WO2016141872A1 - 消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 - Google Patents

消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 Download PDF

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WO2016141872A1
WO2016141872A1 PCT/CN2016/075845 CN2016075845W WO2016141872A1 WO 2016141872 A1 WO2016141872 A1 WO 2016141872A1 CN 2016075845 W CN2016075845 W CN 2016075845W WO 2016141872 A1 WO2016141872 A1 WO 2016141872A1
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powder
powder metallurgy
ball mill
metallurgy superalloy
eliminating
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PCT/CN2016/075845
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English (en)
French (fr)
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刘祖铭
苏鹏飞
黄伯云
段清龙
郭旸
麻梦梅
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中南大学
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Priority to US15/514,826 priority Critical patent/US20170216919A1/en
Publication of WO2016141872A1 publication Critical patent/WO2016141872A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys

Definitions

  • the invention relates to a method for eliminating raw particle boundaries and void defects of powder metallurgy superalloys, and belongs to the field of powder metallurgy materials.
  • the defects of the original particle boundary (PPB), internal pores or heat-induced pores of powder metallurgy superalloys are the main defects of powder superalloys. Once formed, it is difficult to eliminate and seriously reduce the mechanical properties of the alloy.
  • Chinese patent CN102409276A discloses a method for eliminating the boundary of the original particle of powder metallurgy superalloy.
  • the powder metallurgy superalloy after direct hot isostatic pressing is solution treated at high temperature and solid solution at high temperature.
  • the treatment temperature is 1180 ⁇ 1220°C, and the holding time is 1.5 ⁇ 4h, which can effectively eliminate or reduce the original particle boundary.
  • Chinese patent CN102676881A discloses a nickel-based powder metallurgy superalloy which eliminates the boundary of the original particles, and the alloy includes FGH4096 and FGH4097.
  • the hot isostatic pressing temperature of the first step should be higher than the initial melting temperature of the low melting point phase of the alloy powder and lower than 15 ° C above the solidus line of the completely homogenized alloy, the gas pressure should be greater than or equal to 90 MPa, and the time is greater than or Equal to 20 minutes and less than or equal to 1 hour.
  • the heating is stopped, and the powder wrap is cooled with the furnace below cooling to the initial melting temperature of the low melting point phase of the alloy powder, and the heat preservation process is the second step; the holding time of the second step is greater than or equal to 2 hours.
  • the pressure is greater than or equal to 90 MPa, and after the second step is completed, the heating is stopped and cooled to room temperature.
  • the invention can prevent precipitation phases such as carbides from being precipitated along the boundary of the powder original particles, thereby obtaining an alloy in which the microstructure is equiaxed.
  • Chinese patent CN103447341A discloses an equal channel extrusion die for powder high-temperature alloy blanks, which is used for improving the microstructure characteristics of powder high-temperature alloy blanks, and the cross-sections of the blanks after entering the mold are respectively The torsion to the circular section is from the circular section to the elliptical section.
  • This deformation is a combination of torsional shear deformation and extrusion deformation, and realizes a combination of various deformation modes in one extrusion process.
  • the billet undergoes the rotation and shear strain under the action of shear stress, and the shearing and fracture of the crystal grains is realized to achieve the effect of refining the crystal grains.
  • the billet is restricted by the cavity, the intergranular deformation of the billet under compressive stress is difficult, and the development of various microscopic defects existing in the deformable body can be suppressed.
  • the grain refining effect of the invention is obvious, the original particle boundary is completely eliminated, and the comprehensive mechanical properties of the powder high-temperature alloy billet are significantly improved.
  • the above invention is eliminated by treating the green body after the powder is formed.
  • the original boundary of the powder particles is a remedial action taken after the original boundary of the powder particles is formed. Due to process factors, the elimination of the original boundary of the powder particles is limited, or industrial applications cannot be achieved.
