CN107901419A - A kind of method for making annealing treatment regulation and control PA3200 3D printing surface of shaped parts wetabilitys - Google Patents

A kind of method for making annealing treatment regulation and control PA3200 3D printing surface of shaped parts wetabilitys Download PDF

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Publication number
CN107901419A
CN107901419A CN201711390204.0A CN201711390204A CN107901419A CN 107901419 A CN107901419 A CN 107901419A CN 201711390204 A CN201711390204 A CN 201711390204A CN 107901419 A CN107901419 A CN 107901419A
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China
Prior art keywords
annealing
printing
shaped parts
control
time
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CN201711390204.0A
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CN107901419B (en
Inventor
蒋毅坚
魏小波
曾勇
闫胤洲
赵艳
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Beijing University of Technology
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Beijing University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02Thermal after-treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/0009After-treatment of articles without altering their shape; Apparatus therefor using liquids, e.g. solvents, swelling agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE 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
    • B33Y40/00Auxiliary operations or equipment, e.g. for material handling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/0009After-treatment of articles without altering their shape; Apparatus therefor using liquids, e.g. solvents, swelling agents
    • B29C2071/0045Washing using non-reactive liquids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C71/00After-treatment of articles without altering their shape; Apparatus therefor
    • B29C71/02Thermal after-treatment
    • B29C2071/022Annealing

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)

Abstract

A kind of method for making annealing treatment regulation and control PA3200 3D printing surface of shaped parts wetabilitys, belongs to 3D printing technique and medical application fields.The present invention utilizes 3D printing selective laser sintering technology (Selective Laser Sintering, SLS PA3200 3D printing molded parts) are prepared, annealed using tube type vacuum stove to molded part, the tube furnace has easy to operate, high accuracy temperature control, the advantages that working under multiple atmosphere.When the setting heating-up time 13 is small, when soaking time 15 is small, when temperature fall time 13 is small, 160 DEG C of annealing temperature 100 DEG C, the parameter such as annealing atmosphere oxygen, nitrogen makes annealing treatment molded part.After annealing, the contact angle of surface of shaped parts is changed into 60 ° from 121 °, surface wettability is changed into hydrophily by hydrophobicity, Effective Regulation 3200 3D printing surface of shaped parts wetabilitys of PA.

