CN105172154A - Selected region laser sintering and molding method of ultrahigh molecular weight polyethylene - Google Patents
Selected region laser sintering and molding method of ultrahigh molecular weight polyethylene Download PDFInfo
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- CN105172154A CN105172154A CN201510696496.5A CN201510696496A CN105172154A CN 105172154 A CN105172154 A CN 105172154A CN 201510696496 A CN201510696496 A CN 201510696496A CN 105172154 A CN105172154 A CN 105172154A
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Abstract
The invention discloses a selected region laser sintering and molding method of ultrahigh molecular weight polyethylene. The selected region laser sintering and molding method comprises the following steps: (1) heating ultrahigh molecular weight polyethylene powder in selected region laser sintering and molding equipment to a pre-heated temperature; (2) molding the ultrahigh molecular weight polyethylene powder in the selected region laser sintering and molding equipment by adopting pre-set laser scanning speed and output power to obtain a molded piece; and (3) taking out the molded piece and keeping the heat at a temprature of 110-130 DEG C for 8-12 hours, and then cooling to obtain a molded part of the ultrahigh molecular weight polyethylene. The molded part of the ultrahigh molecular weight polyethylene, molded by the method disclosed by the invention, has relatively high mechanical property and size precision, has small transformation shrinkage and is particularly suitable for manufacturing medical auxiliary tools.
Description
Technical field
The invention belongs to 3D printing shaping technical field, particularly relate to a kind of precinct laser sintering forming method of ultra-high molecular weight polyethylene.
Background technology
Precinct laser sintering (SelectiveLaserSintering, be called for short SLS, be also called selective laser sintering) print one of mainstream technology as 3D, to be invented at the mid-80 by doctor CarlDeckard of Texas, USA university the earliest and apply for a patent, after by DTM company (3DSystems purchase) commercialization.SLS is raw material with powder body material, take laser as thermal source, adopts layering-principle of stacking directly to manufacture 3D solid from cad model.The technological parameter of this technology mainly contains: laser power, sweep speed and spacing, preheat temperature and thickness.SLS advantage is that raw material are selected extensively, can be the various powder body materials such as macromolecule, pottery, sand.Compare other 3D printing techniques (as SLA, FDM etc.), need the support of interpolation less during graphics process in early stage, the post-processed relative ease after product machines, the mechanical strength of gained product is high.
Ultra-high molecular weight polyethylene (Ultra-HighMolecularWeightPolyethylene, be called for short UHMWPE) be a kind of linear thermoplastic's crystalline polymers, molecular structure and common polythene are as good as, but due to molecular weight high (viscosity average molecular weigh >100 ten thousand), it has the incomparable resistance to impact of other plastics, wear-resistant, resistance to chemical attack, lower temperature resistance, stress crack resistant, anti-adhesion ability, superior isolation, the performance such as safety and sanitation and self-lubricity.Because UHMWPE has very superior physics, chemistry, mechanical performance, all receive in every profession and trade and apply widely, as the lining material in mining industry industry, the gear in machinery industry, bearing shell etc.UHMWPE equally medically also obtain extensive application, mainly concentrates in the medical materials such as joint replacement materials, organization bracket, blood transfusion apparatus, packaging bag at present.Because it is to biological non-toxicity, UHMWPE has obtained U.S. FDA approval for human-body biological material.
But, though UHMWPE is medically having application, be mostly the standard component taking traditional die methods to produce, preparing in personalized medicine part prior art with UHMWPE and do not relate to.
Summary of the invention
In order to make up above-mentioned the deficiencies in the prior art, the present invention proposes a kind of precinct laser sintering forming method of ultra-high molecular weight polyethylene.
