CN115921861B - Cold isostatic pressing preparation method of metal bar - Google Patents
Cold isostatic pressing preparation method of metal bar Download PDFInfo
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- CN115921861B CN115921861B CN202211540485.4A CN202211540485A CN115921861B CN 115921861 B CN115921861 B CN 115921861B CN 202211540485 A CN202211540485 A CN 202211540485A CN 115921861 B CN115921861 B CN 115921861B
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- 238000009694 cold isostatic pressing Methods 0.000 title claims abstract description 68
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 64
- 239000002184 metal Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003292 glue Substances 0.000 claims abstract description 127
- 238000007789 sealing Methods 0.000 claims abstract description 99
- 238000000034 method Methods 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 28
- 238000011049 filling Methods 0.000 claims abstract description 20
- 238000005056 compaction Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 19
- 229920001971 elastomer Polymers 0.000 claims description 17
- 239000005060 rubber Substances 0.000 claims description 17
- 229910052715 tantalum Inorganic materials 0.000 claims description 12
- 229920002635 polyurethane Polymers 0.000 claims description 11
- 239000004814 polyurethane Substances 0.000 claims description 11
- 229910001362 Ta alloys Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004033 plastic Substances 0.000 claims description 8
- 229920003023 plastic Polymers 0.000 claims description 8
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 2
- 238000010079 rubber tapping Methods 0.000 claims description 2
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- 230000008023 solidification Effects 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012797 qualification Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000004816 latex Substances 0.000 description 3
- 229920000126 latex Polymers 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- FGBJXOREULPLGL-UHFFFAOYSA-N ethyl cyanoacrylate Chemical compound CCOC(=O)C(=C)C#N FGBJXOREULPLGL-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Powder Metallurgy (AREA)
Abstract
The invention provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps: filling metal powder into a sheath for compaction, and then plugging a sealing plug with the side surface coated with first glue into the sheath; after the first glue is solidified, coating second glue at the joint of the sealing plug and the sheath until the second glue is solidified to finish the sealing of the sheath; carrying out cold isostatic pressing treatment on the sealed sheath; then, a hole is formed at the joint of the sheath and the sealing plug, the sheath is inflated to carry out demoulding, the sealing part of the sheath is scratched, and the sealing plug is taken out to obtain the metal bar. In the cold isostatic pressing forming process of the metal powder, the sheath is sealed by adopting different glues, the sealing effect after solidification is good, the operation is simple and convenient, the demolding and the separation are carried out by inflation through the cold isostatic pressing forming, the separation operation of the sheath and the product is simplified, and the product percent of pass is high; the method is simple and convenient to operate, can effectively improve the production efficiency and reduces the cost.
Description
Technical Field
The invention belongs to the technical field of semiconductor targets, and relates to a cold isostatic pressing preparation method of a metal bar.
Background
An integrated circuit is a miniature electronic device, which is prepared by connecting elements such as a transistor, a resistor, a capacitor, an inductor and the like with wiring through a certain process, and is concentrated on a silicon chip to realize a specific function. With the development of the feature size and the wiring width of integrated circuits, copper wiring is gradually used to replace aluminum wiring, but copper wiring is easy to diffuse with silicon of a circuit substrate to form copper-silicon alloy in the use process, and the circuit performance is also affected, so that it is important to plate an inert corrosion-resistant film on the metal interconnection line of the integrated circuits.
The tantalum and the compound thereof have the advantages of hard texture, high ductility, high conductivity, high thermal stability, corrosion resistance and the like, do not form alloy or compound with copper and silicon, can be used as a barrier layer for preventing copper from diffusing, and are widely applied to the industrial fields of chemical industry, microelectronics, electric industry and the like, and the tantalum target is gradually one of key raw materials of the semiconductor industry. Generally, sputtering tantalum targets mainly comprises two main processes of smelting and plastic processing, wherein smelting modes are divided into vacuum arc smelting and vacuum electron beam smelting, the former is mainly adopted at present, high-purity tantalum ingots are obtained through vacuum electron beam smelting, and then plastic deformation is repeatedly carried out on the tantalum ingots, so that tantalum targets with specific sizes are obtained.
