CN104650582B - Based on selective laser sintering Quick-forming polyimides ether ketone material - Google Patents
Based on selective laser sintering Quick-forming polyimides ether ketone material Download PDFInfo
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- CN104650582B CN104650582B CN201410544649.XA CN201410544649A CN104650582B CN 104650582 B CN104650582 B CN 104650582B CN 201410544649 A CN201410544649 A CN 201410544649A CN 104650582 B CN104650582 B CN 104650582B
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- ether ketone
- polyimides
- selective laser
- laser sintering
- antioxidant
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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)
Abstract
The invention discloses a kind of polyimides ether ketone (PIEK) dusty materials for being based on selective laser sintering (Selective Laser Sintering, abbreviation SLS), and component includes: polyimides ether ketone resin, flow promortor, antioxidant；The present invention discloses the preparation methods of polyimides ether ketone material.When polyimides ether ketone powder material provided by the invention is formed for SLS, while guaranteeing excellent mechanical property, high-precision and excellent molding effect, higher heat resistance is provided, SLS product comprehensive performance is effectively improved, is particularly suitable for the manufacturing field high to product performance requirements.
Description
Technical field
The present invention relates to one kind to be based on selective laser sintering polyimides ether ketone powder material, and provides the polyimides ether
The preparation method of ketone powder material.
Background technique
Selective laser sintering (Selective Laser Sintering, abbreviation SLS) technology is last century the nineties
The new and high technology to grow up, it is integrated with the neck such as modern cnc technology, CAD/CAM technology, laser technology and new material
The new results in domain.Selective laser sintering and moulding technology mainly consists of the following steps: (1) establishing the three of product in a computer
Entity CAD model is tieed up, then layered shaping is carried out with delamination software, obtains each processing section information, and be translated into electricity
Signal controls laser scanning system work；(2) swash in the powder for molding material that shaping work table top upper berth sets one layer of dense uniform
Light beam is scanned sintering to powder for molding material according to slice section information under the control of the computer, the powder irradiated by laser beam
End melts and bonds together in subsequent cooling procedure, completes the processing of first level；(3) layer-by-layer powdering, successively sweeps
Burn-back is retouched, using above-mentioned added moulding method, finally produces Three-dimensional Entity Components.Successfully solves computer using SLS technology
In Computer Aided Design the problem of " visible, to can not touch " of three-dimensional modeling.Mock-up quickly is produced, shortens product development week
Phase.
Polymer material and engineering currently used for SLS technology has: polystyrene (PS) powder, nylon (PA) powder, ABS powder
End, polyether-ether-ketone (PEEK) powder etc..Wherein PEEK material) it is a kind of hemicrystalline thermoplastic resin, it is because of good machine
Tool performance and thermal stability are applied to the fields such as aviation.And a kind of current laser sintered heat-proof macromolecule material mainly used
Material, such as aviation field key components and parts, medical field.But the glass transition temperature (Tg) of PEEK is 143 DEG C, fusing point (Tm)
Range is at 330~350 DEG C, and design feature determines such material, and there are still the deficiencies of itself: the lower (Tg of glass transition temperature
=143 DEG C), fusing point is higher (Tm=330-350 DEG C), so that the SC service ceiling temperature of material is low, but temperature is processed in practical operation
Degree is high, and for the two there are implacable contradiction, tracing it to its cause is caused by PEEK semicrystalline structure.Therefore it is deposited in SLS forming process
In biggish contraction distortion, technique controlling difficulty is high, limits the application of such material.
The present invention provides a kind of polyimides ether ketone (PIEK) material for selective laser sintering, is a kind of amorphous new
Type high molecular material.Glass transition temperature (Tg=200 DEG C) with higher and thermal decomposition temperature (450 DEG C or more).For
Selective laser sintering overcomes SLS forming process and shrinks the problems such as change is serious, technique controlling difficulty is high.It is wide to be that one kind has
The SLS high molecular material of prospect.
Summary of the invention
It is an object of the invention to overcome SLS technological deficiency existing for high molecular material PEEK, provide a kind of for selecting
The laser sintered PIEK material of selecting property, the material provide high-fire resistance while guaranteeing excellent mechanical property and molding effect,
Improve SLS product comprehensive performance, is applicable to the manufacture neck high to product intensity, heat resistance susceptibility such as aerospace, medical treatment
Domain.
