CN117600494B - Printing method for improving corrosion resistance and strength of 3D printing collimator - Google Patents

Printing method for improving corrosion resistance and strength of 3D printing collimator Download PDF

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Publication number
CN117600494B
CN117600494B CN202410096509.4A CN202410096509A CN117600494B CN 117600494 B CN117600494 B CN 117600494B CN 202410096509 A CN202410096509 A CN 202410096509A CN 117600494 B CN117600494 B CN 117600494B
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printing
corrosion resistance
strength
powder
collimator
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CN117600494A (en
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胡忠娟
徐林
刘文胜
陆文杰
余伟
韩道镜
郁兀斌
陈世宝
朱晓峰
唐开龙
王涛
仇治勤
罗建军
时晓明
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Anqing Rimet Technology Co ltd
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Anqing Rimet Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/20Direct sintering or melting
    • B22F10/28Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/09Mixtures of metallic powders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/64Treatment of workpieces or articles after build-up by thermal means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/66Treatment of workpieces or articles after build-up by mechanical means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/68Cleaning or washing
    • 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
    • B33Y10/00Processes of additive manufacturing
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

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

Abstract

The invention discloses a printing method for improving corrosion resistance and strength of a 3D printing collimator, which specifically comprises the following steps: (1) Mixing spherical tungsten powder and spherical nickel powder in a certain proportion to obtain mixed powder; (2) drying the mixed powder; (3) Pouring the dried mixed powder into a printing bin of a 3D printer, and when the oxygen content in the printing bin is less than 500ppm, starting to print, and after the printing is finished, obtaining a 3D printing piece; (4) Placing the 3D printing piece and the substrate in a hydrogen atmosphere protection furnace for heat treatment; (5) cutting the heat-treated 3D printed matter from the substrate; (6) Performing sand blasting or abrasive particle flow treatment on the cut 3D printing piece, and removing burrs on the hole wall of the 3D printing piece and cutting burrs generated by cutting; (7) And carrying out ultrasonic cleaning and drying on the 3D printing piece after the deburring to obtain the nickel-tungsten alloy collimator. The invention can simultaneously improve the breaking strength and the corrosion resistance of the collimator.

