CN109759598A - A kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder - Google Patents
A kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder Download PDFInfo
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- CN109759598A CN109759598A CN201910214819.0A CN201910214819A CN109759598A CN 109759598 A CN109759598 A CN 109759598A CN 201910214819 A CN201910214819 A CN 201910214819A CN 109759598 A CN109759598 A CN 109759598A
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Abstract
The invention belongs to 3D printing alloy powder preparation technical fields, more particularly to a kind of 3D printing preparation method of GH4169 Ni-base Superalloy Powder, this method uses vacuum induction melting furnace to prepare GH4169 master alloy coupon first, powder by atomization is carried out with close coupling argon gas atomization technique later,>55 μm of coarse powder is finally removed using ultrasonic vibration classification,<15 μm of fine powder is removed using air current classifying, it is uniform to finally obtain chemical component, narrow particle size distribution (15~55 μm), sphericity is high, oxygen content is low, the GH4169 Ni-base Superalloy Powder of good fluidity, selective laser sintering 3D printing technique is met to the performance requirement of powder, promote the development of selective laser sintering 3D printing technique.
Description
Technical field
The invention belongs to 3D printing alloy powder preparation technical fields, and in particular to a kind of 3D printing is Ni-based with GH4169
The preparation method of superalloy powder.
Background technique
Selective laser sintering technology SLS (Selective Laser Sintering) is selectively layered using laser
Sintering solid powder, and the cured layer of sinter molding is made to be superimposed the part for generating required shape.The technology is that metal parts is direct
A kind of molding method, is one of latest development of metal 3D printing technique.Metal currently used for selective laser sintering technology
Dusty material has titanium alloy, aluminium alloy, stainless steel, nickel base superalloy, cobalt base superalloy etc..
GH4169 alloy belongs to ni-base wrought superalloy, 650 DEG C or less have high tensile strength, yield strength and
Good plasticity has the comprehensive performances such as good anticorrosive, anti-radiation energy, fatigue, fracture toughness, is widely used in aviation boat
It, the industries such as defence and military, petroleum industry.The GH4169 nickel base superalloy part manufactured using traditional handicraft, is respectively present
Component segregation and the low disadvantage of stock utilization, and above-mentioned lack can effectively be overcome using selective laser sintering 3D printing technique
Point.
Powder needed for GH4169 alloy powder for selective laser sintering 3D printing technique is different from prior powder metallurgy
Last characteristic, it is desirable that powdered ingredients uniformly, narrow particle size distribution (15~55 μm), oxygen content is low, sphericity is high and good flowing
Property, the research that the country is carried out for 3D printing technique with Ni-base Superalloy Powder is less, while being limited by domestic powder-making technique,
The main problems such as that there are the preparations of fine grain powder is difficult, powder yield is low, oxygen and other impurity content height.
Summary of the invention
For above-mentioned problems of the prior art and deficiency, the present invention provides a kind of Ni-based height of 3D printing GH4169
The preparation method of temperature alloy powder.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder, this method carry out as steps described below:
Step 1: the GH4169 alloying component according to as defined in GB/T14992-2005 carries out ingredient, and it is molten that vaccum sensitive stove is added in raw material
Refining, casting obtains GH4169 nickel base superalloy bar under vacuum after melting, later the defective part by the excision of alloy bar end to end
Position, and surface is carried out to alloy bar and is stripped off the skin processing, the alloy bar of 90mm × 170mm is obtained after processing, then at bar center
Open the through-hole of 30mm;
Step 2: after the GH4169 bar with through-hole that step 1 is obtained carries out surface clean with dehydrated alcohol, it is molten to be put into atomization
It refines in the alumina crucible of room, the hollow ceramic bar of lower end closed is then passed through into GH4169 bar central through hole, is allowed to block
Thermocouple is put into ceramic bar center and is used to measure molten metal melt temperature by crucible bottom and upper end of leting slip a remark;
Step 3: working chamber is evacuated to 3 × 10-2Pa is hereinafter, applying argon gas makes working chamber be maintained at 0.008Mpa again;
Step 4: alloy being heated to its fusing point or more, and keeps 80~200 DEG C of the degree of superheat, while standing 10~15min;
Step 5: selection atomization argon gas heating temperature sets close-coupled nozzle atomizing pressure, after argon gas is heated to set temperature,
Working chamber's ceramic bar is promoted, atomization gas is opened, so that aluminium alloy is flowed through atomizer with the speed of 2-5kg/min, in spray tower
Form spherical shape GH4169 Ni-base Superalloy Powder;
Step 6: after tower cooler of dusting, collecting GH4169 Ni-base Superalloy Powder, carry out ultrasonic vibration under protection of argon gas
Then screening, the coarse powder of 55 μm of partial size > of removal carry out air current classifying to the fine powder of partial size≤55 μm, 15 μm of < of removal is below
Particle obtains finished product and carries out Vacuum Package.
