GH4169 nickel-based high-temperature alloy for additive manufacturing and heat treatment method thereof
阅读说明：本技术 一种增材制造用gh4169镍基高温合金及其热处理方法 (GH4169 nickel-based high-temperature alloy for additive manufacturing and heat treatment method thereof ) 是由 殷军伟 计霞 刘慧渊 肖静宇 汪承杰 陈志茹 高桦 沈于蓝 郭广浩 余佩鸿 于 2021-08-26 设计创作，主要内容包括：本发明提供了一种增材制造用GH4169镍基高温合金及其热处理方法,所述热处理方法包括以下步骤：将GH4169镍基高温合金依次进行一级热处理、一级冷却、热等静压处理、二级冷却、固溶处理、三级冷却、时效处理以及四级冷却；所述热处理方法优化了热处理工艺,与传统的铸锻件热处理工艺相比,极大地提升了热处理后的GH4169镍基高温合金的力学性能,使其满足研制要求,具有较好的工业化应用前景。(The invention provides a GH4169 nickel-based high-temperature alloy for additive manufacturing and a heat treatment method thereof, wherein the heat treatment method comprises the following steps: sequentially carrying out primary heat treatment, primary cooling, hot isostatic pressing treatment, secondary cooling, solid solution treatment, tertiary cooling, aging treatment and quaternary cooling on the GH4169 nickel-based high-temperature alloy; the heat treatment method optimizes the heat treatment process, greatly improves the mechanical property of the GH4169 nickel-based high-temperature alloy after heat treatment compared with the traditional heat treatment process of the cast and forged piece, enables the alloy to meet the development requirements, and has good industrial application prospect.)
1. A heat treatment method of GH4169 nickel-base superalloy for additive manufacturing is characterized by comprising the following steps:
the GH4169 nickel-based high-temperature alloy is sequentially subjected to primary heat treatment, primary cooling, hot isostatic pressing treatment, secondary cooling, solution treatment, tertiary cooling, aging treatment and quaternary cooling.
2. The heat treatment method according to claim 1, wherein the GH4169 nickel-base superalloy is subjected to pretreatment before being subjected to primary heat treatment;
preferably, the pretreatment comprises purging powder of the GH4169 nickel-base superalloy surface and an inner cavity;
preferably, the purging is performed with compressed gas;
preferably, the GH4169 nickel-based superalloy is fixed on a steel plate through bolts after the pretreatment.
3. The heat treatment method according to claim 1 or 2, wherein the primary heat treatment is performed under vacuum conditions;
preferably, before the primary heat treatment, the vacuum is pumped to 10 DEG-3Pa below;
preferably, the temperature rise rate of the primary heat treatment is 8-12 ℃/min;
preferably, the temperature of the primary heat treatment is increased to 1055-1075 ℃;
preferably, the heat preservation time of the primary heat treatment is 70-100 min;
preferably, the temperature reduction rate of the primary cooling is 2-6 ℃/min;
preferably, the primary cooling is carried out to reduce the temperature to below 100 ℃.
4. The thermal treatment process according to any one of claims 1 to 3, characterized in that the hot isostatic pressing treatment is carried out under a protective atmosphere;
preferably, the step of forming the protective atmosphere comprises: vacuumizing, and introducing protective gas;
preferably, the pressure after the vacuum pumping is 10-3Pa below;
preferably, the protective gas comprises argon or nitrogen;
preferably, the purity of the argon is not less than 99.999%.
5. The heat treatment method according to any one of claims 1 to 4, wherein the temperature rise rate of the hot isostatic pressing treatment is 16 to 19 ℃/min;
preferably, the temperature of the hot isostatic pressing treatment is increased to 1070-1090 ℃;
preferably, the pressure of the hot isostatic pressing is 150-170 MPa;
preferably, the heat preservation time of the hot isostatic pressing treatment is 110-130 min;
preferably, the temperature reduction rate of the secondary cooling is 2-6 ℃/min;
preferably, the secondary cooling is carried out to reduce the temperature to below 100 ℃.
