CN106380610B - The preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies - Google Patents
The preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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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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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/06—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/06—Polysulfones; Polyethersulfones
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Abstract
The present invention provides a kind of laser sintering (SLS) 3D printing preparation methods of polyether sulfone powder supplies, include the following steps：(1) polyether sulfone is placed in the feed bin in Lowtemperaturepulverizer, the liquid nitrogen built in the feed bin is used to polyether sulfone being cooled to 130 DEG C~196 DEG C；(2) polyether sulfone after cooling in step (1) is crushed, it is 110 DEG C~196 DEG C to crush temperature, obtains polyether sulfone just powder；(3) after being sieved the first powder of polyether sulfone in step (2), 100 DEG C are played gradient increased temperatures drying, and heating frequency is 2 DEG C/min~8 DEG C/min, freeze-day with constant temperature 0.5h~2h after being warming up to 130 DEG C；(4) powder being crushed in step (3) is added in grinder, is fully ground to obtain polyether sulfone crude product；(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 2 DEG C/min~8 DEG C/min, freeze-day with constant temperature 0.5h~1h after being warming up to 150 DEG C, obtains laser sintering and moulding 3D printing polyether sulfone powder supplies.
Description
Technical field
The present invention relates to rapid shaping fields, more particularly it relates to a kind of laser sintering (SLS) 3D printing polyethers
The preparation method of sulfone powder supplies.
Background technology
3D printing technique is as emerging material material molding technology, it has also become the important symbol of the 3rd industrial revolution it
One.3D printing originates from late 1970s to the beginning of the eighties, and crucial technical advantage is quick using digitlization means
The labyrinth product for manufacturing unlike material, can be applied to some high-precision advanced manufacturing fields, technical process energy-saving material-saving.
Traditional subtracts material manufacturing technology, general using the methods of cutting, grinding, corrosion and melting, obtains the product of specific shape, then lead to
It crosses the methods of assembled, welding and is combined into product, fabrication cycle is longer, complex procedures, and product rejection rate is high, of high cost.It carries on the back herein
Under scape, 3D printing rapid shaping technique has gradually developed.
Selective laser sintering (selectivelasersintering, SLS) is a kind of 3D printing technique.SLS technology bases
In discrete dynamics models manufacturing theory, by part three-dimensional entity model file along Z-direction hierarchy slicing, and stl file is generated, protected in file
The cross section information of material object parts is deposited, the heat effect of laser is then utilized, according to the slice information of part, by solid powder material
Accumulation is bonded layer by layer, finally shapes part prototype or function part.
Agglomerated material is the key link of SLS technologies development, its forming speed and precision and its physical machine to sintered part
Tool performance plays decisive role, directly influence sintered part application and SLS technologies and other rapid prototyping technologies it is competing
Strive power.Therefore, it is all studying energetically in the influential company of SLS technical aspects such as 3D (DTM), EOS Corp. and laser is provided
Agglomerated material has many scientific research institutions and some to be engaged in the research that the specialized company that material produces is also added to laser sintered material
In exploitation.A variety of laser sintered materials have been developed at present, can be divided into following a few classes by material character：Metal base powder material
Material, ceramic based powdered material, precoated sand, polymer material and engineering etc..Wherein polymer material and engineering include makrolon (PC),
Polystyrene (PS), high impact polyethylene (HIPS).But there are dusty material dispersing uniformity difference to lack for these high molecular materials
It falls into.On the other hand, these materials when carrying out laser sintered due to apparent viscosity height, it is difficult to form fine and close sintered part, it is higher
Porosity cause the mechanical property of sintered part well below the ontology mechanical property of material, therefore, with such polymer make
Sintered part cannot be directly used as functor.The intensity for improving polymer laser sintered part relies primarily on post-processing, and sintered part
The degree that intensity improves depends on the compatibility of agglomerated material and impregnating resin.Therefore, polymerization of the selection for making functor
Object will more consider the compatibility with impregnating resin other than the laser sintered performance of material to be considered.