Further, in step 1, the material composition ratio of the GH4169 nickel base superalloy are as follows: C :≤0.08%,
Cr:17.0~21.0%, Ni:50~55%, Co :≤1.0%, Mo:2.80~3.30%, Al:0.20~0.80%, Ti:0.65~
1.15%, Fe: surplus, Nb:4.75~5.50%, B :≤0.006%, Mg :≤0.01%, Mn :≤0.35%, Si :≤0.35%, P :≤
0.015%, S :≤0.015%, Cu :≤0.30%.
Further, in step 1, smelting temperature is controlled at 1300-1500 DEG C.
Further, in step 3, it is high-purity argon gas that argon gas, which protects gas,.
Further, in step 5, atomization argon gas is high-purity argon gas.
Further, in step 5, atomization argon gas is heated to be 50~500 DEG C.
Further, in step 5, the argon gas atomizing pressure of close-coupled nozzle is 1.5~4.0Mpa.
Compared with prior art, the beneficial effects of the present invention are:
The present invention is directed to selective laser sintering 3D printing technique feature, the 3D printing being prepared GH4169 nickel base superalloy
Powder chemistry ingredient is uniform, oxygen content is low, sphericity is high, hollow sphere rate is low, good fluidity, and particle diameter distribution meets selective laser 3D
15~55 μm of the requirement of printing technique, the recovery rate of fine powder is high, wherein the powder yield of partial size≤55 μm reach 80% with
On, 15~55 μm of partial size of fine powder recovery rate reaches 50% or more, reduces production cost.
Detailed description of the invention
Fig. 1 is GH4169 Ni-base Superalloy Powder particle size distribution curve prepared by embodiment 1;
Fig. 2 is GH4169 Ni-base Superalloy Powder pattern photo prepared by embodiment 1;
Fig. 3 is GH4169 Ni-base Superalloy Powder particle size distribution curve prepared by embodiment 2;
Fig. 4 is GH4169 Ni-base Superalloy Powder pattern photo prepared by embodiment 2;
Fig. 5 is GH4169 Ni-base Superalloy Powder particle size distribution curve prepared by embodiment 3;
Fig. 6 is GH4169 Ni-base Superalloy Powder pattern photo prepared by embodiment 3.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
Embodiment 1
The present invention be a kind of 3D printing GH4169 Ni-base Superalloy Powder preparation method, this method as steps described below into
Row:
Step 1: the GH4169 alloying component according to as defined in GB/T14992-2005 carries out ingredient, and it is molten that vaccum sensitive stove is added in raw material
Refining, smelting temperature are controlled at 1300 DEG C, and casting obtains GH4169 nickel base superalloy bar under vacuum after melting, and GH4169 is Ni-based
The component ratio of high temperature alloy bar are as follows: C :≤0.08%, Cr:17.0~21.0%, Ni:50~55%, Co :≤1.0%, Mo:
2.80~3.30%, Al:0.20~0.80%, Ti:0.65~1.15%, Fe: surplus, Nb:4.75~5.50%, B :≤0.006%,
Mg :≤0.01%, Mn :≤0.35%, Si :≤0.35%, P :≤0.015%, S :≤0.015%, Cu :≤0.30%, later by alloy
Bar excision rejected region end to end, and surface is carried out to alloy bar and is stripped off the skin processing, obtain 90mm × 170mm's after processing
Alloy bar opens the through-hole of 30mm then at bar center;
Step 2: after the GH4169 bar with through-hole that step 1 is obtained carries out surface clean with dehydrated alcohol, it is molten to be put into atomization
It refines in the alumina crucible of room, the hollow ceramic bar of lower end closed is then passed through into GH4169 bar central through hole, is allowed to block
Thermocouple is put into ceramic bar center and is used to measure molten metal melt temperature by crucible bottom and upper end of leting slip a remark;
Step 3: working chamber is evacuated to 3 × 10-2Pa makes working chamber be maintained at 0.008Mpa hereinafter, filling high-purity argon gas again;
Step 4: alloy being heated to its fusing point or more, and keeps 80 DEG C of the degree of superheat, while standing 10min;
Step 5: selecting high-purity argon gas to be atomized argon gas, and atomization argon gas is heated to 50 DEG C, setting close-coupled nozzle atomization pressure
Power be 1.5 Mpa, after argon gas to be atomized is heated to set temperature, promoted working chamber's ceramic bar, open atomization gas, make aluminium alloy with
The speed of 2kg/min flows through atomizer, and spherical shape GH4169 Ni-base Superalloy Powder is formed in spray tower;
Step 6: after tower cooler of dusting, collecting GH4169 Ni-base Superalloy Powder, carry out ultrasonic vibration under protection of argon gas
Then screening, the coarse powder of 55 μm of partial size > of removal carry out air current classifying to the fine powder of partial size≤55 μm, 15 μm of < of removal is below
Particle obtains finished product and carries out Vacuum Package.
