CN105176082A - Composite 3D printing material and preparation method thereof - Google Patents
Composite 3D printing material and preparation method thereof Download PDFInfo
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- CN105176082A CN105176082A CN201510588764.1A CN201510588764A CN105176082A CN 105176082 A CN105176082 A CN 105176082A CN 201510588764 A CN201510588764 A CN 201510588764A CN 105176082 A CN105176082 A CN 105176082A
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- polyetherimide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Developing Agents For Electrophotography (AREA)
Abstract
The invention provides a composite 3D printing material and a preparation method thereof. The composite 3D printing material comprises the following components in parts by weight: 50-100 parts of polyetherimide, 30-100 parts of epoxy resin, 10-30 parts of monocrystal sapphire whisker, 10-30 parts of a coupling agent, 0.1-5 parts of a flatting agent, 0.1-4 parts of a degassing agent and 1-10 parts of a dispersive lubricant. Compared with a traditional polyetherimide material, the composite 3D printing material has relatively high strength and hardness and can be used at the high temperature.
Description
Technical field
The invention belongs to field of compound material, be specifically related to a kind of preparation method of compound 3D printed material.
Background technology
It is a kind of based on digital model file that 3D prints, and applying powder last current state metal or plastics etc. can the rapid shaping techniques of jointing material, are described as the Industrial Revolution again of overturning traditional manufacture.This technology is at jewelry, footwear, industrial design, building, engineering and construction (AEC), dentistry and medical industries, education, geographical information system(GIS), civil engineering work, automobile, and aerospace, gun and other field are applied all to some extent.Since 3D prints birth, change to functional and service product from industry, BUILDINGS MODELS print.And under the intelligence manufacture background in future, 3D printing technique will with other modern technique fusion developments such as internet, cloud computing, Internet of Things, large data.But existing 3D printed material is applied in the problem that the fields such as aerospace automobile also exist insufficient strength, therefore urgently exploitation is a kind of comparatively mates with 3D printer mobility, formability, has the 3D printed material of sufficient intensity and hardness simultaneously.
Monocrystalline sapphire whisker (SinglecrystalsapphireWhisker) is the high purity single crystal of cultivating growth under controlled conditions, its crystalline structure is near-complete, not containing lattice defects such as boundary or grain, dislocation, cavities, have that superior mechanical intensity, heat shock resistance, proportion are little, anti-oxidant, physicals that high abrasion amount and high corrosion resistance etc. are excellent, monocrystalline sapphire whisker becomes the optimal selection of third generation advanced composite material.Intensity and the wear resistance of 3D printing matrix material can be significantly improved.
Summary of the invention
The object of the present invention is to provide a kind of compound 3D printed material and preparation method thereof, the present invention effectively can improve mechanical property, dimensional stability, thermotolerance, the ageing-resistant performance of 3D printing matrix material.Expand polyamide material high-end applications scope in automobile, aerospace.
For realizing above object, technical scheme of the present invention is:
A kind of compound 3D printed material, comprises following component by weight:
Polyetherimide (Polyetherimide) 50 ~ 100 weight part
Epoxy resin 30 ~ 100 weight part
Monocrystalline sapphire whisker 10 ~ 30 weight part
Coupling agent 10 ~ 30 weight part
Flow agent 0.1 ~ 5 weight part
Air release agent 0.1 ~ 4 weight part
Dispersed lubricant 1 ~ 10 weight part.
Described compound 3D printed material, each component preferred weight number is as follows:
Polyetherimide (Polyetherimide) 80 ~ 100 weight part
Epoxy resin 50 ~ 80 weight part
Monocrystalline sapphire whisker 10 ~ 30 weight part
Coupling agent 10 ~ 30 weight part
Flow agent 0.1 ~ 5 weight part
Air release agent 0.1 ~ 4 weight part
Dispersed lubricant 1 ~ 10 weight part.
Described polyetherimide (Polyetherimide) for oxygen index be 47%, density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3; Described epoxy resin is commercially available glycidyl amine epoxy resin.
Described monocrystalline sapphire whisker is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the monocrystalline sapphire whisker that purity (wt%) is 90-99.9%.
Described coupling agent is zirconium class coupling agent; Described flow agent is polydimethylsiloxane or butyl cellulose.
Described air release agent is high-carbon type air release agent, as TYPE air release agent, Viscotrol C or butylbenzene rubber cement; Described dispersed lubricant is polyethylene wax or bis-fatty acid amides.
A preparation method for compound 3D printed material, a, puts into material-compound tank by epoxy resin, dispersed lubricant, coupling agent according to described formula ratio, rapid stirring 1 ~ 3h in heating unit; Monocrystalline sapphire whisker is added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 10 ~ 30min by b; C, at 100 ~ 200 DEG C to add monocrystalline sapphire fiber melting mixing liquid in add polyetherimide, flow agent, air release agent, continue stirring 1 ~ 2h; D, naturally cooling, can obtain compound 3D printed material after crushing and screening.