6. The heat treatment process according to any one of claims 1 to 5, characterized in that the solution treatment is carried out under vacuum conditions;
preferably, before the solution treatment, the vacuum is pumped to 10 DEG-3Pa below;
preferably, the pressure is controlled at 4X 10 during the solution treatment-3Pa below;
preferably, the temperature rise rate of the solution treatment is 16-19 ℃/min;
preferably, the heat preservation time of the solution treatment is 50-70 min;
preferably, the temperature of the solution treatment is increased to 1070-1090 ℃;
preferably, the manner of the tertiary cooling is air cooling;
preferably, the air cooling is performed with a protective gas;
preferably, the protective gas comprises argon or nitrogen;
preferably, the purity of the argon is not lower than 99.999%;
preferably, the absolute pressure in the three-stage cooling process is increased to 45-50 kPa;
preferably, the temperature of the tertiary cooling is reduced to be below 80 ℃.
7. Heat treatment process according to any one of claims 1 to 6, characterized in that the ageing treatment is carried out under vacuum conditions;
preferably, before the aging treatment, the vacuum is pumped to 10 DEG-3Pa below;
preferably, the aging treatment comprises primary treatment and secondary treatment;
preferably, the temperature rise rate of the primary treatment is 16-19 ℃/min;
preferably, the temperature of the primary treatment is increased to 710-730 ℃;
preferably, the heat preservation time of the primary treatment is 6-9 h;
preferably, furnace cooling is performed after the primary treatment;
preferably, the temperature of the secondary treatment is reduced to 610-630 ℃;
preferably, the holding time of the secondary treatment is 6-9 h.
8. The thermal treatment process according to any one of claims 1 to 7, characterized in that the quaternary cooling is air cooling;
preferably, the temperature of the four-stage cooling is reduced to be below 80 ℃.
9. Heat treatment process according to any one of claims 1 to 8, characterized in that it comprises the following steps:
(1) blowing GH4169 nickel-based high-temperature alloy surface and inner cavity with compressed gas to remove powder, fixing on a steel plate with bolts, placing in a vacuum heat treatment furnace, and vacuumizing to 10 deg.C-3Pa below, then heating to 1055-1075 ℃ at the speed of 8-12 ℃/min, preserving the heat for 70-100min, and then heating at the speed of 2-6 ℃/minCooling the furnace to below 100 ℃ in a speed furnace and discharging;
(2) placing the GH4169 nickel-based high-temperature alloy cooled in the step (1) into a hot isostatic pressing furnace, and vacuumizing until the pressure is 10-3Introducing protective gas below Pa, heating to 1070-1090 ℃ at the speed of 16-19 ℃/min, adjusting the pressure to 150-170 MPa, and preserving the temperature for 110-130 min; then furnace cooling is carried out at the speed of 2-6 ℃/min to be below 100 ℃, and discharging is carried out;
(3) placing the GH4169 nickel-based high-temperature alloy cooled in the step (2) into a vacuum heat treatment furnace, and vacuumizing until the pressure is 10-3Pa below, then raising the temperature to 1070-1090 ℃ at the speed of 16-19 ℃/min, preserving the temperature for 50-70min, and controlling the pressure to be 4 multiplied by 10 in the whole process-3Pa below; then introducing protective gas for air cooling, raising the pressure to 45-50 kPa, finally cooling to below 80 ℃ and discharging;
(4) placing the GH4169 nickel-based high-temperature alloy cooled in the step (3) into a vacuum heat treatment furnace, and vacuumizing until the pressure is 10-3Heating to 710-730 ℃ at the speed of 16-19 ℃/min under Pa, and preserving heat for 6-9 h; then cooling to 610 and 630 ℃ along with the furnace, and preserving heat for 6-9 h; then air cooling is carried out, and finally the temperature is cooled to be below 80 ℃ and discharged.
10. An additive manufacturing GH4169 nickel-base superalloy, wherein the additive manufacturing GH4169 nickel-base superalloy is prepared by the heat treatment method of any one of claims 1-9.
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to a GH4169 nickel-based high-temperature alloy for additive manufacturing and a heat treatment method thereof.
Background
Additive manufacturing, often referred to as 3D printing, is widely used in the fields of aerospace, medical treatment, and the like. The forming process is formed by stacking powder or wire materials layer by layer, so that the forming die has the advantages of high material utilization rate and short product production and development period, has almost no limitation on the shape of a product, can directly form complex structures such as grids and cavities, and is often used for manufacturing parts with complex shapes and difficult processing. At present, the additive manufacturing technology using high-energy beam as a heat source is the main development direction of rapid forming of metal parts.
