CN100372638C - Nickel based alloy powder for laser sintering formation, and its prepn. method - Google Patents
Nickel based alloy powder for laser sintering formation, and its prepn. method Download PDFInfo
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- CN100372638C CN100372638C CNB2005100118644A CN200510011864A CN100372638C CN 100372638 C CN100372638 C CN 100372638C CN B2005100118644 A CNB2005100118644 A CN B2005100118644A CN 200510011864 A CN200510011864 A CN 200510011864A CN 100372638 C CN100372638 C CN 100372638C
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Abstract
The present invention provides nickel base alloy powder for rapid laser sintering formation and a preparation method thereof, which belongs to the technical field of nickel base alloy. The powder contains the ingredients of the following weight percentage: 80 to 90% of nickel, 10 to 18% of copper and 1 to 2% of tin. The preparation method comprises the steps that 100 to 200 meshes of pure nickel powder, pure copper powder and pure tin powder are put into a medium frequency induction furnace according to the weight percentage of 80 to 90% of nickel, 10 to 18% of copper and 1 to 2% of tin. The medium frequency induction furnace is heated to 1450 DEG C to 1550 DEG C in an argon atmosphere so that the powder is completely melted and uniformly mixed. The melted metal liquid is poured into a leaking crucible of a water atomizing device, and a water atomizing nozzle is arranged under the leaking crucible. When flowing through the nozzle via a flow guide nozzle, the melted metal liquid is smashed into small droplets by high-speed water flow injected by the nozzle, and the alloy droplets successively fall down in water and are solidified into powder. The present invention has the advantages of small structure, little ingredient segregation, direct large-scale commercialization production for the preparation of the powder, little pollution and simple process.
Description
Technical field
The invention belongs to the nickel-base alloy technical field, particularly a kind of Co-based alloy powder that is used for laser sintering rapid forming and preparation method thereof, this Co-based alloy powder is applicable to laser sintered.
Background technology
At aerospace field, nickel and nickel-base alloy are just being brought into play more and more important effect.Nickel-base alloy generally all has high strength, high-ductility and higher corrosion resistance, is mainly used in processing high-temperature load, corrosion resistant part and equipment, has been subjected to increasing attention at present.Rapid laser-shaping technique is a new and high technology in the manufacturing industry, and it provides a shortcut for short period, many kinds and the low expense that realizes the part manufacturing.The thinking of this technology comes from the inverse process that 3D solid is cut into a series of small unit, by constantly material being added on the uncompleted product by the path of appointment, adopt means chemistry or physics such as polymerization, bonding, sintering, clinkering, solidified liquid or bonding solid material selectively, thus accurately and rapidly produce the prototype or the parts of the shape that requires.
The performance of powder has directly determined the success or failure of laser sintering and moulding.Employed metal dust has the feature that is different from powder metallurgy sintered employed metal dust in laser sintering rapid forming.It requires powder particle spherical in shape, and even particle size distribution is to guarantee good flowability.
But at present commercially available nickel powder or Ni alloy powder are in the laser fast shaping sintering, and spherodization and sintering shrinkage phenomenon are serious, and consequent thermal stress makes part that warpage take place, and has influenced the final performance of product.In addition, most of alloy powders add the mode that adopts the mechanical mixture powder man-hour, owing to be subjected to the influence of powder density, pattern and the difference of fusing point, alloy composition segregation, the even problem of tissue odds appear in laser sintered process easily, be difficult to sinter into fine and close metal parts.
Summary of the invention
The object of the present invention is to provide a kind of Co-based alloy powder that is used for laser sintering rapid forming and preparation method thereof, adopt high speed water atomizing technology of preparing simultaneously, particle diameter, distribution and the grain shape of control powder, to be used for laser sintering rapid forming, realize the shaped object that does not have micro-crack and when sintering, have excellent processability.
Ni alloy powder of the present invention comprises: nickel, copper and three kinds of compositions of tin.Nickel can make profiled member have good mechanical property and mechanical performance, is used in the anti-corrosion part and the equipment of work under the high temperature load.Copper can make the profiled member densification, reduces micro-crack.Tin can make the fusing point of alloy descend, and improves the processability of material.
