CN106432756A - Preparation method for laser sintered polyether ketone powder material for 3D printing - Google Patents
Preparation method for laser sintered polyether ketone powder material for 3D printing Download PDFInfo
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- CN106432756A CN106432756A CN201610846912.XA CN201610846912A CN106432756A CN 106432756 A CN106432756 A CN 106432756A CN 201610846912 A CN201610846912 A CN 201610846912A CN 106432756 A CN106432756 A CN 106432756A
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- ketone
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
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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
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08J2371/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
Abstract
The invention provides a preparation method for a laser sintered polyether ketone powder material for 3D printing. The method comprises the following steps: (1) putting polyether ketone into a stock bin in a low-temperature grinding machine, wherein liquid nitrogen in the stock bin is used for cooling polyether ketone to -150 DEG C to -196 DEG C; (2) crushing the polyether ketone cooled in the step (1) at -140 DEG C to -196 DEG C, thereby obtaining primary polyether ketone powder; (3) screening the primary polyether ketone powder obtained in the step (2), and then performing gradient temperature rise from 90 DEG C and drying, wherein the temperature rise frequency is 2 DEG C/min to 8 DEG C/min, and drying for 0.5h-2h at constant temperature after the temperature is increased to 120 DEG C; (4) adding the powder crushed in the step (3) into a grinding machine and fully grinding, thereby obtaining a rough product of polyether ketone; (5) performing gradient temperature rise from 90 DEG C for drying the rough product of polyether ketone obtained in the step (4), wherein the temperature rise frequency is 2 DEG C/min to 8 DEG C/min, and drying for 0.5h-1h at constant temperature after the temperature is increased to 120 DEG C, thereby obtaining the laser sintered polyether ketone powder material for 3D printing.
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 ketone 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 digitized 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.
Sintered 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 Rapid Prototyping technique
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.
Sintered 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 sintered 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-ketone English name (polyetherketone), abridge PEK, is that main chain is replaced and sub- benzene by ehter bond and ketonic bond
Basic ring connection and a kind of high-performance polymer of being formed, depending on so-called high-performance polymer is the excellent specific property possessing according to it
Justice.Typical polymer is PAEK, formed by aromatic dicarboxylic phenol and difluoro benzophenone high-temperature polycondensation it is also possible to
Formed with aromatic series dihalo thing polycondensation by 4,4- dihydroxy benaophenonel, generally this polymer has high mechanical strength,
Outstanding heat stability (can continuously use under 150 DEG C of high temperature, and flammable low), chemical stability are (at high temperature also very
Stable) and electric property (as insulator), and also to have good processing characteristics.
Polyethers ketone resins is one of top quality so far special engineering plastics, is widely used in the harsh temperature of condition
Measurement, electronic television display engineering, rubber such as manufactures at lining valve used by chemical industry, the pipeline, fine with glass fibre or carbon
The aviation fields such as the cabin of dimension blending manufacture airship and aircraft, helicopter empennage, resistant to elevated temperatures X-ray apparatus, atomic energy dress
Put, acidproof oil well coats and cable material.The high comprehensive performance of polyether-ketone, thermostability highest in PAEK, chemically-resistant
Good, the high temperature steam of property, the good dimension stability after water suction, thermal coefficient of expansion is low, resistance to combustion, and resistance to good fortune is penetrated.Aromatic-polyether ketone resistance toization
Learn medicine function admirable, acid and alkali resistance performance is good, in addition to concentrated sulphuric acid, is hardly invaded candle by every other chemical drugss；Machine
Tool intensity is high, and anti-spiral shell degeneration is strong, is high soft just property resin, all has resistance to impact and abrasion performance within the scope of very wide temperature
Property；Especially it is appreciated that, aromatic-polyether ketone is one of classic resin of fatigue durability.The electrical property of aromatics polyacids ketone is also
Good, it is respectively provided with stable dielectric property and insulating properties in very wide frequency range and temperature range.At fire-retardant aspect, during burning
It is fuming few, be nearly free from corrosive gas.In thermoplastic polymer, the glass transition temperature of polyether-ketone, melt temperature and
Solvent resistance is optimal.There is good engineering propertiess and excellent toughness, more than melt temperature, still have good thermally-stabilised
Property.