  • the above invention patent is not involved in how to eliminate the hole defects of the powder metallurgy superalloy.
  • Hole defects in powder superalloys include internal holes and thermally induced holes.
  • the internal holes are mainly made of powder hollow Residual pores caused by defects, which are pore defects caused by expansion of residual gas during heat treatment. Therefore, powder hollow defects are the main source of void defects in powder superalloys.
  • Powder hollow is a common defect in atomized powder, which is determined by the characteristics of the atomization process and cannot be avoided.
  • the hollow formed inside the atomized powder is completely closed, which is difficult to eliminate in the subsequent powder forming process, and remains in the material to form residual pores.
  • the residual gas enclosed in the atomized hollow defects expands during the subsequent heat treatment to form heat-induced pores or induce cracks. These holes severely degrade the mechanical properties of the powder superalloy, especially the longevity and fatigue properties.
  • the hollow particle ratio of the large particle size powder is relatively high.
  • powder sieving has been used in the art to remove hollow powder.
  • the sieving method removes the large-sized hollow powder, but does not completely remove the hollow powder because the sieved small-sized powder also exhibits hollow defects.
  • the hollow defects that appear in the atomized powder it is usually controlled by a controlled atomization process.
  • the characteristics of the atomization process determine that the hollowness of the powder can only be reduced by controlling the atomization process, and the powder hollow defects cannot be completely eliminated.
  • the invention discloses a method for eliminating the original particle boundary and the hole defect of the powder metallurgy superalloy, firstly
  • the high-temperature alloy powder prepared by the atomization method is mechanically ball-milled to prepare a surface-activated solid powder, and then subjected to powder thermal consolidation forming to prepare a powder metallurgy superalloy.
  • the invention discloses a method for eliminating raw grain boundary and hole defects of a powder metallurgy superalloy, wherein the atomized alloy powder has a particle size of less than or equal to 150 ⁇ m (-100 mesh), preferably 106 ⁇ m (-150 mesh) or less, further preferably 75 ⁇ m (-200 mesh) or less.
  • the invention discloses a method for eliminating the boundary of the original particles of the powder metallurgy superalloy and the defect of the hole.
  • the ball mill used is One of a planetary ball mill, a stirring ball mill, and a drum ball mill is preferably a planetary ball mill.
  • the invention provides a method for eliminating the boundary of raw particles and pore defects of a powder metallurgy superalloy, and the ball milling is carried out under the protection of an inert gas.
  • the invention discloses a method for eliminating the original particle boundary and hole defect of the powder metallurgy superalloy, and the atomized powder is put into the ball mill tank, and the ball ratio is: (8 ⁇ 12) : 1 .
  • the invention discloses a method for eliminating the original particle boundary and the hole defect of the powder metallurgy superalloy, and the atomized powder is put into the ball mill tank, and the ratio of the ball to the material is (8 ⁇ 15) : 1 .
  • the invention discloses a method for eliminating raw grain boundary and hole defects of a powder metallurgy superalloy,
  • the heat consolidation forming is a molding method in hot isostatic pressing, hot extrusion forming, and plasma sintering forming.
  • the invention provides a method for eliminating the original particle boundary and the hole defect of the powder metallurgy superalloy, wherein the hot isostatic pressing is: 1000 ⁇ 1250 °C / 100 ⁇ 150MPa / 4h hot isostatic pressing.
  • the invention discloses a method for eliminating the original particle boundary and the hole defect of the powder metallurgy superalloy.
  • the hot extrusion forming comprises: loading the mixed powder obtained in the first step into a steel sheath, and vacuuming the inside of the jacket to below 10 -1 Pa, Degassing for more than 60 min, sealing welding; then hot extrusion at 900 ⁇ 1200 ° C; the extrusion ratio of the hot extrusion is (6 ⁇ 15): 1 .
  • the invention provides a method for eliminating raw grain boundaries and void defects of a powder metallurgy superalloy, which is: 1000 ⁇ 1250 °C / 40 ⁇ 150MPa / 5 ⁇ 10min plasma sintering.
  • the invention discloses a method for eliminating the original particle boundary and the hole defect of the powder metallurgy superalloy, and solid solution and aging treatment of the high temperature alloy material after the heat consolidation forming;