Polyether sulfone is made with diphenyl ether condensation by the bis- sulphonyl chlorodiphenyl ethers of 4,4'- under anhydrous ferric chloride catalysis.Refraction
Rate 1.85,225 DEG C of glass transition temperature, heat distortion temperature 203 DEG C (1.82MPa).Heat resistance is long between polysulfones and polyarylsulfone (PAS)
180-200 DEG C of phase temperature in use.Ageing-resistant performance is excellent, in 180 DEG C of uses up to 20 years.The good of flame resistance even if burning not
Smoke.Creep resistant is good, and the strain under 150 DEG C and 20MPa pressure only has 2.55%.Polyethersulfone resin (PES) is Britain ICI
A kind of thermoplastic macromolecule material for excellent combination property that company developed in 1972 is the spies few in number being applied
One of kind engineering plastics.It has excellent heat resistance, physical mechanical property, insulation performance etc., and especially having can be
Under high temperature be used continuously and remained in temperature environment jumpy retention property stablize outstanding advantages of, many fields
Through being used widely.But the application in some high-tech sectors at present, such as laser sintering (SLS) 3D printing field, polyether sulfone
There is no be widely used as printed material.
High molecular material applied to SLS technologies should be 10 microns or more, 100 microns of dusty materials below.Powder grain
The too small influence powdering effect of diameter, can then lead to alias very much greatly.In general, high molecular material is due to its distinctive viscoelastic
Property, directly crushing at normal temperatures can make high molecular material be bonded together again because material temperature increases, and crush efficiency is relatively low.
Therefore, generally there are two types of methods for Direct Laser sintering macromolecule and its composite material preparation at present：Deep cooling ballistic method and solvent
The precipitation method.
Deep cooling ballistic method is to make high molecular material that can lead to embrittlement because molecular chain movement ability declines at low temperature, utilizes this
Deep cooling ballistic method may be used to prepare polymer material and engineering in one characteristic.Shape of particle is irregular, and granule size is uneven,
It is difficult to once reach the grain size of desirable amount.Particle diameter distribution is needed repeatedly to sieve, could be used after crushing.Screening, powder repeatedly
It is broken to increase cost, it is therefore necessary to develop a kind of method preparing polyether sulfone powder supplies so that after deep cooling crush,
Powder after crushing is carried out once to prepare the high temperature resistant suitable for 3D printing technique and dipping in regrinding drying process
Polyether sulfone consumptive material of the resin with good compatibility, with uniform grain size, without adding binder, can be conveniently and efficiently
The component of precision, abnormal shape, complexity, high mechanical strength, good stability of the dimension is shaped, and can be used to prepare now unmanned winged
Many parts on machine, microrobot, such as miniature gears, miniature bent axle, miniature connecting rod.
Invention content
The present invention provides a kind of preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies, including following step
Suddenly：
(1) polyether sulfone is placed in the feed bin in Lowtemperaturepulverizer, it is using the liquid nitrogen built in the feed bin that polyether sulfone is cold
But -130 DEG C~-196 DEG C "；
(2) polyether sulfone after cooling in step (1) is crushed, it is -110 DEG C~-196 DEG C to crush temperature, obtains polyether sulfone
First powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 2 DEG C/min~8 DEG C/min, freeze-day with constant temperature 0.5h~2h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, is fully ground to obtain polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 2 DEG C/min~8
DEG C/min, freeze-day with constant temperature 0.5h~1h after being warming up to 150 DEG C, obtain laser sintering and moulding 3D printing polyether sulfone powder supplies.
In one embodiment, the grain size of the polyether sulfone powder is 10 μm -100 μm.
In one embodiment, cooling temperature is -140 DEG C~-180 DEG C in the step (1)
In one embodiment, cooling temperature is -150 DEG C~-170 DEG C in the step (1).
In one embodiment, it is -110 DEG C~-180 DEG C that temperature is crushed in the step (2).
In one embodiment, time 1.2h~1.8h of step (4) grinding.
In one embodiment, time 1.4h~1.6h of step (4) grinding.
In one embodiment, the heating frequency in the step (3), step (5) be 4 DEG C/min~6 DEG C/
min。
In one embodiment, the heating frequency in the step (3), step (5) is 5 DEG C/min.
Another aspect of the present invention provides a kind of laser sintering (SLS) 3D printing polyether sulfone powder, using the preparation
Method is prepared.
