CN106380610A - Method for preparing polyether sulfone powder consumable item for 3D printing of laser sintering and molding - Google Patents
Method for preparing polyether sulfone powder consumable item for 3D printing of laser sintering and molding Download PDFInfo
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- CN106380610A CN106380610A CN201610846566.5A CN201610846566A CN106380610A CN 106380610 A CN106380610 A CN 106380610A CN 201610846566 A CN201610846566 A CN 201610846566A CN 106380610 A CN106380610 A CN 106380610A
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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 invention provides a method for preparing a polyether sulfone powder consumable item for 3D printing of laser sintering and molding, comprising the following steps: (1) placing polyether sulfone in a stock bin of a low-temperature mill, liquid nitrogen in the stock bin being used for cooling polyether sulfone to -130 DEG C to -196 DEG C; (2) smashing polyether sulfone cooled in step (1) with a smashing temperature of -110 DEG C to -196 DEG C, so as to obtain initial polyether sulfone powder; (3) after screening the initial polyether sulfone powder in step (2), drying the same by gradient temperature increase from 100 DEG C, a temperature increasing frequency being 2 DEG C/min-8 DEG C/min, and drying at a constant temperature for 0.5 h to 2 h after the temperature is increased to 130 DEG C; (4) adding smashed powder in step (3) into a grinding miller, and fully grinding to obtain a polyether sulfone raw product; and (5) drying the polyether sulfone raw product in step (4) at an increased temperature by gradient temperature increase from 100oC,the temperature increasing frequency being 2 DEG C/min-8 DEG C/min, and drying at a constant temperature for 0.5 h to 2 h after the temperature is increased to 150 DEG C, so as to obtain the polyether sulfone powder consumable item for 3D printing of laser sintering and molding.
Description
Technical field
A kind of the present invention relates to rapid shaping field, more particularly it relates to laser sintering (SLS) 3D printing polyethers
The preparation method of sulfone powder consumptive material.
Background technology
3D printing technique is as emerging materials processing forming technique, 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 its crucial technical advantage is quick using digitlization means
Manufacture the labyrinth product of unlike material, can be applicable to some high-grade, precision and advanced advanced manufacture fields, technical process energy-saving material-saving.
Traditional subtracts material manufacturing technology, typically adopts the method such as cutting, grinding, corrosion and melting, obtains the product of given shape, then lead to
Cross the Combination of Methods such as assembled, welding and become product, fabrication cycle is longer, complex procedures, and product rejection rate is high, high cost.Here is carried on the back
Under scape, 3D printing rapid shaping technique gradually grows up.
Selective laser sintering (selective laser sintering, SLS) is a kind of 3D printing technique.SLS technology
Based on discrete dynamics models manufacturing theory, by part three-dimensional entity model file along Z-direction hierarchy slicing, and generate stl file, in file
The cross section information of in store material object parts, then utilizes the heat effect of laser, according to the slice information of part, by pressed powder material
Bed of material layer bonding is piled up, and finally shapes part prototype or function part.
Agglomerated material is the key link of SLS technology development, and it is to the forming speed of sintered part and precision and its physical machine
Tool performance plays decisive role, directly influences the competing of the application of sintered part and SLS technology and other RP techniques
Strive power.Therefore, all studying energetically and laser is being provided in the influential company of SLS technical elements such as 3D (DTM), EOS Corp.
Agglomerated material, has the specialized company that a lot of scientific research institutions are engaged in material production with some to be also added to the research of laser sintered material
In the middle of exploitation.Develop multiple laser sintered material at present, following a few class can be divided into 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 Merlon (PC),
Polystyrene (PS), high impact polyethylene (HIPS).But there is lacking of dusty material dispersing uniformity difference in these macromolecular materials
Fall into.On the other hand, these materials when carrying out laser sintered because apparent viscosity is high it is difficult to form fine and close sintered part, higher
Porosity lead to the body mechanical property well below material for the mechanical property of sintered part, therefore, make of such polymer
Sintered part can not be directly used as functor.The intensity 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, select the polymerization for making functor
Thing, in addition to the laser sintered performance of material to be considered, more will consider the compatibility with impregnating resin.