Technical problem of the present invention is solved by following technical scheme:
A precinct laser sintering forming method for ultra-high molecular weight polyethylene, comprises the steps:
(1) ultra-high molecular weight polyethylene powder is heated to preheat temperature in precinct laser sintering former;
(2) adopt predetermined laser scanning speed and power output to make described ultra-high molecular weight polyethylene powder shaping in precinct laser sintering former, obtain profiled member;
(3) take out described profiled member, at the temperature of 110 ~ 130 DEG C, be incubated 8 ~ 12h, cooling afterwards obtains the molded article of ultra-high molecular weight polyethylene.
Preferably, in step (2), described predetermined laser scanning speed and power output are determined by following formula: v=k α, wherein: α represents laser output power ratio, 0 < α≤1, the peak power of the real output/laser instrument of α=laser instrument; ν represents laser scanning speed; The span of k is 2 ~ 6.
Preferably, k is determined by below formula:
Wherein:
Δ T represents the temperature difference of lf processing temperature and preheat temperature;
C represents the specific heat capacity of ultra-high molecular weight polyethylene powder;
K represents the laser absorption rate of ultra-high molecular weight polyethylene powder;
P
maxrepresent the peak power of laser instrument;
ρ represents the density of ultra-high molecular weight polyethylene powder;
D represents the spot diameter of laser;
S represents the thickness of laser-transmitting ultra-high molecular weight polyethylene powder.
Preferably, the mean molecule quantity of described ultra-high molecular weight polyethylene powder is 200 ~ 4,000,000, and particle diameter is 30 ~ 60 μm.
Preferably, the described preheat temperature in described step (1) is 130 ~ 150 DEG C.
Preferably, the heating fluorescent tube in described precinct laser sintering former adopts rebuilding, as follows:
Lower floor is made up of four heating lamp circumference of cannon bone quadrates, wherein the length direction of two heating fluorescent tubes is parallel with the direction of displacement of powder-laying roller in described precinct laser sintering former, and the length direction of other two heating fluorescent tubes is vertical with the direction of displacement of powder-laying roller in described precinct laser sintering former;
To heat above fluorescent tube at two parallel with the direction of displacement of powder-laying roller in described precinct laser sintering former and be also provided with also parallel with the direction of displacement of powder-laying roller in a described precinct laser sintering former heating fluorescent tube separately in addition.
Preferably, the rated power of described heating fluorescent tube is 200 ~ 500W.
The present invention compared with prior art, comprise following advantage: the precinct laser sintering forming method that the invention provides a kind of ultra-high molecular weight polyethylene, molded article mechanical property, the dimensional accuracy of shaping ultra-high molecular weight polyethylene are all higher, deformation retract is little, is particularly useful for the manufacture of medical auxiliary tool.
Accompanying drawing explanation
Fig. 1 is the distribution mode of the heating fluorescent tube in the specific embodiment of the invention;
Fig. 2 is the temperature line of each measurement point in the different heating lighting tube combination lower area in Fig. 1.
Detailed description of the invention
Below contrast accompanying drawing and combine preferred embodiment the invention will be further described.
UHMWPE is a kind of crystalline polymer material, molecular weight is more than 1,000,000, processing fluidity of molten is poor, and viscosity is high, and shaping after-contraction distortion is larger, these all limit the shaping application of the SLS of UHMWPE, inventor, after analyzing the shaping many factors of the SLS that affects UHMWPE, obtains following technical scheme, in a specific embodiment, a precinct laser sintering forming method for ultra-high molecular weight polyethylene, comprises the steps:
(1) ultra-high molecular weight polyethylene powder is heated to preheat temperature in precinct laser sintering former;
(2) adopt predetermined laser scanning speed and power output to make described ultra-high molecular weight polyethylene powder shaping in precinct laser sintering former, obtain profiled member;
(3) take out described profiled member, at the temperature of 110 ~ 130 DEG C, be incubated 8 ~ 12h, cooling afterwards obtains the molded article of ultra-high molecular weight polyethylene.