Compared with prior art, beneficial effects of the present invention：
Preparation method provided by the invention uses gradient increased temperature process, shortens the arid cycle of polyether sulfone so that polyethers
Sulfone is effectively dried, and the frequency of the gradient increased temperature used has efficiently controlled water in polyether sulfone for 2 DEG C/min~8 DEG C/min
Point, impurity go out, the polyether sulfone powder for preparing uniform grading provides guarantee.On the other hand, in deep cooling crush method
After obtaining the first powder of polyether sulfone, using the method for drying-grinding-drying so that the size tunable of polyether sulfone has obtained and dipping
Polyether sulfone powder supplies of the resin with good compatibility, with uniform grain size, without adding binder, overcome existing
The powder diameter that deep cooling ballistic method obtains is uneven, it is difficult to become good laser sintering (SLS) 3D printing polyether sulfone powder supplies
Deficiency, saved production cost, it is simple for process, be suitble to industrialization continuous production.
Specific implementation mode
The present invention provides a kind of preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies, including following step
Suddenly：
(1) polyether sulfone is placed in the feed bin in Lowtemperaturepulverizer, it is using the liquid nitrogen built in the feed bin that polyether sulfone is cold
But -130 DEG C~-196 DEG C "；
(2) polyether sulfone after cooling in step (1) is crushed, it is -110 DEG C~-196 DEG C to crush temperature, obtains polyether sulfone
First powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 2 DEG C/min~8 DEG C/min, freeze-day with constant temperature 0.5h~2h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, is fully ground to obtain polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 2 DEG C/min~8
DEG C/min, freeze-day with constant temperature 0.5h~1h after being warming up to 150 DEG C, obtain laser sintering and moulding 3D printing polyether sulfone powder supplies.
Selective Laser Sintering
Selective Laser Sintering (SelectiveLaserSintering) is one important in rapid shaping technique
Branch, it is integrated with Fundamental Course of Mechanic Manufacturing, laser technology, material science, modern scientist engineering, computer technology, modern test
The technologies such as technology and CAD/CAM theoretical foundations and application.The technology can manufacture out part prototype in a relatively short period of time
And mold, it is widely used in the every field of machine-building.The technology is based on layering-principle of stacking, and profit is computerizedd control
The movement locus of high energy laser beam utilizes the high energy melting metal powder of laser beam, after waiting for that laser facula is removed, molten metal
Quickly solidification again.Whole process be exactly laser facula movement from point to surface, then by the process in face to body, each part be by
Forming face is layering.The technology path of SLS process is corresponding CAD model to be established first against part, by mould
Type imports formation system and carries out step section, and each layer obtained is sliced the geological information for including section, generates STL format texts
Part.Then the track that high energy laser beam is sliced along each layer under control of the computer is scanned, and is melted in the region
Metal powder.It waits for repaving next layer of powder after one layer, repeats above procedure until part forming.
Laser sintered 3D printing polyether sulfone powder supplies molding application, feature on 3D printer are：By laser
Sintering 3D printing polyether sulfone powder supplies are added in the powder supply cylinder of selective laser sintering and moulding machine, and powdering idler wheel is by powder material
Material is equably layered in processing plane and is heated to processing temperature, and laser sends out laser, and computer controlled laser is opened
The angle of pass and scanner so that laser beam is scanned in processing plane according to corresponding two-dimensional slice shape, laser beam
After inswept, workbench moves down a thickness, then powdering, and laser beam flying obtains laser sintered part repeatedly, wherein swashing
The mode that light beam scans in processing plane scans for subregion.
The preheating temperature of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 70~85 DEG C；Preferably, described
The preheating temperature of laser sintering and moulding 3D printing polyether sulfone powder supplies is 70~80 DEG C；It is highly preferred that it is described it is laser sintered at
The preheating temperature of type 3D printing polyether sulfone powder supplies is 75 DEG C.
The input energy density of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.1~0.4J/mm3；It is excellent
The input energy density of selection of land, the laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.2~0.3J/mm3；More preferably
The input energy density on ground, the laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.28J/mm3.
The laser power of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 10~60W；Preferably, described to swash
The laser power of light sinter molding 3D printing polyether sulfone powder supplies is 15~30W.
The sweep speed of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 1500~2000mm/s；It is preferred that
The sweep speed on ground, the laser sintering and moulding 3D printing polyether sulfone powder supplies is 1800~2000mm/s；It is highly preferred that institute
The sweep speed for stating laser sintering and moulding 3D printing polyether sulfone powder supplies is 1900mm/s.
The sintering spacing of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.1~0.2mm；Preferably, institute
The sintering spacing for stating laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.15~0.18mm；It is highly preferred that the laser
The sintering spacing of sinter molding 3D printing polyether sulfone powder supplies is 0.16mm.