The percentage by weight of various elements is in the alloy powder that can be used for rapid laser-shaping technique that the present invention developed: nickel is 80-90%, is preferably 82-86%.When nickel content was higher than 90 weight %, powder can produce violent contraction when sintering, be unfavorable for moulding; Nickel content is lower than 80 weight %, and then the mechanical performance of product can variation.The ratio of copper is 10-18 weight %, is preferably 13-16 weight %.When the content of copper was higher than 18 weight %, the mechanical property of final products can descend significantly; When copper content was lower than 10 weight %, the thermal stress of product can increase, and makes difficult forming.The percentage by weight of tin is 1-2%.When tin content was higher than 2 weight %, powder was easily oxidized in sintering, increased the defective of profiled member; When tin content is lower than 1 weight %, powder fusing point height, molding effect is undesirable.
The preparation of powder of the present invention is with 100-200 purpose pure nickel powder, pure copper powder and pure tin powder according to percentage by weight are: nickel is 80-90%, copper is 10-18 weight %, tin is that 1-2% puts into intermediate frequency furnace, under argon gas atmosphere, be heated to 1450～1550 ℃, powder is melted fully and mix, bottom pour ladle crucible with melt metal liquid streamer entry atomization plant, below the bottom pour ladle crucible, be equipped with water atomizing nozzle, when melt metal liquid stream is flowed through nozzle by the water conservancy diversion mouth, the high-velocity flow that is penetrated by nozzle smashes into droplet, and alloy liquid droplet drops on and is frozen into powder in the water subsequently.
From phasor shown in Figure 1 (arrow indication zone for powder constituent of the present invention district) as can be known, the fusing point of manganese ternary alloy powder is lower than 1453 degrees centigrade and 1084 degrees centigrade of fine copper of pure nickel between 1054-1068 degree centigrade.Be beneficial to laser sintering and moulding.
For the Co-based alloy powder of being invented, its average particulate diameter should especially preferably use spheric granules less than accumulation horizon thickness.The Ni alloy powder average particulate diameter is too small, causes the powder reunion easily, reduces the flowability of powder, makes it be difficult to form highdensity powder bed, and the effect generation owing to laser irradiation is splashed when sintering, is difficult to realize the high accuracy moulding of part.
Consider above-mentioned factor, the present invention adopts existing water atomization technology to prepare the Ni-Cu-Sn manganese ternary alloy powder, and adopt water atomization powder process to have remarkable advantages: (1) tissue is tiny, and component segregation is little; (2) can enlarge the kind and the composition range of alloy element; (3) have the large-scale commercial applications production advantage of direct preparation powder, pollute for a short time, technology is simple.After powder is made, through carrying out sintering after necessary screening and the deoxidation.
Description of drawings
Fig. 1 is an ambrose alloy tin ternary phase diagrams of the present invention.
Fig. 2 is a Ni-Cu-Sn powder EDAX results of the present invention, and transverse axis is an accelerating potential, and the longitudinal axis is a diffraction peak intensity; The content that shows Ni among the figure is the highest, is Cu and Sn secondly.
Fig. 3 is an alloy powder stereoscan photograph of the present invention.
Fig. 4 is a 75-100 micron Ni-Cu-Sn powder SEM photo of the present invention.
Fig. 5 is a 100-150 micron Ni-Cu-Sn powder SEM photo of the present invention.
Fig. 6 is Ni-Cu-Sn powder X-ray RD result, and transverse axis is the angle of diffraction, and the longitudinal axis is a diffraction peak intensity.