GH4169 is a precipitation hardening type nickel-based high-temperature alloy, the optimal use temperature range is-253-650 ℃, the alloy has a series of excellent performances such as good corrosion resistance, weldability, oxidation resistance, high tensile strength, yield strength, plasticity and the like in the temperature range, and still has high tensile strength, creep strength, fatigue strength and rupture strength at 700 ℃, and the alloy is widely applied to aerospace, nuclear energy, petroleum industry and extrusion dies. However, as the additive manufacturing mostly adopts laser forming, the solidification time after the metal melting is less than 10-4And therefore, the performance, especially the plasticity, of the part can hardly meet the requirements of the traditional process. Meanwhile, the heat treatment process of the traditional casting and forging piece is difficult to match with the additive manufacturing high-temperature alloy part. Special heat treatment regimes are therefore required to match the requirements of the additively manufactured part.
CN109763081A discloses a heat treatment process of a nickel-based precipitation hardening type superalloy, which comprises the following process steps: 1) heating the nickel-based precipitation hardening superalloy to 480-520 ℃ in an air furnace, and preserving heat for 30-40 min to obtain a preheated superalloy product; 2) transferring the high-temperature alloy product preheated in the step 1) into another heating furnace, heating the high-temperature alloy product to 1080-1100 ℃ in advance in the heating furnace, timing after the preheated high-temperature alloy product is put into the heating furnace, keeping the temperature for 10-15 min after the temperature in the heating furnace is restored to 1080-1100 ℃, and discharging the high-temperature alloy product out of the heating furnace for air cooling; 3) heating the high-temperature alloy product subjected to solid solution in the step 2) to 740-760 ℃, preserving heat for 3-5 hours, cooling by filling argon, and aging to obtain a high-temperature alloy finished product. The yield strength of the high-temperature alloy part treated by the heat treatment process is low, and is only 765MPa at most, and needs to be further improved.
CN110846600A discloses a multi-step reversion heat treatment method for additive manufacturing of single crystal nickel-based superalloy, comprising the following steps: cleaning a surface impurity crystal layer introduced in an additive manufacturing process of the single crystal nickel-based high-temperature alloy manufactured by the additive manufacturing process, determining the volume fraction of a gamma 'phase at room temperature of the single crystal nickel-based high-temperature alloy manufactured by the additive manufacturing process, taking a temperature value corresponding to the first percentage of the volume fraction of the gamma' phase at room temperature as a first step temperature, preserving heat at the first step temperature for a first time period, reducing the volume fraction of the gamma 'phase by a second percentage as a second step temperature, preserving heat at the second step temperature for a second time period, continuously circulating until the temperature is raised to a temperature interval corresponding to the third percentage of the volume fraction of the gamma' phase, preserving heat at the step temperature for an M time period, wherein M is a natural number, and performing standard heat treatment on the single crystal nickel-based high-temperature alloy manufactured by the additive manufacturing process after the step recovery heat treatment to obtain the single crystal nickel-based high-temperature alloy; the heat treatment method has complex steps and long time, and is not beneficial to industrial application.
In conclusion, how to improve the heat treatment method for the additive manufacturing of the nickel-based superalloy, further improve the performance of the nickel-based superalloy, and meet the use requirements becomes a problem to be solved at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide the GH4169 nickel-based high-temperature alloy for additive manufacturing and the heat treatment method thereof, and the heat treatment method greatly improves the performance of the GH4169 nickel-based high-temperature alloy after heat treatment by optimizing the heat treatment process, so that the GH4169 nickel-based high-temperature alloy meets the development requirements and has a good industrial application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a heat treatment method of a GH4169 nickel-base superalloy for additive manufacturing, which comprises the following steps:
the GH4169 nickel-based high-temperature alloy is sequentially subjected to primary heat treatment, primary cooling, hot isostatic pressing treatment, secondary cooling, solution treatment, tertiary cooling, aging treatment and quaternary cooling.
According to the heat treatment method, firstly, material stress is removed through primary heat treatment, possible metallurgical defects (air holes, cracks and the like) are eliminated through a hot isostatic pressing process, the grain level of a matrix is controlled, then delta phases precipitated in the primary heat treatment process in the previous stage, the hot isostatic pressing furnace cooling process and the solid solution heating process are dissolved to the maximum extent through solid solution treatment, and a fine crystal structure containing less delta phases is obtained; compared with the traditional heat treatment process for referencing the existing forged casting, the heat treatment method greatly improves the mechanical property of the alloy and is beneficial to industrial production.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the GH4169 nickel-based high-temperature alloy is pretreated before primary heat treatment.
