing silicon carbide ceramic part and near-net-shape forming preparation method thereof |
| CN113735590A (en) * | 2021-09-29 | 2021-12-03 | 北京理工大学 | Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material |
| CN113735590B (en) * | 2021-09-29 | 2022-06-28 | 北京理工大学 | Preparation method and product of high-temperature-resistant electromagnetic wave-absorbing ceramic matrix composite material |
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