CN109762336A - A kind of 3D printing composite wire and preparation method thereof - Google Patents
A kind of 3D printing composite wire and preparation method thereof Download PDFInfo
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- CN109762336A CN109762336A CN201910051771.6A CN201910051771A CN109762336A CN 109762336 A CN109762336 A CN 109762336A CN 201910051771 A CN201910051771 A CN 201910051771A CN 109762336 A CN109762336 A CN 109762336A
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Abstract
The invention belongs to 3D printing technique fields, and in particular to a kind of 3D printing composite wire and preparation method thereof.The component and mass percent of 3D printing composite wire of the invention are as follows: polyetherimide (PEI): 65%~85%；Polyether-ether-ketone (PEEK): 10%~30%；Carbon fiber: 0.1%~10%；Coupling agent: 0.1%~3%；Lubricant: 0.2%~4%.Preparation method includes melting extrusion granulation and melting extrusion wire drawing.The present invention solves the manufacture requirement that existing 3D printing wire rod is unable to satisfy aerospace parts；Suitable for simplifying manufacturing process, having saved manufacturing cost to complicated being customized of aircraft components 3D printing, the use temperature upper limit and mechanical performance of wire rod are improved, the suitable application area of 3D printing wire rod has been widened.
Description
Technical field
The invention belongs to 3D printing technique fields, and in particular to a kind of 3D printing composite wire and preparation method thereof.
Background technique
3D printing, also known as increasing material manufacturing are directly successively processed by machine realization, are superimposed as according to three-dimensional data
The technique of shape generates entity with this.Different from the method for conventionally employed production mold and traditional die casting, this no mold freedom at
The technology of shape gets rid of the constraint of space geometry and design technology, can design arbitrary structures and be transformed into physical product, open up significantly
Wide making space, shortens the manufacturing cycle, reduces manufacturing cost and risk, become nowadays emerging intelligence manufacture field
Bellwether.In December, 2017,12 department such as the Ministry of Industry and Information Technology, State Development and Reform Commission print and distribute " increasing material manufacturing (3D printing)
Industry development action plan (2017-2020) ", it mentions in the works, arrives the year two thousand twenty, increasing material manufacturing industry annual sales revenue is super
20,000,000,000 yuan are crossed, average annual growth rate is 30% or more.Key core technologies reach international synchronized development level, and technological equipment is substantially full
Sufficient industrial application demand, ecosystem construction is significant perfect, realizes that scale application, Overseas Development ability are obvious in certain fields
It is promoted.For role positioning during " made in China " is to " Chinese intelligence is made ", 3D printing is to develop the core of intelligence manufacture
One of technology has irreplaceable role.
Currently, most widely used is still fused glass pellet (FDM) technology in 3D printing technique, as a kind of
Can be by the printing technique method of various thermoplastic polymer wire rods heating fusing and then successively accumulation molding, principle is simple, operates
Easy, saving raw material, printing period at low cost are short, are most widely used, also just have to Guan Chong in numerous 3D printing techniques
The status wanted.
However, the polymer wire for being applied to FDM printing technique is still mainly each with ABS, PLA, PC, PP, PE, nylon etc.
Class often uses thermoplastic engineering plastic and its composite material for being modified enhancing in the majority, these materials are generally existing low using temperature,
Mechanical strength is poor, and combination process is complicated, and additive is various, the very limited problem of practical ranges, especially in aerospace
In terms of equal engineer applications almost can not practical application, current existing 3D printing consumptive material type is difficult to meet already growing
The market demand.
Polyetherimide (PEI) and polyether-ether-ketone (PEEK) are common aeronautical material, and heat distortion temperature is high, are had both excellent
Different mechanical property has wide spectrum chemical resistance, fire resistance and low cause cigarette, and creep resistant and excellent size stability,
It is widely used in fireman's helmet, aircraft interior trim, aerospace component and each position component of automobile etc. out of my cabin.They are as aviation
Grade Particular thermoplastic's resin has the high-fire resistance, chemical resistance for being directed to that any FDM thermoplastic can not all be reached on the market
And excellent mechanical property.Carbon fiber, which is a kind of phosphorus content, very excellent has both well processed in 95% or more mechanical property
The carbon material of performance belongs to very crucial reinforcing material as the grand strategy goods and materials for developing defence and military and national economy.