Description

Printing method for improving corrosion resistance and strength of 3D printing collimator
Technical Field
The invention relates to the technical field of 3D printing tungsten collimators, in particular to a printing method for improving corrosion resistance and strength of a 3D printing collimator.
Background
The development of CT machine (computed tomography) technology is rapid, and the development of the CT machine is currently advanced to the fifth generation, wherein an X-ray detector is a core component for checking and imaging, relates to the assembly and the debugging of up to thousands of high-precision parts, and is a key step and technology for ensuring the performance of the whole CT machine and controlling the production cost. The X-ray detector of the CT machine consists of three main parts, namely an X-ray collimator, a collimator bracket and a photoelectric conversion module. Along with the development of medical imaging industry and the demand of high-precision diagnosis and treatment, the structure of the X-ray collimator is more and more complex and diversified, so that the X-ray collimator is produced by adopting a selective laser melting 3D printing technology (SLM).
SLM technology has evolved over the years to mature in printing of many metal powders, such as iron, titanium, nickel, etc., but is relatively headache for pure tungsten (W) prints. This is because tungsten possesses an extremely high melting point (3410 ℃) and is the most refractory metal in nature. In essence, the SLM technology melts and welds spherical tungsten particles with the high energy of the laser, and the laser does not completely melt the entire tungsten sphere, but only a portion of the surface of the tungsten sphere, after rapidly sweeping the spherical tungsten powder in the print area due to the high melting point of tungsten. Thus, although the entire tungsten article can be finally print-molded, its structural strength is always poor.
Currently, in order to increase the intensity of the tungsten collimator, the printing parameters are generally adjusted, such as increasing the printing power, reducing the scanning speed, and the like. However, increasing the printing power tends to cause a sharp rise in temperature in the print cartridge, and the partial area of the material is highly stressed, and serious distortion occurs after the 3D printed material is cut from the substrate. In addition, the scanning speed is reduced, so that the production efficiency is greatly reduced.
In addition, the 3D printed tungsten product is usually printed by spherical powder of several micrometers to tens of micrometers, and the spherical powder has small particles, high surface activity and insufficient laser melting welding, so that the printed part is easy to be oxidized and corroded in a high-temperature and humid environment.
Disclosure of Invention
The invention aims to overcome the defects and the shortcomings of the prior art and provide a printing method for improving the corrosion resistance and strength of a 3D printing collimator so as to improve the breaking strength and corrosion resistance of the collimator at the same time.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a printing method for improving corrosion resistance and strength of a 3D printing collimator is characterized by comprising the following steps of: the method specifically comprises the following steps:
s1, mixing: mixing spherical tungsten powder and spherical nickel powder to obtain mixed powder, wherein the mass fraction of the spherical nickel powder is 1-3%, and the mass fraction of the spherical tungsten powder is 97-99%;
s2, drying: putting the mixed powder into a vacuum drying oven for drying;
S3.3D printing: pouring the dried mixed powder into a printing bin of a 3D printer, and when the oxygen content in the printing bin is less than 500ppm, starting to print, and after the printing is finished, obtaining a 3D printing piece;
s4, heat treatment: placing the 3D printing piece and the substrate in a hydrogen atmosphere protection furnace for heat treatment;
s5, cutting: cutting the 3D printing piece after heat treatment from the substrate;
s6, deburring: performing sand blasting or abrasive particle flow treatment on the cut 3D printing piece, and removing burrs on the hole wall of the 3D printing piece and cutting burrs generated by cutting;
s7, cleaning and drying: and carrying out ultrasonic cleaning and drying on the 3D printing piece after the deburring to obtain the nickel-tungsten alloy collimator.
Further, in the step S1, before mixing the spherical tungsten powder and the spherical nickel powder, the spherical tungsten powder and the spherical nickel powder with the granularity of 5-45 mu m, which accord with normal distribution, have the sphericity of more than 95% and the oxygen content of less than 100ppm are selected.
In the step S1, the spherical tungsten powder and the spherical nickel powder are put into a mixer for uniform mixing for 30-180min.
Further, during mixing, nitrogen is filled into the mixer for protection.
Further, in the step S2, the drying time is 30-240 min, the drying temperature is 60-110 ℃, and the vacuum degree of the vacuum drying oven is less than 10 -2 Pa。
Further, in the step S3, after the door of the printing bin is closed, argon is blown into the printing bin to perform degassing, so that the oxygen content in the printing bin is less than 500ppm.
Further, in the step S3, the printing power of the 3D printer is 50-240W, the scanning speed is 200-1000mm/S, and the thickness of the printing layer is 1.5-4 filaments/layer.
Further, in the step S4, the heat treatment temperature is 500-1000 ℃ and the heat preservation time is 2-8h.
In step S5, a 3D printed material is cut off against the surface of the substrate by using a slow wire cutting method.