In a preferred embodiment, mainly comprise raw-material preferably, the uniformity in temperature field, the determination of preheat temperature, the optimization etc. of laser technical parameters, also namely can by the following technical solutions in one or any combination:
Set up the Mathematical Modeling of laser processing procedure, calculate the relation deriving laser scanning speed ν and laser output power ratio α, both are linear, in step (2), predetermined laser scanning speed and power output are determined by following formula: v=k α, wherein: α represents laser output power ratio, 0 < α≤1, the peak power of the real output/laser instrument of α=laser instrument; ν represents laser scanning speed; The span of k is 2 ~ 6.K then can be determined by below formula:
Wherein:
Δ T represents the temperature difference of lf processing temperature and preheat temperature;
C represents the specific heat capacity of ultra-high molecular weight polyethylene powder;
K represents the laser absorption rate of ultra-high molecular weight polyethylene powder;
P
maxrepresent the peak power of laser instrument;
ρ represents the density of ultra-high molecular weight polyethylene powder;
D represents the spot diameter of laser;
S represents the thickness of laser-transmitting ultra-high molecular weight polyethylene powder.
Laser power and sweep speed reflect the emittance size within the unit interval in powder forming surface, directly determine powder body melting degree and final Forming Quality.Linear relationship according to the derivation of equation out laser power and sweep speed: ν=k α, wherein the range of choice of k is preferably 2 ~ 6.What k value represented is the size that material accepts laser energy, and k value is less, and energy is higher, and it is high that material absorption melting transfers liquid phase accounting to, and crystallisation by cooling is shaping, and density, mechanical property and surface quality are also relatively high, but crystalline phase is many, and deformation retract is large; Otherwise energy is little, material component melting, crystallisation by cooling is few mutually, and deformation retract is little, but the index such as density, mechanical property is corresponding lower.The density that suitable Energy transmission can make the shaping acquisition of powder certain, profiled member shrinks also unlikely excessive simultaneously.Power is larger, and the energy of laser irradiation is larger, and absorbed energy melting degree is higher, and the transformation of solid-liquid now occurs, and mobility is also better, and the phase of individual layer is also more even.Meanwhile, energy is higher, and the thickness of laser penetration powder is also higher, and melt-processed makes bonding between layers also better.But energy is higher, the temperature difference of processing district and periphery is also larger, and the phenomenon that the contraction in cooling procedure causes stress to be concentrated is also more serious, and macromolecular material thermal degradation can occur under too high energy, affects apparent property and the mechanical property of profiled member.Sweep speed is the speed that galvanometer rotary reflection laser makes laser conduct, and sweep speed has reacted in unit are the time accepting laser emission processing, have impact on the energy absorption of powder.Sweep speed is larger, and the time of Laser Processing is shorter, otherwise longer.Under same power output, sweep speed is larger, and the irradiation energy that powder accepts is fewer, and the part of crystal heat absorption melting is fewer, and structure degree of irregularity is higher, and vice versa.Therefore, inventor is found by theory calculate and experimental verification and obtains above preferred power and sweep speed combination, while improving mechanical property, also takes into account minimizing deformation retract, realizes best molding effect.
The particle diameter of UHMWPE powder is less, and the formed precision of profiled member is better, and roughness is little, and surface gloss is high, is conducive to improving Forming Quality.Particle granules nodularization degree is higher, and the bulk density of powder body material is higher, and mobility is better, is conducive to the flatness in powder bed powder process and improves profiled member density and mechanical property.If the particle diameter of UHMWPE powder is excessive or domain size distribution is uneven, all easily cause surface of shaped parts coarse, formed precision is poor.Particle aggregation, nodularization degree is low, causes poor fluidity, processing difficulties.If the molecular weight of UHMWPE powder is too high, viscosity increases, processing difficulties; Molecular weight is too low, and poor mechanical property easily buckling deformation occurs.Therefore, optimizing UHMWPE powder selects mean molecule quantity to be 200 ~ 4,000,000, and particle diameter is 30 ~ 60 μm, the superfine powder of good sphericity (spherical or almost spherical), self-control can be selected for the UHMWPE that SLS is shaping in this enforcement, also can select commercially available TICONA company GUR
tMwith Mitsui Chemicals MIPELON
tMat least one in the trade mark.
