CN107033294A - It is a kind of for conductive UV-cured resin composite of laser 3D printing and preparation method thereof - Google Patents
It is a kind of for conductive UV-cured resin composite of laser 3D printing and preparation method thereof Download PDFInfo
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- CN107033294A CN107033294A CN201710267430.3A CN201710267430A CN107033294A CN 107033294 A CN107033294 A CN 107033294A CN 201710267430 A CN201710267430 A CN 201710267430A CN 107033294 A CN107033294 A CN 107033294A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of for conductive UV-cured resin composite of laser 3D printing and preparation method thereof, the composite is made up of following parts by weight of component：Cationic prepolymer 15~25, cationic photoinitiator 1~3, cationic reactive diluent 5~20, free radical type prepolymer 20~50, radical photoinitiator (sensitising agent) 1~2, coupling agent 0.05~1, toughener 1~2, plasticizer 1~2, nano-silver thread 0.1~1.Preparation method is：Using high-speed stirred, ultrasonic wave be scattered, vacuum defoamation technique, then composite and its product are formed under the irradiation of laser ultraviolet.Prepared composite fluidity is excellent, and molding shrinkage is low, and light sensitivity is high, and electric conductivity reaches below 10 Ω cm that impact flexibility is up to 4kJ/m2More than, it is adapted to laser ultraviolet light solidification 3D printing rapid shaping, the 3D printing product conductive available for requirement is prepared.
Description
Technical field
The present invention relates to 3D printing field of material preparation, more particularly to a kind of conductive UV-curing for laser 3D printing
Change resin composite materials and preparation method thereof.
Background technology
In recent years, rapid shaping has obtained significant progress, wherein three-dimensional (3D) printing technique is increasingly mature and industrialization,
In the gradually popularization and application of the fields such as bioengineering, Aero-Space, building, design.3D printing has several, wherein, laser ultraviolet light
Solidification 3D printing technique is quickly grown, using UV-cured resin, quick under 365nm or so laser to be by liquid crosslinking
Solid, then prints 3D products layer by layer.The use of more UV-cured resin is mainly at present epoxy resin and third
Olefin(e) acid esters.This resinoid is insulator in itself, and its specific insulation is up to 1013Ω cm, some application fields such as electronics electricity
Gas, household electrical appliances, military equipment, communication apparatus etc. need conductive articles, and the UV-cured resin of current insulation can not just expire
Sufficient application demand.The method of many conventional addition conductive agents of conduction of polymer, conventional conductive agent has conductive black, stainless steel fine
Dimension etc., but its addition is big, it is larger to the Effect on Mechanical Properties of composite.
The content of the invention
Based on the problems of prior art, it is an object of the invention to provide a kind of conduction for laser 3D printing is purple
Outer light-cured resin composite and preparation method thereof, its electric conductivity is high, and mechanical property is good.
The purpose of the present invention is achieved through the following technical solutions：
Embodiment of the present invention provides a kind of conductive UV-cured resin composite for laser 3D printing, by such as
The component composition of lower parts by weight：
Embodiment of the present invention also provides a kind of conductive UV-cured resin composite for laser 3D printing
Preparation method, for preparing the conductive UV-cured resin composite of the present invention for laser 3D printing, including
Following steps：
Each component is taken by the conductive UV-cured resin composite-material formula of the present invention for laser 3D printing；
Each component is added in container, is stirred 3 minutes with magnet rotor, the mixture being stirred then is put into ultrasonic wave clear
Wash after being vibrated 30 minutes in device and take out；
Prepare batten mould, mould binding face smears one layer of vaseline；
Start ultra-violet curing case, and adjust mould rack height, light intensity is fixed on 50mw/ ㎝2, mixture is instilled into mould
Levelling in tool, is put into vacuum drying chamber and froth breaking is vacuumized at 20~30 DEG C 30 minutes, is then irradiated in ultra-violet curing case,
Ultraviolet wavelength is 365nm, and batten irradiates 1 minute per face, irradiates two-sided rear taking-up, that is, obtains the conduction for laser 3D printing
UV-cured resin composite.