Further, in the step S7, the frequency of ultrasonic waves is 25-53KHz, the cleaning time is 5-30min, and the water temperature is 25-80 ℃; the drying temperature is 50-120 ℃, and the drying time is 5-120min.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a certain proportion (1-3%) of spherical nickel powder is added into the spherical tungsten powder, and the two spherical powders are uniformly mixed, so that nickel-tungsten alloy can be generated during printing, the alloyed nickel-tungsten phase not only obviously improves the breaking strength of a collimator product (from 150N to 220N), but also greatly improves the corrosion resistance (the neutral salt spray test time can be increased from 2 hours to 72 hours).
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, a printing method for improving corrosion resistance and strength of a 3D printing collimator specifically includes the following steps:
step one, mixing: selecting spherical tungsten powder and spherical nickel powder with the granularity of 5-45 mu m, conforming to normal distribution, the sphericity of more than 95 percent and the oxygen content of less than 100ppm, and uniformly mixing the spherical tungsten powder and the spherical nickel powder in a mixer for 150min according to a certain proportion, namely, the mass fraction of the spherical nickel powder is 3 percent, the mass fraction of the spherical tungsten powder is 97 percent, thereby obtaining mixed powder.
The particle size of 5-45 μm is to match the thickness of the printed layer; the normal distribution is met, so that the compactness of the printing material is ensured, and the breaking strength is ensured; the sphericity is more than 95 percent, so as to ensure the fluidity of the powder, thereby ensuring the uniformity of powder spreading; the oxygen content is < 100ppm in order to ensure the purity of the powder.
In addition, since a certain amount of mechanical energy is applied to the powder during mixing, the mixer needs to be purged with nitrogen gas to protect the powder from oxidation.
Step two, drying: and (5) putting the mixed powder into a vacuum drying oven for drying.
Specifically, the drying time is 180min, the drying temperature is 90 ℃, and the vacuum degree of a vacuum drying oven is less than 10 -2 Pa。
Step three, 3D printing: pouring the dried mixed powder into a printing bin of a 3D printer, closing a bin door of the printing bin, blowing argon into the printing bin for degassing, and when the oxygen content in the printing bin is less than 500ppm, starting to print, and after printing, obtaining a 3D printing piece.
Specifically, the printing power of the 3D printer is 180W, the scanning speed is 600mm/s, and the thickness of the printing layer is 2 wires/layer.
Step four, heat treatment: and placing the 3D printing part and the substrate in a hydrogen atmosphere protection furnace for heat treatment.
Specifically, the heat treatment temperature is 700 ℃, and the heat preservation time is 6 hours.
Step five, cutting: and cutting the 3D printed part after heat treatment from the substrate by adopting a cutting mode of a slow wire.
Step six, deburring: and carrying out sand blasting treatment or abrasive particle flow treatment on the cut 3D printing piece, and removing burrs on the hole wall of the 3D printing piece and cutting burrs generated by cutting.
Step seven, cleaning and drying: and carrying out ultrasonic cleaning and drying on the 3D printing piece after the deburring to obtain the nickel-tungsten alloy collimator.
Specifically, the frequency of ultrasonic wave is 45KHz, the cleaning time is 20min, and the water temperature is 60 ℃; the drying temperature is 100 ℃ and the drying time is 90min.
The invention is further described below with reference to the accompanying drawings:
according to the invention, the laser energy of the 3D printer is utilized, nickel is fully melted (the melting point of nickel is 1453 ℃) while scanning, meanwhile, tungsten and nickel are partially alloyed to form a tungsten-nickel alloy phase, so that the binding force between powders can be obviously improved, and the breaking strength of a product is improved. At the same time, nickel and the nickel-tungsten phase formed have excellent corrosion resistance and are difficult to oxidize even in high temperature humid air.
Under the precondition that other technological parameters and conditions are unchanged, when the mass fraction of the spherical nickel powder is 0%, 0.5%, 1%, 2% and 3%, respectively, 3D printing tests are respectively carried out, and breaking strength tests and neutral salt spray tests are respectively carried out on the printed nickel tungsten alloy collimator, wherein specific test data are shown in the following table:
TABLE 1 Effect of Nickel doping on the intensity of 3D printing collimators
Sample number Proportion of Nickel (mass fraction) Breaking strength (N)
1 0.00% 151
2 0.50% 157
3 1.00% 166
4 2.00% 190
5 3.00% 221
TABLE 2 Effect of Nickel doping on the Corrosion resistance of 3D printing collimators
Sample number Proportion of Nickel (mass fraction) Neutral salt spray test time (h)
1 0.00% 2
2 0.50% 5
3 1.00% 12
4 2.00% 36
5 3.00% 72
As shown in tables 1 and 2, when the mass fraction of the spherical nickel powder is 1-3%, the fracture strength and the corrosion resistance of the collimator (nickel tungsten alloy collimator) obtained by 3D printing are obviously improved.
Specifically, when the mass fraction of the spherical nickel powder is 3%, the breaking strength of the collimator (nickel tungsten alloy collimator) obtained by 3D printing is improved to 221N, and the neutral salt spray test time is improved to 72h, so that the breaking strength of the collimator product is obviously improved, and the corrosion resistance of the collimator is greatly improved.
Although the present disclosure describes embodiments, not every embodiment is described in terms of a single embodiment, and such description is for clarity only, and one skilled in the art will recognize that the embodiments described in the disclosure as a whole may be combined appropriately to form other embodiments that will be apparent to those skilled in the art.
Therefore, the above description is only of the preferred embodiments of the present application and is not intended to limit the scope of the present application; all changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.