  • the solid solution process parameter is: 1000 to 1250 ° C heat preservation After 1 ⁇ 2h, air cooling, aging treatment process parameters are: 700 ⁇ 900 °C insulation 4 ⁇ 10h, air cooling.
  • the patent proposes mechanical ball milling treatment on the atomized powder to improve the surface activity of the powder and eliminate the hollow inside the powder particles. Defects, thereby eliminating the original boundary of the powder particles, internal pores and heat-induced pores, improving the overall mechanical properties.
  • the atomized powder is ball milled to activate the surface of the powder , obtain high surface active powder, can effectively eliminate the original boundary of the powder and improve the interfacial bonding strength during hot consolidation forming; the powder is deformed by ball milling to eliminate the hollow inside the powder particles Defects and solidification shrinkage, a completely solid powder is obtained, and the gas enclosed in the powder hollow is released, thereby effectively eliminating internal pores and heat-induced pores during heat consolidation forming, and improving comprehensive mechanical properties; atomization powder is ball-milled Deformation is favorable for recrystallization to form equiaxed crystal structure and improve performance.
  • a method for eliminating the original particle boundary and void defects of a powder metallurgy superalloy ball milling the atomized prealloyed powder After treatment, a high surface active solid powder is obtained, and then thermal consolidation forming is performed to prepare a powder metallurgy superalloy.
  • the invention has simple process and high production efficiency, and is favorable for large-scale preparation and application.
  • Figure 1 is a metallographic microstructure of a Rene 104 nickel-based superalloy prepared by plasma sintering of an atomized nickel-base superalloy powder in the comparative example of the present invention.
  • SEM scanning electron microscope
  • FIG. 3 is a cross-sectional SEM image of a powder of a nickel-based superalloy atomized powder after mechanical ball milling according to Embodiment 1 of the present invention
  • FIG. 4 is a metallographic microstructure of a Rene104 nickel-based superalloy prepared by plasma sintering after atomization of an atomized nickel-base superalloy powder according to Embodiment 1 of the present invention.
  • Plasma sintering is carried out, the process parameters are 1150 ° C / 40 MPa / heat for 5 min, and then solution treatment: 1180 ° C solid solution / 1h / furnace cooling, and then 815 ° C / 8h aging treatment, to obtain a nickel-based superalloy.
  • Figure 1 is a view showing the microstructure of a Rene 104 nickel-base superalloy prepared in the present comparative example, and a significant original grain boundary can be observed, as shown by the points indicated by 1, 2 in Fig. 1.
  • the gas atomized Rene104 nickel-based prealloyed powder was placed in a ball mill tank, and the ball to material ratio was 10:1. Under the protection of argon, ball milling was carried out in a planetary ball mill with a ball milling speed of 250 r/min and a ball milling time of 1.5 h to obtain a ball-milled nickel-base superalloy powder.
  • the ball-milled nickel-base superalloy powder was plasma-sintered at 1150 ° C / 40 MPa, kept for 5 min, and then solution treated: 1180 ° C solid solution / 1 h / furnace cold, and then 815 ° C / 8 h aging treatment, to obtain a nickel-based superalloy.
  • FIG. 2 is a scanning electron microscopy (SEM) image of the atomized powder section of the present embodiment, in which some of the powders have obvious hollow defects, as indicated by 3, 4, 5, and 6 in FIG.
  • Fig. 3 is a SEM image of the powder cross section of the atomized powder after mechanical ball milling of the present embodiment, and no powder hollow phenomenon was observed.
  • Figure 4 is a metallographic microstructure of the nickel-based powder superalloy prepared in this example, and no significant original grain boundaries were observed.
  • Gas atomized Rene104 nickel-based prealloyed powder is loaded into a ball mill tank, and ball milling is performed in an agitated ball mill under argon protection.
  • the ball milling speed was 100 r/min, and the ball milling time was 3 h, and the ball-milled nickel-base superalloy powder was obtained.
  • the ball mill powder is placed in a steel jacket, vacuum degassed, welded and sealed; hot extrusion at 1100 °C, the extrusion ratio is 10:1 , obtain high density nickel-based alloy bar; finally solid solution at 1115 °C 1h+1170 °C solid solution 3h / air cooling, 845 °C aging 4h + 760 °C aging 8h / air cooling , a nickel-based superalloy is obtained.