As seen from the above technical solution provided by the invention, it is provided in an embodiment of the present invention for laser 3D printing
Conductive UV-cured resin composite and preparation method thereof, its advantage is：
The present invention in UV-cured resin composite by adding nano silver wire, toughener as conductive agent
Afterwards, conductivity of composite material is greatly improved, and the performance such as impact flexibility, bending strength, bending modulus, heat distortion temperature is protected
Hold, while the viscosity increase of composite is few, remain in that high light sensitivity, the solidification 3D printing of laser ultraviolet light can be met
Requirement.In a word, the combination property of composite prepared by the present invention is greatly improved, and the dimensional stability of obtained product increases
Plus, so as to be conducive to improving the precision of printing product., can be with it is of special importance that the electric conductivity of composite is increased substantially
Suitable for conductive 3D printing product, so as to expand the application field of UV-cured resin and its 3D printing product.
The present invention is namely based on above-mentioned background, and nano silver wire is combined with light-cured resin, then adds coupling agent, toughener
Solidify 3D printing composite etc. conductive ultraviolet light has been prepared, extend the application field of 3D printing technique.
Embodiment
With reference to the particular content of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made,
Belong to protection scope of the present invention.
The embodiment of the present invention provides a kind of conductive UV-cured resin composite for laser 3D printing, by as follows
The component composition of parts by weight：
In above-mentioned composite, cationic prepolymer uses the epoxide equivalent to be for 100~400g/eg, room temperature viscosity
8000~15000mPas epoxy resin；Be preferred to use epoxide equivalent be 200~400g/eg, room temperature viscosity be 10000~
12000mPas epoxy resin.Molecular weight of epoxy resin is avoided using this epoxy resin too high, melting viscosity is big, shadow
Ring print speed；Molecular weight of epoxy resin is too low, the problem of Mechanical Properties of Products is bad.
The cationic photoinitiator is cation sulfosalt class, it is preferred to use mixed type triaryl sulphur hexafluorophosphoric acid
The mixture of any of salt and mixed type triaryl sulphur hexafluoro antimonate or both.
In above-mentioned composite, cationic reactive diluent is the mixture of epoxycyclohexyl ester and oxetanes,
The part by weight of epoxy cyclohexyl ester and oxetanes is 1 in mixture:0.5~1；It is preferred to use 3,4- epoxycyclohexyl first
By weight the 1 of acid -3,4- epoxycyclohexanecarboxylates and oxetanes:0.7 mixture.
The free radical type prepolymer is the acrylate of two or trifunctional, and room temperature viscosity is 50~500mPas.It is excellent
Choosing, free radical type prepolymer is using (3) ethoxyquin trimethylolpropane trimethacrylate or (3) third oxidation trimethylolpropanes
Triacrylate.
In above-mentioned composite, radical photoinitiator (sensitising agent) is benzophenone；It is preferred to use 1- hydroxyl rings
Hexyl Benzophenone.
The coupling agent is silane coupling agent；It is preferred that it is preferred that γ-glycydoxy trimethoxy silane
(KH-560), γ aminopropyltriethoxy silane (KH-550), γ-methacryloxypropyl trimethoxy silane
(KH-570) any or their mixture.
The toughener is that MBS is hud typed elastomer, and core is the polybutadiene rubber of crosslinking, plays toughening effect；Shell
For methylmethacrylate polymer, the compatibility with epoxy resin and acrylic resin is good.
In above-mentioned composite, nano silver wire is used as conductive agent, using a diameter of 5~50nm, 100~200 μm of length
Nano silver wire.Because the nano silver wire used is long fibre shape, addition can form conductive network on a small quantity, therefore assign composite wood
Expect electric conductivity.
In above-mentioned composite, plasticizer is triphenyl phosphate (TPP), and composite wood is on the one hand improved using this plasticizer
The toughness of material；On the other hand also there is fire retardation.