Claims (10)

1. A printing method for improving corrosion resistance and strength of a 3D printing collimator is characterized by comprising the following steps of: the method specifically comprises the following steps:
s1, mixing: mixing spherical tungsten powder and spherical nickel powder to obtain mixed powder, wherein the mass fraction of the spherical nickel powder is 1-3%, and the mass fraction of the spherical tungsten powder is 97-99%;
s2, drying: putting the mixed powder into a vacuum drying oven for drying;
S3.3D printing: pouring the dried mixed powder into a printing bin of a 3D printer, and when the oxygen content in the printing bin is less than 500ppm, starting to print, and after the printing is finished, obtaining a 3D printing piece;
s4, heat treatment: placing the 3D printing piece and the substrate in a hydrogen atmosphere protection furnace for heat treatment;
s5, cutting: cutting the 3D printing piece after heat treatment from the substrate;
s6, deburring: performing sand blasting or abrasive particle flow treatment on the cut 3D printing piece, and removing burrs on the hole wall of the 3D printing piece and cutting burrs generated by cutting;
s7, cleaning and drying: and carrying out ultrasonic cleaning and drying on the 3D printing piece after the deburring to obtain the nickel-tungsten alloy collimator.
2. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1, characterized by: in the step S1, before the spherical tungsten powder and the spherical nickel powder are mixed, the spherical tungsten powder and the spherical nickel powder with the granularity of 5-45 mu m, which accord with normal distribution, have the sphericity more than 95% and the oxygen content less than 100ppm are selected.
3. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1 or 2, characterized by: in the step S1, spherical tungsten powder and spherical nickel powder are put into a mixer for uniform mixing for 30-180min.
4. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 3, characterized by: during mixing, nitrogen is filled into the mixer for protection.
5. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1, characterized by: in the step S2, the drying time is 30-240 min, the drying temperature is 60-110 ℃, and the method is characterized in thatThe vacuum degree of the vacuum drying box is less than 10 -2 Pa。
6. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1, characterized by: in the step S3, after the bin gate of the printing bin is closed, argon is blown into the printing bin to carry out degassing, so that the oxygen content in the printing bin is less than 500ppm.
7. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1 or 6, characterized by: in the step S3, the printing power of the 3D printer is 50-240W, the scanning speed is 200-1000mm/S, and the thickness of the printing layer is 1.5-4 filaments/layer.
8. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1, characterized by: in the step S4, the heat treatment temperature is 500-1000 ℃, and the heat preservation time is 2-8h.
9. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1, characterized by: in the step S5, a 3D printed material is cut off against the surface of the substrate by using a cutting method of a slow wire.
10. A printing method for improving the corrosion resistance and strength of a 3D printing collimator according to claim 1, characterized by: in the step S7, the frequency of ultrasonic waves is 25-53KHz, the cleaning time is 5-30min, and the water temperature is 25-80 ℃; the drying temperature is 50-120 ℃, and the drying time is 5-120min.
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CN115533091A (en) * 2022-10-11 2022-12-30 中南大学 3D printing preparation method of high-density tungsten alloy
CN116275103A (en) * 2023-02-25 2023-06-23 湖南顶立科技股份有限公司 Tungsten nickel iron component and preparation method thereof
CN116422906A (en) * 2023-03-03 2023-07-14 安庆瑞迈特科技有限公司 Method for improving performance of laser 3D printing tungsten and tungsten alloy grid
CN116512132A (en) * 2023-03-28 2023-08-01 安庆瑞迈特科技有限公司 Method for removing burrs of 3D printing collimator by using liquid sand blasting
CN116479300A (en) * 2023-04-28 2023-07-25 湖南顶立科技股份有限公司 3D printing method of high-strength high-toughness tungsten alloy member and tungsten alloy member
CN116604036A (en) * 2023-05-18 2023-08-18 安庆瑞迈特科技有限公司 3D printing method for tungsten and tungsten alloy grating
CN116855810A (en) * 2023-07-07 2023-10-10 湖南云箭集团有限公司 Additive manufacturing method of high specific gravity tungsten alloy complex structure
CN116921696A (en) * 2023-07-20 2023-10-24 中国科学院重庆绿色智能技术研究院 Forming method for forming tungsten-based composite material based on laser 3D printing
CN116949320A (en) * 2023-09-21 2023-10-27 苏州倍丰智能科技有限公司 Superalloy powder for 3D printing, preparation method and printing method

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