CN107880490B - A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing - Google Patents
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- 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
- B33Y10/00—Processes of additive manufacturing
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- 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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Abstract
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing, the present invention relates to 4D printing technique fields.The technical issues of being confined to thermoplastic resin material and photocuring thermoset resin material the invention solves current 3D printing and 4D printing.Method: one, each component is weighed；Two, it mixes, centrifugally operated, then de-bubble；Three, chopped carbon fiber, mechanical stirring is added.The method of 4D printing: composite material is packed into the propeller socket of printer, is successively printed using computer model；Then, product solidification is taken out.Preparation process of the present invention is simple, operates and is easy product intensity height, the structural member deflection printed is big, and recovery of shape speed is fast.Composite material prepared by the present invention prints field for 4D.
Description
Technical field
The present invention relates to 4D printing technique fields.
Background technique
The Si Kailadibici of Massachusetts Institute Technology is complete by one in California, USA TED conference within 2013
Whole experiment illustrates 4D printing technique to participant.4D printing is to increase time dimension on the basis of traditional 3D printing
Degree, the structural member printed by 3D printer can occur change in shape with the time, realize that complicated shape is integrally melted into
Type.The key of 4D printing is that printed material is a kind of intellectual material, can be actively according to presetting under the conditions of dynamic excitation
Path occur change in shape.
Printing technique be it is a kind of designed a model based on Computerized three-dimensional, by the way that software hierarchy is discrete and numerical control molding system,
The special materials such as polymer, metal, inorganic matter are subjected to layer-by-layer accumulation molding, produce the emerging technology of physical product.Although
4D printing technique receives the extensive concern of various fields, but at present there are still many problems, especially printing shape memory is poly-
Close object and its composite material.4D prints shape-memory polymer and leads in biomedicine, aerospace, robot, automobile, electronics etc.
Domain has potential application prospect.Currently, mainly passing through the printing type of fusion sediment and solvent direct write in field of biomedicine
Realize the printing shaping of thermoplastic material.Due to the application limitation in fields such as aerospace, automobiles of thermoplastic material, research
The printing of thermosetting polymer has very important significance, and specifically promotes to make to the progress of intellectual material and manufacturing process
With.
Summary of the invention
The invention solves current 3D printings and 4D printing to be confined to thermoplastic resin material and photocuring thermosetting property tree
The technical issues of rouge material, and provide it is a kind of suitable for 4D printing thermosetting epoxy resin based composites preparation method and
The method for carrying out 4D printing.
It is a kind of suitable for 4D printing thermosetting epoxy resin based composites preparation method, specifically according to the following steps into
Row:
One, 65~75 parts of epoxy resin, 15~20 parts of low temperature curing agents, 1~3 part of carbon Nanowire are weighed according to mass fraction
Dimension, 5~15 parts of thickening fillers and 2~4 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
The method that a kind of thermosetting epoxy resin based composites suitable for 4D printing carry out 4D printing, is specifically pressed
Following steps carry out:
A kind of thermosetting epoxy resin based composites suitable for 4D printing of above-mentioned preparation are packed into pushing away for printer
Into in device socket, successively printed using computer model；Then, take out product temperature be 100~130 DEG C under the conditions of into
Row solidification, curing time are 3~5h；The syringe needle internal diameter of the printer is 0.8~1.5mm, and print speed is 0.1~5.0mm/
s。
The beneficial effects of the present invention are: the present invention is prepared for a kind of thermoset epoxy base shape memory suitable for 4D printing
Composite printing material, and provide a kind of printing technology of 4D printing thermosetting material.It is special compared with thermoplastic material printing
Point is that preparation process is simple, and operation is easy, and product intensity is high, and the structural member deflection printed is big, and recovery of shape speed is fast
Deng.
Composite material prepared by the present invention prints field for 4D.
Detailed description of the invention
Fig. 1 is the optical microscopy structure chart of chopped carbon fiber described in embodiment one；
Fig. 2 is the shape of product Recovery Process figure (a-b-c-d-e-f) that embodiment one prints.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.