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 sedimentation 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.But the shape of particle being obtained using deep cooling ballistic method
Irregularly, granule size is uneven, is difficult to once reach the particle diameter of desirable amount.Particle diameter distribution, needs repeatedly to sieve, pulverizes it
After could use.Screening, pulverizing increased cost it is therefore necessary to develop a kind of side preparing polyethers ketone powder consumptive material repeatedly
Method is so that after deep cooling crush, carrying out regrinding dry run to the powder after pulverizing, preparing and be suitable to 3D printing technique
High temperature resistant and impregnating resin there is the good compatibility, the polyether-ketone consumption having uniform particle diameter, need not adding binding agent
Material, can conveniently and efficiently shape the part of precision, abnormal shape, complexity, high mechanical strength, good stability of the dimension, and can be used to make
For the many parts on UAV now, 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 polyethers ketone powder consumptive material, walks including following
Suddenly：
(1) polyether-ketone is inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for polyether-ketone is cold
But to -150 DEG C～-196 DEG C；
(2) polyether-ketone after cooling in step (1) is pulverized, pulverize temperature and be -140 DEG C～-196 DEG C, obtain polyether-ketone
Just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 DEG C；
(4) powder pulverized in step (3) is added in grinder, be fully ground and obtain polyether-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 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 120 DEG C, obtain laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
In one embodiment, the particle diameter of described polyethers ketone powder is 10 μm -100 μm.
In one embodiment, in described step (1), chilling temperature is -155 DEG C～-180 DEG C
In one embodiment, in described step (1), chilling temperature is -160 DEG C～-170 DEG C.
In one embodiment, pulverize temperature in described step (2) and be -150 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.The present invention
On the other hand provide a kind of laser sintering (SLS) 3D printing polyethers ketone powder, prepared using described preparation method.
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-ketone so that polyethers
Ketone is effectively dried, and the frequency of the gradient increased temperature of employing is effectively controlled water in polyether-ketone for 2 DEG C/min～8 DEG C/min
Point, the going out of impurity, guarantee is provided for the polyethers ketone powder preparing uniform grading.On the other hand, in deep cooling crush method
Obtain polyether-ketone just after powder, using drying-grinding-drying method so that the size tunable of polyether-ketone, obtained and dipping
Resin has the good compatibility, the polyethers ketone 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 polyethers ketone powder consumptive material
Deficiency, saved production cost, process is simple, suitable industrialization continuously produces.
Specific embodiment
The present invention provides a kind of preparation method of laser sintering (SLS) 3D printing polyethers ketone powder consumptive material, walks including following
Suddenly：
(1) polyether-ketone is inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for polyether-ketone is cold
But to -150 DEG C～-196 DEG C；
(2) polyether-ketone after cooling in step (1) is pulverized, pulverize temperature and be -140 DEG C～-196 DEG C, obtain polyether-ketone
Just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 DEG C；
(4) powder pulverized in step (3) is added in grinder, be fully ground and obtain polyether-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 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 120 DEG C, obtain laser sintering and moulding 3D printing polyethers ketone 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 basiss 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 the SLS course of processing 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 of described laser sintered 3D printing polyethers ketone powder consumptive material molding on 3D printer, feature is：By laser
Sintering 3D printing polyethers ketone 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 scanning device 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 polyethers ketone powder consumptive material is 70～85 DEG C；Preferably, described
The preheating temperature of laser sintering and moulding 3D printing polyethers ketone 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 polyethers ketone powder consumptive material is 75 DEG C.
The input energy density of described laser sintering and moulding 3D printing polyethers ketone 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 polyethers ketone powder consumptive material is 0.2～0.3J/mm3；More preferably
Ground, the input energy density of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 0.28J/mm3.
The laser power of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 10～60W；Preferably, described sharp
The laser power of light sinter molding 3D printing polyethers ketone powder consumptive material is 15～30W.
The sweep speed of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 1500～2000mm/s；Preferably
Ground, the sweep speed of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 1800～2000mm/s；It is highly preferred that institute
The sweep speed stating laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 1900mm/s.
The sintering spacing of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 0.1～0.2mm；Preferably, institute
The sintering spacing stating laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 0.15～0.18mm；It is highly preferred that described laser
The sintering spacing of sinter molding 3D printing polyethers ketone powder consumptive material is 0.17mm.