Polyether sulfone is by the double sulphonyl chlorodiphenyl ether of 4,4'- under anhydrous ferric chloride catalysis, prepared with diphenyl ether condensation.Refraction
Rate 1.85,225 DEG C of vitrification point, 203 DEG C of heat distortion temperature (1.82MPa).Heat resistance is between polysulfones and polyarylsulfone (PAS), long
Phase uses temperature 180-200 DEG C.Ageing-resistant performance is excellent, in 180 DEG C of uses up to 20 years.Even if flame resistance is good. burn also not
It is fuming.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 of excellent combination property in exploitation in 1972 for the company, is the spy few in number being applied
Plant one of engineering plastics.It has excellent heat resistance, physical and mechanical properties, insulating properties etc., and particularly having can be
Continuously use under high temperature and remain to keep the outstanding advantages such as stable performance, in many fields in temperature environment jumpy
Through being used widely.But the application in some high-tech sectors at present, such as laser sintering (SLS) 3D printing field, polyether sulfone
It is not widely used as printed material.
The macromolecular material being applied to SLS technology should be more than 10 microns, less than 100 microns of dusty material.Powder grain
The too little impact powdering effect in footpath, then can lead to alias greatly very much.In general, macromolecular material is due to its distinctive viscoelastic
Property, directly pulverizing at normal temperatures understands because material temperature raises make macromolecular material again be bonded together, and crush efficiency is relatively low.
Therefore, current Direct Laser sintering macromolecule and its composite preparation typically have two methods：Deep cooling ballistic method and solvent
The precipitation method.
Deep cooling ballistic method is to make macromolecular material can lead to embrittlement because molecular chain movement ability declines at low temperature, utilizes this
One characteristic, can prepare polymer material and engineering using deep cooling ballistic method.Shape of particle is irregular, and granule size is uneven,
It is difficult to once reach the particle diameter of desirable amount.Particle diameter distribution, could use after the multiple screening of needs, pulverizing.Screening, powder repeatedly
Broken increased cost it is therefore necessary to develop a kind of method preparing polyether sulfone powder consumptive material so that after deep cooling crush,
Powder after pulverizing is carried out, once in regrinding dry run, prepare and be suitable to the high temperature resistant of 3D printing technique and dipping
Resin has good compatibility, the polyether sulfone consumptive material having uniform particle diameter, need not adding binding agent, can be conveniently and efficiently
Shape precision, abnormal shape, the part of complexity, high mechanical strength, good stability of the dimension, and can be used to prepare now unmanned winged
Many parts on machine, microrobot, such as miniature gears, miniature bent axle, miniature connecting rod.
Content of the invention
The present invention provides a kind of preparation method of laser sintering (SLS) 3D printing polyether sulfone powder consumptive material, walks including following
Suddenly：
(1) polyether sulfone is inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for polyether sulfone is cold
But to -130 DEG C～-196 DEG C；
(2) polyether sulfone after cooling in step (1) is pulverized, pulverize temperature and be -110 DEG C～-196 DEG C, obtain polyether sulfone
Just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification 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 pulverized in step (3) is added in grinder, be fully ground and obtain polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification 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 consumptive material.
In one embodiment, the particle diameter of described polyether sulfone powder is 10 μm -100 μm.
In one embodiment, in described step (1), chilling temperature is -140 DEG C～-180 DEG C
In one embodiment, in described step (1), chilling temperature is -150 DEG C～-170 DEG C.
In one embodiment, pulverize temperature in described step (2) and be -110 DEG C～-180 DEG C.
In one embodiment, time 1.2h～1.8h that described step (4) is ground.
In one embodiment, time 1.4h～1.6h that described step (4) is ground.
In one embodiment, described step (3), the intensification frequency in step (5) be 4 DEG C/min～6 DEG C/
min.
In one embodiment, described step (3), the intensification frequency in step (5) are 5 DEG C/min.
Another aspect of the present invention provides a kind of laser sintering (SLS) 3D printing polyether sulfone powder, using described preparation
Method prepares.
Compared with prior art, beneficial effects of the present invention：
The preparation method that the present invention provides adopts 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 of employing has efficiently controlled water in polyether sulfone for 2 DEG C/min～8 DEG C/min
Point, the going out of impurity, guarantee is provided for the polyether sulfone powder preparing uniform grading.On the other hand, in deep cooling crush method
Obtain polyether sulfone just after powder, using drying-grinding-drying method so that the size tunable of polyether sulfone, obtained and dipping
Resin has good compatibility, the polyether sulfone powder consumptive material having uniform particle diameter, need not adding binding agent, overcomes existing
The powder diameter that deep cooling ballistic method obtains uneven it is difficult to become good laser sintering (SLS) 3D printing polyether sulfone powder consumptive material
Deficiency, saved production cost, process is simple, be suitable for that industrialization is continuous to be produced.
