WO2013018957A1 - 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법 - Google Patents
마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법 Download PDFInfo
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- WO2013018957A1 WO2013018957A1 PCT/KR2011/009519 KR2011009519W WO2013018957A1 WO 2013018957 A1 WO2013018957 A1 WO 2013018957A1 KR 2011009519 W KR2011009519 W KR 2011009519W WO 2013018957 A1 WO2013018957 A1 WO 2013018957A1
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- tungsten carbide
- target temperature
- mold
- sintered body
- temperature
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000003466 welding Methods 0.000 title claims abstract description 34
- 238000003756 stirring Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract 6
- 239000000843 powder Substances 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 50
- 238000005245 sintering Methods 0.000 claims abstract description 35
- 238000000465 moulding Methods 0.000 claims abstract description 17
- 238000011049 filling Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000007770 graphite material Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims description 33
- 125000006850 spacer group Chemical group 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 21
- 230000000630 rising effect Effects 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 1
- 239000010941 cobalt Substances 0.000 abstract description 16
- 229910017052 cobalt Inorganic materials 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 14
- 238000002844 melting Methods 0.000 abstract description 13
- 230000008018 melting Effects 0.000 abstract description 11
- 239000010959 steel Substances 0.000 abstract description 11
- 229910000831 Steel Inorganic materials 0.000 abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 7
- 238000005299 abrasion Methods 0.000 abstract description 6
- 238000001994 activation Methods 0.000 abstract description 6
- 230000004913 activation Effects 0.000 abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010936 titanium Substances 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract 2
- 230000000996 additive effect Effects 0.000 abstract 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 12
- 229910052721 tungsten Inorganic materials 0.000 description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 9
- 239000010937 tungsten Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 238000009770 conventional sintering Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- GJNGXPDXRVXSEH-UHFFFAOYSA-N 4-chlorobenzonitrile Chemical compound ClC1=CC=C(C#N)C=C1 GJNGXPDXRVXSEH-UHFFFAOYSA-N 0.000 description 1
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000003562 lightweight material Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- 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
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
- B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
- B23K20/1245—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding characterised by the apparatus
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5626—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on tungsten carbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Definitions
- the present invention relates to a method for manufacturing a tungsten carbide sintered body for friction stir welding tools, and more particularly, has a high density, high strength, high toughness and high wear resistance in a short time in a single process using a discharge plasma sintering process.
- Friction Stir Welding a cost-melting solid-state joint, is used in the process of joining lightweight materials. This is being applied.
- friction stir welding technology has been applied to various industries such as titanium, steel, stainless steel, nickel alloy, and other high-melting materials such as titanium, steel, stainless steel, and nickel alloys. have.
- Tungsten carbide has a melting point of 2600 ° C and a density of 15.7 g / cm 3 and cobalt (Co) has a melting point of 1459 ° C and a density of 8.9 g / cm 3 and tungsten carbide-cobalt is called cemented carbide. It is used for various purposes because of its advantages and advantages of metal. Tungsten carbide has high melting point, high strength and abrasion resistance, and is used in various applications such as machining tools, abrasion resistant tools, cutting tools, and molds.
- tungsten carbide-cobalt manufacturing technology which has been in the spotlight as a tool for solid-state friction stir welding, can be largely classified into a melting / casting method and a powder metallurgy method.
- dissolution / casting and powder metallurgy are the most common methods for sintering and manufacturing tungsten carbide-cobalt, which has the advantage of lowering the manufacturing cost due to easy mass production, but has limitations in grain control and densification.
- the powder metallurgy technology has the advantage of producing high toughness and high strength tungsten carbide-cobalt due to the homogeneous phase distribution, fine grain control, easy to manufacture high melting point materials, and the range of composition and composition ratio of design freedom. Recently, it is being actively applied as an alternative to the melting / casting method.
- the applicant has applied for a method of manufacturing a tungsten carbide-cobalt sintered body to be used for a tool material for solid-state friction stir welding using a discharge plasma sintering process.
- the present invention was created in order to solve the above requirements, the growth of particles of tungsten carbide sintered body to be used for the tool material for solid-state friction stir welding, while sintering by the discharge plasma sintering apparatus using only the tungsten carbide powder using pulse current activation method Highly homogeneous structure of high melting point with high density, high strength, high toughness, and high wear resistance can be obtained in a short time with a single process that can be controlled. The process cost is lower than that of HP or HIP, and there is almost no difference in physical properties between inside and outside. It is an object of the present invention to provide a method for producing a tungsten carbide sintered body for a friction stir welding tool.
- Tungsten carbide sintered body manufacturing method for friction stir welding tool for achieving the above object is a.
- a filling step of filling tungsten carbide (WC) powder into a mold made of graphite material I. Mounting the mold filled with the tungsten carbide powder in a chamber of a discharge plasma sintering apparatus; All. Evacuating the chamber; la.
- the final target temperature of the molding step is 1410 to 2000 °C is applied.