The electron beam furnace smelting is usually used for metal bars, and the forming of the electron beam furnace smelting usually needs cold isostatic pressing and sintering processes, wherein the cold isostatic pressing is one of the most main forming means of powder metallurgy, a sheath is usually needed to be selected as a die, the selected sheath material and structure have direct influence on the formability of a pressed blank and the quality of a product, and meanwhile, the cold isostatic pressing sheath has certain technical requirements in use, and particularly the sealing operation of the sheath is shown. CN 204321190U discloses a sheath for powder metallurgy cold isostatic pressing, the sheath is a bag-shaped sheath with an opening at one end, a sealing plug is arranged at the opening end of the sheath, and a transition pad is arranged between the sealing plug and the material; through adopting and putting the transition backing plate in the material top, refill rubber sealing plug, use the iron wire to tie up the seal after the final pre-vacuumizing. However, in the sealing operation of iron wire binding, the technical experience of operators is important, and the tightness degree, the number of threads, the positions of falling threads and the like of iron wire binding are key factors influencing the yield of pressed billets, so that the operation is complex, and the production efficiency is influenced.
CN 103920880a discloses a method for preparing tantalum and tantalum alloy bars, which comprises the following steps: loading prepared tantalum or tantalum alloy powder into a cylindrical rubber sleeve, kneading, sealing, placing into a cold isostatic press, pressurizing, maintaining pressure, releasing pressure, completing cold isostatic pressing, and demolding to obtain a tantalum rod pressed compact; the method comprises the steps of plugging in a rubber plug, discharging air in the rubber jacket, binding the rubber plug part by using an iron wire to form a blank strip, uniformly kneading the blank strip, clamping by using a clamping plate, and fixing by using an elastic band.
In summary, when preparing the metal bar by cold isostatic pressing, a proper packing mode needs to be selected, so that the packing tightness can be ensured, the operation is simplified, the working efficiency can be improved, and the cost is reduced.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a cold isostatic pressing preparation method of a metal bar, wherein in the cold isostatic pressing process of metal powder, different glues are matched for sealing a sheath, and demoulding separation is carried out by inflation after cold isostatic pressing; the method has the advantages of good tightness of the sheath, simple and convenient operation, effective improvement of production efficiency and cost reduction.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps:
(1) Filling metal powder into a sheath for compaction, and then plugging a sealing plug with the side surface coated with first glue into the sheath;
(2) After the first glue in the step (1) is solidified, coating second glue at the joint of the sealing plug and the sheath until the second glue is solidified to finish the sealing of the sheath;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2);
(4) And (3) after cold isostatic pressing treatment, perforating at the joint of the sheath and the sealing plug, inflating into the sheath to demold, then scribing the sealing part of the sheath, and taking out the sealing plug to obtain the metal bar.
In the invention, when preparing the metal bar, the cold isostatic pressing method is one of the powder metallurgy forming methods, the selection and sealing operation of the sheath are important factors influencing the performance of the formed product, when the sheath is sealed, different glues are used in a matching way, the gap between the sealing plug and the sheath is fully filled while the sheath is packaged, a good sealing effect is achieved after solidification, the operation is simple and convenient, after the cold isostatic pressing treatment is carried out for forming, the sheath and the formed bar are separated in a pore opening and inflation mode, after the sealing plug is drawn out from the sealing position, the metal bar can also be directly taken out, the separation operation of the sheath and the product is simplified, and the density and strength of the obtained metal bar are higher; the method disclosed by the invention is simple and convenient to operate, can effectively improve the production efficiency and reduces the cost.
The following technical scheme is a preferred technical scheme of the invention, but is not a limitation of the technical scheme provided by the invention, and the technical purpose and beneficial effects of the invention can be better achieved and realized through the following technical scheme.
In a preferred embodiment of the present invention, the material of the metal powder in the step (1) includes any one of tantalum, tantalum alloy, niobium or niobium alloy.
Preferably, the particle size of the metal powder in the step (1) is 3 to 20. Mu.m, for example, 3 μm, 4 μm, 5 μm, 6 μm, 8 μm, 10 μm, 12 μm, 15 μm or 20 μm, etc., but not limited to the recited values, and other non-recited values within the range of the values are equally applicable.
Preferably, the material of the sheath in the step (1) comprises any one of rubber, latex or plastic.
Preferably, the shape of the sheath in step (1) is rod-like.
According to the preferred technical scheme, the material of the sealing plug in the step (1) comprises rubber or polyurethane.
