CN107901419B - A method of annealing regulation PA3200 3D printing surface of shaped parts wetability - Google Patents

A method of annealing regulation PA3200 3D printing surface of shaped parts wetability Download PDF

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Publication number
CN107901419B
CN107901419B CN201711390204.0A CN201711390204A CN107901419B CN 107901419 B CN107901419 B CN 107901419B CN 201711390204 A CN201711390204 A CN 201711390204A CN 107901419 B CN107901419 B CN 107901419B
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China
Prior art keywords
annealing
printing
shaped parts
molded part
wetability
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CN201711390204.0A
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CN107901419A (en
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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 method of annealing regulation PA3200 3D printing surface of shaped parts wetability 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 part) is prepared, it is annealed using tube type vacuum furnace to molded part, the tube furnace has many advantages, such as easy to operate, high accuracy temperature control, can work under multiple atmosphere.Setting heating-up time 1-3 hours, soaking time 1-5 hours, temperature fall time 1-3 hours, 100 DEG C -160 DEG C of annealing temperature, the parameters such as annealing atmosphere oxygen, nitrogen made annealing treatment molded part.After annealing, the contact angle of surface of shaped parts becomes 60 ° from 121 °, surface wettability is changed into hydrophily by hydrophobicity, Effective Regulation 3200 3D printing surface of shaped parts wetability of PA.

