CN113102753B - Indirect 3D printing tungsten-based alloy part degreasing sintering method - Google Patents
Indirect 3D printing tungsten-based alloy part degreasing sintering method Download PDFInfo
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- CN113102753B CN113102753B CN202010034919.8A CN202010034919A CN113102753B CN 113102753 B CN113102753 B CN 113102753B CN 202010034919 A CN202010034919 A CN 202010034919A CN 113102753 B CN113102753 B CN 113102753B
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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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a degreasing and sintering method for indirectly 3D printed tungsten-based alloy parts, which comprises the steps of placing a tungsten-based alloy blank prepared by metal powder extrusion molding in an atmosphere furnace, introducing protective or reducing atmosphere in the whole process, heating to a proper temperature range at a multi-step slow heating rate for heat preservation for degreasing, heating to a sintering temperature range at a slow heating rate for sintering, and cooling to room temperature at a slow cooling rate to obtain a high-performance tungsten-based alloy. The invention ensures that the obtained tungsten-based alloy sintered part has no defects of cracking, residual binder, deformation and the like. The method lays a good foundation for indirectly printing tungsten-based alloy parts with high density and good forming precision by 3D.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly provides a degreasing and sintering method for indirectly 3D-printed tungsten-based alloy parts.
Background
Metal additive manufacturing (3D printing) is a new near-net-shape forming technology for parts, which is the hottest nowadays, and has attracted extensive attention and been widely used due to its advantages of being suitable for manufacturing parts with complex geometric shapes, uniform tissue structures and high performance. Currently, metal additive manufacturing technology includes the following ways: the direct forming technology of the metal powder directly acted by laser comprises Selective Laser Melting (SLM), selective Electron Beam Melting (EBM) and Laser Melting Deposition (LMD); the second is indirect 3D printing technology based on mixing of metal powder with binder, including injection molding (PIM) and metal extrusion. However, the manufacturing techniques of selective laser melting, selective electron beam melting and direct laser melting deposition have high requirements on the original powder, and require that the metal powder has a certain sphericity, a certain particle size range, good fluidity and loose packing density. The metal injection molding process needs spherical powder with proper particle size, and the development and manufacturing of molds with different shapes are needed for different formed parts, so that the economic cost is high. Based on the defects of additive manufacturing, the metal extrusion forming technology has no strict requirements on the sphericity and the fluidity of the original powder, and a special die is not needed in the forming process. Therefore, the metal extrusion forming technology can become an indirect 3D printing technology with great potential.
The indirect 3D printing technology for metal extrusion forming mainly comprises four processes of mixing metal powder and a binder, printing forming, degreasing and sintering. For the shaped blank, the subsequent degreasing and sintering process parameter setting is a key process for ensuring the structure and the performance of the shaped piece. The atmosphere, gas flow, degreasing heating rate and degreasing temperature used in the thermal degreasing process have great influence on the decomposition rate of the binder. If too large air flow is used, the defects of bubbling, collapse, cracking and the like of the degreased blank can be caused by violent decomposition of the binder due to high temperature rise rate and high degreasing temperature. The sintering process of the degreased blank adopts a proper heating rate, a sintering temperature interval and a cooling rate so as to avoid the defects of deformation, collapse, cracking and the like of the hot degreased blank in the sintering process.