The thickness in monolayer of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.1~0.2mm；Preferably, institute
The thickness in monolayer for stating laser sintering and moulding 3D printing polyether sulfone powder supplies is 0.12~0.18mm；It is highly preferred that the laser
The thickness in monolayer of sinter molding 3D printing polyether sulfone powder supplies is 0.16mm.
The present invention uses vibromill deep cooling crush.Material is cooled down in hopper with immersing in liquid nitrogen, is entered through screw(-type) feeder
Vibromill, and carry out deep cooling crush.As needed, liquid nitrogen is also added in pulverizer, to keep crushing at a lower temperature.
Grinding device includes feed hopper, liquid nitrogen tank, vibrator, warehouse for finished product, air blower, batcher, cooling storehouse, airtight valve.
Cooling storehouse is added from top in material, moves down；Liquid nitrogen is added from bottom and moves up.This reverse movement impregnates
Formula cools down, and material can be cooled to -130 DEG C~-196 DEG C.The cooling device of low-temperature grinding includes feed bin, screw(-type) feeder, guarantor
Warm layer, star valve, liquid nitrogen entrance.
The grinder is the desk-top flour mills of Guangzhou great Xiang electro mechanical devices Co., Ltd DX-40, motor speed
1420r/min。
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -196 DEG C, cooling 3h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -196 DEG C to crush temperature, crushes 1.5h,
Obtain polyether sulfone just powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 5 DEG C/min, freeze-day with constant temperature 2h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grinding
2h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 5 DEG C/min, is risen
Temperature obtains laser sintering and moulding 3D printing polyether sulfone powder supplies to freeze-day with constant temperature 1h after 150 DEG C.
Embodiment 2
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -180 DEG C, cooling 3.5h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -180 DEG C to crush temperature, crushes 1.5h,
Obtain polyether sulfone just powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 5 DEG C/min, freeze-day with constant temperature 2h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grinding
1.8h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 5 DEG C/min, is risen
Temperature obtains laser sintering and moulding 3D printing polyether sulfone powder supplies to freeze-day with constant temperature 1h after 150 DEG C.
Embodiment 3
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -140 DEG C, cooling 4h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -150 DEG C to crush temperature, crushes 2h, obtains
To powder at the beginning of polyether sulfone；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 5 DEG C/min, freeze-day with constant temperature 0.5h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, is fully ground under the conditions of 1420r/min, ground
1.6h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 5 DEG C/min, is risen
Temperature obtains laser sintering and moulding 3D printing polyether sulfone powder supplies to freeze-day with constant temperature 1h after 150 DEG C.
Embodiment 4
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -196 DEG C, cooling 3h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -196 DEG C to crush temperature, crushes 1.5h,
Obtain polyether sulfone just powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 5 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grinding
2h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 5 DEG C/min, is risen
Temperature to freeze-day with constant temperature 0.5h after 150 DEG C, obtain laser sintering and moulding 3D printing polyether sulfone powder supplies.
Embodiment 5
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -130 DEG C, cooling 2h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -110 DEG C to crush temperature, crushes 2h, obtains
To powder at the beginning of polyether sulfone；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 2 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grinding
2h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 6 DEG C/min, is risen
Temperature to freeze-day with constant temperature 0.5h after 150 DEG C, obtain laser sintering and moulding 3D printing polyether sulfone powder supplies.
Embodiment 5
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -140 DEG C, cooling 2.5h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is 134 DEG C to crush temperature, crushes 1.5h,
Obtain polyether sulfone just powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 4 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grinding
2h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 6 DEG C/min, is risen
Temperature obtains laser sintering and moulding 3D printing polyether sulfone powder supplies to freeze-day with constant temperature 0.5h after 150 DEG C.
Embodiment 6
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -162 DEG C, cooling 2h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -196 DEG C to crush temperature, crushes 2.5h,
Obtain polyether sulfone just powder；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradients
Heat up drying, and heating frequency is 8 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grinding
2h obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played to gradient increased temperature drying at 100 DEG C, heating frequency is 8 DEG C/min, is risen
Temperature obtains laser sintering and moulding 3D printing polyether sulfone powder supplies to freeze-day with constant temperature 0.5h after 150 DEG C.