The specific embodiment
Embodiment 1:
Pure nickel powder, pure copper powder and the pure tin powder of commercially available 75-150 micron are put into intermediate frequency furnace according to percentage by weight at 84: 14.4: 1.6, under argon gas atmosphere, be heated to 1500 degrees centigrade, powder is melted fully and mix.Bottom pour ladle crucible with melt metal liquid streamer entry atomization plant, below the bottom pour ladle crucible, be equipped with water atomizing nozzle, when melt metal liquid stream was flowed through nozzle by the water conservancy diversion mouth, the high-velocity flow that is penetrated by nozzle smashed into droplet, and alloy liquid droplet drops on and is frozen into powder in the water subsequently.Fig. 2 makes Ni-Cu-Sn powder EDAX results, and as we know from the figure, the content of Ni is the highest, is 85.17 weight %, is Cu secondly, is 13.58 weight %, and Sn is 1.25 weight %.Close with theoretical value.Fig. 3 is obtained powder stereoscan photograph of the present invention.As can be seen from Figure 3, therefore starting powder particle diameter skewness uses standard screen that alloy powder of the present invention is sieved.The screening back selects 75-100 micron powder to use as the laser Fast Sintering, and as shown in Figure 4, it is spherical that powder particle is, and particle diameter is evenly distributed, and has good mobility, is convenient to by the powder feeder powder feeding, thereby carries out laser sintered.
Fig. 6 is the XRD analysis result of powder, and as can be seen from Figure 6, mainly by Ni, the solid solution of Cu is formed, but also contains a certain amount of oxygen, has formed Ni in the alloy powder
2CuO
3Therefore, after screening, powder is carried out deoxidation treatment.
Powder is placed hydrogenation furnace, rise to 550 degrees centigrade, be incubated after 2 hours and take out with the programming rate of 5 centigrade per minutes.After tested, the 0.68 weight % of 75-100 micron powder oxygen content before by hydrogenation drops to 0.38 weight %.
Through above processing alloy powder, can directly be applied in the laser fast shaping sintering.The part densification of institute's moulding is shunk for a short time, and the tendency of cracking is little, can adapt to needs widely.
Embodiment 2:
Pure nickel powder, pure copper powder and the pure tin powder of commercially available 75-150 micron are put into intermediate frequency furnace according to percentage by weight at 90: 9: 1, under argon gas atmosphere, be heated to 1550 degrees centigrade, powder is melted fully and mix.With the bottom pour ladle crucible of melt metal liquid streamer entry atomization plant, the nozzle that makes water fogging places the crucible bottom, and the high-velocity flow that nozzle penetrates is crashed to pieces into droplet to melt metal liquid stream, alloy liquid droplet is dropped on be frozen into powder in the water.Through above processing alloy powder, the nodularization degree is good, and powder diameter is thinner.Through screening, select the powder of 100-150 micron to carry out sintering, as shown in Figure 5.This spheroidizing of powder degree is good, even particle size distribution.Insulation is 2 hours in 550 degrees centigrade hydrogenation furnace, carries out deoxidation.After tested, the 0.77 weight % of the 100-150 micron powder oxygen content after the hydrogenation before by hydrogenation drops to 0.42 weight %, and the powder after the processing can directly be applied in the laser fast shaping sintering.The part shape of institute's moulding is regular, even tissue, good mechanical property.
Embodiment 3:
Pure nickel powder, pure copper powder and the pure tin powder of commercially available 75-150 micron are put into intermediate frequency furnace according to percentage by weight at 80: 18: 2, under argon gas atmosphere, be heated to 1450 degrees centigrade, powder is melted fully and mix.Melt metal liquid stream injects the bottom pour ladle crucible, and the high-velocity flow that nozzle is penetrated is crashed to pieces into droplet to melt metal liquid stream, alloy liquid droplet is dropped on be frozen into powder in the water.Through screening, select the powder of 100-150 micron to carry out sintering, as shown in Figure 5.This powder particle is spherical in shape substantially, and even particle size distribution is fit to laser fast shaping.Insulation is 2 hours in 550 degrees centigrade hydrogenation furnace, carries out deoxidation.After tested, the 0.77 weight % of the 100-150 micron powder oxygen content after the hydrogenation before by hydrogenation drops to 0.42 weight %, and the powder after the processing can directly be applied in the laser fast shaping sintering, is used for moulding compact metal part.