Preferably, the pretreatment comprises purging powder of the GH4169 nickel-base superalloy surface and the inner cavity.
Preferably, the purging is performed with compressed gas.
According to the invention, the cleaning of the powder on the surface and the inner cavity of the GH4169 nickel-based high-temperature alloy is beneficial to protecting equipment, and meanwhile, the phenomenon that the powder in the inner cavity of the alloy is burnt and agglomerated to block the internal structure of a workpiece is avoided.
The standard for checking whether powder on the surface and in the inner cavity of the GH4169 nickel-based superalloy is cleaned or not is as follows: and arranging the dust-free cloth dipped with the alcohol at an air outlet for inspection, and cleaning the dust-free cloth if the dust-free cloth is not dipped with the powder.
Preferably, the GH4169 nickel-based superalloy is fixed on a steel plate through bolts after the pretreatment.
In the invention, the GH4169 nickel-based superalloy is printed on the substrate, so the GH4169 nickel-based superalloy and the substrate are treated as a whole in the whole heat treatment process.
In the present invention, the deformation of the GH4169 nickel-base superalloy and the substrate can be prevented by fixing them to the steel sheet.
In a preferred embodiment of the present invention, the primary heat treatment is performed under vacuum.
Preferably, before the primary heat treatment, the vacuum is pumped to 10 DEG-3Pa or less, e.g. 10-5Pa、5×10-5Pa、10- 4Pa、5×10-4Pa or 10-3Pa, etc., but are not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the temperature increase rate of the first-stage heat treatment is 8 to 12 ℃/min, such as 8 ℃/min, 9 ℃/min, 10 ℃/min, 11 ℃/min, or 12 ℃/min, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the primary heat treatment is carried out at a temperature of 1055 to 1075 ℃, for example 1055 ℃, 1060 ℃, 1065 ℃, 1070 ℃ or 1075 ℃, but the temperature is not limited to the recited values, and other values not recited in the above range are also applicable.
In the present invention, the temperature of the primary heat treatment is controlled. If the temperature is too high, the crystal grains can be coarsened, so that the material is softened; if the temperature is too low, the delta phase and the Laves phase are difficult to dissolve, resulting in less strengthening phase precipitation during subsequent aging.
Preferably, the first heat treatment is carried out for a period of 70-100min, such as 70min, 80min, 90min or 100min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature reduction rate of the primary cooling is 2-6 ℃/min, such as 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min or 6 ℃/min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the primary cooling is to a temperature below 100 ℃, such as 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
In a preferred embodiment of the present invention, the hot isostatic pressing is performed in a protective atmosphere.
Preferably, the step of forming the protective atmosphere comprises: vacuumizing and introducing protective gas.
Preferably, the pressure after the vacuum pumping is 10-3Pa or less, e.g. 10-5Pa、5×10-5Pa、10-4Pa、5×10-4Pa or 10-3Pa, etc., but are not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the protective gas comprises argon or nitrogen.
Preferably, the purity of the argon is not less than 99.999%.
In the invention, protective gas is introduced after vacuum pumping, so that the pressure in the furnace reaches 10-30 MPa, and protective atmosphere is formed. And then, carrying out the next heating operation, and adjusting the pressure to a set value after the temperature is stable.
In a preferred embodiment of the present invention, the heat-up rate of the hot isostatic pressing is 16 to 19 ℃/min, for example, 16 ℃/min, 17 ℃/min, 18 ℃/min, 19 ℃/min, etc., but the heat-up rate is not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable.
Preferably, the hot isostatic pressing treatment is carried out at a temperature of 1070 to 1090 ℃, for example 1070 ℃, 1075 ℃, 1080 ℃, 1085 ℃ or 1090 ℃, but the hot isostatic pressing treatment is not limited to the recited values, and other values not recited in the numerical range are also applicable.
In the present invention, the temperature of the hot isostatic pressing treatment needs to be controlled. If the temperature is too high, the crystal grains are coarsened, so that the material is softened; if the temperature is too low, the effect of improving the density cannot be achieved.
Preferably, the hot isostatic pressing pressure is 150 to 170MPa, such as 150MPa, 155MPa, 160MPa, 165MPa or 170MPa, but is not limited to the recited values, and other values not recited in this range are also applicable.
Preferably, the holding time for the hot isostatic pressing treatment is 110-.