Specific embodiment 1: a kind of thermosetting epoxy resin based composites system suitable for 4D printing of present embodiment
Preparation Method specifically sequentially includes the following steps:
One, 65~75 parts of epoxy resin, 15~20 parts of low temperature curing agents, 1~3 part of carbon Nanowire are weighed according to mass fraction
Dimension, 5~15 parts of thickening fillers and 2~4 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: asphalt mixtures modified by epoxy resin described in step 1
Rouge is one of bisphenol A type epoxy resin, propanepoxy resin, phenolic aldehyde multi-epoxy resin and glycerol epoxy resin
Or several combinations.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: it is low described in step 1
Warm curing agent is the combination of one or more of polyamide, polyetheramine, fatty amine, aliphatic cyclic amine and aromatic amine.Other and specific reality
It is identical to apply mode one or two.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 1
The fibre length for stating carbon nano-fiber is 5-50 μm.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 1
Stating thickening filler is the combination of one or more of bentonite, kaolin, montmorillonite, bauxite and dextrin.Other and specific reality
It is identical to apply one of mode one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: in step 1 from
Heart operation is that control centrifugation rate is 500~2000 revs/min, and centrifugation time is 5~10min.Other and specific embodiment
One of one to five is identical.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: being removed in step 1
Bubble condition is that control centrifugation rate is 1000~3000 revs/min, and centrifugation time is 10~20min.Other and specific embodiment party
One of formula one to six is identical.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: institute in step 1
The fibre length for stating root chopped carbon fiber is 1~8mm.It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: machine in step 3
Tool speed of agitator is 100 revs/min, time 2min.It is other identical as one of specific embodiment one to eight.
Specific embodiment 10: a kind of thermosetting epoxy resin base suitable for 4D printing described in specific embodiment one is multiple
The method that condensation material carries out 4D printing, specifically sequentially includes the following steps:
A kind of thermosetting epoxy resin based composites suitable for 4D printing prepared by specific embodiment one are packed into
In the propeller socket of printer, successively printed using computer model；Then, taking out product in temperature is 100~130
Solidified under the conditions of DEG C, curing time is 3~5h；The syringe needle internal diameter of the printer is 0.8~1.5mm, and print speed is
0.1~5.0mm/s.
Using following embodiment verifying beneficial effects of the present invention:
Embodiment one:
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing of the present embodiment, specifically by following
Step carries out:
One, 65 parts of epoxy resin, 20 parts of low temperature curing agents, 3 parts of carbon nano-fibers, 8 parts of thickenings are weighed according to mass fraction
Filler and 4 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
Wherein, epoxy resin described in step 1 is bisphenol A type epoxy resin.
Low temperature curing agent described in step 1 is polyetheramine.
The fibre length of carbon nano-fiber described in step 1 is 5.0-50.0 μm.
Thickening filler described in step 1 is bentonite.
It is 1000 revs/min that centrifugally operated, which is control centrifugation rate, in step 1, centrifugation time 10min.
It is 2000 revs/min that de-bubble condition, which is control centrifugation rate, in step 1, centrifugation time 20min.
The fibre length of root chopped carbon fiber described in step 1 is 1.0~8.0mm.
Mechanical stirring revolving speed is 100 revs/min in step 3, time 2min.
A kind of thermosetting epoxy resin based composites suitable for 4D printing of preparation are packed into the propeller of printer
In socket, successively printed using computer model；Then, product is taken out to be solidified under the conditions of temperature is 120 DEG C, Gu
The change time is 3h；The syringe needle internal diameter of the printer is 1.5mm, print speed 2.0mm/s.
The product that the present embodiment is obtained carries out recovery of shape test under the conditions of temperature is 180 DEG C, is returned in 10s just
Beginning shape.
The optical microscopy structure chart of chopped carbon fiber described in the present embodiment is as shown in Figure 1；
The shape of product Recovery Process figure (a-b-c-d-e-f) of the present embodiment printing is as shown in Fig. 2, wherein f is structure
Permanent shape, a are the temporary shapes of structure.It is about from the time that temporary shapes are returned to permanent shape as seen from Figure 2
10.0s。
Embodiment two:
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing of the present embodiment, specifically by following
Step carries out:
One, 68 parts of epoxy resin, 17 parts of low temperature curing agents, 2 parts of carbon nano-fibers, 10 parts of thickenings are weighed according to mass fraction
Filler and 3 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
Wherein, epoxy resin described in step 1 is bisphenol A type epoxy resin.
Low temperature curing agent described in step 1 is polyamide.
The fibre length of carbon nano-fiber described in step 1 is 5.0-50.0 μm.
Thickening filler described in step 1 is montmorillonite.
It is 2000 revs/min that centrifugally operated, which is control centrifugation rate, in step 1, centrifugation time 5min.