Comparative example 1
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) polyether sulfone is placed in the feed bin in Lowtemperaturepulverizer, the liquid nitrogen built in the feed bin is used for polyether sulfone is cold
But to -198 DEG C；
(2) polyether sulfone after cooling in step (1) is pulverized, it is -198 DEG C to crush temperature, obtains polyether sulfone just powder.
Comparative example 2
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder supplies, includes the following steps：
(1) cooling storehouse is added from top in 10g polyether sulfones, moved down；Liquid nitrogen is added from bottom and moves up, reverse to transport
Material is cooled to -196 DEG C, cooling 2h by dynamic immersion type cooling；
(2) polyether sulfone after cooling is crushed by vibrator in step (1), and it is -196 DEG C to crush temperature, crushes 2.5h,
Obtain polyether sulfone just powder；
(3) it after powder at the beginning of being warmed to room temperature polyether sulfone in step (2) is sieved, is placed in control heat riser, 130 DEG C of items
Dry 0.5h under part；
(4) powder being crushed in step (3) is added in grinder, under the conditions of 1420r/min, grinds 1.2h, obtain
To polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is placed in heat riser, dry 0.5h, obtains laser under the conditions of 150 DEG C
Sinter molding 3D printing polyether sulfone powder supplies.
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, comparative example 2 are auspicious greatly using Guangzhou
The desk-top flour mills of electro mechanical devices Co., Ltd DX-40, motor speed 1420r/min.
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, comparative example 1,2 granularity of comparative example are surveyed
The pilot production American-European gram Instrument Ltd.'s electric-resistivity method particle size analyzer image method particle size analyzer in Zhuhai.
1 particle size range test result of table
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, comparative example 1, comparative example 2 are prepared into
The laser sintering and moulding 3D printing polyether sulfone powder supplies arrived, the molding application on 3D printer.
Laser sintered 3D printing polyether sulfone powder supplies are added in the powder supply cylinder of selective laser sintering and moulding machine, are spread
Dusty material is equably layered in processing plane and is heated to processing temperature by powder idler wheel, and laser sends out laser, computer
Control laser switch and scanner angle so that laser beam processing plane on according to corresponding two-dimensional slice shape into
Row scanning, after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying obtains laser repeatedly
The mode that sintered part, wherein laser beam scan in processing plane scans for subregion；The laser sintering and moulding 3D printing is poly-
The preheating temperature of ether sulfone powder supplies is 76 DEG C；The input energy of the laser sintering and moulding 3D printing polyether sulfone powder supplies is close
Degree is 0.25J/mm3；The laser power of the laser sintering and moulding 3D printing polyether sulfone powder supplies is 16W；The laser is burnt
The sweep speed for forming type 3D printing polyether sulfone powder supplies is 1800mm/s；The laser sintering and moulding 3D printing polyether sulfone powder
The sintering spacing of last consumptive material is 0.15mm；The thickness in monolayer of the laser sintering and moulding 3D printing polyether sulfone powder supplies is
0.15mm.The result that the polyether sulfone 3D printing finished product being prepared by the polyether sulfone powder is tested for the property is as follows.
Performance test
Tensile property:Test for tensile strength is carried out on CMT5504 type electronic universal mechanics machines, by GB/T1040-
Standard batten, tensile speed 5mm/s is made in 1992 standards.
Bending property:Bending property experiment is carried out on CMT5504 type electronic universal mechanics machines, by GB/T9341-
Standard batten, test speed 2mm/min is made in 2008 standards.
Non-notch sample simple beam impact strength:It is impacted on XJC-25Z type mechanical combination balance weight impact testing machines
Experiment, standard batten, impact energy 2J are made by GB/T1043-1993.
2 the performance test results of table
From above-mentioned granularity, the performance test results as can be seen that when the process using gradient increased temperature impacts legal system to deep cooling
It when the first powder of standby obtained polyether sulfone is dried, obtains polyether sulfone powder diameter and is evenly distributed, have with impregnating resin good
Compatibility well, the polyether sulfone consumptive material without adding binder.It is to apply condition almost without external force by laser sintered principle
Lower rapidoprint makes the drip molding being sintered out have very strong physical property and chemical property, and the contrived experiment material proposed
The scheme of material is easy quickly, great reduced time and economizes on resources.