Preferably, the cooling rate of the secondary cooling is 2-6 ℃/min, such as 2 ℃/min, 3 ℃/min, 4 ℃/min, 5 ℃/min or 6 ℃/min, but not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the secondary cooling is to a temperature below 100 ℃, such as 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃ or 100 ℃, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
In a preferred embodiment of the present invention, the solution treatment is performed under vacuum.
Preferably, before the solution treatment, the vacuum is pumped to 10 DEG-3Pa or less, e.g. 10-5Pa、5×10-5Pa、10-4Pa、5×10-4Pa or 10-3Pa, etc., but are not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the pressure is controlled at 4X 10 during the solution treatment-3Pa or less, e.g. 10-5Pa、5×10- 5Pa、10-4Pa、5×10-4Pa、10-3Pa or 4X 10-3Pa, etc., but are not limited to the recited values, and the range of valuesValues not listed by him are equally applicable.
Preferably, the rate of temperature increase in the solution treatment is 16 to 19 ℃/min, for example, 16 ℃/min, 17 ℃/min, 18 ℃/min, 19 ℃/min, and the like, but is not limited to the values listed, and other values not listed within the range of values are also applicable.
Preferably, the holding time for the solution treatment is 50 to 70min, such as 50min, 55min, 60min, 65min or 70min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the solution treatment is carried out at a temperature of 1070 to 1090 ℃, for example, 1070 ℃, 1075 ℃, 1080 ℃, 1085 ℃ or 1090 ℃, but the temperature is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are also applicable.
In the present invention, the temperature of the solution treatment has a certain influence on the properties of the final alloy. If the temperature is too high, the crystal grains can be coarsened, so that the material is softened; if the temperature is too low, the delta phase and the Laves phase are difficult to dissolve, resulting in less strengthening phase precipitation during subsequent aging.
Preferably, the manner of the tertiary cooling is air cooling.
In the invention, the air cooling is adopted to obtain a faster cooling speed, and the growth of crystal grains due to the slow cooling speed and the repeated precipitation of the Laves phase and the delta phase are avoided.
Preferably, the air cooling is performed with a protective gas.
Preferably, the protective gas comprises argon or nitrogen.
Preferably, the purity of the argon is not less than 99.999%.
Preferably, the absolute pressure during the three-stage cooling is increased to 45 to 50kPa, such as 45kPa, 46kPa, 47kPa, 48kPa, 49kPa, or 50kPa, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature of the tertiary cooling is reduced to 80 ℃ or less, such as 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
As a preferable embodiment of the present invention, the aging treatment is performed under a vacuum condition.
Preferably, before the aging treatment, the vacuum is pumped to 10 DEG-3Pa or less, e.g. 10-5Pa、5×10-5Pa、10-4Pa、5×10-4Pa or 10-3Pa, etc., but are not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the aging treatment comprises primary treatment and secondary treatment.
Preferably, the temperature increase rate of the first stage treatment is 16 to 19 ℃/min, such as 16 ℃/min, 17 ℃/min, 18 ℃/min, 19 ℃/min, and the like, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the first stage treatment is carried out at a temperature of 710 to 730 ℃, for example 710 ℃, 715 ℃, 720 ℃, 725 ℃ or 730 ℃, but the temperature is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the first treatment is carried out for a holding time of 6 to 9 hours, such as 6 hours, 6.5 hours, 7 hours, 7.5 hours, 8 hours, 8.5 hours, or 9 hours, but not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, the primary treatment is followed by furnace cooling.
In the present invention, the temperature reduction rate after the first-stage treatment is not more than 50 ℃/h, for example, 30 ℃/h, 35 ℃/h, 40 ℃/h, 45 ℃/h or 50 ℃/h, etc., but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
Preferably, the secondary treatment is cooled to 610-630 deg.C, such as 610 deg.C, 615 deg.C, 620 deg.C, 625 deg.C or 630 deg.C, but not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the holding time of the secondary treatment is 6-9h, such as 6h, 6.5h, 7h, 7.5h, 8h, 8.5h or 9h, etc., but not limited to the recited values, and other values not recited in the range of values are also applicable.
In a preferred embodiment of the present invention, the four-stage cooling mode is air cooling.