The composite material of fibre reinforced is widely used in the military industry fields such as aircraft manufacturing, shipbuilding, rocket manufacture.Therefore, with poly-
Etherimide (PEI), polyether-ether-ketone (PEEK) are binary resin matrix, then are equipped with the efficient humidification of carbon fiber, are conducts
The best complex material system of 3D printing aircraft components wire rod；So far there are no such 3D printing composite systems to apply
In manufacture aircraft components or other field.
Summary of the invention
In view of the above situation of the prior art, the object of the present invention is to provide a kind of 3D printing composite wire and its preparations
Method.3D printing composite wire of the invention solves the manufacture requirement that existing 3D printing wire rod is unable to satisfy aerospace parts, can
Suitable for simplifying manufacturing process to complicated being customized of aircraft components 3D printing, manufacturing cost is saved, the use of wire rod is improved
Temperature upper limit and mechanical performance widen the suitable application area of 3D printing wire rod.
In the first aspect of the present invention, a kind of 3D printing composite wire, component and mass percent are provided are as follows: polyethers
Acid imide (PEI): 65%~85%；Polyether-ether-ketone (PEEK): 10%~30%；Carbon fiber: 0.1%~10%；Coupling agent:
0.1%~3%；Lubricant: 0.2%~4%.
The weight average molecular weight Mw of the polyetherimide is the g/mol of 40,000 g/mol~60,000, the weight average molecular weight of polyether-ether-ketone
Mw is the g/mol of 30,000 g/mol~50,000.
The carbon fiber is chopped carbon fiber, and the length is one of 1mm, 3mm and 5mm or their any ratios
The mixture of example.
The coupling agent is vinyl three (methoxyethoxy) silane, anilinomethyl trimethoxy silane, methacrylic acid
One of the complex compound of chromium chloride, two (methylacryloyl) isostearoyl base isopropyl titanates or their any group
It closes.
The lubricant is N, N '-ethylenebisstearamide (EBSA), palmitinic acid, zinc stearate, atoleine, oxidation
One of polyethylene wax, dimethyl silicone polymer or their any combination.
In another aspect of the invention, a kind of a kind of preparation side of 3D printing composite wire as described above is provided
Method, comprising:
Melting extrusion is granulated: the coupling agent weighed up, lubricant are added to the polyetherimide after drying, polyether-ether-ketone two
In first resin matrix, through double screw extruder after being thoroughly mixed uniformly, under conditions of temperature is 350 DEG C~450 DEG C into
Row melt blending and extruding pelletization, in extrusion process, by add fine mouth be gradually added into it is dry after carbon fiber, it is water cooled, air-cooled,
Composite master batch is obtained after pelletizing；
Melting extrusion wire drawing: compound through single screw rod resin wire drawing machine drought after the abundant desiccant dehumidification of composite master batch
Wire rod, then shape wire is collected by disk wrapping wire；The heating temperature of the resin wire drawing machine is 320 DEG C~400 DEG C, is obtained
The diameter of wire rod is 1.75mm ± 0.05mm.
The present invention provides a kind of composite wire and preparation method thereof of 3D printing.The present invention uses aviation-grade Special Resin
3D printing wire rod is prepared for the carbon fibre reinforced composite of binary matrix, existing 3D printing wire rod is solved and is unable to satisfy aviation
The manufacture requirement of component；Suitable for simplifying manufacturing process to complicated being customized of aircraft components 3D printing, manufacture has been saved
Cost improves the use temperature upper limit and mechanical performance of wire rod, has widened the suitable application area of 3D printing wire rod.
Specific embodiment
Objects, technical solutions and advantages for a clearer understanding of the present invention, below with reference to embodiment, to the present invention into
Row is further described.