In described step a, Heating temperature is 80 ~ 120 DEG C, and stirring velocity is 400 ~ 750r/min.
In step c, stirring velocity is 450 ~ 1000r/min.
Use EOSP396 model 3D printer, adopt powder sintered shaping (SelectedLaserSintering is called for short SLS) technology, utilize infrared laser to carry out powdered material powder sintered shaping.Described monocrystalline sapphire whisker researches and develops preparation by monocrystalline sapphire whisker team of Dongguan Shenzhen Research Institute of Tsinghua University innovation center, and select diameter 0.1 ~ 5 micron, length is the monocrystalline sapphire whisker of 5 ~ 100 microns.Selected monocrystalline sapphire whisker density is 4g/cm3, and purity (wt%) is about 99%.
The invention has the beneficial effects as follows:
Beneficial effect:
(1) a kind of compound 3D printed material of the present invention is compared with traditional polyamide material, and compound 3D printed material of the present invention has higher bending elastic modulus, tensile strength, dimensional stability and thermal distoftion temperature, can at high temperature use.
(2) a kind of compound 3D printed material process of the present invention is simple, is easy to suitability for industrialized production
(3) a kind of compound 3D printed material raw material of the present invention is cheap, wide material sources, and has good environmental benefit and economic benefit.
Accompanying drawing explanation
Accompanying drawing 1 illustrates the preparation flow figure of compound 3D printed material.
Embodiment
The present invention is described in further detail by embodiment.
Embodiment 1
(1) 50 weight parts water glyceramine based epoxy resins, 1 weight account polyethylene wax, 10 weight part zirconium class coupling agents are put into material-compound tank, in 80 DEG C, stir 1h with 400r/min.
(2) 10 weight part monocrystalline sapphire whiskers are added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 10min.
(3) at 100 DEG C, add 80 weight part polyetherimides, 0.1 weight part polydimethylsiloxane, 0.1 weight part TYPE air release agent in above-mentioned mixed solution, 450r/min continues to stir 2h.
(4) naturally cooling, can obtain compound 3D printed material after crushing and screening.
Embodiment 2
(1) 60 weight parts water glyceramine based epoxy resins, 5 weight account polyethylene waxes, 15 weight part zirconium class coupling agents are put into material-compound tank, in 90 DEG C, stir 1.5h with 450r/min.
(2) 15 weight part monocrystalline sapphire whiskers are added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 15min.
(3) at 100 DEG C, add 80 weight part polyetherimides, 0.2 weight part polydimethylsiloxane, 0.3 weight part Viscotrol C in above-mentioned mixed solution, 500r/min continues to stir 2h.
(4) naturally cooling, can obtain compound 3D printed material after crushing and screening.
Embodiment 3
(1) 70 weight parts water glyceramine based epoxy resins, 7 weight account polyethylene waxes, 20 weight part zirconium class coupling agents are put into material-compound tank, in 90 DEG C, stir 2h with 500r/min.
(2) 20 weight part monocrystalline sapphire whiskers are added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 15min.
(3) at 150 DEG C, in above-mentioned mixed solution, add 80 weight part polyetherimides, 0.5 weight part gather butyl cellulose, 0.1 weight part Viscotrol C, 600r/min continue stir 2h.
(4) naturally cooling, can obtain compound 3D printed material after crushing and screening.
Embodiment 4
(1) 70 weight parts water glyceramine based epoxy resins, 8 weight part bis-fatty acid amides, 30 weight part zirconium class coupling agents are put into material-compound tank, in 100 DEG C, stir 3h with 600r/min.
(2) 25 weight part monocrystalline sapphire whiskers are added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 15min.
(3) at 175 DEG C, in above-mentioned mixed solution, add 80 weight part polyetherimides, 0.7 weight part gather butyl cellulose, 0.5 weight part butylbenzene rubber cement, 700r/min continue stir 2h.
(4) naturally cooling, can obtain compound 3D printed material after crushing and screening.
Embodiment 5
(1) 80 weight parts water glyceramine based epoxy resins, 10 weight account polyethylene waxes, 20 weight part zirconium class coupling agents are put into material-compound tank, in 100 DEG C, stir 3h with 750r/min.
(2) 30 weight part monocrystalline sapphire whiskers are added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 30min.
(3) at 200 DEG C, in above-mentioned mixed solution, add 80 weight part polyetherimides, 1 weight part gather butyl cellulose, 1 weight part butylbenzene rubber cement, 1000r/min continue stir 2h.
(4) naturally cooling, can obtain compound 3D printed material after crushing and screening.