Specific embodiment
The present invention provides a kind of preparation method of laser sintering (SLS) 3D printing polyether sulfone powder consumptive material, walks including following
Suddenly：
(1) polyether sulfone is inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for polyether sulfone is cold
But to -130 DEG C～-196 DEG C；
(2) polyether sulfone after cooling in step (1) is pulverized, pulverize temperature and be -110 DEG C～-196 DEG C, obtain polyether sulfone
Just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification 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 pulverized in step (3) is added in grinder, be fully ground and obtain polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification 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 consumptive material.
Selective Laser Sintering
Selective Laser Sintering (Selective Laser Sintering) is important one in rapid shaping technique
Individual branch, it is integrated with Fundamental Course of Mechanic Manufacturing, laser technology, material science, modern scientist engineering, computer technology, modern survey
The technology such as examination technology and CAD/CAM theoretical foundation and application.It is former that this technology can manufacture out part in the short period of time
Type and mould, are widely used in the every field of machine-building.This technology is based on layering-principle of stacking, using computer control
The movement locus of high energy laser beam processed, using the high energy melting metal dust of laser beam, after treating that laser facula is removed, metal
Liquid and rapid solidification.Whole process is exactly that laser facula moves from point to surface, then the process by face to body, and each part is
It is layering by forming face and form.The technology path of SLS process is to set up corresponding CAD model first against part, will
Model imports formation system and carries out step section, the geological information that each layer of section obtaining comprises section, generates STL form literary composition
Part.Then high energy laser beam is scanned along the track of each layer of section under control of the computer, melts in this region
Metal dust.Repave next layer of powder after one layer is terminated, repeat above procedure up to part forming.
The application that described laser sintered 3D printing polyether sulfone powder consumptive material is molded on 3D printer, feature is：By laser
Sintering 3D printing polyether sulfone powder consumptive material is added in the confession powder cylinder of selective laser sintering and moulding machine, and powdering roller is by powder material
Material is equably layered in processing plane and is heated to processing temperature, and laser instrument sends laser, the opening of computer controlled laser
Close and scanner angle so that laser beam processing plane on be scanned according to corresponding two-dimensional slice shape, laser beam
After inswept, workbench moves down a thickness, then powdering, laser beam flying, so repeatedly, obtains laser sintered part, wherein sharp
Light beam mode of scanning in processing plane scans for subregion.
The preheating temperature of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 70～85 DEG C；Preferably, described
The preheating temperature of laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 70～80 DEG C；It is highly preferred that described laser sintered one-tenth
The preheating temperature of type 3D printing polyether sulfone powder consumptive material is 75 DEG C.
The input energy density of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.1～0.4J/mm3；Excellent
Selection of land, the input energy density of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.2～0.3J/mm3；More preferably
Ground, the input energy density of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.28J/mm3.
The laser power of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 10～60W；Preferably, described sharp
The laser power of light sinter molding 3D printing polyether sulfone powder consumptive material is 15～30W.
The sweep speed of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 1500～2000mm/s；Preferably
Ground, the sweep speed of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 1800～2000mm/s；It is highly preferred that institute
The sweep speed stating laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 1900mm/s.
The sintering spacing of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.1～0.2mm；Preferably, institute
The sintering spacing stating laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.15～0.18mm；It is highly preferred that described laser
The sintering spacing of sinter molding 3D printing polyether sulfone powder consumptive material is 0.16mm.
The thickness in monolayer of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.1～0.2mm；Preferably, institute
The thickness in monolayer stating laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 0.12～0.18mm；It is highly preferred that described laser
The thickness in monolayer of sinter molding 3D printing polyether sulfone powder consumptive material is 0.16mm.
The present invention adopts vibromill deep cooling crush.Material is cooled down with immersing in liquid nitrogen in hopper, enters through screw(-type) feeder
Vibromill, and carry out deep cooling crush.As needed, also add liquid nitrogen in pulverizer, to keep being pulverized at a lower temperature.
Reducing mechanism includes feed hopper, liquid nitrogen tank, vibrator, warehouse for finished product, air blast, batcher, cooling storehouse, airtight valve.
Material adds cooling storehouse from top, moves down；From bottom, addition moves up liquid nitrogen.This reverse movement soaks
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.