The thickness in monolayer of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 0.1～0.2mm；Preferably, institute
The thickness in monolayer stating laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 0.12～0.18mm；It is highly preferred that described laser
The thickness in monolayer of sinter molding 3D printing polyethers ketone powder consumptive material is 0.17mm.
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, aerator, 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 chiller 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 company limited 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 polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 2h, obtain
To polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 5 DEG C/min, heats up
The freeze-day with constant temperature 1h to after 120 DEG C, obtains laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Embodiment 2
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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 4h；
(2) polyether-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -180 DEG C, pulverizes 2h, obtain
To polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 5 DEG C/min, heats up
The freeze-day with constant temperature 1h to after 120 DEG C, obtains laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Embodiment 3
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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 -155 DEG C, cools down 4h；
(2) polyether-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -150 DEG C, pulverizes 3h, obtain
To polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 5 DEG C/min, heats up
The freeze-day with constant temperature 0.5h to after 120 DEG C, obtains laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Embodiment 4
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 1.5h,
Obtain polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 DEG C；
(4) powder pulverized in step (3) is added in grinder, under the conditions of 1420r/min is fully ground, grind
1.5h, obtains polyether-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 5 DEG C/min, heats up
The freeze-day with constant temperature 0.5h to after 120 DEG C, obtain laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Embodiment 5
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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 -160 DEG C, cools down 2h；
(2) polyether-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -160 DEG C, pulverizes 2h, obtain
To polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 6 DEG C/min, heats up
The freeze-day with constant temperature 0.5h to after 120 DEG C, obtain laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Embodiment 5
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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 -150 DEG C, cools down 2.5h；
(2) polyether-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -140 DEG C, pulverizes 1.5h,
Obtain polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 6 DEG C/min, heats up
The freeze-day with constant temperature 0.5h to after 120 DEG C, obtains laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Embodiment 6
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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 2.5h；
(2) polyether-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 3h, obtain
To polyether-ketone just powder；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is played gradient increased temperature at 90 DEG C to be dried, intensification frequency is 8 DEG C/min, heats up
The freeze-day with constant temperature 0.5h to after 120 DEG C, obtains laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Comparative example 1
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) polyether-ketone is inserted in the feed bin in Lowtemperaturepulverizer, the built-in liquid nitrogen of described feed bin is used for polyether-ketone is cold
But to -198 DEG C；
(2) will be crushed for the polyether-ketone after cooling in step (1), pulverize temperature and be -198 DEG C, obtain polyether-ketone just powder.
Comparative example 2
The laser sintering (SLS) 3D printing preparation method of polyethers ketone powder consumptive material, comprises the steps：
(1) 10g polyether-ketone 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-ketone after cooling in step (1) is vibrated ball mill and pulverizes, and pulverizes temperature and is -196 DEG C, pulverizes 2.5h,
Obtain polyether-ketone just powder；
(3), after being warmed to room temperature polyether-ketone in step (2) just powder is sieved, it is placed in control heat riser, 120 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-ketone crude product；
(5) polyether-ketone crude product in step (4) is placed in heat riser, 0.5h is dried under the conditions of 120 DEG C, obtains
To laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
Grind using described in embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, comparative example 2
Grinder is the desk-top flour mill of Guangzhou great Xiang electro mechanical devices company limited 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 polyethers ketone powder consumptive material arriving, the application of molding on 3D printer.