Abstract

一种消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法，对雾化粉末进行机械球磨处理，然后进行粉末热固结成形，制备粉末冶金高温合金。

Description

消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法
技术领域
本发明涉及 一种消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法， 属于粉末冶金材料领域。
背景技术
粉末冶金高温合金的原始颗粒边界(PPB)、内部孔洞或热诱导孔洞等缺陷是粉末高温合金的主要缺陷，一旦形成，很难消除，严重降低合金的力学性能。
针对粉末冶金高温合金原始颗粒边界缺陷，中国专利CN102409276A，公开了一种消除粉末冶金高温合金原始颗粒边界的方法，对直接热等静压后的粉末冶金高温合金进行高温固溶处理，高温固溶处理温度为1180～1220℃，保温时间为1.5～4h，能够有效地消除或减弱原始颗粒边界。中国专利CN102676881A，公开了一种消除原始颗粒边界的镍基粉末冶金高温合金，该合金包括FGH4096和FGH4097，此两种合金在冶炼过程中另加入质量百分数为0.15-0.9%的Hf，加入元素Hf在粉末颗粒内部形成MC型碳化物，以减少在原始颗粒边界析出，从而使直接热等静压后的镍基粉末冶金高温合金进行标准热处理后，消除镍基粉末冶金高温合金中的原始颗粒边界，在力学性能上表现为改善了合金的缺口敏感性。中国专利CN103551573A，公开了一种可避免原始颗粒边界相析出的高温合金粉末热等静压工艺。其中，第一步的热等静压温度应高于合金粉末的低熔点相的初熔温度且低于完全均匀化合金的固相线以上15℃，气体压力应大于或等于90MPa，时间大于或等于20分钟且小于或等于1个小时。第一步完成后，停止加热，将粉末包套随炉冷却至合金粉末的低熔点相的初熔温度以下保温，保温过程即为第二步；第二步的保持时间大于或等于2小时，以保证第一步后冷却过程中形成的低熔点相能够在保温过程中完全溶解，压力大于或等于90MPa，第二步完成后停止加热随炉冷却至室温。该发明可以避免碳化物等析出相沿粉末原始颗粒边界析出，从而得到致密且显微组织为等轴晶的合金。中国专利CN103447341A，公开了一种粉末高温合金制坯的等通道挤压模具，用于改善粉末高温合金坯料组织特征，坯料进入模具后，其截面分别经 过圆截面到椭圆截面扭转到圆截面，这种变形为扭转剪切变形和挤压变形的结合，实现了一道次挤压过程中多种变形模式的组合。在变形扭转过渡段，由于椭圆扭转面的扭转变形，坯料在剪切应力的作用下，发生转动和剪切应变，实现晶粒的剪切破碎，达到细化晶粒的效果。同时，由于坯料受到型腔的限制，处于压应力状态下的坯料晶间变形困难，可抑制变形体原存在的各种微观缺陷的发展。该发明晶粒细化效果明显，原始颗粒边界消除彻底，粉末高温合金坯料的综合力学性能得到明显提高。
上述发明都是通过对粉末成形后的坯体进行处理来消除 粉末颗粒原始边界，是在粉末颗粒原始边界形成之后采取的补救措施。受工艺因素的制约，粉末颗粒原始边界的消除效果有限，或无法实现工业应用。
对于如何消除 粉末冶金高温合金的孔洞缺陷，上述发明专利则没有涉及。
粉末高温合金中的孔洞缺陷包括内部孔洞和热诱导孔洞。其中，内部孔洞主要是 由粉末 空心 缺陷导致的残留孔洞，热诱导孔洞是残留气体在热处理过程中产生膨胀导致的孔洞缺陷。 因此，粉末空心缺陷是导致粉末高温合金出现 孔洞缺陷的主要来源。
粉末空心是雾化粉末中普遍存在的缺陷，这是雾化工艺特点决定的，无法避免。雾化粉末内部形成的空心是完全封闭的，在后续粉末成形过程中难以消除，残留在材料内部形成残留孔洞。封闭在雾化空心缺陷中的残留气体，在随后的热处理过程中发生膨胀，形成热诱导孔洞，或诱发裂纹。这些孔洞严重降低粉末高温合金的力学性能，特别是持久寿命和疲劳性能。