The embodiment of the present invention also provides a kind of system of the conductive UV-cured resin composite for laser 3D printing
Preparation Method, the conductive UV-cured resin composite for laser 3D printing above-mentioned for preparing, comprises the following steps：
Each component is taken by the above-mentioned conductive UV-cured resin composite-material formula for laser 3D printing；
Each component is added in container, is stirred 3 minutes with magnet rotor, the mixture being stirred then is put into ultrasonic wave clear
Wash after being vibrated 30 minutes in device and take out；
Prepare batten mould, mould binding face smears one layer of vaseline；
Start ultra-violet curing case, and adjust mould rack height, light intensity is fixed on 50mw/ ㎝2, mixture is instilled into mould
Levelling in tool, is put into vacuum drying chamber and froth breaking is vacuumized at 20~30 DEG C 30 minutes, is then irradiated in ultra-violet curing case,
Ultraviolet wavelength is 365nm, and batten irradiates 1 minute per face, irradiates two-sided rear taking-up, that is, obtains the conduction for laser 3D printing
UV-cured resin composite.
Specifically, the preparation method is：It is weighed into by formula rate in 1000ml beakers, adds magnet rotor stirring 3
Minute, then the mixture being stirred is put into after being shaken 30 minutes in ultrasonic cleaner and taken out.Can by ultrasonication
To improve the dispersion mixing uniformity of each component.Prepare batten mould, mould binding face, which smears one layer of vaseline, prevents liquid from letting out
Leak and conveniently stripped.Ultra-violet curing case is started, and adjusts mould rack height, light intensity is fixed on 50mw/ ㎝2.By liquid
Body instills levelling in mould, is put into vacuum drying chamber at 20~30 DEG C and vacuumizes froth breaking 30 minutes, is then placed in ultra-violet curing
Irradiate, ultraviolet wavelength is 365nm, batten irradiates 1 minute per face, taken out after irradiation is two-sided, test performance in case.
Conductive UV-cured resin composite for laser 3D printing prepared by the present invention, is a kind of composition,
It has high fluidity, better photosensitivity, high conductivity and high tenacity, and shrinkage factor is low, printing precision is high, it is adaptable to laser ultraviolet
3D printing rapid shaping.
The embodiment of the present invention is specifically described in further detail below.
Performance test methods in following examples are as follows：
Viscosity：With reference to GB/T22235-2008, using viscosity of the Brookfield DV3T rheometers to liquid photosensitive resin
It is measured, test temperature is 23 DEG C, and each sample collection is averaged twice.
Tensile strength and elongation at break：Carried out according to GB/T 1040-2006 standards.
Bending strength and bending modulus：Carried out according to GB/T 9341-2008 standards.
Simple beam impact strength：Carried out according to GB/T1043-2008 standards.
Heat distortion temperature：Carried out according to GB/T1634-2004 standards；Maximum deflection direct stress 0.46MPa, programming rate：2
℃/min。
Molding shrinkage：The measure of cure shrinkage uses bottle method, is determined using QBB type coating hydrometer jar at 23 DEG C
Liquid resinous density pLiquid, the density p of illumination postcure resin is obtained with densitometerGu, cure shrinkage is calculated with reference to ISO3521
Rate, formula is as follows：
Specific insulation：Carried out according to GB/T1410-2006 standards
Comparative example and embodiment 1~3：
Comparative example and the formula of embodiment 1~3 are shown in Table 1, and table 1 below is the formula table of comparative example and embodiment 1~3：
It is weighed into by the formula rate of above-mentioned table 1 in 1000ml beakers, adds magnet rotor and stir 3 minutes, then will
The mixture being stirred is put into vibrations in ultrasonic cleaner and taken out after 30 minutes.Each component can be improved by ultrasonication
Dispersion mixing uniformity.Prepare batten mould, mould binding face, which smears one layer of vaseline, prevents liquid leakage and convenient de-
Mould.Ultra-violet curing case is started, and adjusts mould rack height, light intensity is fixed on 50mw/ ㎝2.Liquid is instilled in mould
Levelling, is put into vacuum drying chamber at 20~30 DEG C and vacuumizes froth breaking 30 minutes, is then placed in ultra-violet curing case and irradiates, ultraviolet
Line wavelength is 365nm, and batten irradiates 1 minute per face, is taken out after irradiation is two-sided, test performance.