It is 2000 revs/min that de-bubble condition, which is control centrifugation rate, in step 1, centrifugation time 10min.
The fibre length of root chopped carbon fiber described in step 1 is 1.0~8.0mm.
Mechanical stirring revolving speed is 100 revs/min in step 3, time 2min.
A kind of thermosetting epoxy resin based composites suitable for 4D printing of preparation are packed into the propeller of printer
In socket, successively printed using computer model；Then, product is taken out to be solidified under the conditions of temperature is 100 DEG C, Gu
The change time is 5h；The syringe needle internal diameter of the printer is 1.0mm, print speed 1.0mm/s.
The product that the present embodiment is obtained carries out recovery of shape test under the conditions of temperature is 180 DEG C, is returned in 20s just
Beginning shape.
Embodiment three:
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing of the present embodiment, specifically by following
Step carries out:
One, 70 parts of epoxy resin, 18 parts of low temperature curing agents, 2 parts of carbon nano-fibers, 8 parts of thickenings are weighed according to mass fraction
Filler and 2 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
Wherein, epoxy resin described in step 1 is that bisphenol A type epoxy resin and propanepoxy resin press quality
Than being combined for 8: 2.
Low temperature curing agent described in step 1 is polyetheramine.
The fibre length of carbon nano-fiber described in step 1 is 5.0-50.0 μm.
Thickening filler described in step 1 is dextrin.
It is 2000 revs/min that centrifugally operated, which is control centrifugation rate, in step 1, centrifugation time 5min.
It is 2000 revs/min that de-bubble condition, which is control centrifugation rate, in step 1, centrifugation time 10min.
The fibre length of root chopped carbon fiber described in step 1 is 1.0~8.0mm.
Mechanical stirring revolving speed is 100 revs/min in step 3, time 2min.
A kind of thermosetting epoxy resin based composites suitable for 4D printing of preparation are packed into the propeller of printer
In socket, successively printed using computer model；Then, product is taken out to be solidified under the conditions of temperature is 120 DEG C, Gu
The change time is 3h；The syringe needle internal diameter of the printer is 1.5mm, print speed 1.0mm/s.
The product that the present embodiment is obtained carries out recovery of shape test under the conditions of temperature is 120 DEG C, is returned in 50s just
Beginning shape.
Example IV:
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing of the present embodiment, specifically by following
Step carries out:
One, 72 parts of epoxy resin, 18 parts of low temperature curing agents, 2 parts of carbon nano-fibers, 6 parts of thickenings are weighed according to mass fraction
Filler and 2 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
Wherein, epoxy resin described in step 1 is phenolic aldehyde multi-epoxy resin.
Low temperature curing agent described in step 1 is that aliphatic cyclic amine and aromatic amine are 1: 1 combination in mass ratio.
The fibre length of carbon nano-fiber described in step 1 is 5.0-50.0 μm.
Thickening filler described in step 1 is that bentonite and kaolin are 1: 1 mixing in mass ratio.
It is 1000 revs/min that centrifugally operated, which is control centrifugation rate, in step 1, centrifugation time 10min.
It is 2000 revs/min that de-bubble condition, which is control centrifugation rate, in step 1, centrifugation time 10min.
The fibre length of root chopped carbon fiber described in step 1 is 1.0~8.0mm.
Mechanical stirring revolving speed is 100 revs/min in step 3, time 2min.
A kind of thermosetting epoxy resin based composites suitable for 4D printing of preparation are packed into the propeller of printer
In socket, successively printed using computer model；Then, product is taken out to be solidified under the conditions of temperature is 120 DEG C, Gu
The change time is 3h；The syringe needle internal diameter of the printer is 1.2mm, print speed 5.0mm/s.
The product that the present embodiment is obtained carries out recovery of shape test under the conditions of temperature is 150 DEG C, is returned in 20s just
Beginning shape.
Embodiment five:
A kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing of the present embodiment, specifically by following
Step carries out:
One, 75 parts of epoxy resin, 15 parts of low temperature curing agents, 3 parts of carbon nano-fibers, 5 parts of thickenings are weighed according to mass fraction
Filler and 2 parts of chopped carbon fibers；
Two, by the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler mix, carry out from
Heart operation, then de-bubble obtain uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out
Mechanical stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing.
Wherein, epoxy resin described in step 1 is bisphenol A type epoxy resin and glycerol epoxy resin is 8 in mass ratio
: 2 combinations.