目前雾化工艺制备的粉末中，大粒径粉末的空心率比较高。长期以来，本领域采取粉末筛分的方法去除空心粉。筛分方法可以去除大尺寸空心粉末，但不能完全去除空心粉末，因为过筛的小尺寸粉末也会出现空心缺陷。 针对雾化粉末出现的空心缺陷，通常采用控制雾化工艺来进行控制。但是，雾化工艺特点决定了通过控制雾化工艺只能降低粉末空心率，不能完全消除粉末空心缺陷。
针对粉末 空心缺陷导致的粉末高温合金材料内部孔洞和热诱导孔洞，国内外未见通过消除雾化合金粉末空心缺陷，进而消除内部孔洞和热诱导孔洞的公开报道。
至今为止，国内外未见通过球磨处理消除雾化合金粉末空心缺陷，获得表面活化的实心粉末，进而消除粉末颗粒原始边界、内部孔洞和热诱导孔洞的公开报道。
发明内容
本发明的目的在于提供一种消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞缺陷的方法， 首先 对雾化法制备的高温合金粉末进行机械球磨处理， 制备得到表面活化的实心粉末， 然后进行粉末 热 固结成形， 制备粉末冶金高温合金。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷 的方法，所述 雾化合金粉末 的粒度小于等于 150 μ m （-100目 ） ， 优选为小于等于106 μ m （ -150 目），进一步优选为小于等于75 μ m （ -200 目 ） 。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷 的方法，球磨时，所用球磨机为 行星式球磨机、搅拌式球磨机、滚筒式球磨机中的一种，优选为行星式球磨机。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷的方法， 球磨在惰性气体保护下进行。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷的方法， 将雾化粉末 入球磨罐，球料比 : (8~12) : 1 ，在行星式球磨机中球磨，球磨转速为 250~350r/min ， 时间为 1~4h 。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷的方法， 将雾化粉末 入球磨罐，球料比为 (8~15) : 1 ，在搅拌球磨机中球磨，球磨转速为 60~150r/min ， 时间为 2 ～ 6h ；
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷 的方法， 热固结成形采用热等静压成形、热挤压成形、等离子烧结成形中的一种成型方式。
本发明一种消除粉末冶金高温合金原始颗粒边界和孔洞 缺陷 的方法，所述热等静压成形是： 1000 ～ 1250 ℃ /100 ～ 150MPa/4h 热等静压成形 。
本发明一种消除粉末冶金高温合金原始颗粒边界和孔洞 缺陷 的方法，所述热挤压成形是：将步骤一所得混合粉末 装入钢包套，对包套内抽真空至10-1Pa以下，除气60 min以上，封焊；然后在900 ~1200℃进行热挤压成 形 ；所述热挤压成 形 的挤压比为（ 6~15 ） : 1 。
本发明一种消除粉末冶金高温合金 原始颗粒边界和孔洞 缺陷 的方法，所述等离子烧结成形是： 1000 ～ 1250 ℃ /40 ～ 150MPa/5 ～ 10min 等离子烧结成形 。
本发明一种消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法，将热固结成形后的高温合金材料进行固溶和时效处理； 固溶工艺参数为： 1000 ～ 1250 ℃保温 1~2h 后，空冷，时效处理工艺参数为： 700 ～ 900 ℃保温 4 ～ 10h ，空冷 。
本发明的优点和积极效果：