Another object of the present invention is to provide the preparation methods of above-mentioned PIEK material.
A kind of PIEK material for selective laser sintering provided by the invention, is composed of the following components: PIEK
Resin, flow promortor, antioxidant；Each component is matched by following portions by weight:
PIEK resin 94-99
Flow promortor 0.5-5
Antioxidant 0.5-1
Above-mentioned PIEK resin is provided by Qingdao Zhong Ke new material Co., Ltd.
Above-mentioned flow promortor is one or more of nano silica, nano aluminium oxide, nano calcium oxide.
Above-mentioned antioxidant is Hinered phenols antioxidant, and Hinered phenols antioxidant is preferably p-hydroxyanisole, to benzene two
Phenol, the tertiary base of 2,6- bis- are to phenyl methylcarbamate, 1,3,5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6- bis-
Tert-butyl -4- methyl-phenol, 2, one or more of 2 '-bis- (4- methyl-6-tert butyl-phenol) methane.
According to above-mentioned each group distribution ratio, the PIEK dusty material for selective laser sintering is prepared according to the following steps: will
PIEK resin, flow promortor, antioxidant are added in mixing agitator, stir evenly, and by 120 meshes, obtain for selectivity
Laser sintered PIEK dusty material.
By gained PIEK dusty material be used for SLS former AMA600 forming, gained molded part by ASTM standard into
Row performance test.
Specific implementation method
Embodiment 1
PIEK resin 950g is weighed, nano silica 45g, p-hydroxyanisole 5g are put into mixing agitator, stirring
Uniformly, 120 meshes are crossed.The laser sintered PIEK dusty material of selecting property to obtain the final product.
Above-mentioned gained PIEK dusty material, preparation technology parameter are as follows: laser power are shaped on SLS former AMA600
50W, scanning speed 2000mm/s, be sintered spacing 0.1mm, sinter layer thickness 0.1mm, 180 DEG C of preheating temperature；By gained SLS at
Shape part is tested for the property by ASTM standard.Tensile strength 67MPa, bending strength 131MPa, bending modulus 3820MPa are intact
Mouth impact strength 191J/m2, 205 DEG C of glass transition temperature, 457 DEG C of thermal decomposition start temperature (weightlessness 5%).
Embodiment 2
PIEK resin 980g is weighed, nano silica 12g, p-hydroxyanisole 8g are put into mixing agitator, stirring
Uniformly, 120 meshes are crossed.The laser sintered PIEK dusty material of selecting property to obtain the final product.
Above-mentioned gained PIEK dusty material, preparation technology parameter are as follows: laser power are shaped on SLS former AMA600
50W, scanning speed 2000mm/s, be sintered spacing 0.1mm, sinter layer thickness 0.1mm, 180 DEG C of preheating temperature；By gained SLS at
Shape part is tested for the property by ASTM standard.Tensile strength 71MPa, bending strength 134MPa, bending modulus 3870MPa are intact
Mouth impact strength 193J/m2, 204 DEG C of glass transition temperature, 460 DEG C of thermal decomposition start temperature (weightlessness 5%).
Embodiment 3
PIEK resin 980g, nano calcium oxide 10g are weighed, to the tertiary base of 2,6- bis- to phenyl methylcarbamate 10g, is put into mixing agitator
In, it stirs evenly, crosses 120 meshes.The laser sintered PIEK dusty material of selecting property to obtain the final product.
Above-mentioned gained PIEK dusty material, preparation technology parameter are as follows: laser power are shaped on SLS former AMA600
50W, scanning speed 2000mm/s, be sintered spacing 0.1mm, sinter layer thickness 0.1mm, 180 DEG C of preheating temperature；By gained SLS at
Shape part is tested for the property by ASTM standard.Tensile strength 73MPa, bending strength 137MPa, bending modulus 3900MPa are intact
Mouth impact strength 197J/m2, 208 DEG C of glass transition temperature, 465 DEG C of thermal decomposition start temperature (weightlessness 5%).