In the invention, the step (1) of plugging the sealing plug into the sheath means that the opening end of the sheath is plugged by the sealing plug.
Preferably, the first glue of step (1) comprises an acrylate glue, preferably 502 glue; wherein the 502 glue is mainly prepared from alpha-ethyl cyanoacrylate, and then tackifier, stabilizer, flexibilizer, polymerization inhibitor and the like are added.
In the preferred embodiment of the present invention, the curing time of the first glue in the step (2) is 1 to 20min, for example, 1min, 3min, 5min, 8min, 10min, 12min, 15min, 18min or 20min, but not limited to the recited values, and other non-recited values in the range of the values are equally applicable.
Preferably, the second glue of step (2) comprises an AB glue or a polyurethane glue.
Preferably, the A component in the AB glue comprises acrylic modified epoxy resin, and the B component comprises modified amine.
In a preferred embodiment of the present invention, the mass ratio of the first glue to the second glue is 1-3, for example, 1, 1.25, 1.5, 1.8, 2, 2.25, 2.5, 2.7 or 3, but not limited to the recited values, and other non-recited values within the range are equally applicable.
In the invention, the first glue and the second glue are used during the sealing of the sheath, the dosage of the first glue is relatively large, the main gluing function is realized, and the second glue has the waterproof function while the sealing is supplemented.
Preferably, the second glue in step (2) is cured for a period of time ranging from 1 to 20min, such as 1min, 3min, 5min, 6min, 8min, 10min, 12min, 15min, 18min or 20min, but not limited to the recited values, and other non-recited values within the range are equally applicable.
In a preferred embodiment of the present invention, the pressure of the cold isostatic pressing in the step (3) is 100 to 300MPa, for example, 100MPa, 150MPa, 200MPa, 250MPa or 300MPa, etc., but the present invention is not limited to the values listed, and other values not listed in the range of values are equally applicable.
Preferably, the pressure of the cold isostatic pressing of step (3) is provided by a cold isostatic pressing device.
Preferably, the time of cold isostatic pressing in step (3) is 5-60 min, for example 5min, 10min, 15min, 20min, 25min, 30min, 40min, 50min or 60min, etc., but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferable technical scheme of the invention, the tapping in the step (4) is performed by a screwdriver.
Preferably, the opening in the step (4) is positioned at the adhesion position of the glue.
Preferably, the aperture of the opening in step (4) is 4-7 mm, for example 4mm, 4.5mm, 5mm, 5.5mm, 6mm, 6.5mm or 7mm, but is not limited to the recited values, and other non-recited values within this range are equally applicable.
As a preferred technical scheme of the invention, the inflating in the step (4) is as follows: and filling air into the sheath from the opening by adopting an air gun.
Preferably, the gas charged in step (4) is air.
Preferably, the jacket is separated from the formed bar after demolding in the step (4).
As a preferable technical scheme of the invention, the sealing part of the sheath in the step (4) is cut by adopting a flat cutter, and a wallpaper cutter is preferable.
Preferably, the shape of the metal bar in the step (4) is cylindrical or prismatic.
Preferably, the length-diameter ratio or the length-diameter ratio of the metal bar in the step (4) is 1-10, such as 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
As a preferable technical scheme of the invention, the preparation method comprises the following steps:
(1) Filling metal powder into a sheath for compaction, wherein the metal powder is made of any one of tantalum, tantalum alloy, niobium or niobium alloy, the particle size is 3-20 mu m, the sheath is made of any one of rubber, latex or plastic, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of rubber or polyurethane, and the first glue comprises acrylate glue;
(2) After 1-20 min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, wherein the second glue comprises AB glue or polyurethane glue, the mass ratio of the first glue to the second glue is 1-3, and after 1-20 min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 100-300 MPa, and the time is 5-60 min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 4-7 mm, filling gas into the sheath by adopting an air gun to finish demoulding, and then, scribing the sealing part of the sheath by adopting a flat cutter and taking out the sealing plug to obtain the metal bar.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the method, in the cold isostatic pressing forming process of the metal powder, different glues are used together to seal the sheath, the sealing effect after solidification is good, the operation is simple and convenient, after the cold isostatic pressing forming, demolding and separation are carried out through inflation, the separation operation of the sheath and a product is simplified, the production efficiency is high, the sheath leakage in the cold isostatic pressing process is prevented, and the product qualification rate is high;
(2) The method disclosed by the invention is simple and convenient to operate, can effectively improve the production efficiency and reduces the cost.