本专利提出对雾化粉末进行机械球磨 处理，提高粉末表面活性， 消除粉末颗粒内部 空心 缺陷，从而消除粉末颗粒原始边界、内部孔洞和热诱导孔洞，提高综合力学性能。
雾化粉末经过球磨处理， 使粉末表面活化 ，获得高表面活性粉末，在热固结成形时，可以有效消除粉末原始边界，提高界面结合强度 ； 粉末经球磨产生变形，消除粉末颗粒内部 空心 缺陷和凝固缩孔，获得完全实心粉末，封闭在粉末空心中的气体得到释放，从而 在热固结成形时有效 消除内部孔洞和热诱导孔洞，改善综合力学性能；雾化 粉末经过球磨处理 产生变形，有利于再结晶形成等轴晶组织，提高性能。
综上所述， 一种消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法，对 雾化预合金粉末进行球磨 处理，获得高表面活性实心粉末，再进行热固结成形，制备得到粉末冶金高温合金 。本发明工艺简单，生产效率高，有利于规模化制备和应用。
附图说明
附图1是本发明对比例采用雾化镍基高温合金粉末进行等离子烧结成形制备的Rene104镍基高温合金金相显微组织。
附图2是本发明实施例1镍基高温合金雾化粉末截面扫描电镜（SEM）图
附图3是本发明实施例1镍基高温合金雾化粉末经机械球磨后的粉末截面SEM图
附图4是本发明实施实例1雾化镍基高温合金粉末经机械球磨后，等离子烧结成形制备的Rene104镍基高温合金金相显微组织。
从附图1的金相观察结果可知， 雾化粉末直接成形制备的镍基高温合金显微组织出现了明显的原始颗粒边界（PPB），附图1中的1、2所指示均为原始颗粒边界。
从附图2的 SEM观察结果可知，实施实例1中部分雾化粉末出现了明显的空心缺陷，附图2中3、4、5、6均为空心缺陷。
从附图3的 SEM观察结果可知，实施实例1中雾化粉末经机械球磨后，粉末截面没有观察到空心现象。
从附图4的光学显微镜观察结果可知，实施例1制备的镍基高温合金显微组织，没有观察到明显的原始颗粒边界。
具体实施方式
下面结合具体实施方式对本发明作进一步说明。
对比例：雾化粉末直接等离子烧结制备Rene104镍基高温合金
将气体雾化Rene104镍基预合金粉末（成分为 Ni-13Co-16Cr-4Mo-4W-2.2Al-3.7Ti-0.77Nb （ wt% ） ）进行等离子烧结，工艺参数为1150℃/40MPa/保温5min，再进行固溶处理：1180℃固溶/1h/炉冷，然后进行815℃/8h时效处理,得到镍基高温合金。
附图1是本对比例制备的Rene104镍基高温合金的显微组织，可以观察到明显的原始颗粒边界，见附图1中的1、2所指示的部位。
实施例1：
将气体雾化Rene104镍基预合金粉末装入球磨罐， 球料比 : 10 : 1 ， 在氩气保护下，在行星球磨机中进行球磨，球磨转速为250r/min，球磨时间为1.5h， 得到球磨镍基高温合金粉末。
将球磨镍基高温合金粉末在1150℃/40MPa进行等离子烧结，保温5min，然后进行固溶处理：1180℃固溶/1h/炉冷，然后进行815℃/8h时效处理,得到镍基高温合金。
附图2是本实施例雾化粉末截面扫描电镜（SEM）图片，图中部分粉末出现了明显的空心缺陷，见附图2中3、4、5、6所指示。附图3为本实施例雾化粉末经机械球磨后，粉末截面SEM图，没有观察到粉末空心现象。附图4是本实施例制备的镍基粉末高温合金的金相显微组织，没有观察到明显的原始颗粒边界。
实施例2：
将气体雾化Rene104镍基预合金粉末装入球磨罐，在氩气保护中， 在搅拌式球磨机中球磨 ，球磨转速为100r/min，球磨时间为3h， 得到球磨镍基高温合金粉末。
将球磨粉末装入钢包套，抽真空除气、焊封；在 1100 ℃ 进行热挤压成型，挤压比为 10 : 1 ，获得高致密度的镍基合金棒材； 最后在 1115 ℃ 固溶 1h+1170℃固溶3h/ 空冷， 845 ℃ 时效 4h+760℃时效8h/ 空冷 ，得到镍基高温合金。