The tungsten-based alloy mainly takes tungsten as a hard phase (85-99 percent by mass) and takes nickel, copper or nickel, iron and other components as a binding phase. The tungsten-based alloy has the advantages of high density, high strength, high ductility, high ray absorption capacity, good toughness, low thermal expansion coefficient and the like, so the tungsten-based alloy is widely applied to aerospace, national defense and military industry, nuclear industry and civil industry, such as a gyroscope rotor in a satellite navigation system and a counterweight and damping material on an airplane; conventional military weapons such as kinetic energy armor piercing bombs, fragile bombs, armor-breaking bombs and shrapnel bombs, international thermonuclear fusion test materials and the like. Tungsten-based alloy parts are generally formed by adopting the traditional sintering and machining technology, and the technology is relatively difficult to form for the tungsten-based alloy which is brittle at room temperature, high in cost and high in equipment requirement. Recently, research on extrusion forming 3D printing technology of tungsten-based alloy parts is developed by many scientific research units, and results show that the extrusion forming indirect 3D printing technology has great advantages in tungsten-based alloy part forming. However, at present, the subsequent degreasing sintering forming process of indirectly 3D printing tungsten-based alloy blank is not mature, and various process flows and parameters need to be formulated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides the degreasing and sintering method for indirectly 3D printing the tungsten-based alloy parts, has very important engineering significance, and effectively fills the blank field. After the tungsten-based alloy blank is degreased by adopting a thermal degreasing process, the paraffin-based binder on the surface of the metal particles is completely pyrolyzed, and a good foundation is laid for subsequent sintering. After the hot degreasing blank adopts the parameters of the two-step sintering process, the tungsten-based alloy part with high density and good forming precision can be obtained. The method lays a good foundation for indirectly printing the high-performance tungsten-based alloy parts in 3D.
The technical purpose of the invention is realized by the following technical scheme.
A degreasing and sintering method for indirectly 3D printing tungsten-based alloy parts comprises the following steps:
in step 1, the indirect 3D printing method is paraffin-based binder metal extrusion molding.
In step 1, the tungsten-based alloy is 96W-2.7Ni-1.3Fe (W-96 wt%, ni-2.7 wt%, fe-1.3 wt%).
In step 1, the temperature rise rate is 1-5 ℃/min.
In the step 1, the mode of multi-stage slow heating rate is that the temperature is kept for 1-5 min at 50-100 ℃ per liter.
In the step 1, the temperature is kept for 3 to 5 hours at 500 to 600 ℃.
In step 1, the inert shielding gas is argon, helium or nitrogen (purity 99.999 vol.%).
In step 1, the reducing atmosphere is hydrogen (purity 99.999 vol.%), argon-hydrogen gas mixture, and the volume ratio of argon to hydrogen is 1:9, purity 99.999vol.%.
2, continuously placing the tungsten-based alloy subjected to thermal degreasing in an atmosphere furnace, and continuously heating to 1400-1500 ℃ in inert protective gas or reducing atmosphere for heat preservation for 0.5-3 h;
in step 2, the temperature rise rate is 1 to 10 ℃/min, preferably 1 to 5 ℃/min.
In step 2, the inert shielding gas is argon, helium or nitrogen (purity 99.999 vol.%); the reducing atmosphere is hydrogen (purity is 99.999 vol.%), argon-hydrogen gas mixture, and the volume ratio of argon to hydrogen is 1:9, purity 99.999vol.%.
In step 2, the temperature is kept at 1400-1500 ℃ for 1-3 h.
And 3, after the heat preservation in the step 2 is finished, cooling the tungsten-based alloy to room temperature in an atmosphere furnace, inert protective gas or reducing atmosphere.
In step 3, the inert shielding gas is argon, helium or nitrogen (purity 99.999 vol.%); the reducing atmosphere is hydrogen (purity is 99.999 vol.%), argon-hydrogen gas mixture, and the volume ratio of argon to hydrogen is 1:9, purity 99.999vol.%.
In step 3, the cooling rate is 1-5 ℃/min
In the technical scheme of the invention, the gas flow with the gas flow rate of 50-100 ml/min is introduced into the atmosphere furnace so as to ensure that the atmosphere furnace is in inert protective gas or reducing atmosphere.
Compared with the prior art, the degreasing sintering method for the tungsten-based alloy part has the following advantages: (1) Compared with the complex processes such as the chemical degreasing-thermal degreasing-sintering three-step process and the like, the degreasing-sintering parameters of the indirect 3D printing tungsten-based alloy part formulated by the invention have the advantages of simple operation process, good stability, strong operability and the like. (2) The degreasing-sintering parameters established by the invention ensure that the degreased sample does not have paraffin-based binder, the sintered sample does not have the defects of deformation, collapse, cracks, holes and the like, and the sintered sample has high sintering density and good sintering formability. (3) The invention provides a basis for preparing high-performance defect-free tungsten-based alloy parts by indirect 3D printing.