Through analyzing, GH4169 Ni-base Superalloy Powder oxygen content prepared by embodiment 1 is 0.024%, passes through Fig. 1,2
As can be seen that the satellite ball that powder sphericity is preferable, only a small amount of, is calculated after screening, 55 μm of partial size or less powder are received
Yield reaches 81%.
Embodiment 2
The present invention be a kind of 3D printing GH4169 Ni-base Superalloy Powder preparation method, this method as steps described below into
Row:
Step 1: the GH4169 alloying component according to as defined in GB/T14992-2005 carries out ingredient, and it is molten that vaccum sensitive stove is added in raw material
Refining, smelting temperature are controlled at 1400 DEG C, and casting obtains GH4169 nickel base superalloy bar under vacuum after melting, and GH4169 is Ni-based
The component ratio of high temperature alloy bar are as follows: C :≤0.08%, Cr:17.0~21.0%, Ni:50~55%, Co :≤1.0%, Mo:
2.80~3.30%, Al:0.20~0.80%, Ti:0.65~1.15%, Fe: surplus, Nb:4.75~5.50%, B :≤0.006%,
Mg :≤0.01%, Mn :≤0.35%, Si :≤0.35%, P :≤0.015%, S :≤0.015%, Cu :≤0.30%, later by alloy
Bar excision rejected region end to end, and surface is carried out to alloy bar and is stripped off the skin processing, obtain 90mm × 170mm's after processing
Alloy bar opens the through-hole of 30mm then at bar center;
Step 2: after the GH4169 bar with through-hole that step 1 is obtained carries out surface clean with dehydrated alcohol, it is molten to be put into atomization
It refines in the alumina crucible of room, the hollow ceramic bar of lower end closed is then passed through into GH4169 bar central through hole, is allowed to block
Thermocouple is put into ceramic bar center and is used to measure molten metal melt temperature by crucible bottom and upper end of leting slip a remark;
Step 3: working chamber is evacuated to 3 × 10-2Pa makes working chamber be maintained at 0.008Mpa hereinafter, filling high-purity argon gas again;
Step 4: alloy being heated to its fusing point or more, and keeps 130 DEG C of the degree of superheat, while standing 12min;
Step 5: selecting high-purity argon gas to be atomized argon gas, and atomization argon gas is heated to 300 DEG C, setting close-coupled nozzle atomization pressure
Power be 3.0 Mpa, after argon gas to be atomized is heated to set temperature, promoted working chamber's ceramic bar, open atomization gas, make aluminium alloy with
The speed of 3kg/min flows through atomizer, and spherical shape GH4169 Ni-base Superalloy Powder is formed in spray tower;
Step 6: after tower cooler of dusting, collecting GH4169 Ni-base Superalloy Powder, carry out ultrasonic vibration under protection of argon gas
Then screening, the coarse powder of 55 μm of partial size > of removal carry out air current classifying to the fine powder of partial size≤55 μm, 15 μm of < of removal is below
Particle obtains finished product and carries out Vacuum Package.
Through analyzing, GH4169 Ni-base Superalloy Powder oxygen content prepared by embodiment 2 is 0.025%, passes through Fig. 3,4
As can be seen that powder sphericity is preferable, there are a small amount of satellite balls, are calculated after screening, and 55 μm of partial size or less powder are received
Yield reaches 83%.