Claims (10)

1 、 消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法， 其特征在于：首先 对雾化法制备的高温 合金粉末进行机械 球磨处理， 制备得到表面活化的实心粉末， 然后进行粉末热固结成形， 制备粉末冶金高温合金 。
2 、根据权利要求 1 所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于： 所述 雾化合金粉末的粒度小于等于 150 μ m 。
3 、 根据权利要求 1 所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于： 球磨时，所用球磨机为行星式球磨机、搅拌式球磨机、滚筒式球磨机中的一种。
4 、 根据权利要求 3 所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于：球磨在惰性气体保护下进行。
5 、 根据权利要求 3 所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于：将雾化粉末入球磨罐，球料比 : (8~12) : 1 ，在行星式球磨机中球磨，球磨转速为 250~350r/min
， 时间为 1~4h 。
6 、 根据权利要求 3 所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于：将雾化粉末入球磨罐，球料比为 (8~15) : 1 ，在搅拌球磨机中球磨，球磨转速为 60~150r/min ， 时间为 2 ～ 6h 。
7 、根据权利要求 1-6 任意一项所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于： 热 固结 成形采用热等静压成形、热挤压成形、等离子烧结成形中的一种成型方式 。
8 、 根据权利要求 7 所述的 消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于：
热等静压成形工艺参数是： 1000 ～ 1250 ℃ /100 ～ 150MPa/4h ；
热挤压成形工艺参数是 ：在 900~1200℃进行热挤压成形；所述热挤压成形的挤压比为（6~15 ） : 1 ；
等离子烧结成形工艺参数是： 1000 ～ 1250 ℃ /40 ～ 150MPa/5 ～ 10min 。
9 、根据权利要求 8 所述的消除粉末冶金高温合金原始颗粒边界和孔洞缺陷的方法 ，其特征在于： 将热固结成形后的高温合金材料进行固溶和时效处理 。
10 、根据权利要求 9 所述的消除粉末冶金高温合金原始颗粒边界
和孔洞缺陷的方法，其特征在于： 固溶处理工艺参数为： 1000 ～ 1250 ℃ 保温 1~2h
，空冷；时效处理工艺参数为： 700 ～ 900 ℃ 保温 4 ～ 10h ，空冷 。
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Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105344436B (zh) * 2015-03-09 2017-11-21 中南大学 一种消除雾化合金粉末空心缺陷的方法
GB2565063B (en) 2017-07-28 2020-05-27 Oxmet Tech Limited A nickel-based alloy
CN108611507B (zh) * 2018-04-25 2020-06-05 北京航空航天大学 一种基于粉末再加工的热等静压近净成形方法
WO2020059059A1 (ja) * 2018-09-19 2020-03-26 技術研究組合次世代３Ｄ積層造形技術総合開発機構 金属積層造形用粉末およびその製造方法と、積層造形装置およびその制御プログラム
CN110116203A (zh) * 2019-06-06 2019-08-13 西北有色金属研究院 一种消除镍基粉末高温合金原始颗粒边界的方法
CN111238956B (zh) * 2020-01-08 2021-08-27 中南大学 一种粉末合金制备与热固结成形工艺开发高通量方法
CN111647764A (zh) * 2020-04-20 2020-09-11 中南大学 一种镍基粉末高温合金及其成型方法
CN112045188A (zh) * 2020-09-04 2020-12-08 中国航发北京航空材料研究院 一种粉末高温合金卧式挤压模芯及其制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040096350A1 (en) * 2002-11-18 2004-05-20 Advanced Materials Products, Inc. Method for manufacturing fully dense metal sheets and layered composites from reactive alloy powders
CN101418393A (zh) * 2008-12-01 2009-04-29 昆明贵金属研究所 AgCuV合金材料制备新方法
CN101649401A (zh) * 2009-07-20 2010-02-17 温州宏丰电工合金有限公司 Ag-Ni-氧化物电触头材料及其制备方法
CN102534297A (zh) * 2010-12-16 2012-07-04 北京有色金属研究总院 一种热膨胀系数呈梯度变化的合金材料及其制备方法
CN103551573A (zh) * 2013-10-22 2014-02-05 中国科学院金属研究所 可避免原始颗粒边界相析出的高温合金粉末热等静压工艺
WO2014175555A1 (ko) * 2013-04-25 2014-10-30 배은영 고성능 센더스트 압분자심 코아 및 그 제조방법

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4073648A (en) * 1974-06-10 1978-02-14 The International Nickel Company, Inc. Thermoplastic prealloyed powder
CN1239723C (zh) * 2000-12-20 2006-02-01 昆明贵金属研究所 铜基合金电真空触头材料及其制备方法
CN103240412B (zh) * 2013-05-22 2014-10-15 北京科技大学 一种近终形制备粉末超合金的方法
KR20150017089A (ko) * 2013-08-06 2015-02-16 창원대학교 산학협력단 우수한 초고온 기계적 특성을 갖는 내열합금의 열처리 방법 및 그에 의한 합금

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040096350A1 (en) * 2002-11-18 2004-05-20 Advanced Materials Products, Inc. Method for manufacturing fully dense metal sheets and layered composites from reactive alloy powders
CN101418393A (zh) * 2008-12-01 2009-04-29 昆明贵金属研究所 AgCuV合金材料制备新方法
CN101649401A (zh) * 2009-07-20 2010-02-17 温州宏丰电工合金有限公司 Ag-Ni-氧化物电触头材料及其制备方法
CN102534297A (zh) * 2010-12-16 2012-07-04 北京有色金属研究总院 一种热膨胀系数呈梯度变化的合金材料及其制备方法
WO2014175555A1 (ko) * 2013-04-25 2014-10-30 배은영 고성능 센더스트 압분자심 코아 및 그 제조방법
CN103551573A (zh) * 2013-10-22 2014-02-05 中国科学院金属研究所 可避免原始颗粒边界相析出的高温合金粉末热等静压工艺

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