Preferably, the quaternary cooling is carried out to a temperature of 80 ℃ or less, for example, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred embodiment of the present invention, the heat treatment method includes the steps of:
(1) blowing GH4169 nickel-based high-temperature alloy surface and inner cavity with compressed gas to remove powder, fixing on a steel plate with bolts, placing in a vacuum heat treatment furnace, and vacuumizing to 10 deg.C-3Heating to 1055-1075 ℃ at the speed of 8-12 ℃/min under Pa, preserving heat for 70-100min, and then furnace-cooling to below 100 ℃ at the speed of 2-6 ℃/min to discharge;
(2) placing the GH4169 nickel-based high-temperature alloy cooled in the step (1) into a hot isostatic pressing furnace, and vacuumizing until the pressure is 10-3Introducing protective gas below Pa, heating to 1070-1090 ℃ at the speed of 16-19 ℃/min, adjusting the pressure to 150-170 MPa, and preserving the temperature for 110-130 min; then furnace cooling is carried out at the speed of 2-6 ℃/min to be below 100 ℃, and discharging is carried out;
(3) placing the GH4169 nickel-based high-temperature alloy cooled in the step (2) into a vacuum heat treatment furnace, and vacuumizing until the pressure is 10-3Pa below, then raising the temperature to 1070-1090 ℃ at the speed of 16-19 ℃/min, preserving the temperature for 50-70min, and controlling the pressure to be 4 multiplied by 10 in the whole process-3Pa below; then introducing protective gas for air cooling, raising the pressure to 45-50 kPa, finally cooling to below 80 ℃ and discharging;
(4) placing the GH4169 nickel-based high-temperature alloy cooled in the step (3) into a vacuum heat treatment furnace, and vacuumizing until the pressure is 10-3Heating to 710-730 ℃ at the speed of 16-19 ℃/min under Pa, and preserving heat for 6-9 h; then cooled to 630 ℃ along with the furnaceWarming for 6-9 h; then air cooling is carried out, and finally the temperature is cooled to be below 80 ℃ and discharged.
In another aspect, the invention provides a GH4169 nickel-base superalloy prepared by the heat treatment method.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the heat treatment method, the material stress is removed through primary heat treatment, the hot isostatic pressing, the solution treatment, the aging treatment and other processes are combined, and the conditions in the treatment process are controlled, so that the mechanical property of the GH4169 nickel-based high-temperature alloy is effectively improved, and the R of the GH4169 nickel-based high-temperature alloy is enabled to be 650 DEG CmReach more than 1112MPa, Rp0.2More than 990MPa, more than 21.5 percent of elongation after fracture and more than 43 percent of reduction of area; under the conditions of 650 ℃ and 620MPa loading force, the lasting life reaches 136h, and the elongation reaches more than 13.5 percent;
(2) the heat treatment process is simple in flow and has a good industrial application prospect.
Drawings
FIG. 1 is a gold phase diagram of a GH4169 nickel-base superalloy provided by example 1 of the present invention after heat treatment.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a heat treatment method of GH4169 nickel-base superalloy for additive manufacturing, which comprises the following steps:
(1) blowing GH4169 nickel-based superalloy surface and inner cavity with compressed nitrogen to remove powder, fixing on a steel plate with bolts, placing in a vacuum heat treatment furnace, and vacuumizing to 10 deg.C-3Pa, then increased at a rate of 10 ℃/minHeating to 1065 ℃, preserving the heat for 90min, and then furnace-cooling to 100 ℃ at the speed of 5 ℃/min to discharge;
(2) placing the GH4169 nickel-based high-temperature alloy cooled in the step (1) into a hot isostatic pressing furnace, and vacuumizing until the pressure is 10-3Pa, introducing argon, heating to 1080 ℃ at the speed of 17 ℃/min, adjusting the pressure to 160MPa, and keeping the temperature for 120 min; then furnace cooling is carried out at the speed of 4 ℃/min to 90 ℃ and discharging is carried out;
(3) placing the GH4169 nickel-based high-temperature alloy cooled in the step (2) into a vacuum heat treatment furnace, and vacuumizing until the pressure is 10-3Pa, heating to 1080 deg.C at 17 deg.C/min, maintaining for 60min, and controlling pressure at 4 × 10-3Pa below; then introducing argon gas for air cooling, raising the pressure to 45kPa, finally cooling to 80 ℃ and discharging;
(4) placing the GH4169 nickel-based high-temperature alloy cooled in the step (3) into a vacuum heat treatment furnace, and vacuumizing until the pressure is 10-3Pa, then raising the temperature to 720 ℃ at the speed of 18 ℃/min, and preserving the temperature for 8 h; then cooling to 620 ℃ with the furnace, and preserving heat for 8 hours; then air cooling is carried out, and finally the mixture is cooled to 80 ℃ and discharged.