Embodiment 3
The present invention be a kind of 3D printing GH4169 Ni-base Superalloy Powder preparation method, this method as steps described below into
Row:
Step 1: the GH4169 alloying component according to as defined in GB/T14992-2005 carries out ingredient, and it is molten that vaccum sensitive stove is added in raw material
Refining, smelting temperature are controlled at 1500 DEG C, and casting obtains GH4169 nickel base superalloy bar under vacuum after melting, and GH4169 is Ni-based
The component ratio of high temperature alloy bar are as follows: C :≤0.08%, Cr:17.0~21.0%, Ni:50~55%, Co :≤1.0%, Mo:
2.80~3.30%, Al:0.20~0.80%, Ti:0.65~1.15%, Fe: surplus, Nb:4.75~5.50%, B :≤0.006%,
Mg :≤0.01%, Mn :≤0.35%, Si :≤0.35%, P :≤0.015%, S :≤0.015%, Cu :≤0.30%, later by alloy
Bar excision rejected region end to end, and surface is carried out to alloy bar and is stripped off the skin processing, obtain 90mm × 170mm's after processing
Alloy bar opens the through-hole of 30mm then at bar center;
Step 2: after the GH4169 bar with through-hole that step 1 is obtained carries out surface clean with dehydrated alcohol, it is molten to be put into atomization
It refines in the alumina crucible of room, the hollow ceramic bar of lower end closed is then passed through into GH4169 bar central through hole, is allowed to block
Thermocouple is put into ceramic bar center and is used to measure molten metal melt temperature by crucible bottom and upper end of leting slip a remark;
Step 3: working chamber is evacuated to 3 × 10-2Pa makes working chamber be maintained at 0.008Mpa hereinafter, filling high-purity argon gas again;
Step 4: alloy being heated to its fusing point or more, and keeps 200 DEG C of the degree of superheat, while standing 15min;
Step 5: selecting high-purity argon gas to be atomized argon gas, and atomization argon gas is heated to 500 DEG C, setting close-coupled nozzle atomization pressure
Power be 4.0 Mpa, after argon gas to be atomized is heated to set temperature, promoted working chamber's ceramic bar, open atomization gas, make aluminium alloy with
The speed of 5kg/min flows through atomizer, and spherical shape GH4169 Ni-base Superalloy Powder is formed in spray tower;
Step 6: after tower cooler of dusting, collecting GH4169 Ni-base Superalloy Powder, carry out ultrasonic vibration under protection of argon gas
Then screening, the coarse powder of 55 μm of partial size > of removal carry out air current classifying to the fine powder of partial size≤55 μm, 15 μm of < of removal is below
Particle obtains finished product and carries out Vacuum Package.
Through analyzing, GH4169 Ni-base Superalloy Powder oxygen content prepared by embodiment 3 is 0.028%, passes through Fig. 5,6
As can be seen that powder sphericity is preferable, there are a small amount of satellite balls, are calculated after screening, and 55 μm of partial size or less powder are received
Yield reaches 84%.
Claims (7)
1. a kind of 3D printing preparation method of GH4169 Ni-base Superalloy Powder, which is characterized in that this method is according to following
Step carries out:
Step 1: the GH4169 alloying component according to as defined in GB/T14992-2005 carries out ingredient, and it is molten that vaccum sensitive stove is added in raw material
Refining, casting obtains GH4169 nickel base superalloy bar under vacuum after melting, later the defective part by the excision of alloy bar end to end
Position, and surface is carried out to alloy bar and is stripped off the skin processing, the alloy bar of 90mm × 170mm is obtained after processing, then at bar center
Open the through-hole of 30mm;
Step 2: after the GH4169 bar with through-hole that step 1 is obtained carries out surface clean with dehydrated alcohol, it is molten to be put into atomization
It refines in the alumina crucible of room, the hollow ceramic bar of lower end closed is then passed through into GH4169 bar central through hole, is allowed to block
Thermocouple is put into ceramic bar center and is used to measure molten metal melt temperature by crucible bottom and upper end of leting slip a remark;
Step 3: working chamber is evacuated to 3 × 10-2Pa is hereinafter, applying argon gas makes working chamber be maintained at 0.008Mpa again;
Step 4: alloy being heated to its fusing point or more, and keeps 80~200 DEG C of the degree of superheat, while standing 10~15min;
Step 5: selection atomization argon gas heating temperature sets close-coupled nozzle atomizing pressure, after argon gas is heated to set temperature,
Working chamber's ceramic bar is promoted, atomization gas is opened, so that aluminium alloy is flowed through atomizer with the speed of 2-5kg/min, in spray tower
Form spherical shape GH4169 Ni-base Superalloy Powder;
Step 6: after tower cooler of dusting, collecting GH4169 Ni-base Superalloy Powder, carry out ultrasonic vibration under protection of argon gas
Then screening, the coarse powder of 55 μm of partial size > of removal carry out air current classifying to the fine powder of partial size≤55 μm, 15 μm of < of removal is below
Particle obtains finished product and carries out Vacuum Package.