The present invention provides a kind of 3D printing composite wire, it is characterised in that: the mass percent of its each component are as follows: poly-
Etherimide (PEI): 65%~85%；Polyether-ether-ketone (PEEK): 10%~30%；Carbon fiber: 0.1%~10%；Coupling agent:
0.1%~3%；Lubricant: 0.2%~4%.
The weight average molecular weight Mw of the polyetherimide is the g/mol of 40,000 g/mol~60,000, the weight average molecular weight of polyether-ether-ketone
Mw is the g/mol of 30,000 g/mol~50,000.
The carbon fiber is chopped carbon fiber, and the length is one of 1mm, 3mm and 5mm or several any ratios
The mixture of example.
The coupling agent is vinyl three (methoxyethoxy) silane, anilinomethyl trimethoxy silane, methacrylic acid
One of the complex compound of chromium chloride, two (methylacryloyl) isostearoyl base isopropyl titanates or several any ratios
The mixture of example.
The lubricant is N, N '-ethylenebisstearamide (EBSA), palmitinic acid, zinc stearate, atoleine, oxidation
The mixture of one of polyethylene wax, dimethyl silicone polymer or several arbitrary proportions.
The present invention also provides a kind of preparation methods of 3D printing composite wire as described above, which is characterized in that preparation
Steps are as follows:
1. melting extrusion is granulated: the coupling agent weighed up, lubricant are added to the polyetherimide after drying, polyether-ether-ketone
In resin matrix, through double screw extruder after being thoroughly mixed uniformly, carried out under conditions of temperature is 350 DEG C~450 DEG C
Melt blending and extruding pelletization, in extrusion process, by add fine mouth be gradually added into it is dry after carbon fiber, it is water cooled, air-cooled, cut
Composite master batch is obtained after grain.
2. melting extrusion wire drawing: multiple through single screw rod resin wire drawing machine drought after the abundant desiccant dehumidification of composite master batch
Zygonema material, then shape wire is collected by disk wrapping wire, the heating temperature of the resin wire drawing machine is 320 DEG C~400 DEG C, wire rod
Diameter is 1.75mm ± 0.05mm.
It is aircraft components and its most structure of accessory, complex-shaped, there is irregular asymmetry curved surface or fine
Internal structure, small volume, while it being also contemplated that a possibility that it is fabricated and economy, including manufacturing cost, manufacture week
The complexity of phase, manufacture risk and technical process etc. factor.For these urgent problems, the present invention is utilized
3D printing intelligent Manufacturing Technology enhances the innovation mode that extraordinary compound resin combines with novel carbon fiber, has developed with polyethers acyl
Two kinds of aviation-grade Particular thermoplastic resins of imines (PEI) and polyether-ether-ketone (PEEK) are made as binary resin matrix with carbon fiber
3D printing composite wire prepared by composite material for reinforcing material, have on the market any thermoplasticity 3D printing wire rod all without
High-fire resistance, chemical resistance and the excellent mechanical property heat distortion temperature height that method is reached are, it can be achieved that aircraft interior trim, navigates out of my cabin
The customization 3D printing of each position aircraft component such as empty space flight component, can push the research and production of aircraft components it is more intelligent,
Lean, high efficiency and economization.In addition, preparation is simple, safe operation environmental protection, mass production can be achieved.
Embodiment 1
By the vacuum dried case of the masterbatch resin of polyetherimide, polyether-ether-ketone in 120 DEG C desiccant dehumidification 4 hours, carbon fiber
Vacuum dried case is tieed up in 70 DEG C after desiccant dehumidification 2 hours, weigh 1g coupling agent, 1g lubricant be added to it is dry after 65g it is poly-
In the hybrid resin of etherimide and 30g polyether-ether-ketone, through double screw extruder after being thoroughly mixed uniformly, it is in temperature
Carry out melt blending and extruding pelletization under conditions of 360 DEG C, in extrusion process, pass through add fine mouth be gradually added into it is dry after 3g carbon
Fiber (length 1mm) obtains composite master batch after water cooled, air-cooled, pelletizing.