Drawings
FIG. 1 shows SEM photographs (a) of the tungsten-based alloy of 96W-2.7Ni-1.3Fe prepared in example 1 of the present invention by hot degreasing and SEM photographs (b) of a cross section after sintering.
FIG. 2 shows SEM photographs (a) of the tungsten-based alloy of 96W-2.7Ni-1.3Fe prepared in example 2 of the present invention by hot degreasing and SEM photographs (b) of the cross-section after sintering.
FIG. 3 shows SEM pictures (a) and (b) of a sintered cross section of a 96W-2.7Ni-1.3Fe tungsten-based alloy prepared in example 3 of the present invention.
FIG. 4 shows SEM pictures (a) of the tungsten-based alloy of 96W-2.7Ni-1.3Fe prepared in example 4 of the present invention after hot degreasing, SEM pictures (b) of the cross section after sintering, and a drawn blank and a sintered part (c).
Detailed Description
The features of the present invention are further described below by way of examples, but the present invention is not limited to the following examples.
Example 1
Will be printed by indirect 3D to a size of 5 x 5mm 3 The 96W-2.7Ni-1.3Fe (W-96 wt%, ni-2.7 wt%, fe-1.3 wt%) tungsten-based alloy blank is placed in an atmosphere furnace, argon gas (with the purity of 99.999 vol%) with the flow rate of 50ml/min is introduced, the temperature rise rate is 1 ℃/min, the temperature is kept for 1min when the temperature per liter is higher than 100 ℃, the temperature is kept for 3h when the temperature is raised to 400 ℃, so as to remove paraffin-based binder, the temperature is raised to 1450 ℃ at the temperature rise rate of 1 ℃/min, and the temperature is kept for 2h. And finally, cooling to room temperature at a cooling rate of 1 ℃/min in an argon (with purity of 99.999 vol.%) atmosphere with a flow rate of 50ml/min to obtain the tungsten-based alloy sintered piece. As shown in FIG. 1, the tungsten-based alloy parts have no residual paraffin-based binder on the surface after thermal degreasing, and the cross-sectional SEM image after sintering shows that the sample has no voids and bubbles.
Example 2
Will be printed by indirect 3D to a size of 5 x 7mm 3 Putting the 96W-2.7Ni-1.3Fe tungsten-based alloy blank in an atmosphere furnace, introducing hydrogen (with the purity of 99.999 vol.%) with the flow rate of 60ml/min, heating up to 3 ℃/min, keeping the temperature for 3min at 50 ℃ per rise, heating up to 500 ℃, keeping the temperature for 2h to remove paraffin-based binder, and heating up to 2 ℃/minAnd keeping the temperature at 1450 ℃ for 3h. And after the heat preservation is finished, cooling to room temperature at a cooling rate of 3 ℃/min in a hydrogen (with the purity of 99.999 vol.%) atmosphere with the flow rate of 60ml/min, and taking out to obtain the tungsten-based alloy sintered piece. It can be seen in fig. 2 that the sample has no paraffin-based binder on the particle surface after thermal degreasing, and the sample has no deformation and collapse because there are no gaps between tungsten particles and the binder phase (ternary phase of tungsten, nickel and iron) between the tungsten particles on the section of the sintered part.
Example 3
Will be 5 x 7 x 5mm in size by indirect 3D printing 3 The 96W-2.7Ni-1.3Fe tungsten-based alloy blank is placed in an atmosphere furnace, hydrogen (with the purity of 99.999 vol.%) is introduced at the flow rate of 70ml/min, the heating rate is 5 ℃/min, the temperature is kept for 3min at the temperature of 100 ℃ per liter, the temperature is increased to 600 ℃, the temperature is kept for 3h to remove paraffin-based binder, the temperature is increased to 1500 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1h, and then the temperature is reduced to room temperature at the cooling rate of 5 ℃/min in the atmosphere of hydrogen (with the purity of 99.999 vol.%) at the flow rate of 70ml/min and then the blank is taken out. As can be seen in FIG. 3, after the sample is subjected to thermal degreasing at 600 ℃ for 3h, no paraffin-based binder remains on the surfaces of the particles, and the particles are connected compactly without holes and without cracking after being sintered at 1500 ℃.