Laser sintered 3D printing polyethers ketone 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 scanning device 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 ketone powder consumptive material is 78 DEG C；The input energy of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is close
Spend for 0.25J/mm3；The laser power of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is 18W；Described laser burns
The sweep speed forming type 3D printing polyethers ketone powder consumptive material is 1700mm/s；Described laser sintering and moulding 3D printing polyether-ketone powder
The sintering spacing of last consumptive material is 0.17mm；The thickness in monolayer of described laser sintering and moulding 3D printing polyethers ketone powder consumptive material is
0.17mm.The result that the polyether-ketone 3D printing finished product being prepared by described polyethers ketone 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
| Tensile strength (MPa) | Bending strength (MPa) | Impact strength (breach) (J/m) | |
| Embodiment 1 | 87.53 | 148.68 | 78.02 |
| Embodiment 2 | 85.28 | 147.56 | 74.16 |
| Embodiment 3 | 85.23 | 147.66 | 75.63 |
| Embodiment 4 | 86.47 | 147.10 | 74.98 |
| Embodiment 5 | 85.56 | 146.98 | 75.61 |
| Embodiment 6 | 86.28 | 147.12 | 76.30 |
| Embodiment 7 | 85.98 | 147.28 | 76.84 |
| Comparative example 1 | 65.23 | 109.36 | 45.12 |
| Comparative example 2 | 72.74 | 123.64 | 58.97 |
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-ketone obtaining is dried, obtains polyether-ketone powder diameter and be evenly distributed, with impregnating resin have good
The compatibility got well, the polyether-ketone 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-ketone so that polyethers
Ketone is effectively dried, and the frequency of the gradient increased temperature of employing is effectively controlled water in polyether-ketone for 2 DEG C/min～8 DEG C/min
Point, the going out of impurity, guarantee is provided for the polyethers ketone powder preparing uniform grading.On the other hand, in deep cooling crush method
Obtain polyether-ketone just after powder, using drying-grinding-drying method so that the size tunable of polyether-ketone, obtained and dipping
Resin has the good compatibility, the polyethers ketone 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 polyethers ketone powder consumptive material
Deficiency, saved production cost, process is simple, suitable industrialization continuously produces.
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 numerical rangies 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 polyethers ketone powder consumptive material it is characterised in that including following walking
Suddenly：
(1) polyether-ketone 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-ketone-
150 DEG C～-196 DEG C；
(2) polyether-ketone after cooling in step (1) is pulverized, pulverize temperature and be -140 DEG C～-196 DEG C, obtain polyether-ketone just powder
End；
(3) after first for polyether-ketone in step (2) powder being sieved, it is placed in controllable heat riser, 90 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 120 DEG C；
(4) powder pulverized in step (3) is added in grinder, be fully ground and obtain polyether-ketone crude product；(5) by step
(4) in, polyether-ketone crude product plays gradient increased temperature at 90 DEG C and is dried, and intensification frequency is 2 DEG C/min～8 DEG C/min, is warming up to 120 DEG C
Freeze-day with constant temperature 0.5h～1h afterwards, obtains laser sintering and moulding 3D printing polyethers ketone powder consumptive material.
2. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyethers ketone powder consumptive material, its feature exists
In the particle diameter of described polyethers ketone powder is 10 μm -100 μm.
3. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyethers ketone powder consumptive material, its feature exists
In in described step (1), chilling temperature is -155 DEG C～-180 DEG C.
4. the laser sintering (SLS) 3D printing as claimed in claim 3 preparation method of polyethers ketone powder consumptive material, its feature exists
In in described step (1), chilling temperature is -160 DEG C～-170 DEG C.
5. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyethers ketone powder consumptive material, its feature exists
In in described step (2), pulverizing temperature is -150 DEG C～-180 DEG C.
6. the laser sintering (SLS) 3D printing as claimed in claim 1 preparation method of polyethers ketone 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 polyethers ketone 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 polyethers ketone 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 polyethers ketone 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 polyethers ketone powder it is characterised in that adopt claim 1-9 any one
Preparation method described in claim prepares.
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| CN1954022A (en) * | 2004-03-21 | 2007-04-25 | 丰田赛车有限公司 | Powder for rapid prototyping and associated production method |
| CN103980690A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | 3D printing modified polyether ketone resin material and preparation method |
| US20150061195A1 (en) * | 2013-08-29 | 2015-03-05 | Scott DeFelice | Method For Analytically Determining SLS Bed Temperatures |
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| CN1954022A (en) * | 2004-03-21 | 2007-04-25 | 丰田赛车有限公司 | Powder for rapid prototyping and associated production method |
| 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 |
| US20150061195A1 (en) * | 2013-08-29 | 2015-03-05 | Scott DeFelice | Method For Analytically Determining SLS Bed Temperatures |
| CN103980690A (en) * | 2014-04-30 | 2014-08-13 | 中国科学院化学研究所 | 3D printing modified polyether ketone resin material and preparation method |
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| CN109796610A (en) * | 2019-03-06 | 2019-05-24 | 武汉理工大学 | The preparation method of polyether-ether-ketone nano-powder with lamellar structure |
| CN109796610B (en) * | 2019-03-06 | 2022-07-08 | 武汉理工大学 | Preparation method of polyetheretherketone nano-powder with lamellar structure |
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