- the filling step includes a pre-pressurizing process of filling the dried tungsten carbide powder into the mold and preliminarily pressurized to a pressure of 1400 to 1600kg f using a molding press and maintained for 5 to 15 minutes.
- the molding step is to maintain the inside of the mold filled with the tungsten carbide powder at a pressure of 30 to 100MPa, la-1. Firstly heating the tungsten carbide powder in the mold to a first target temperature at a temperature increase rate of 60 ° C./min to 150 ° C./min; D-2. Maintaining the primary target temperature for 1 to 10 minutes; D-3. Heating the secondary tungsten carbide powder in the mold to a secondary target temperature at a temperature increase rate of 30 ° C./min to 80 ° C./min; D-4. Maintaining the secondary target temperature for 1 to 10 minutes; D-5.
- the seventh final target temperature for 1 to 10 minutes; wherein the primary target temperature is 550 ° C to 650 ° C, the secondary target temperature is 900 ° C to 1005 ° C, and the third target Temperature is 1010 °C to 1105 °C, the fourth target temperature is 1110 °C to 1205 °C, the fifth target temperature is 1210 °C to 1305 °C, the sixth target temperature is 1310 °C to 1405 °C, 7 The next final target temperature is 1410 °C to 2000 °C is applied.
- the relative density of the sintered tungsten carbide sintered body is formed to be 99.5% or more.
- tungsten carbide is suitably used for the tool for friction stir welding using the pulse current activation method as the discharge plasma sintering apparatus.
- the sintered body can be manufactured and manufactured by using only tungsten carbide single material excluding the sintering aid such as cobalt, which simplifies the manufacturing process and lowers the cost. Has the advantage of providing higher toughness, higher wear resistance and higher strength when have.
- FIG. 1 is a view schematically showing a discharge plasma sintering apparatus applied to the tungsten carbide sintered body manufacturing method for a friction stir welding tool according to the present invention
- FIG. 2 is a photograph taken by a scanning electron microscope of tungsten carbide powder before the sintering step applied to the tungsten carbide sintered body manufacturing method for friction stir welding tool according to the present invention
- FIG. 3 is a graph showing the XRD component analysis results for the tungsten carbide powder before the sintering process applied in FIG.
- 5 and 6 are photographs of a tungsten carbide sintered body having a diameter of 65.5 mm and a thickness of 30 mm or more having a relative density of 99.8% or more manufactured at a heating rate of 35 ° C./min at a target temperature of 1400 to 2000 ° C. under a pressure of 70 MPa.
- FIG. 8 is a photograph taken after the friction stir welding test process is mounted on a SS400 (tensile strength 400 MPa) steel plate by mounting the tungsten carbide tool of FIG.
- FIG. 10 is a photograph showing a shape after a test process of 50 m or more with the tungsten carbide tool of FIG. 7;
- FIG. 11 is a graph illustrating a change in weight while the tungsten carbide tool of FIG. 7 is subjected to a mounting test process of 50 m or more.
- FIG. 12 is a graph showing an XRD component analysis result of the sintered compact of FIG. 5.
- FIG. 1 is a view schematically showing a discharge plasma sintering apparatus applied to the tungsten carbide sintered body manufacturing method for a friction stir welding tool according to the present invention.
- the discharge plasma sintering apparatus 100 includes a chamber 110, a cooling unit 120, a current supply unit 130, a temperature detection unit 140, a pump 150, a pressurizer 160, and a main controller ( 170 and an operation unit 180.
- the upper electrode 211 and the lower electrode 212 are provided in the chamber 110 so as to be spaced apart from each other, and although not shown, the upper and lower electrodes 211 and 212 are formed to allow the coolant to flow through for dissipation. have.
- the cooling unit 120 is configured to distribute the cooling water to the cooling water distribution pipes provided on the inner wall of the chamber 110 and the cooling water distribution pipes provided on the upper and lower electrodes 211 and 212.
- the current supply unit 130 is controlled by the main controller 170 through the upper and lower electrodes 211 and 212 to apply a pulse current.
- the temperature detection unit 140 is preferably applied to the infrared temperature detection method for detecting the temperature through the see-through window provided in the chamber 110.
- the pump 150 is configured to discharge the bet inside the chamber 110 to the outside.
- the pressurizer 160 is installed to pressurize the tungsten carbide powder 205 filled in the mold 200.
- a cylinder structure capable of raising and lowering the lower electrode 212 is applied.
- the main controller 170 controls the cooling unit 120, the current supply unit 130, the pump 150, and the pressurizer 160 according to an operation command set through the operation unit 180, and is detected by the temperature detector 140.
- the temperature information is received and displayed through a display unit (not shown).
- Mold 200 is formed in a cylindrical shape, the receiving groove is formed to fill the tungsten carbide powder in the center.