Described grinder is the desk-top flour mill 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 consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -196 DEG C, cools down 3h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 1.5h,
Obtain polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 5 DEG C/min, freeze-day with constant temperature 2h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
2h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 5 DEG C/min, rises
Temperature freeze-day with constant temperature 1h to after 150 DEG C, obtains laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Embodiment 2
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -180 DEG C, cools down 3.5h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -180 DEG C, pulverizes 1.5h,
Obtain polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 5 DEG C/min, freeze-day with constant temperature 2h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
1.8h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 5 DEG C/min, rises
Temperature freeze-day with constant temperature 1h to after 150 DEG C, obtains laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Embodiment 3
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -140 DEG C, cools down 4h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -150 DEG C, pulverizes 2h, obtain
To polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 5 DEG C/min, freeze-day with constant temperature 0.5h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, be fully ground under the conditions of 1420r/min, grind
1.6h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 5 DEG C/min, rises
Temperature freeze-day with constant temperature 1h to after 150 DEG C, obtains laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Embodiment 4
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -196 DEG C, cools down 3h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 1.5h,
Obtain polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 5 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
2h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 5 DEG C/min, rises
Temperature freeze-day with constant temperature 0.5h to after 150 DEG C, obtain laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Embodiment 5
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -130 DEG C, cools down 2h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -110 DEG C, pulverizes 2h, obtain
To polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 2 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
2h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 6 DEG C/min, rises
Temperature freeze-day with constant temperature 0.5h to after 150 DEG C, obtain laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Embodiment 5
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -140 DEG C, cools down 2.5h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is 134 DEG C, pulverizes 1.5h,
Obtain polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 4 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
2h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 6 DEG C/min, rises
Temperature freeze-day with constant temperature 0.5h to after 150 DEG C, obtains laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Embodiment 6
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -162 DEG C, cools down 2h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 2.5h,
Obtain polyether sulfone just powder；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradients
Intensification drying, intensification frequency is 8 DEG C/min, freeze-day with constant temperature 1.5h after being warming up to 130 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
2h, obtains polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is played gradient increased temperature at 100 DEG C to be dried, intensification frequency is 8 DEG C/min, rises
Temperature freeze-day with constant temperature 0.5h to after 150 DEG C, obtains laser sintering and moulding 3D printing polyether sulfone powder consumptive material.
Comparative example 1
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) polyether sulfone is inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for polyether sulfone is cold
But to -198 DEG C；
(2) will be crushed for the polyether sulfone after cooling in step (1), pulverize temperature and be -198 DEG C, obtain polyether sulfone just powder.
Comparative example 2
The laser sintering (SLS) 3D printing preparation method of polyether sulfone powder consumptive material, comprises the steps：
(1) 10g polyether sulfone is added cooling storehouse from top, move down；From bottom, addition moves up liquid nitrogen, reverse fortune
Dynamic immersion type cooling, material is cooled to -196 DEG C, cools down 2h；
(2) polyether sulfone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 2.5h,
Obtain polyether sulfone just powder；
(3), after being warmed to room temperature polyether sulfone in step (2) just powder is sieved, it is placed in control heat riser, 130 DEG C of bars
0.5h is dried under part；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min, grind 1.2h, obtain
To polyether sulfone crude product；
(5) polyether sulfone crude product in step (4) is placed in heat riser, 0.5h is dried under the conditions of 150 DEG C, obtains laser
Sinter molding 3D printing polyether sulfone powder consumptive material.
Embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, comparative example 2 adopt Guangzhou auspicious greatly
The desk-top flour mill 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, comparative example 2 granularity are surveyed
Pilot production Zhuhai America and Europe's gram Instrument Ltd.'s electric-resistivity method particle size analyzer image method particle size analyzer.
Table 1 particle size range test result
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 consumptive material arriving, the application of shaping on 3D printer.
Laser sintered 3D printing polyether sulfone powder consumptive material is added in the confession powder cylinder of selective laser sintering and moulding machine, paving
Dusty material is equably layered in processing plane and is heated to processing temperature by powder roller, and laser instrument sends laser, computer
Control the switch of laser instrument and the angle of scanner so that laser beam enters according to corresponding two-dimensional slice shape in processing plane
Row scanning, after laser beam is inswept, workbench moves down a thickness, then powdering, and laser beam flying so repeatedly, obtains laser
Sintered part, the wherein laser beam mode of scanning in processing plane scans for subregion；Described laser sintering and moulding 3D printing gathers
The preheating temperature of ether sulfone powder consumptive material is 76 DEG C；The input energy of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is close
Spend for 0.25J/mm3；The laser power of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is 16W；Described laser burns
The sweep speed forming type 3D printing polyether sulfone powder consumptive material is 1800mm/s；Described laser sintering and moulding 3D printing polyether sulfone powder
The sintering spacing of last consumptive material is 0.15mm；The thickness in monolayer of described laser sintering and moulding 3D printing polyether sulfone powder consumptive material is
0.15mm.The result that the polyether sulfone 3D printing finished product being prepared by described polyether sulfone powder carries out performance test is as follows.