Detailed Description
For better illustrating the present invention, the technical scheme of the present invention is convenient to understand, and the present invention is further described in detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
The invention provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps of:
(1) Filling metal powder into a sheath for compaction, and then plugging a sealing plug with the side surface coated with first glue into the sheath;
(2) After the first glue in the step (1) is solidified, coating second glue at the joint of the sealing plug and the sheath until the second glue is solidified to finish the sealing of the sheath;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2);
(4) And (3) after cold isostatic pressing treatment, perforating at the joint of the sheath and the sealing plug, inflating into the sheath to demold, then scribing the sealing part of the sheath, and taking out the sealing plug to obtain the metal bar.
The following are exemplary but non-limiting examples of the invention:
example 1:
the embodiment provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps:
(1) Filling tantalum metal powder into a sheath for compaction, wherein the average particle size of the metal powder is 5 mu m, the sheath is made of rubber, a sealing plug with the side surface coated with first glue is plugged into the sheath, the sealing plug is made of rubber, and the first glue is 502 glue;
(2) After 2min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, the second glue is AB glue, the component A in the AB glue is acrylic acid modified epoxy resin, the component B is modified amine, the mass ratio of the first glue to the second glue is 1:1, and after 5min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 150MPa, and the time is 45min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 5mm, filling air into the sheath by adopting an air gun to finish demoulding, and then, cutting the sealing part of the sheath by adopting a wallpaper knife, and taking out the sealing plug to obtain the tantalum metal bar.
In the embodiment, the tantalum metal bar is prepared by the method, the tightness of the sheath is good, the qualification rate of the obtained bar product is high, the operation is simple and convenient, and the production efficiency is high.
Example 2:
the embodiment provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps:
(1) Filling tantalum metal powder into a sheath for compaction, wherein the average particle size of the metal powder is 3 mu m, the sheath is made of plastic, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of polyurethane, and the first glue is 502 glue;
(2) After 5min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, the second glue is AB glue, the component A in the AB glue is acrylic acid modified epoxy resin, the component B is modified amine, the mass ratio of the first glue to the second glue is 3:1, and after 6min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 200MPa, and the time is 20min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 4mm, filling air into the sheath by adopting an air gun to finish demoulding, and then, cutting the sealing part of the sheath by adopting a wallpaper knife, and taking out the sealing plug to obtain the tantalum metal bar.
In the embodiment, the tantalum metal bar is prepared by the method, the tightness of the sheath is good, the qualification rate of the obtained bar product is high, the operation is simple and convenient, and the production efficiency is high.
Example 3:
the embodiment provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps:
(1) Filling tantalum alloy metal powder into a sheath for compaction, wherein the average particle size of the metal powder is 10 mu m, the sheath is made of latex, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of polyurethane, and the first glue is 502 glue;
(2) After 1min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, the second glue is AB glue, the component A in the AB glue is acrylic acid modified epoxy resin, the component B is modified amine, the mass ratio of the first glue to the second glue is 2:1, and after 8min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 300MPa, and the time is 15min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 5.5mm, filling air into the sheath by adopting an air gun to finish demoulding, and then, cutting the sealing part of the sheath by adopting a wallpaper knife, and taking out the sealing plug to obtain the tantalum alloy metal bar.
In the embodiment, the tantalum alloy metal bar is prepared by the method, the tightness of the sheath is good, the qualification rate of the obtained bar product is high, the operation is simple and convenient, and the production efficiency is high.
Example 4:
the embodiment provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps:
(1) The preparation method comprises the steps of filling niobium metal powder into a sheath for compaction, wherein the average particle size of the metal powder is 15 mu m, the sheath is made of rubber, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of polyurethane, and the first glue is acrylate glue;
(2) After 15min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, the second glue is polyurethane glue, the mass ratio of the first glue to the second glue is 1.5:1, and after 10min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 225MPa, and the time is 10min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 6mm, filling air into the sheath by adopting an air gun to finish demoulding, and then, cutting the sealing part of the sheath by adopting a wallpaper knife, and taking out the sealing plug to obtain the niobium metal bar.