Low temperature curing agent described in step 1 is polyetheramine.
The fibre length of carbon nano-fiber described in step 1 is 5-50 μm.
Thickening filler described in step 1 is that bentonite and dextrin are 1: 1 combination in mass ratio.
It is 1000 revs/min that centrifugally operated, which is control centrifugation rate, in step 1, centrifugation time 10min.
It is 3000 revs/min that de-bubble condition, which is control centrifugation rate, in step 1, centrifugation time 10min.
The fibre length of root chopped carbon fiber described in step 1 is 1.0~8.0mm.
Mechanical stirring revolving speed is 100 revs/min in step 3, time 2min.
A kind of thermosetting epoxy resin based composites suitable for 4D printing of preparation are packed into the propeller of printer
In socket, successively printed using computer model；Then, product is taken out to be solidified under the conditions of temperature is 130 DEG C, Gu
The change time is 3h；The syringe needle internal diameter of the printer is 1.5mm, print speed 5.0mm/s.
The product that the present embodiment is obtained carries out recovery of shape test under the conditions of temperature is 150 DEG C, is returned in 20s just
Beginning shape.
Claims (6)
1. a kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing, it is characterised in that this method is specific
It sequentially includes the following steps:
One, 65 ~ 75 parts of epoxy resin, 15 ~ 20 parts of low temperature curing agents, 1 ~ 3 part of carbon nano-fiber, 5 ~ 15 are weighed according to mass fraction
Part thickening filler and 2 ~ 4 parts of chopped carbon fibers；
Two, the weighed epoxy resin of step 1, low temperature curing agent, carbon nano-fiber and thickening filler are mixed, carries out centrifugation behaviour
Make, then de-bubble obtains uniform epoxy resin composite material；
Three, the weighed chopped carbon fiber of step 1 is added in the epoxy resin composite material that step 2 obtains, is carried out mechanical
Stirring obtains the thermosetting epoxy resin based composites for being suitable for 4D printing；Wherein carbon nano-fiber in step 1
Fibre length be 5-50 μm；The fibre length of chopped carbon fiber is 1 ~ 8mm；Thickening filler is bentonite, kaolin, illiteracy take off
The combination of one or more of soil, bauxite and dextrin；
Wherein using the method that the thermosetting epoxy resin based composites of step 3 preparation carry out 4D printing: by thermoset epoxy
Polymer matrix composites are packed into the propeller socket of printer, are successively printed using computer model；Then, it takes out and produces
Product are solidified under the conditions of temperature is 100 ~ 130 DEG C, and curing time is 3 ~ 5h；The syringe needle internal diameter of the printer be 0.8 ~
1.5mm, print speed are 0.1 ~ 5.0mm/s.
2. a kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing according to claim 1,
It is characterized in that epoxy resin described in step 1 is bisphenol A type epoxy resin, phenolic aldehyde multi-epoxy resin and glycerol epoxy tree
The combination of one or more of rouge.
3. a kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing according to claim 1,
It is characterized in that low temperature curing agent described in step 1 is one of polyamide, polyetheramine, fatty amine, aliphatic cyclic amine and aromatic amine
Or several combinations.
4. a kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing according to claim 1,
It is characterized in that it is 500 ~ 2000 revs/min that centrifugally operated, which is control centrifugation rate, in step 2, centrifugation time is 5 ~ 10min.
5. a kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing according to claim 1,
It is characterized in that in step 2 de-bubble condition be control centrifugation rate be 1000 ~ 3000 revs/min, centrifugation time be 10 ~
20min。
6. a kind of thermosetting epoxy resin based composites preparation method suitable for 4D printing according to claim 1,
It is characterized in that mechanical stirring revolving speed is 100 revs/min in step 3, time 2min.
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| CN112980143A (en) * | 2021-02-10 | 2021-06-18 | 上海东杰高分子材料有限公司 | Composition and material for 3D printing and preparation and printing methods thereof |
| CN113881279A (en) * | 2021-11-03 | 2022-01-04 | 中国科学院兰州化学物理研究所 | 3D printing shape memory epoxy resin ink, preparation method and application thereof, and 3D printing epoxy resin |
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| US9222007B2 (en) * | 2012-09-13 | 2015-12-29 | GM Global Technology Operations LLC | Shape memory polymer which functions as a dry adhesive clamp and methods of making and using the same |
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