The mechanical property of embodiment 3 is tested, the results are shown in following table:
Table 1 embodiment 3 prepares the mechanical property of compound 3D printed material
| Mechanical property | Numerical value | Unit | Testing standard |
| Tensile modulus | 1098000 | Pound | ISO527-1/-2 |
| Tensile strength | 73500 | Pound | ISO527-1/-2 |
| Elongation at break | 3.1 | % | ISO527-1/-2 |
Shown by above data, embodiments of the invention 3 tensile modulus, tensile strength are very high, with the obvious advantage.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. a compound 3D printed material, comprises following component by weight:
Polyetherimide (Polyetherimide) 50 ~ 100 weight part
Epoxy resin 30 ~ 100 weight part
Monocrystalline sapphire whisker 10 ~ 30 weight part
Coupling agent 10 ~ 30 weight part
Flow agent 0.1 ~ 5 weight part
Air release agent 0.1 ~ 4 weight part
Dispersed lubricant 1 ~ 10 weight part.
2. compound 3D printed material according to claim 1, each composition weight number is as follows:
Polyetherimide (Polyetherimide) 80 ~ 100 weight part
Epoxy resin 50 ~ 80 weight part
Monocrystalline sapphire whisker 10 ~ 30 weight part
Coupling agent 10 ~ 30 weight part
Flow agent 0.1 ~ 5 weight part
Air release agent 0.1 ~ 4 weight part
Dispersed lubricant 1 ~ 10 weight part.
3. compound 3D printed material according to claim 1, described polyetherimide (Polyetherimide) for oxygen index be 47%, density is the commercially available polyetherimide of 1.28 ~ 1.42g/cm3; Described epoxy resin is commercially available glycidyl amine epoxy resin.
4. compound 3D printed material according to claim 1, described monocrystalline sapphire whisker is diameter 0.1 ~ 5 micron, and length is 5 ~ 100 microns, and density is 4g/cm3, the monocrystalline sapphire whisker that purity (wt%) is 90-99.9%.
5. compound 3D printed material according to claim 1, described coupling agent is zirconium class coupling agent; Described flow agent is polydimethylsiloxane or butyl cellulose.
6. compound 3D printed material according to claim 1, described air release agent is high-carbon type air release agent, as TYPE air release agent, Viscotrol C or butylbenzene rubber cement; Described dispersed lubricant is polyethylene wax or bis-fatty acid amides.
7. a preparation method for compound 3D printed material, a, puts into material-compound tank by epoxy resin, dispersed lubricant, coupling agent according to described formula ratio, rapid stirring 1 ~ 3h in heating unit; Monocrystalline sapphire whisker is added the mixing liquid of above-mentioned melting at ultrasonic lower concussion 10 ~ 30min by b; C, at 100 ~ 200 DEG C to add monocrystalline sapphire fiber melting mixing liquid in add polyetherimide, flow agent, air release agent, continue stirring 1 ~ 2h; D, naturally cooling, can obtain compound 3D printed material after crushing and screening.
8. the preparation method of compound 3D printed material according to claim 7, in described step a, Heating temperature is 80 ~ 120 DEG C, and stirring velocity is 400 ~ 750r/min.
9. the preparation method of compound 3D printed material according to claim 7, in step c, stirring velocity is 450 ~ 1000r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510588764.1A CN105176082A (en) | 2015-09-16 | 2015-09-16 | Composite 3D printing material and preparation method thereof |
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| CN201510588764.1A CN105176082A (en) | 2015-09-16 | 2015-09-16 | Composite 3D printing material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819743A (en) * | 2016-03-29 | 2016-08-03 | 杭州电子科技大学 | Method for preparing gem and jade devices with three-dimensional printing technology |
| CN106279817A (en) * | 2016-08-23 | 2017-01-04 | 四川金利声乐电子科技有限公司 | A kind of material for 3D printing and preparation method thereof |
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|---|---|---|---|---|
| WO1988009356A1 (en) * | 1987-05-29 | 1988-12-01 | Otsuka Kagaku Kabushiki Kaisha | Resin composition for scroll type compressor members and process for manufacturing scroll type compressor parts |
| CN1210117A (en) * | 1998-07-09 | 1999-03-10 | 厦门大学 | Production of composite material with stereospecific whisker strengthened polymer |
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| CN101410459A (en) * | 2006-03-30 | 2009-04-15 | 旭化成化学株式会社 | Resin composition and molded product thereof |
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2015
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| CN1210117A (en) * | 1998-07-09 | 1999-03-10 | 厦门大学 | Production of composite material with stereospecific whisker strengthened polymer |
| CN1659234A (en) * | 2002-04-11 | 2005-08-24 | 通用电气公司 | Filler reinforced polyether imide resin composition and molded article thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819743A (en) * | 2016-03-29 | 2016-08-03 | 杭州电子科技大学 | Method for preparing gem and jade devices with three-dimensional printing technology |
| CN106279817A (en) * | 2016-08-23 | 2017-01-04 | 四川金利声乐电子科技有限公司 | A kind of material for 3D printing and preparation method thereof |
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Application publication date: 20151223 |
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