In the embodiment, the niobium metal bar is prepared by the method, the tightness of the sheath is good, the qualification rate of the obtained bar product is high, the operation is simple and convenient, and the production efficiency is high.
Example 5:
the embodiment provides a cold isostatic pressing preparation method of a metal bar, which comprises the following steps:
(1) Filling niobium alloy metal powder into a sheath for compaction, wherein the average particle size of the metal powder is 8 mu m, the sheath is made of plastic, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of rubber, and the first glue is 502 glue;
(2) After 10min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, the second glue is polyurethane glue, the mass ratio of the first glue to the second glue is 2.5:1, and after 5min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 120MPa, and the time is 60min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 7mm, filling air into the sheath by adopting an air gun to finish demoulding, and then, cutting the sealing part of the sheath by adopting a wallpaper knife, and taking out the sealing plug to obtain the niobium alloy metal bar.
In the embodiment, the niobium alloy metal bar is prepared by the method, the tightness of the sheath is good, the qualification rate of the obtained bar product is high, the operation is simple and convenient, and the production efficiency is high.
Comparative example 1:
this comparative example provides a method for cold isostatic pressing of metal bars, which refers to the method in example 1, differing only in: the operation of step (2) is not included.
In the comparative example, the side surface of the sealing plug is coated by only adopting the first glue when the sheath is sealed, the sealing property of the sheath is poor, the uniformity of stress of the powder at each part cannot be ensured during cold isostatic pressing, the uniformity of the obtained product is lower, and the part cannot be molded.
Comparative example 2:
this comparative example provides a method for cold isostatic pressing of metal bars, which refers to the method in example 1, differing only in: the operation of opening holes and inflating in the step (4) is not included.
In this comparative example, after the sheath was cold isostatic pressed, the sealing part was directly scratched, and the sealing plug was taken out, but at this time, the metal bar was tightly bonded to the side of the main body of the sheath, and the metal bar was difficult to directly take out, and thereafter, the metal bar was easily damaged during taking out.
It can be seen from the above examples and comparative examples that in the cold isostatic pressing process of metal powder, the method of the invention seals the sheath by adopting different glues to cooperate, has good sealing effect after solidification, is simple and convenient to operate, simplifies the separation operation of the sheath and the product by demolding and separating through inflation after cold isostatic pressing, has high production efficiency, prevents sheath leakage in the cold isostatic pressing process, and has high product qualification rate; the method is simple and convenient to operate, can effectively improve the production efficiency and reduces the cost.
The present invention is described in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e., it does not mean that the present invention must be practiced depending on the above detailed methods. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions for the method of the present invention, addition of auxiliary steps, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
Claims (23)
1. A method for preparing a metal bar by cold isostatic pressing, characterized in that the preparation method comprises the following steps:
(1) Filling metal powder into a sheath and compacting, wherein the sheath is made of rubber or plastic, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of rubber, and the first glue comprises acrylic ester glue;
(2) After the first glue in the step (1) is solidified, coating second glue at the joint of the sealing plug and the sheath, wherein the second glue comprises AB glue or polyurethane glue, and sealing the sheath after the second glue is solidified;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2);
(4) And (3) after cold isostatic pressing treatment, perforating at the joint of the sheath and the sealing plug, inflating into the sheath to demold, then scribing the sealing part of the sheath, and taking out the sealing plug to obtain the metal bar.
2. The method according to claim 1, wherein the metal powder in step (1) is made of any one of tantalum, tantalum alloy, niobium or niobium alloy.
3. The method according to claim 1, wherein the metal powder in step (1) has a particle size of 3 to 20 μm.
4. The method of claim 1, wherein the sheath of step (1) is rod-shaped.
5. The method of claim 1, wherein the first glue in step (1) is 502 glue.
6. The preparation method of claim 1, wherein the first glue in step (2) is cured for 1-20 min.
7. The method of claim 1, wherein the AB glue comprises an acrylic modified epoxy resin as component a and a modified amine as component B.
8. The preparation method of claim 1, wherein the mass ratio of the first glue to the second glue is 1-3.
9. The preparation method of claim 1, wherein the second glue in step (2) is cured for 1-20 min.
10. The method according to claim 1, wherein the pressure of the cold isostatic pressing in the step (3) is 100-300 mpa.
11. The method of claim 1, wherein the cold isostatic pressure of step (3) is provided by a cold isostatic press.
12. The method according to claim 1, wherein the cold isostatic pressing in step (3) is performed for a period of 5-60 min.