Preheat temperature is one of key factor affecting Forming Quality, and UHMWPE is as the one of crystalline polymer, and fusing point is at about 145 DEG C, and in temperature-rise period, material experienced by rigidity elastomeric state, flexible low bullet state until change amorphous molten state.Molecule segment is elevated to setting in motion on vitrification point in temperature, and crystal structure continues heat absorption until disintegrated completely near fusing point, and now volume change is maximum, material generation warpage and distortion.If preheat temperature is too low, UHMWPE experienced by the complete procedure from room temperature to fusing point, and Volume Changes accumulation is large, and having a strong impact on Forming Quality even cannot be shaping.Therefore preheat temperature is selected near fusing point, reduces volume discontinuities to the shaping impact caused as far as possible.Meanwhile, preheat temperature is conducive to the temperature gradient reducing laser processing area and periphery, reduces the formation of stress and the generation of warpage.But the selection of preheat temperature can not be too high, temperature is too high makes molecule segment generation crosslinked, and molecular weight rises, and viscosity increases, and in process, the mobility of powder is greatly affected, and forming process can be made to carry out smoothly.In present embodiment, preheat temperature is differential scanning calorimetry (differentialscanningcalorimetry, the DSC) curve by analyzing UHMWPE, determines, between 130 ~ 150 DEG C, to be conducive to the uniformity in temperature field.
The Uniformity of Temperature Field of SLS forming room is weighed with the change of the curve of measurement point temperature, obtains the heating lighting tube combination putting into practice the optimization confirmed thus.In this example, heating fluorescent tube in precinct laser sintering former adopts rebuilding, as follows: lower floor is by four heating fluorescent tubes (the selection gist firing rate of heating lamp tube power and heating uniformities, the quartz infrared heating lamps pipe of preferred rated power 200 ~ 500W, 500W is adopted in a specific embodiment) surround square composition (as the L1 in Fig. 1, L2, shown in L3 and L4), wherein the length direction of two heating fluorescent tubes is parallel with the direction of displacement of powder-laying roller in precinct laser sintering former, the length direction of other two heating fluorescent tubes is vertical with the direction of displacement of powder-laying roller in described precinct laser sintering former, to heat above fluorescent tube at two parallel with the direction of displacement of powder-laying roller in precinct laser sintering former and be also provided with also parallel with the direction of displacement of powder-laying roller in a described precinct laser sintering former heating fluorescent tube (as shown in L5 and L7 in Fig. 1) (the quartz infrared heating lamps pipe of preferred rated power 200 ~ 500W, adopts 300W in a specific embodiment) separately in addition and form.
The uniformity in temperature field is one of key factor affecting Forming Quality, if temperature field is uneven, profiled member in process between layers, with layer diverse location occur the temperature difference, easily cause internal stress formed and concentrate, cause buckling deformation, having a strong impact on Forming Quality even cannot be shaping.
In present embodiment, the defining method of Uniformity of Temperature Field is the measurement point temperature by diverse location in thermal field under adopting contact thermocouple to measure different heating lighting tube combination, finally draws temperature curve, compares the smoothness of each temperature curve.As shown in Figure 1, for heating the distribution map of fluorescent tube, under different heating lighting tube combinations, measure each point for measuring temperature (T1 ~ T8 in longitudinally (direction vertical with the direction of displacement of powder-laying roller), spacing between every two adjacent points for measuring temperature is 43mm) temperature, the uniformity of drafting pattern evaluate temperature field, as shown in Figure 2, for measurement point temperature line each in different heating lighting tube combination lower area, it is less that temperature curve represents each point temperature difference gently, can think that Uniformity of Temperature Field is better, determine optimum heating lighting tube combination with this.Wherein, the sequence number of the lighting tube combination in figure is shown in below table 1, as shown in Figure 2, compared to other lighting tube combinations, under L1+L2+L3+L4+L5+L7 heats the combination (the 3# curve in Fig. 2) of fluorescent tube, to be linked to be temperature curve the mildest for each measurement point, rise and fall minimum, namely think that Uniformity of Temperature Field is best, therefore, lighting tube combination is preferably when being L1+L2+L3+L4+L5+L7, more uniform temperature field can be obtained, thus reduce the profiled member contraction distortion problem caused because temperature field is uneven.