Description

A kind of method for making annealing treatment regulation and control PA3200 3D printing surface of shaped parts wetabilitys
Technical field
The present invention relates to 3D printing technique and medical application fields, particularly devise a kind of annealing regulation and control PA3200 The method of 3D printing surface of shaped parts wetability.
Background technology
PA3200 be it is a kind of by micro-meter scale bead filling PA2200 white powder, have excellent mechanical performance and Biocompatibility.At present, the main molding mode of PA3200 is 3D printing selective laser sintering (SLS) technology.SLS is that one kind makes Little particle (polymer, ceramics) is successively sintered into the rapid shaping technique of entity with high power laser light, it is fast with shaping speed, The features such as precision is high.Excellent mechanical performance and life are had based on the molding PA3200 3D printings molded part of 3D printing SLS technologies Thing compatibility, there is huge application prospect, including suture, trachea bracket, passage, conduit etc. in medical field.It is applied to The element of medical field need to have good biocompatibility, it is desirable to which element surface is smooth, and hydrophily is presented in wetability.But base Hydrophobicity is presented in the molding PA3200 3D printings surface of shaped parts wetability of SLS technologies, this is serious to limit it in medical treatment Application in field.Therefore, it is necessary to be surface-treated to PA3200 3D printing molded parts, regulate and control its surface wettability, be allowed to Reach the requirement of medical field application.
At present, the method for being surface-treated regulation and control wetability for PA classes elements material mainly has:
1. plasma processing method:This method is mainly contacted using the air-flow of upper state with surface of shaped parts, causes table Face pattern and chemical composition change, so as to achieve the purpose that to regulate and control wetability.For PA class materials, the air-flow master of upper state If nitrogen and oxygen plasma.Although the method can efficiently realize the regulation and control to surface of shaped parts wetability, also can be right The feature on surface impacts.
2. surface coated treatment method:This method mainly prepares one layer of hydrophobic or hydrophilic coating in surface of shaped parts, Coating is adhered to surface, achievees the purpose that to regulate and control wetability.The method very effective can realize regulation and control surface of shaped parts Wetability, but coating is unstable, easily comes off.
3. laser radiation treatment method:This method handles surface of shaped parts using the high-energy of laser, makes the table of molded part Face pattern changes with chemical composition, so as to achieve the purpose that to regulate and control surface of shaped parts wetability.The method can be quick, has The realization regulation and control PA class surface of shaped parts wetabilitys of effect, but PA3200 is directed to, laser irradiation fails the change for causing surface wettability Change.
4. the method for annealing:This method for a period of time, then slowly cools down again mainly by molded part High temperature storage, Surface of shaped parts pattern and chemical composition is caused to change so as to achieve the purpose that to regulate and control its wetability during this.This side Method can effectively realize the surface wettability of regulation and control PA class molded parts, and easy to operate, and flow is simple.It is several compared to other Method, its advantage essentially consist in the annealing temperature that can accurately control under different atmosphere, so as to reach accuracy controlling molded part table The purpose of face wetability, and not yet occur at present for the wetability for making annealing treatment regulation and control PA3200 3D printing molded parts Relevant report.
Therefore, the present invention is using the wetability of annealing method regulation and control PA3200 3D printing surface of shaped parts, this method stream Journey is simple, can effectively realize the regulation and control of the wetability to PA3200 3D printing surface of shaped parts.
The content of the invention
The object of the present invention is to provide a kind of side for making annealing treatment regulation and control PA3200 3D printing surface of shaped parts wetabilitys Method.
What the purpose of the present invention was achieved through the following technical solutions:
1) PA3200 3D printing molded parts are prepared using 3D printing SLS technologies, are dipped in alcohol solvent cleaning afterwards, It is subsequently dipped to be cleaned by ultrasonic in ultra-pure water, is finally putting into drying box and dries, sample is prepared and completed;
2) parameters such as the heating-up time in annealing process, soaking time, temperature fall time, annealing temperature, atmosphere are designed, are set The program of annealing furnace, after it is ready to complete, is placed in the 3D printing molded part completed is handled through step 1) in stove;
3) vacuum tube furnace is used, when heating-up time 1-3 is small in annealing process, when soaking time 1-5 is small, temperature fall time 1- 3 it is small when, 100 DEG C -160 DEG C of annealing temperature, annealing atmosphere is oxygen or nitrogen;
The present invention is to utilize the heating made annealing treatment under different atmosphere, insulation, temperature-fall period, makes surface of shaped parts pattern Change with chemical composition, realize the purpose of regulation and control PA3200 3D printing surface of shaped parts wetabilitys.Not yet move back at present The method of the wetability of fire processing regulation and control PA3200 3D printing molded parts.This method has obvious innovative:
1) material that this method uses is PA3200, its forming technique is using 3D printing precinct laser sintering (SLS) Technology;
2) this method uses tube type vacuum stove, which has easy to operate, high accuracy temperature control, work under multiple atmosphere The advantages that.When heating-up time 1-3 is small in annealing process, when soaking time 1-5 is small, when temperature fall time 1-3 is small, annealing temperature 100℃-160℃;
3) this method carries out under oxygen or nitrogen atmosphere, is printed as by controlling annealing temperature to regulate and control PA32003D The surface wettability of type part, whole set process is easy to operate, and flow is simple.
Brief description of the drawings
Fig. 1 is the 3D shapings of annealing regulation and control PA3200 3D printing surface of shaped parts wetability methods of the present invention Part surface wettability variation diagram (wetability is characterized with contact angle)
Embodiment
The specific embodiment of the invention is described in further details below in conjunction with the accompanying drawings:
The first step:PA3200 3D printing molded parts are prepared using 3D printing SLS technologies
This step is intended to the excellent PA3200 3D printing molded parts of processability, can be divided into and prepare data, shaping, rear place Manage three processes:
1) data are prepared:This process mainly establishes molded part threedimensional model using magics softwares and saves as STL (3D is beaten Stamp type professional format) form, the model having been had built up afterwards using rapid section software RP Tools sections, will then cut Piece file is imported in PSW 3.7 software of machine operation (this in order to control), is saved as with section and elevation information .eosjz file, finally by this file copy into 3.7 softwares of printer EOS P396 machine computers PSW, loading, this To prepare data procedures;
2) it is molded:This process primary operational EOS P396 machines carry out the shaping of molded part, prepare moulding cylinder before being molded, will Moulding cylinder rises to pre- powdering 9mm after highest, and preheat powder bed 2 it is small when, machine can be under software control according to shaping afterwards The cross section information of every layer of part carries out successively sintering process, is 0.12mm per layer thickness, until whole molded part is completed;
3) post-process:This process mainly takes out molded part and carries out the cleaning of surface powder.After the completion of shaping, due to shaping Cylinder temperature is higher, and natural cooling 10 can be taken off when small.Surface of shaped parts and internal dust are cleared up using high pressure air rifle afterwards, Alcohol solvent cleaning is then dipped in, is subsequently dipped to be cleaned by ultrasonic in ultra-pure water, is finally putting into drying box and dries, sample is Post processing is completed.
Second step:Annealing parameter is designed, is made annealing treatment
According to the fusing point of PA3200 and the heating-up time of pertinent literature investigation design annealing, soaking time, during cooling Between, temperature, the parameter such as atmosphere, design parameter for heating-up time 1-3 it is small when, when soaking time 1-5 is small, when temperature fall time 1-3 is small, 100 DEG C -160 DEG C of annealing temperature, annealing atmosphere are oxygen or nitrogen.Afterwards by the ready PA3200 3D printings of previous step Molded part is placed in tube type vacuum stove, then operates annealing furnace, will be vacuumized in stove and oxygen or nitrogen are filled with stove, is checked The closure and circulation of whole gas circuit;Annealing furnace program is finally set according to above-mentioned parameter, proceeds by annealing.
3rd step:Surface wettability detects
Refering to Fig. 1, the surface wettability of molded part is characterized by contact angle, and contact angle is less than 90 °, and surface presents hydrophilic Property, for contact angle more than 90 °, hydrophobicity is presented in surface, and contact angle is detected with OCA20 contact angle measurements.Without stepping back 121 ° of the surface of shaped parts contact angle of processing, is presented hydrophobic surface, and the surface of shaped parts contact angle by annealing is reachable 60 °, hydrophilic surface is presented.This result shows that, annealing can realize regulation and control PA3200 3D printings surface of shaped parts wetting Property, surface of shaped parts wetability is changed into hydrophily from hydrophobicity.