Example 4
Placing a 96W-2.7Ni-1.3Fe tungsten-based alloy drawing piece blank subjected to indirect 3D printing in an atmosphere furnace, introducing argon gas (the purity is 99.999 vol.%) at the flow rate of 100ml/min, keeping the temperature at the rate of 3 ℃/min for 5min at the temperature of 100 ℃ per liter, heating to 700 ℃, keeping the temperature for 2h, removing paraffin-based binder, then heating to 1480 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 2h, and then cooling to room temperature at the cooling rate of 1 ℃/min in the argon gas (the purity is 99.999 vol.%) at the flow rate of 100ml/min to obtain a tungsten-based alloy sintering piece. In fig. 4, it can be seen that after the tungsten-based alloy sintered part is subjected to heat preservation at 700 ℃ for 2 hours, the paraffin-based binder completely disappears, the section of the sintered part has no holes and cracks, the particle interface has no gaps, the sample of the tensile part has no deformation and collapse, and the formability is good.
The adjustment of the process parameters according to the content of the invention realizes the degreasing and sintering of indirect 3D printing tungsten-based alloy parts, and the performance of the invention is basically consistent with that of the invention. The invention being thus described by way of example, it should be understood that any simple alterations, modifications or other equivalent alterations as would be within the skill of the art without the exercise of inventive faculty, are within the scope of the invention.
Claims (5)
1. The method for degreasing and sintering the indirect 3D printing tungsten-based alloy part is characterized by comprising the following steps of:
step 1, placing a tungsten-based alloy blank subjected to indirect 3D printing in an atmosphere furnace, heating to 400-700 ℃ in inert protective gas or reducing atmosphere by adopting a multi-stage slow heating rate mode, and preserving heat for 2-5 hours to completely remove paraffin-based binder and complete thermal degreasing; the mode of multi-stage slow heating rate is that the temperature is kept for 1-5 min at 50-100 ℃ per liter, and the heating rate is 1-5 ℃/min; the indirect 3D printing mode is paraffin-based binder metal extrusion molding, and the tungsten-based alloy is 96W-2.7Ni-1.3Fe;
2, continuously placing the tungsten-based alloy subjected to thermal degreasing in an atmosphere furnace, and continuously heating to 1400-1500 ℃ in inert protective gas or reducing atmosphere for heat preservation for 0.5-3 h; the heating rate is 1-10 ℃/min;
step 3, after the heat preservation in the step 2 is finished, cooling the tungsten-based alloy to room temperature in an atmosphere furnace, inert protective gas or reducing atmosphere, wherein the cooling rate is 1-5 ℃/min;
and introducing gas flow with the gas flow rate of 50-100 ml/min into the atmosphere furnace so as to enable the atmosphere furnace to be in inert protective gas or reducing atmosphere.
2. The method for degreasing and sintering the indirect 3D printing tungsten-based alloy part as claimed in claim 1, wherein in the step 1, the temperature is kept at 500-600 ℃ for 3-5 h.
3. The method for degreasing and sintering the indirect 3D printing tungsten-based alloy part as claimed in claim 1, wherein in the step 2, the temperature rise rate is 1-5 ℃/min, and the temperature is maintained at 1400-1500 ℃ for 1-3 h.
4. The method for degreasing and sintering the tungsten-based alloy part for indirect 3D printing as claimed in claim 1, wherein the inert protective gas is argon, helium or nitrogen.
5. The indirect 3D printing tungsten-based alloy part degreasing sintering method as claimed in claim 1, wherein the reducing atmosphere is hydrogen gas or an argon-hydrogen gas mixture, and the volume ratio of argon gas to hydrogen gas is 1:9.
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