Table 1: the heating lighting tube combination of experiment
| Experiment sequence number | Heating lighting tube combination |
| 1# | L1+L2+L3+L4+L5 |
| 2# | L1+L2+L3+L4+L5+L6 |
| 3# | L1+L2+L3+L4+L5+L7 |
| 4# | L1+L2+L3+L4+L6+L7 |
| 5# | L1+L2+L3+L4+L6+L8 |
| 6# | L1+L2+L3+L4+L5+L6+L7 |
| 7# | L1+L2+L3+L4+L5+L6+L7+L8 |
The selection of the holding temperature in step (3) is according to the lower temperature province of the crystalline rate in the DSC curve of UHMWPE, and generally lower than fusing point, make internal stresses release, each phase uniformity improves.After profiled member processing, the Volume Changes that the crystallization process due to UHMWPE produces, inner inevitably exist remaining stress.Crystalline rate near vitrification point and fusing point is minimum, therefore holding temperature is set near fusing point, crystalline rate can be made to keep low level, each position of profiled member is slowly crystallization evenly, internal stress slow releasing comes, the warpage caused due to stress also can slowly be calmed down, and internal flaw is eliminated, and dimensional accuracy and mechanical property all can be improved to some extent.
UHMWPE powder in the present invention, after SLS forming room is uniformly distributed, by predetermined heating fluorescent tube combined heated to preheat temperature, then is increased to processing temperature by after laser irradiation energy, now the powder body material melt-flow of laser irradiation region, cooling aftershaping.The application prospect that the SLS of UHMWPE is molded over medical field is long-range, especially medical auxiliary tool aspect, as manufactured medical auxiliary apparatus, implant, joint tissue etc., the data model of patient positions is set up by scanning and CAD means, defect is wherein repaired or designs rational implant etc., SLS is utilized to produce the personalized part of UHMWPE, these parts can better coincide the structure of patient positions, the physiology brought due to break-in alleviating patient is painful, accelerates the rehabilitation speed of patient simultaneously.The concrete steps utilizing SLS to manufacture UHMWPE medical auxiliary tool can comprise:
(1) the characteristic 3 D coordinate of scan patients body part, forms image digitization file;
(2) based on scan image design medical auxiliary tool model, after section, SLS equipment is imported;
(3) arrange according to above-mentioned technological parameter, use UHMWPE raw material to start processing;
(4) layering prints and manufactures, and obtains the personalized medicine accessory coincide with patient positions, and carries out post processing;
(5) profiled member is carried out to the test of the aspects such as surface quality, formed precision and mechanical property;
(6) pieces O.K. is applied to patient positions, assessment result of use.
Each technological parameter can be selected and combine arbitrarily in the scope of giving above, for the effect of process parameter optimizing is described, carries out contrast test.The concrete Selecting parameter of some embodiments and comparative example (thickness of shape layer is set to d=0.2mm) sees the following form 2, and result of the test is in table 3.
Table 2: molding technique parameter
The quality evaluation of table 3:SLS test specimen
Wherein: density refers to the actual density of sample and the ratio of solid density; Molding shrinkage is the difference of actual size and design size and the ratio of design size.
Go back from upper table 2 with table 3: comparative example 1 is compared with embodiment 1, and suitable preheat temperature contributes to improving density, reduces contraction distortion.Comparative example 2 and comparative example 3 illustrate respectively when k value too low or too high time, the large or poor mechanical property of sample contraction distortion can be caused.In embodiments of the invention, when k value is moderate, the sample taking into account mechanical property and dimensional accuracy can be obtained.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For those skilled in the art, without departing from the inventive concept of the premise, some equivalent to substitute or obvious modification can also be made, and performance or purposes identical, all should be considered as belonging to protection scope of the present invention.