Preparation method provided by the invention uses gradient increased temperature process, shortens the arid cycle of polyether sulfone so that polyethers
Sulfone is effectively dried, and the frequency of the gradient increased temperature used is effectively controlled water in polyether sulfone for 2 DEG C/min~8 DEG C/min
Point, impurity go out, the polyether sulfone powder for preparing uniform grading provides guarantee.On the other hand, in deep cooling crush method
After obtaining the first powder of polyether sulfone, using the method for drying-grinding-drying so that the size tunable of polyether sulfone has obtained and dipping
Polyether sulfone powder supplies of the resin with good compatibility, with uniform grain size, without adding binder, overcome existing
The powder diameter that deep cooling ballistic method obtains is uneven, it is difficult to become good laser sintering (SLS) 3D printing polyether sulfone powder supplies
Deficiency, saved production cost, it is simple for process, be suitble to industrialization continuous production.
Embodiment above-mentioned is merely illustrative, some features for explaining the method for the invention.Appended right
It is required that it is intended to the range as wide as possible for requiring to be contemplated that, and embodiments as presented herein is only according to all possible reality
Apply the explanation of the embodiment of the selection of the combination of example.Therefore, the purpose of applicant is that the attached claims are not illustrated this
The exemplary selectional restriction of the feature of invention.Some numberical ranges used also include son in the claims
Range, the variation in these ranges should also be construed to be covered by the attached claims in the conceived case.
Claims (10)
1. a kind of preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies, which is characterized in that including walking as follows
Suddenly：
(1) by polyether sulfone be placed in Lowtemperaturepulverizer in feed bin in, using the liquid nitrogen built in the feed bin by polyether sulfone cooling-
130 DEG C~-196 DEG C "；
(2) polyether sulfone after cooling in step (1) is crushed, it is -110 DEG C~-196 DEG C to crush temperature, obtains polyether sulfone just powder
End；
(3) it after being sieved the first powder of polyether sulfone in step (2), is placed in controllable heat riser, 100 DEG C are played gradient increased temperatures
Dry, heating frequency is 2 DEG C/min~8 DEG C/min, freeze-day with constant temperature 0.5h~2h after being warming up to 130 DEG C；
(4) powder being crushed in step (3) is added in grinder, is fully ground to obtain polyether sulfone crude product；
(5) by polyether sulfone crude product in step (4) at 100 DEG C rise gradient increased temperature drying, heating frequency for 2 DEG C/min~8 DEG C/
Min, freeze-day with constant temperature 0.5h~1h after being warming up to 150 DEG C obtain laser sintering and moulding 3D printing polyether sulfone powder supplies.
2. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as described in claim 1, feature exist
In the grain size of the polyether sulfone powder is 10 μm -100 μm.
3. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as described in claim 1, feature exist
In cooling temperature is -140 DEG C~-180 DEG C in the step (1).
4. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as claimed in claim 3, feature exist
In cooling temperature is -150 DEG C~-170 DEG C in the step (1).
5. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as described in claim 1, feature exist
In it is -110 DEG C~-180 DEG C to crush temperature in the step (2).
6. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as described in claim 1, feature exist
In time 1.2h~1.8h of step (4) grinding.
7. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as claimed in claim 6, feature exist
In time 1.4h~1.6h of step (4) grinding.
8. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as described in claim 1, feature exist
In the heating frequency in the step (3), step (5) is 4 DEG C/min~6 DEG C/min.
9. the preparation method of laser sintering (SLS) 3D printing polyether sulfone powder supplies as claimed in claim 8, feature exist
In the heating frequency in the step (3), step (5) is 5 DEG C/min.
10. a kind of laser sintering (SLS) 3D printing polyether sulfone powder, which is characterized in that use claim 1-9 any one
Preparation method described in claim is prepared.
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| CN108976796A (en) * | 2018-07-09 | 2018-12-11 | 湖南华曙高科技有限责任公司 | Polyaryl thioether sulfone composite material and preparation method for selective laser sintering |
| CN109749442B (en) * | 2018-12-17 | 2021-07-23 | 浙江大学宁波理工学院 | Polyimide powder material for selective laser sintering and preparation method and application thereof |
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| CN104109343A (en) * | 2014-08-01 | 2014-10-22 | 中国科学院重庆绿色智能技术研究院 | High-flowability plastic composite powder material and preparation method thereof |
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| CN104109343A (en) * | 2014-08-01 | 2014-10-22 | 中国科学院重庆绿色智能技术研究院 | High-flowability plastic composite powder material and preparation method thereof |
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