Performance test
Tensile property:CMT5504 type electronic universal mechanics machine carries out test for tensile strength, by GB/T1040-
1992 standards make standard batten, and draw speed is 5mm/s.
Bending property:CMT5504 type electronic universal mechanics machine carries out bending property test, by GB/T9341-
2008 standards make standard batten, and test speed is 2mm/min.
Non-notch sample simple beam impact strength:XJC-25Z type mechanical combination balance weight impact testing machine is impacted
Test, makes standard batten by GB/T 1043-1993, and impact energy is 2J.
Table 2 the performance test results
As can be seen that working as, legal system is impacted to deep cooling using the process of gradient increased temperature from above-mentioned granularity, the performance test results
When the first powder of the standby polyether sulfone obtaining is dried, obtains polyether sulfone powder diameter and be evenly distributed, with impregnating resin have good
The compatibility got well, the polyether sulfone consumptive material that binding agent need not be added.It is almost without external force applying condition by laser sintered principle
Lower rapidoprint makes the drip molding sintering out have very strong physical property and chemical property, and the contrived experiment material proposing
The scheme of material is easy quick, great reduced time and economizing on resources.
The preparation method that the present invention provides adopts 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 of employing is effectively controlled water in polyether sulfone for 2 DEG C/min～8 DEG C/min
Point, the going out of impurity, guarantee is provided for the polyether sulfone powder preparing uniform grading.On the other hand, in deep cooling crush method
Obtain polyether sulfone just after powder, using drying-grinding-drying method so that the size tunable of polyether sulfone, obtained and dipping
Resin has good compatibility, the polyether sulfone powder consumptive material having uniform particle diameter, need not adding binding agent, overcomes existing
The powder diameter that deep cooling ballistic method obtains uneven it is difficult to become good laser sintering (SLS) 3D printing polyether sulfone powder consumptive material
Deficiency, saved production cost, process is simple, be suitable for that industrialization is continuous to be produced.
Aforesaid embodiment is merely illustrative, for explaining some features of the method for the invention.Appended right
Require the scope as wide as possible being intended to require 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 appended claim is not illustrated this
The selectional restriction of the example of feature of invention.Some number ranges used also include son within the claims
Scope, the change in these scopes also should be construed to be covered by appended claim in the conceived case.
Claims (10)
1. a kind of laser sintering (SLS) 3D printing with the preparation method of polyether sulfone powder consumptive material it is characterised in that including following walking
Suddenly：
(1) polyether sulfone to be inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for being cooled to polyether sulfone-
130 DEG C～-196 DEG C；
(2) polyether sulfone after cooling in step (1) is pulverized, pulverize temperature and be -110 DEG C～-196 DEG C, obtain polyether sulfone just powder
End；
(3) after first for polyether sulfone in step (2) powder being sieved, it is placed in controllable heat riser, 100 DEG C are played gradient increased temperatures
It is dried, intensification 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 pulverized in step (3) is added in grinder, be fully ground and obtain polyether sulfone crude product；
(5) by polyether sulfone crude product in step (4) 100 DEG C rise gradient increased temperatures be dried, intensification frequency be 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 consumptive material.
2. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyether sulfone powder consumptive material, its feature exists
In the particle diameter of described polyether sulfone powder is 10 μm -100 μm.
3. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyether sulfone powder consumptive material, its feature exists
In in described step (1), chilling temperature is -140 DEG C～-180 DEG C.
4. the laser sintering (SLS) 3D printing as claimed in claim 3 preparation method of polyether sulfone powder consumptive material, its feature exists
In in described step (1), chilling temperature is -150 DEG C～-170 DEG C.
5. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyether sulfone powder consumptive material, its feature exists
In in described step (2), pulverizing temperature is -110 DEG C～-180 DEG C.
6. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyether sulfone powder consumptive material, its feature exists
In time 1.2h～1.8h that described step (4) is ground.
7. the laser sintering (SLS) 3D printing as claimed in claim 6 preparation method of polyether sulfone powder consumptive material, its feature exists
In time 1.4h～1.6h that described step (4) is ground.
8. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyether sulfone powder consumptive material, its feature exists
In the intensification frequency in described step (3), step (5) is 4 DEG C/min～6 DEG C/min.
9. the laser sintering (SLS) 3D printing as claimed in claim 8 preparation method of polyether sulfone powder consumptive material, its feature exists
In the intensification frequency in described step (3), step (5) is 5 DEG C/min.
10. a kind of laser sintering (SLS) 3D printing with polyether sulfone powder it is characterised in that adopt claim 1-9 any one
Preparation method described in claim prepares.
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