The GH4169 nickel-based high-temperature alloy subjected to heat treatment in the embodiment is characterized by a metallographic microscope, and the metallographic structure diagram of the GH4169 nickel-based high-temperature alloy is shown in FIG. 1. As can be seen from fig. 1, the crystal grain size is small, and many recrystallized grains are present.
Example 2:
the present example provides a heat treatment method of an additive manufacturing GH4169 nickel-base superalloy, which is referenced to the heat treatment method of example 1, except that: the temperature of the solution treatment in the step (3) was 1100 ℃.
Example 3:
the present example provides a heat treatment method of an additive manufacturing GH4169 nickel-base superalloy, which is referenced to the heat treatment method of example 1, except that: the temperature of the solution treatment in the step (3) was 1130 ℃.
Example 4:
the present example provides a heat treatment method of an additive manufacturing GH4169 nickel-base superalloy, which is referenced to the heat treatment method of example 1, except that: the temperature of hot isostatic pressing in step (2) was 1175 ℃.
Example 5:
the present example provides a heat treatment method of an additive manufacturing GH4169 nickel-base superalloy, which is referenced to the heat treatment method of example 4, except that: the temperature of the solution treatment in the step (3) was 1100 ℃.
Example 6:
the present example provides a heat treatment method of an additive manufacturing GH4169 nickel-base superalloy, which is referenced to the heat treatment method of example 4, except that: the temperature of the solution treatment in the step (3) was 1130 ℃.
The tensile mechanical properties at 650 ℃ of the GH4169 nickel-base superalloy after heat treatment of examples 1-6 were measured, and the results are shown in Table 1; the results of the measurements of the durability of the GH4169 Ni-based superalloy subjected to the heat treatment in examples 1 to 3 under the loading force conditions of 650 ℃ and 620MPa are shown in Table 2.
TABLE 1
Rm(Mpa)
Rp0.2(Mpa)
A(％)
Z(％)
Example 1
1112
990
21.5
43
Example 2
1006
854
21
26
Example 3
1027
872
18.5
24
Example 4
966
808.5
34
34.5
Example 5
1018.5
864.5
14
20.5
Example 6
997.5
840
21.5
21.5
Technical index
≥960
≥860
≥3
≥10
Wherein R ismTensile strength; rp0.2Is the yield strength; a is elongation after fracture; z is the reduction of area.
TABLE 2
Loading force (Mpa)
Test time/h
Elongation (%)
Example 1
620
136
13.5
Example 2
620
137
8.5
Example 3
620
132
6
Technical index
620
≥23
≥3
Embodiment 1 adopts the heat treatment method of the invention, effectively improves the mechanical properties of GH4169 nickel-based superalloy; examples 2 and 3 increased the solution treatment temperature during treatment, resulting in a decrease in tensile strength, yield strength, elongation after fracture, and reduction of area; example 4 elevated hiping temperature during treatment, although increasing elongation after break, the tensile strength and yield strength decreased significantly; examples 5 and 6 increase the temperature of both hot isostatic pressing and solution treatment, resulting in a decrease in mechanical properties.
As for the durability, it can be seen from Table 2 that the increase in the solution treatment temperature, although not so much affecting the time, results in a serious decrease in the elongation.
It can be seen from the above embodiments that the heat treatment method of the invention firstly removes the material stress through the primary heat treatment, then combines the hot isostatic pressing, the solution treatment, the aging treatment and other processes, and effectively improves the mechanical properties of the GH4169 nickel-based high-temperature alloy by controlling the conditions in the treatment process, so that the R of the GH4169 nickel-based high-temperature alloy is reduced to 650 DEG CmReach more than 1112MPa, Rp0.2More than 990MPa, more than 21.5 percent of elongation after fracture and more than 43 percent of reduction of area; under the conditions of 650 ℃ and 620MPa loading force, the lasting life reaches 136h, and the elongation reaches more than 13.5 percent; the heat treatment process is simple in flow and has a good industrial application prospect.
The applicant states that the present invention is illustrated by the above examples to show the product and detailed method of the present invention, but the present invention is not limited to the above products and detailed method, i.e. it is not meant that the present invention must rely on the above products and detailed method to be carried out. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
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