Claims (7)
1. a precinct laser sintering forming method for ultra-high molecular weight polyethylene, is characterized in that, comprise the steps:
(1) ultra-high molecular weight polyethylene powder is heated to preheat temperature in precinct laser sintering former;
(2) adopt predetermined laser scanning speed and power output to make described ultra-high molecular weight polyethylene powder shaping in precinct laser sintering former, obtain profiled member;
(3) take out described profiled member, at the temperature of 110 ~ 130 DEG C, be incubated 8 ~ 12h, cooling afterwards obtains the molded article of ultra-high molecular weight polyethylene.
2. the precinct laser sintering forming method of ultra-high molecular weight polyethylene according to claim 1, it is characterized in that: in step (2), described predetermined laser scanning speed and power output are determined by following formula: v=k α, wherein: α represents laser output power ratio, 0 < α≤1, the peak power of the real output/laser instrument of α=laser instrument; ν represents laser scanning speed; The span of k is 2 ~ 6.
3. the precinct laser sintering forming method of ultra-high molecular weight polyethylene according to claim 2, is characterized in that: k is determined by below formula:
Wherein:
Δ T represents the temperature difference of lf processing temperature and preheat temperature;
C represents the specific heat capacity of ultra-high molecular weight polyethylene powder;
K represents the laser absorption rate of ultra-high molecular weight polyethylene powder;
P
maxrepresent the peak power of laser instrument;
ρ represents the density of ultra-high molecular weight polyethylene powder;
D represents the spot diameter of laser;
S represents the thickness of laser-transmitting ultra-high molecular weight polyethylene powder.
4. the precinct laser sintering forming method of ultra-high molecular weight polyethylene according to claim 1, is characterized in that: the mean molecule quantity of described ultra-high molecular weight polyethylene powder is 200 ~ 4,000,000, and particle diameter is 30 ~ 60 μm.
5. the precinct laser sintering forming method of ultra-high molecular weight polyethylene according to claim 1, is characterized in that: the described preheat temperature in described step (1) is 130 ~ 150 DEG C.
6. the precinct laser sintering forming method of ultra-high molecular weight polyethylene according to claim 1, is characterized in that: the heating fluorescent tube in described precinct laser sintering former adopts rebuilding, as follows:
Lower floor is made up of four heating lamp circumference of cannon bone quadrates, wherein the length direction of two heating fluorescent tubes is parallel with the direction of displacement of powder-laying roller in described precinct laser sintering former, and the length direction of other two heating fluorescent tubes is vertical with the direction of displacement of powder-laying roller in described precinct laser sintering former;
To heat above fluorescent tube at two parallel with the direction of displacement of powder-laying roller in described precinct laser sintering former and be also provided with also parallel with the direction of displacement of powder-laying roller in a described precinct laser sintering former heating fluorescent tube separately in addition.
7. the precinct laser sintering forming method of ultra-high molecular weight polyethylene according to claim 6, is characterized in that: the rated power of described heating fluorescent tube is 200 ~ 500W.
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| CN106726013A (en) * | 2016-11-29 | 2017-05-31 | 淮阴工学院 | A kind of manufacturing process of low mill ultra-high molecular weight polyethylene composite material hip cotyle |
| CN107686577A (en) * | 2016-08-04 | 2018-02-13 | 中国石油化工股份有限公司 | A kind of polyethylene composition and application and laser sintering processes and three-dimensional article |
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| CN111055493A (en) * | 2018-10-16 | 2020-04-24 | 中国石油化工股份有限公司 | Laser sintering forming device and forming method |
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| CN112743835A (en) * | 2020-12-25 | 2021-05-04 | 聊城市东昌府区妇幼保健院 | Medical protective clothing and manufacturing method thereof |
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