Embodiment 4
Weigh PIEK resin 960g, nano-silica aluminium 30g, p-hydroxyanisole 10g are put into mixing agitator, stir
Uniformly, 120 meshes are crossed.The laser sintered PIEK dusty material of selecting property to obtain the final product.
Above-mentioned gained PIEK dusty material, preparation technology parameter are as follows: laser power are shaped on SLS former AMA600
50W, scanning speed 2000mm/s, be sintered spacing 0.1mm, sinter layer thickness 0.1mm, 180 DEG C of preheating temperature；By gained SLS at
Shape part is tested for the property by ASTM standard.Tensile strength 70MPa, bending strength 135MPa, bending modulus 3890MPa are intact
Mouth impact strength 195J/m2, 207 DEG C of glass transition temperature, 461 DEG C of thermal decomposition start temperature (weightlessness 5%).
Claims (3)
1. the polyimides ether ketone powder material based on selective laser sintering, it is characterised in that the polyimides ether ketone powder material
Material is composed of the following components: polyimides ether ketone resin, flow promortor, antioxidant；
The each component is matched by following portions by weight: polyimides ether ketone resin 94-99 flow promortor 0.5-5 antioxidant 0.5-1；
The antioxidant is Hinered phenols antioxidant；Hinered phenols antioxidant is p-hydroxyanisole, hydroquinone, 2,6-
Two tertiary bases are to phenyl methylcarbamate, 1,3,5- trimethyls -2,4,6- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene, 2,6- di-t-butyl -
4- methyl-phenol, 2, one or more of 2 '-bis- (4- methyl-6-tert butyl-phenol) methane.
2. material according to claim 1, it is characterized in that the flow promortor be nano silica, it is nano oxidized
One or more of aluminium, nano calcium oxide.
3. the preparation method of the polyimides ether ketone powder described in claim 1 based on selective laser sintering, are as follows: by poly- Asia
Amidogen ether ketone powder adds in mixing agitator, then adds flow promortor, antioxidant, stirs evenly, and by 120 meshes, is made described
The polyimides ether ketone powder material based on selective laser sintering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410544649.XA CN104650582B (en) | 2014-09-30 | 2014-09-30 | Based on selective laser sintering Quick-forming polyimides ether ketone material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410544649.XA CN104650582B (en) | 2014-09-30 | 2014-09-30 | Based on selective laser sintering Quick-forming polyimides ether ketone material |
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| CN104650582A CN104650582A (en) | 2015-05-27 |
| CN104650582B true CN104650582B (en) | 2019-03-19 |
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| CN114437500B (en) * | 2021-12-22 | 2023-06-30 | 重庆交通大学绿色航空技术研究院 | Polyether-ether-ketone composite powder for laser selective sintering and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827689A (en) * | 2004-12-21 | 2006-09-06 | 德古萨公司 | Polyarylene ether ketone powder, molding containing the same and method for preparing the same |
| CN102886900A (en) * | 2011-07-21 | 2013-01-23 | 赢创德固赛有限公司 | Improved component characteristics through rays in laser sintering |
| CN103709737A (en) * | 2013-12-05 | 2014-04-09 | 吴江中瑞机电科技有限公司 | High-molecular composite powder material for SLS and preparation method therefor |
-
2014
- 2014-09-30 CN CN201410544649.XA patent/CN104650582B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1827689A (en) * | 2004-12-21 | 2006-09-06 | 德古萨公司 | Polyarylene ether ketone powder, molding containing the same and method for preparing the same |
| CN102886900A (en) * | 2011-07-21 | 2013-01-23 | 赢创德固赛有限公司 | Improved component characteristics through rays in laser sintering |
| CN103709737A (en) * | 2013-12-05 | 2014-04-09 | 吴江中瑞机电科技有限公司 | High-molecular composite powder material for SLS and preparation method therefor |
Non-Patent Citations (2)
| Title |
|---|
| "聚亚胺酮系列聚合物研究进展";张林等;《功能材料》;20101231;第2010年论文集卷;388-392 |
| "聚亚胺醚酮的分子设计、合成及玻璃化转变的分子模拟";徐艺等;《高分子材料科学与工程》;20121231;第28卷(第12期);1-4 |
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Granted publication date: 20190319 Termination date: 20200930 |