2. a kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder as described in claim 1, feature exist
In, in step 1, the material composition ratio of the GH4169 nickel base superalloy are as follows: C :≤0.08%, Cr:17.0~21.0%,
Ni:50~55%, Co :≤1.0%, Mo:2.80~3.30%, Al:0.20~0.80%, Ti:0.65~1.15%, Fe: surplus, Nb:
4.75~5.50%, B :≤0.006%, Mg :≤0.01%, Mn :≤0.35%, Si :≤0.35%, P :≤0.015%, S :≤
0.015%, Cu :≤0.30%.
3. a kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder as described in claim 1, feature exist
In in step 1, smelting temperature is controlled at 1300-1500 DEG C.
4. a kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder as described in claim 1, feature exist
In in step 3, it is high-purity argon gas that argon gas, which protects gas,.
5. a kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder as described in claim 1, feature exist
In in step 5, atomization argon gas is high-purity argon gas.
6. a kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder as described in claim 1, feature exist
In in step 5, atomization argon gas is heated to be 50~500 DEG C.
7. a kind of preparation method of 3D printing GH4169 Ni-base Superalloy Powder as described in claim 1, feature exist
In in step 5, the argon gas atomizing pressure of close-coupled nozzle is 1.5~4.0Mpa.
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CN111394608A (en) * | 2020-03-31 | 2020-07-10 | 金川集团股份有限公司 | Preparation method of copper alloy powder for selective laser melting additive manufacturing |
CN112024898A (en) * | 2020-07-23 | 2020-12-04 | 江苏威拉里新材料科技有限公司 | Preparation method of GH5188 powder for 3D printing |
CN112809010A (en) * | 2020-12-29 | 2021-05-18 | 辽宁冠达新材料科技有限公司 | Preparation method of GH5188 cobalt-based high-temperature alloy powder for 3D printing |
CN113042741A (en) * | 2021-03-15 | 2021-06-29 | 中天上材增材制造有限公司 | Preparation method of metal powder or alloy powder for 3D printing and energy-saving automatic system |
CN113084181A (en) * | 2021-04-12 | 2021-07-09 | 辽宁冠达新材料科技有限公司 | Preparation method of GH3230 nickel-based superalloy powder for 3D printing |
CN113369484A (en) * | 2021-06-08 | 2021-09-10 | 金川镍钴研究设计院有限责任公司 | Method for preparing low-oxygen-content vacuum gas atomization 3D printing high-temperature alloy powder |
CN114054775A (en) * | 2021-11-22 | 2022-02-18 | 北京钢研高纳科技股份有限公司 | Aging strengthening type nickel-based superalloy 3D printing process and manufactured 3D printing piece |
WO2022041255A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Method for preparing nano-phase reinforced nickel-based high-temperature alloy using micron ceramic particles |
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Cited By (9)
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CN111394608A (en) * | 2020-03-31 | 2020-07-10 | 金川集团股份有限公司 | Preparation method of copper alloy powder for selective laser melting additive manufacturing |
CN112024898A (en) * | 2020-07-23 | 2020-12-04 | 江苏威拉里新材料科技有限公司 | Preparation method of GH5188 powder for 3D printing |
WO2022041255A1 (en) * | 2020-08-30 | 2022-03-03 | 中南大学 | Method for preparing nano-phase reinforced nickel-based high-temperature alloy using micron ceramic particles |
CN112809010A (en) * | 2020-12-29 | 2021-05-18 | 辽宁冠达新材料科技有限公司 | Preparation method of GH5188 cobalt-based high-temperature alloy powder for 3D printing |
CN113042741A (en) * | 2021-03-15 | 2021-06-29 | 中天上材增材制造有限公司 | Preparation method of metal powder or alloy powder for 3D printing and energy-saving automatic system |
CN113084181A (en) * | 2021-04-12 | 2021-07-09 | 辽宁冠达新材料科技有限公司 | Preparation method of GH3230 nickel-based superalloy powder for 3D printing |
CN113369484A (en) * | 2021-06-08 | 2021-09-10 | 金川镍钴研究设计院有限责任公司 | Method for preparing low-oxygen-content vacuum gas atomization 3D printing high-temperature alloy powder |
CN114054775A (en) * | 2021-11-22 | 2022-02-18 | 北京钢研高纳科技股份有限公司 | Aging strengthening type nickel-based superalloy 3D printing process and manufactured 3D printing piece |
CN114054775B (en) * | 2021-11-22 | 2022-12-06 | 北京钢研高纳科技股份有限公司 | Aging strengthening type nickel-based high-temperature alloy 3D printing process and manufactured 3D printing piece |
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Application publication date: 20190517 |