Description

A method of annealing regulation PA3200 3D printing surface of shaped parts wetability
Technical field
The present invention relates to 3D printing technique and medical application fields, especially devise a kind of annealing regulation PA3200 The method of 3D printing surface of shaped parts wetability.
Background technique
PA3200 is a kind of white powder by micro-meter scale bead filling PA2200, with excellent mechanical performance and Biocompatibility.Currently, the main molding mode of PA3200 is 3D printing selective laser sintering (SLS) technology.SLS is that one kind makes The rapid shaping technique for successively sintering little particle (polymer, ceramics) into entity with high power laser light, has shaping speed fast, The features such as precision is high.There is excellent mechanical performance and life based on the molding PA3200 3D printing molded part of 3D printing SLS technology Object compatibility has huge application prospect, including suture, trachea bracket, channel, conduit etc. in medical field.It is applied to The element of medical field need to have good biocompatibility, it is desirable that element surface is smooth, and hydrophily is presented in wetability.However base Hydrophobicity is presented in the molding PA3200 3D printing surface of shaped parts wetability of SLS technology, 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 part, regulates and controls its surface wettability, be allowed to Reach the requirement of medical field application.
Currently, mainly having for the method for PA class elements material surface treatment regulation wetability:
1. plasma processing method: this method is mainly contacted using the air-flow of upper state with surface of shaped parts, and table is caused Face pattern and chemical component change, to achieve the purpose that regulate and control wetability.For PA class material, the air-flow master of upper state If nitrogen and oxygen plasma.Although the method can efficiently realize the regulation to surface of shaped parts wetability, also can be right The functionality 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 regulate and control wetability.The method can very effective realization regulation surface of shaped parts Wetability, but coating is unstable, is easy to fall off.
3. laser irradiation 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 component, to achieve the purpose that regulate and control surface of shaped parts wetability.The method can be quick, has The realization of effect regulates and controls PA class surface of shaped parts wetability, but is directed to PA3200, and laser irradiation fails the change for causing surface wettability Change.
4. make annealing treatment method: this method mainly by molded part High temperature storage for a period of time, then slowly cool down again, Surface of shaped parts pattern and chemical component is caused to change during this to achieve the purpose that regulate and control its wetability.This side Method can effectively realize the surface wettability of regulation PA class molded part, and easy to operate, and process is simple.It is several compared to other Method, advantage essentially consist in the annealing temperature that can accurately control under different atmosphere, to reach accuracy controlling molded part table The purpose of face wetability, and not yet occur regulating and controlling the wetability of PA3200 3D printing molded part for annealing at present Relevant report.
Therefore, wetability of the present invention using annealing method regulation PA3200 3D printing surface of shaped parts, this method stream Journey is simple, can effectively realize the regulation of the wetability to PA3200 3D printing surface of shaped parts.
Summary of the invention
The object of the present invention is to provide a kind of sides of annealing regulation PA3200 3D printing surface of shaped parts wetability Method.
What the purpose of the present invention was achieved through the following technical solutions:
1) PA3200 3D printing molded part is prepared using 3D printing SLS technology, is dipped in alcohol solvent cleaning later, It is subsequently dipped to be cleaned by ultrasonic in ultrapure water, is finally putting into drying box and dries, sample is prepared and completed;
2) heating-up time in annealing process, soaking time, temperature fall time, annealing temperature, the parameters such as atmosphere, setting are designed The program of annealing furnace is placed in furnace after it is ready to complete by the 3D printing molded part completed is handled through step 1);
3) vacuum tube furnace is used, heating-up time 1-3 hour in annealing process, soaking time 1-5 hours, temperature fall time 1- 3 hours, 100 DEG C -160 DEG C of annealing temperature, annealing atmosphere was oxygen or nitrogen;
The present invention is to make surface of shaped parts pattern using heating, the heat preservation, temperature-fall period made annealing treatment under different atmosphere It changes with chemical component, realizes the purpose of regulation PA3200 3D printing surface of shaped parts wetability.It not yet moves back at present The method of the wetability of fire processing regulation PA3200 3D printing molded part.This method has apparent innovative:
1) material that this method uses is PA3200, and forming technique is using 3D printing precinct laser sintering (SLS) Technology;
2) this method uses tube type vacuum furnace, which has easy to operate, high accuracy temperature control, work under multiple atmosphere The advantages that.Heating-up time 1-3 hour in annealing process, soaking time 1-5 hours, temperature fall time 1-3 hours, annealing temperature 100℃-160℃;
3) this method carries out under oxygen or nitrogen atmosphere, regulates and controls PA32003D by control annealing temperature and is printed as The surface wettability of type part, whole set process is easy to operate, and process is simple.
Detailed description of the invention
Fig. 1 is the 3D molding of annealing regulation PA3200 3D printing surface of shaped parts wetability method of the present invention Part surface wettability variation diagram (wetability is characterized with contact angle)
Specific embodiment
The specific embodiment of the invention is described in further details with reference to the accompanying drawing:
Step 1: preparing PA3200 3D printing molded part using 3D printing SLS technology
This step is intended to the excellent PA3200 3D printing molded part of processability, can be divided into and prepare data, molding, rear place Manage three processes:
1) prepare data: this process mainly establishes molded part threedimensional model using magics software and saves as STL (3D is beaten Stamp type professional format) format, the model having had built up is sliced using rapid section software RP Tools later, will then be cut Piece file imports in PSW 3.7 (this be the software for controlling machine and running), is stored as with section and elevation information .eosjz file, finally by this file copy into 3.7 software of printer EOS P396 machine computer PSW, load, this To prepare data procedures;
2) form: this process primary operational EOS P396 machine carries out the molding of molded part, prepares moulding cylinder before forming, will Moulding cylinder rises to pre- powdering 9mm after highest, and preheats powder bed 2 hours, and machine can be under software control according to molding later The cross section information of every layer of part carries out layer-by-layer sintering process, and every thickness degree is 0.12mm, until entire 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 molding, due to molding Cylinder temperature is higher, can be taken off within natural cooling 10 hours.Surface of shaped parts and internal dust are cleared up using high pressure air rifle later, It is then dipped in alcohol solvent cleaning, is subsequently dipped to be cleaned by ultrasonic in ultrapure water, is finally putting into drying box and dries, sample is Post-processing is completed.
Step 2: design annealing parameter, is made annealing treatment
According to the fusing point of PA3200 and the heating-up time of pertinent literature investigation design annealing, soaking time, when cooling Between, temperature, the parameters such as atmosphere, design parameter be heating-up time 1-3 hours, soaking time 1-5 hours, temperature fall time 1-3 hours, 100 DEG C -160 DEG C of annealing temperature, annealing atmosphere is oxygen or nitrogen.Later by the ready PA3200 3D printing of previous step Molded part is placed in tube type vacuum furnace, then operates annealing furnace, will vacuumize in furnace and oxygen or nitrogen are filled in furnace, is checked The closure and circulation of entire gas circuit;Annealing furnace program is finally arranged according to above-mentioned parameter, starts to be made annealing treatment.
Step 3: surface wettability detects
Refering to fig. 1, the surface wettability of molded part is characterized by contact angle, and less than 90 °, surface presents hydrophilic contact angle Property, for contact angle greater than 90 °, hydrophobicity is presented in surface, and contact angle is detected with OCA20 contact angle measurement.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 may be implemented regulation PA3200 3D printing surface of shaped parts wetting Property, so that surface of shaped parts wetability is become hydrophily from hydrophobicity.

Claims (1)

1. a kind of method of annealing regulation PA3200 3D printing surface of shaped parts wetability, which is characterized in that this method packet Include following steps:
1) PA3200 3D printing molded part is prepared using 3D printing selective laser sintering technology, molded part is immersed into ethyl alcohol later Solvent cleaning, is subsequently dipped to be cleaned by ultrasonic in ultrapure water, is finally putting into drying box and dries, and sample is prepared and completed;
2) journey of annealing furnace is arranged in the heating-up time in design annealing process, soaking time, temperature fall time, annealing temperature, atmosphere Sequence is placed in furnace after it is ready to complete by the 3D printing molded part completed is handled through step 1);
3) tube type vacuum furnace is used, heating-up time 1-3 hour in annealing process, soaking time 1-5 hours, temperature fall time 1-3 was small When, 100 DEG C -160 DEG C of annealing temperature, annealing atmosphere is oxygen or nitrogen.
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

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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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