The vacuum dried case of composite master batch after desiccant dehumidification 4 hours, is squeezed in 120 DEG C through single screw rod resin wire drawing machine travel
Composite wire out, then molding is collected by disk wrapping wire and obtains composite wire, the heating temperature of the resin wire drawing machine is 350
DEG C, the diameter of obtained wire rod is 1.75mm ± 0.05mm.
Embodiment 2
By the vacuum dried case of the masterbatch resin of polyetherimide, polyether-ether-ketone in 130 DEG C desiccant dehumidification 3.5 hours, carbon
The vacuum dried case of fiber after desiccant dehumidification 2 hours, weighs 1g coupling agent in 75 DEG C, 2g lubricant be added to it is dry after 85g
In the hybrid resin of polyetherimide and 10g polyether-ether-ketone, through double screw extruder after being thoroughly mixed uniformly, it is in temperature
Carry out melt blending and extruding pelletization under conditions of 370 DEG C, in extrusion process, pass through add fine mouth be gradually added into it is dry after 2g carbon
Fiber (length 3mm) obtains composite master batch after water cooled, air-cooled, pelletizing.
The vacuum dried case of composite master batch after desiccant dehumidification 4 hours, is squeezed in 125 DEG C through single screw rod resin wire drawing machine travel
Composite wire out, then molding is collected by disk wrapping wire and obtains composite wire, the heating temperature of the resin wire drawing machine is 360
DEG C, the diameter of obtained wire rod is 1.75mm ± 0.05mm.
Embodiment 3
By the vacuum dried case of the masterbatch resin of polyetherimide, polyether-ether-ketone in 140 DEG C desiccant dehumidification 3 hours, carbon fiber
Vacuum dried case is tieed up in 75 DEG C after desiccant dehumidification 2 hours, weigh 2g coupling agent, 2g lubricant be added to it is dry after 70g it is poly-
In the hybrid resin of etherimide and 16g polyether-ether-ketone, through double screw extruder after being thoroughly mixed uniformly, it is in temperature
Carry out melt blending and extruding pelletization under conditions of 370 DEG C, in extrusion process, pass through add fine mouth be gradually added into it is dry after 10g
Carbon fiber (combination of the arbitrary proportion of length 1mm and 3mm carbon fiber), obtains composite master batch after water cooled, air-cooled, pelletizing.
The vacuum dried case of composite master batch after desiccant dehumidification 3 hours, is squeezed in 140 DEG C through single screw rod resin wire drawing machine travel
Composite wire out, then molding is collected by disk wrapping wire and obtains composite wire, the heating temperature of the resin wire drawing machine is 380
DEG C, the diameter of obtained wire rod is 1.75mm ± 0.05mm.
Embodiment 4
By the vacuum dried case of the masterbatch resin of polyetherimide, polyether-ether-ketone in 150 DEG C desiccant dehumidification 2 hours, carbon fiber
Vacuum dried case is tieed up in 70 DEG C after desiccant dehumidification 2 hours, weigh 1.5g coupling agent, 2.5g lubricant be added to it is dry after
In the hybrid resin of 68g polyetherimide and 20g polyether-ether-ketone, through double screw extruder after being thoroughly mixed uniformly, in temperature
Degree is carries out melt blending and extruding pelletization under conditions of 400 DEG C, in extrusion process, by add fine mouth be gradually added into it is dry after
8g carbon fiber (combination of the arbitrary proportion of the carbon fiber of length 3mm and 5mm), obtains compound mother after water cooled, air-cooled, pelletizing
Grain.
The vacuum dried case of composite master batch after desiccant dehumidification 4 hours, is squeezed in 120 DEG C through single screw rod resin wire drawing machine travel
Composite wire out, then molding is collected by disk wrapping wire and obtains composite wire, the heating temperature of the resin wire drawing machine is 330
DEG C, the diameter of obtained wire rod is 1.75mm ± 0.05mm.