The performance of comparative example and embodiment 1~3 is shown in Table 2, and table 2 below is being beaten for laser 3D for comparative example and embodiment 1~3
The performance of the conductive UV-cured resin composite of print：
As can be seen from the above Table 2, the present invention adds specific nano silver wire in UV-cured resin composite
After conductive agent, toughener, conductivity of composite material is greatly improved, impact flexibility, bending strength, bending modulus, thermal deformation
The performances such as temperature are maintained, while the viscosity increase of composite is few, remains in that high light sensitivity, can meet laser
Ultraviolet light solidifies the requirement of 3D printing.In a word, the combination property of composite prepared by the present invention is greatly improved, obtained product
Dimensional stability increase so that be conducive to improve printing product precision.It is of special importance that the electric conductivity of composite is big
Amplitude is improved, and goes for conductive 3D printing product, so as to expand the application of UV-cured resin and its 3D printing product
Field.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (10)
1. a kind of conductive UV-cured resin composite for laser 3D printing, it is characterised in that by following parts by weight
Component composition：
2. a kind of conductive UV-cured resin composite for laser 3D printing according to claim 1, it is special
Levy and be, the cationic prepolymer use epoxide equivalent be 8000 for 100~400g/eg, room temperature viscosity~
15000mPas epoxy resin；
The cationic photoinitiator is cation sulfosalt class.
3. a kind of conductive UV-cured resin composite for laser 3D printing according to claim 2, it is special
Levy and be,
The cationic prepolymer uses epoxide equivalent to be 10000~12000mPas for 200~400g/eg, room temperature viscosity
Epoxy resin；
The cation sulfosalt class uses mixed type triaryl sulphur hexafluorophosphate and mixed type triaryl sulphur hexafluoro antimony
The mixture of any of hydrochlorate or both.
4. a kind of conductive UV-cured resin for laser 3D printing according to any one of claims 1 to 3 is combined
Material, it is characterised in that the cationic reactive diluent is the mixture of epoxycyclohexyl ester and oxetanes, mixing
The part by weight of epoxy cyclohexyl ester and oxetanes is 1 in thing:0.5~1；
The free radical type prepolymer is the acrylate of two or trifunctional, and room temperature viscosity is 50~500mPas.
5. a kind of conductive UV-cured resin composite for laser 3D printing according to claim 4, it is special
Levy and be, the free radical type prepolymer is using (3) ethoxyquin trimethylolpropane trimethacrylate or (3) third three hydroxyl first of oxidation
Base propane triacrylate.
6. a kind of conductive UV-cured resin for laser 3D printing according to any one of claims 1 to 3 is combined
Material, it is characterised in that the radical photoinitiator is benzophenone；
The coupling agent is silane coupling agent；
The toughener is that MBS is hud typed elastomer.
7. a kind of conductive UV-cured resin composite for laser 3D printing according to claim 6, it is special
Levy and be, the benzophenone uses 1- hydroxy cyclohexyl phenylketones；
The silane coupling agent uses γ-glycydoxy trimethoxy silane, gamma-amino propyl triethoxy
Any of silane, γ-methacryloxypropyl trimethoxy silane or their mixture.
8. a kind of conductive UV-cured resin for laser 3D printing according to any one of claims 1 to 3 is combined
Material, it is characterised in that a diameter of 5~50nm of nano silver wire, 100~200 μm of length.
9. a kind of conductive UV-cured resin for laser 3D printing according to any one of claims 1 to 3 is combined
Material, it is characterised in that the plasticizer is triphenyl phosphate.