Claims (2)
1. Co-based alloy powder that is used for laser sintering rapid forming, it is characterized in that: the percentage by weight of the various elements of composition of powder is: nickel is 82-86%, and copper is 13-16 weight %, and tin is 1-2%.
2. method for preparing the described Co-based alloy powder of claim 1, it is characterized in that: with 100-200 purpose pure nickel powder, pure copper powder and pure tin powder according to percentage by weight are: nickel is 82-86%, copper is 13-16 weight %, tin is that 1-2% puts into intermediate frequency furnace, under argon gas atmosphere, be heated to 1450～1550 ℃, powder is melted fully and mix, bottom pour ladle crucible with melt metal liquid streamer entry atomization plant, below the bottom pour ladle crucible, be equipped with water atomizing nozzle, when melt metal liquid stream is flowed through nozzle by the water conservancy diversion mouth, the high-velocity flow that is penetrated by nozzle smashes into droplet, and alloy liquid droplet drops on and is frozen into powder in the water subsequently.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100118644A CN100372638C (en) | 2005-06-03 | 2005-06-03 | Nickel based alloy powder for laser sintering formation, and its prepn. method |
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| CNB2005100118644A CN100372638C (en) | 2005-06-03 | 2005-06-03 | Nickel based alloy powder for laser sintering formation, and its prepn. method |
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| CN100372638C true CN100372638C (en) | 2008-03-05 |
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| CN102416480B (en) * | 2011-11-24 | 2013-05-15 | 浦江汇凯粉体科技有限公司 | Method for preparing copper-tin-nickel alloy powder by water atomization |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0499101A (en) * | 1990-08-07 | 1992-03-31 | Mitsubishi Materials Corp | Cu-ni series alloy powder and manufacture thereof |
| CN1078674A (en) * | 1992-05-08 | 1993-11-24 | 北京粉末冶金研究所 | Produce the method for alloy powder |
| US5303617A (en) * | 1990-02-27 | 1994-04-19 | Taiho Kogyo Co., Ltd. | Sliding material |
| EP0715916A2 (en) * | 1994-12-09 | 1996-06-12 | Ford Motor Company Limited | An iron or copper based powder composition |
| EP0930115A1 (en) * | 1996-07-20 | 1999-07-21 | Special Melted Products Limited | Production of iron or nickel-based products |
| CN2398039Y (en) * | 1999-11-23 | 2000-09-27 | 北京科因技术开发有限公司 | High-pressure water atomized powder making device |
| CN1594653A (en) * | 2004-06-24 | 2005-03-16 | 上海工程技术大学 | Method for assembling nickel base nano WC/Co composite plating on stainless steel surface using laser |
-
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- 2005-06-03 CN CNB2005100118644A patent/CN100372638C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5303617A (en) * | 1990-02-27 | 1994-04-19 | Taiho Kogyo Co., Ltd. | Sliding material |
| JPH0499101A (en) * | 1990-08-07 | 1992-03-31 | Mitsubishi Materials Corp | Cu-ni series alloy powder and manufacture thereof |
| CN1078674A (en) * | 1992-05-08 | 1993-11-24 | 北京粉末冶金研究所 | Produce the method for alloy powder |
| EP0715916A2 (en) * | 1994-12-09 | 1996-06-12 | Ford Motor Company Limited | An iron or copper based powder composition |
| EP0930115A1 (en) * | 1996-07-20 | 1999-07-21 | Special Melted Products Limited | Production of iron or nickel-based products |
| CN2398039Y (en) * | 1999-11-23 | 2000-09-27 | 北京科因技术开发有限公司 | High-pressure water atomized powder making device |
| CN1594653A (en) * | 2004-06-24 | 2005-03-16 | 上海工程技术大学 | Method for assembling nickel base nano WC/Co composite plating on stainless steel surface using laser |
Non-Patent Citations (1)
| Title |
|---|
| Ni基金属粉末激光快速制造的研究. 张剑锋，沈以赴，赵剑锋，黄因慧，余承业.航空学报，第23卷第3期. 2002 * |
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