Claims (2)

  1. A kind of 1. method for making annealing treatment regulation and control PA3200 3D printing surface of shaped parts wetabilitys, it is characterised in that this method bag Include following steps:
    1) PA3200 3D printing molded parts are prepared using 3D printing selective laser sintering technology, molded part is immersed into ethanol afterwards Solvent cleans, and is subsequently dipped to be cleaned by ultrasonic in ultra-pure water, is finally putting into drying box and dries, and sample is prepared and completed;
    2) heating-up time in design annealing process, soaking time, temperature fall time, annealing temperature, atmosphere, set the journey of annealing furnace Sequence, after it is ready to complete, is placed in the 3D printing molded part completed is handled through step 1) in stove;
    3) tube type vacuum stove is used, when heating-up time 1-3 is small in annealing process, when soaking time 1-5 is small, temperature fall time 1-3 is small When, 100 DEG C -160 DEG C of annealing temperature, annealing atmosphere is oxygen or nitrogen.
  2. 2. the method for annealing regulation and control PA3200 3D printing surface of shaped parts wetabilitys according to claim 1, it is special Sign is by controlling the heating-up time, soaking time, temperature fall time, annealing temperature, atmosphere one or several, regulate and control molded part Surface wettability.
CN201711390204.0A 2017-12-21 2017-12-21 A method of annealing regulation PA3200 3D printing surface of shaped parts wetability Active CN107901419B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102796909A (en) * 2012-01-31 2012-11-28 重庆润泽医药有限公司 Method for preparing porous tantalum medical implant material through three-dimensional printing forming
CN103740963A (en) * 2012-01-31 2014-04-23 重庆润泽医药有限公司 Method for preparing porous tantalum medical implant material by selective laser sintering formation
CN103785835A (en) * 2014-03-04 2014-05-14 山东大学 Manufacturing method for preventing deforming and cracking when large-size complex titanium alloy parts are in three-dimensional printing
US9592530B2 (en) * 2012-11-21 2017-03-14 Stratasys, Inc. Additive manufacturing with polyamide consumable materials
CN107073825A (en) * 2014-10-29 2017-08-18 惠普发展公司,有限责任合伙企业 Three-dimensional (3D) Method of printing

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102796909A (en) * 2012-01-31 2012-11-28 重庆润泽医药有限公司 Method for preparing porous tantalum medical implant material through three-dimensional printing forming
CN103740963A (en) * 2012-01-31 2014-04-23 重庆润泽医药有限公司 Method for preparing porous tantalum medical implant material by selective laser sintering formation
US9592530B2 (en) * 2012-11-21 2017-03-14 Stratasys, Inc. Additive manufacturing with polyamide consumable materials
CN103785835A (en) * 2014-03-04 2014-05-14 山东大学 Manufacturing method for preventing deforming and cracking when large-size complex titanium alloy parts are in three-dimensional printing
CN107073825A (en) * 2014-10-29 2017-08-18 惠普发展公司,有限责任合伙企业 Three-dimensional (3D) Method of printing

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Application publication date: 20180413

Assignee: Luoyang Jingrui Industrial Technology Co.,Ltd.

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Denomination of invention: A method of annealing treatment to regulate the surface wettability of PA3200 3D printed molded parts

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Denomination of invention: A method of annealing treatment to regulate the surface wettability of PA3200 3D printed molded parts

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