Embodiment 5
By the vacuum dried case of the masterbatch resin of polyetherimide, polyether-ether-ketone in 120 DEG C desiccant dehumidification 4 hours, carbon fiber
Vacuum dried case is tieed up in 80 DEG C after desiccant dehumidification 1.5 hours, weigh 0.5g coupling agent, 1g lubricant be added to it is dry after
In the hybrid resin of 70g polyetherimide and 28g polyether-ether-ketone, through double screw extruder after being thoroughly mixed uniformly, in temperature
Degree is carries out melt blending and extruding pelletization under conditions of 420 DEG C, in extrusion process, by add fine mouth be gradually added into it is dry after
0.5g carbon fiber (length 5mm) obtains composite master batch after water cooled, air-cooled, pelletizing.
The vacuum dried case of composite master batch after desiccant dehumidification 3 hours, is squeezed in 140 DEG C through single screw rod resin wire drawing machine travel
Composite wire out, then molding is collected by disk wrapping wire and obtains composite wire, the heating temperature of the resin wire drawing machine is 400
DEG C, the diameter of obtained wire rod is 1.75mm ± 0.05mm.
Claims (6)
1. a kind of 3D printing composite wire, component and mass percent are as follows: polyetherimide: 65%~85%；Polyethers ether
Ketone: 10%~30%；Carbon fiber: 0.1%~10%；Coupling agent: 0.1%~3%；Lubricant: 0.2%~4%.
2. 3D printing composite wire described in accordance with the claim 1, wherein the weight average molecular weight of the polyetherimide is 40,000
The g/mol of g/mol~60,000, the weight average molecular weight of polyether-ether-ketone are the g/mol of 30,000 g/mol~50,000.
3. 3D printing composite wire described in accordance with the claim 1, wherein the carbon fiber is chopped carbon fiber, length is
Any combination of any one or they in 1mm, 3mm and 5mm.
4. 3D printing composite wire described in accordance with the claim 1, wherein the coupling agent is three (methoxy (ethoxy) of vinyl
Base) silane, anilinomethyl trimethoxy silane, the complex compound of methacrylate-chromic chloride, two (methylacryloyl) different tristearin
One of acyl group isopropyl titanate or their any combination.
5. 3D printing composite wire described in accordance with the claim 1, wherein the lubricant is N, N '-ethylenebis stearoyl
One of amine, palmitinic acid, zinc stearate, atoleine, oxidized polyethylene wax, dimethyl silicone polymer or their times
Meaning combination.
6. a kind of preparation method of 3D printing composite wire described in accordance with the claim 1, comprising:
Melting extrusion is granulated: the coupling agent weighed up, lubricant are added to the polyetherimide after drying, polyether-ether-ketone binary tree
In aliphatic radical body, through double screw extruder after being thoroughly mixed uniformly, melted under conditions of temperature is 350 DEG C~450 DEG C
Melt and simultaneously extruding pelletization is blended, in extrusion process, passes through the carbon fiber for adding fine mouth to be gradually added into after drying, water cooled, air-cooled, pelletizing
After obtain composite master batch；
Melting extrusion wire drawing: after the abundant desiccant dehumidification of composite master batch, through single screw rod resin wire drawing machine drought composite wire,
Shape wire is collected by disk wrapping wire again；The heating temperature of the resin wire drawing machine is 320 DEG C~400 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111424333A (en) * | 2020-05-08 | 2020-07-17 | 广安长明高端产业技术研究院 | Electrostatic spinning PEEK/low-melting-point metal composite fiber, 3D printing consumable material and preparation method thereof |
| CN111761844A (en) * | 2020-06-30 | 2020-10-13 | 诺思贝瑞新材料科技（苏州）有限公司 | Continuous fiber composite material for 3D printing and preparation method and device thereof |
| CN112251830A (en) * | 2020-10-22 | 2021-01-22 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | Oriented carbon nanotube reinforced nylon composite material, and preparation method and application thereof |
| WO2021214400A1 (en) * | 2020-04-21 | 2021-10-28 | Safran | Composition for additive manufacturing |
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| CN112251830B (en) * | 2020-10-22 | 2023-04-11 | 江西省纳米技术研究院 | Oriented carbon nanotube reinforced nylon composite material, and preparation method and application thereof |
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