13. The method of claim 1, wherein the tapping in step (4) is performed with a screwdriver.
14. The method of claim 1, wherein the openings in step (4) are located at glue joints.
15. The method according to claim 1, wherein the pore diameter of the opening in the step (4) is 4-7 mm.
16. The method of claim 1, wherein the inflating of step (4) is: and filling air into the sheath from the opening by adopting an air gun.
17. The method of claim 1, wherein the gas introduced in step (4) is air.
18. The method of claim 1, wherein the post-mold jacket of step (4) is separated from the molded bar.
19. The method of claim 1, wherein the jacket seal of step (4) is scored using a flat knife.
20. The method of claim 19, wherein the jacket seal of step (4) is scored using a wallpaper knife.
21. The method of claim 1, wherein the metal bar in step (4) is cylindrical or prismatic in shape.
22. The method of claim 21, wherein the metal bar in step (4) has an aspect ratio or aspect ratio of 1 to 10.
23. The preparation method according to claim 1, characterized in that the preparation method comprises the steps of:
(1) Filling metal powder into a sheath for compaction, wherein the metal powder is made of any one of tantalum, tantalum alloy, niobium or niobium alloy, the particle size is 3-20 mu m, the sheath is made of rubber or plastic, a sealing plug with a side surface coated with first glue is plugged into the sheath, the sealing plug is made of rubber, and the first glue comprises acrylate glue;
(2) After 1-20 min, the first glue is solidified, a second glue is coated at the joint of the sealing plug and the sheath, wherein the second glue comprises AB glue or polyurethane glue, the mass ratio of the first glue to the second glue is 1-3, and after 1-20 min, the second glue is solidified, so that the sheath sealing is completed;
(3) Carrying out cold isostatic pressing treatment on the sealed sheath in the step (2), wherein the pressure of the cold isostatic pressing is 100-300 MPa, and the time is 5-60 min;
(4) And (3) after cold isostatic pressing treatment, perforating the joint of the sheath and the sealing plug by adopting a screwdriver, wherein the aperture of the perforating is 4-7 mm, filling gas into the sheath by adopting an air gun to finish demoulding, and then tearing the sealing part of the sheath by adopting a flat cutter and taking out the sealing plug to obtain the metal bar.
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| JP2003137653A (en) * | 2001-10-24 | 2003-05-14 | Ishizuka Kenkyusho:Kk | Method of manufacturing composite sintered compact and reaction vessel for the same |
| CN201020536Y (en) * | 2007-04-29 | 2008-02-13 | 西北有色金属研究院 | Jacket for cold isostatic moulding in powder metallurgy |
| CN201132215Y (en) * | 2007-12-10 | 2008-10-15 | 西北有色金属研究院 | Isostatic cool pressing forming die for filter tube with closing end |
| CN102189261A (en) * | 2011-05-30 | 2011-09-21 | 华中科技大学 | Densification method of porous workpiece |
| CN204321190U (en) * | 2014-12-04 | 2015-05-13 | 北京有色金属研究总院 | A kind of jacket for cold isostatic moulding in powder metallurgy |
| CN113136554A (en) * | 2021-04-26 | 2021-07-20 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method thereof |
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2022
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003137653A (en) * | 2001-10-24 | 2003-05-14 | Ishizuka Kenkyusho:Kk | Method of manufacturing composite sintered compact and reaction vessel for the same |
| CN201020536Y (en) * | 2007-04-29 | 2008-02-13 | 西北有色金属研究院 | Jacket for cold isostatic moulding in powder metallurgy |
| CN201132215Y (en) * | 2007-12-10 | 2008-10-15 | 西北有色金属研究院 | Isostatic cool pressing forming die for filter tube with closing end |
| CN102189261A (en) * | 2011-05-30 | 2011-09-21 | 华中科技大学 | Densification method of porous workpiece |
| CN204321190U (en) * | 2014-12-04 | 2015-05-13 | 北京有色金属研究总院 | A kind of jacket for cold isostatic moulding in powder metallurgy |
| CN113136554A (en) * | 2021-04-26 | 2021-07-20 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method thereof |
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| CN115921861A (en) | 2023-04-07 |
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