10. the preparation method of a kind of conductive UV-cured resin composite for laser 3D printing, it is characterised in that use
In the conductive UV-cured resin composite for laser 3D printing described in preparation any one of claim 1 to 9, including
Following steps：
The conductive UV-cured resin composite-material formula for laser 3D printing as described in any one of claim 1 to 9
Take each component；
Each component is added in container, is stirred 3 minutes with magnet rotor, the mixture being stirred then is put into ultrasonic cleaner
Middle vibration is taken out after 30 minutes；
Prepare batten mould, mould binding face smears one layer of vaseline；
Start ultra-violet curing case, and adjust mould rack height, light intensity is fixed on 50mw/ ㎝2, mixture is instilled in mould
Levelling, is put into vacuum drying chamber and froth breaking is vacuumized at 20~30 DEG C 30 minutes, is then irradiated in ultra-violet curing case, ultraviolet
Line wavelength is 365nm, and batten irradiates 1 minute per face, takes out, that is, is obtained for the conductive ultraviolet of laser 3D printing after irradiation is two-sided
Light-cured resin composite.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956363A (en) * | 2018-05-21 | 2018-12-07 | 青海泰丰先行锂能科技有限公司 | A kind of detection method of lithium ion battery material sintering anteroposterior contraction rate |
| CN109517112A (en) * | 2018-11-21 | 2019-03-26 | 中山大简科技有限公司 | A kind of conductive photosensitive resin composition for photocuring rapid prototyping |
| CN111471140A (en) * | 2020-05-19 | 2020-07-31 | 深圳永昌和科技有限公司 | Magnetic control 3D printing ultraviolet curing conductive material and preparation method thereof |
| CN111875771A (en) * | 2020-08-05 | 2020-11-03 | 北京石油化工学院 | Preparation method of hyperbranched polyurethane acrylate resin for UV (ultraviolet) photocuring |
| CN113402923A (en) * | 2021-06-16 | 2021-09-17 | 深圳市撒比斯科技有限公司 | 3D laser photosensitive printing conductive ink for integrated circuit and preparation method thereof |
| CN114986902A (en) * | 2022-06-07 | 2022-09-02 | 丽水学院 | Preparation method of high-performance DLP-3D printing material applied to oral medical field |
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| CN105713332A (en) * | 2016-04-14 | 2016-06-29 | 北京石油化工学院 | Ultraviolet-curable resin composite for laser 3D printing and preparation method of ultraviolet-curable resin composite |
| CN106380806A (en) * | 2016-09-28 | 2017-02-08 | 北京石油化工学院 | Conductive polylactic acid composite material composition for hot-melt 3D printing and preparation method thereof |
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2017
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105713332A (en) * | 2016-04-14 | 2016-06-29 | 北京石油化工学院 | Ultraviolet-curable resin composite for laser 3D printing and preparation method of ultraviolet-curable resin composite |
| CN106380806A (en) * | 2016-09-28 | 2017-02-08 | 北京石油化工学院 | Conductive polylactic acid composite material composition for hot-melt 3D printing and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956363A (en) * | 2018-05-21 | 2018-12-07 | 青海泰丰先行锂能科技有限公司 | A kind of detection method of lithium ion battery material sintering anteroposterior contraction rate |
| CN109517112A (en) * | 2018-11-21 | 2019-03-26 | 中山大简科技有限公司 | A kind of conductive photosensitive resin composition for photocuring rapid prototyping |
| CN111471140A (en) * | 2020-05-19 | 2020-07-31 | 深圳永昌和科技有限公司 | Magnetic control 3D printing ultraviolet curing conductive material and preparation method thereof |
| CN111875771A (en) * | 2020-08-05 | 2020-11-03 | 北京石油化工学院 | Preparation method of hyperbranched polyurethane acrylate resin for UV (ultraviolet) photocuring |
| CN113402923A (en) * | 2021-06-16 | 2021-09-17 | 深圳市撒比斯科技有限公司 | 3D laser photosensitive printing conductive ink for integrated circuit and preparation method thereof |
| CN114986902A (en) * | 2022-06-07 | 2022-09-02 | 丽水学院 | Preparation method of high-performance DLP-3D printing material applied to oral medical field |
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Application publication date: 20170811 |
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