- the current applied to the mold 200 from the upper and lower electrodes 211 and 212 is concentrated to increase the temperature raising efficiency and reduce unnecessary energy consumption. It is preferable to provide a spacer between the electrodes 211 and 212. That is, an outer diameter is formed between the upper electrode 211 for applying an electric field in the mold 200 and the upper punch 215 entering from the upper direction in the mold 200 toward the upper punch 215, and the graphite material is formed. First to third upper spacers 221, 222, and 223 are provided. In addition, between the lower punch 216 extending from the lower electrode 212 and entering the inside from the lower direction of the mold 200 toward the lower punch 216, the outer diameter is made smaller and the first to the first to be made of graphite material. Third lower spacers 231 to 233 are provided.
- the first upper spacers 221 and the first lower spacers 231 have a diameter of 350 mm and a thickness of 30 mm.
- the second upper spacers 222 and the second lower spacers 232 have a diameter of 300 mm and a thickness. 60 mm is applied, and the third upper spacer 223 and the third lower spacer 233 have a diameter of 100 to 200 mm and a thickness of 15 to 30 mm.
- the method for producing a tungsten carbide sintered body for a friction stir welding tool using a pulse current activation method using the discharge plasma sintering apparatus according to the present invention is subjected to a filling step, a mounting step, a vacuuming step, a molding step, and a cooling step.
- the filling step is filling the sintered tungsten carbide (WC) powder into the mold 200 made of graphite material.
- the material applied in the filling step is applied only to tungsten carbide powder alone.
- FIG. 2 shows a photograph of a tungsten carbide powder prepared for filling under a scanning electron microscope.
- the tungsten carbide powder has a purity of 99.95% and a particle size of 0.5 ⁇ m. It is in a state.
- FIG. 3 the XRD component analysis of the tungsten carbide powder applied in FIG. 2 is shown in FIG. 3, and impurities such as W 2 C were not included.
- the sintering target tungsten carbide powder does not contain impurities other than the tungsten carbide component.
- the lower punch 216 is inserted into the lower portion of the discharge plasma sintering mold 200 and the tungsten carbide powder is filled into the mold 200, and then the upper punch 215 is inserted into the upper portion of the mold 200.
- the adhesion between the powder particles is increased by preliminary pressurization for 5 to 15 minutes at a pressure of 1400 to 1600 kgf using a molding press.
- a mounting step of mounting the mold 200 in the chamber 110 of the discharge plasma sintering apparatus 100 is performed.
- the upper and lower spacers 221, 222, 223, 231, 232 and 233 described above are mounted between the upper and lower electrodes 211 and 212 of the mold 200.
- the vacuumization step is to make the internal space of the chamber 110 in a vacuum state, and discharge the air inside the chamber 110 through the pump 150 to make a vacuum state.
- the inside of the chamber 110 may be evacuated to 6 Pa to 1 ⁇ 10 ⁇ 3 Pa.
- contamination of the initial tungsten carbide powder due to impurities and oxidation of the inside of the chamber 110 may be caused. Can be.
- the molding step is a step of applying a current to the tungsten carbide powder for shaping.
- the pressurizer 160 is operated to maintain a pressure of 30 to 100 MPa, preferably 70 MPa, to the tungsten carbide powder 205 in the mold 200.
- the tungsten carbide powder in the mold 200 is heated in accordance with the elevated temperature and isothermal patterns. At this time, it is preferable to set the final target temperature of the mold 200 to 1410 ° C to 2000 ° C. If the sintering temperature is 1410 ° C or less, the sintered body is not formed and a sintered body having low density is produced. In addition, when the final sintering target temperature is 2000 °C or more, the grains of the sintered body rapidly grow and melt (melting) adversely affect the mechanical properties.
- the molding process first, to the first target temperature of 550 °C to 650 °C at a temperature increase rate of 60 °C / min to 150 °C / min for the tungsten carbide powder 205 in the mold 200 Car temperature rises.
- the primary target temperature is set to 600 ° C.
- the primary target temperature is kept isothermal for 1 to 10 minutes.
- the temperature of the tungsten carbide powder 205 in the mold 200 is increased to a secondary target temperature of 900 ° C. to 1005 ° C. at a temperature increase rate of 30 ° C./min to 80 ° C./min.
- the secondary target temperature is set to 1000 ° C.
- the secondary target temperature is kept isothermal for 1 to 10 minutes.
- the temperature of the tungsten carbide powder 205 in the mold 200 is increased to a third target temperature of 1010 ° C. to 1105 ° C. at a temperature rising rate of 10 ° C./min to 80 ° C./min.
- the third target temperature is set to 1100 ° C.
- the third target temperature is kept isothermal for 1 to 10 minutes.
- the temperature of the tungsten carbide powder 205 in the mold 200 is increased to a fourth target temperature of 1110 ° C. to 1205 ° C. at a temperature rising rate of 10 ° C./min to 80 ° C./min.
- the 4th target temperature is set to 1200 degreeC.
- the fourth target temperature is kept isothermal for 1 to 10 minutes.
- the temperature of the tungsten carbide powder 205 in the mold 200 is increased to the fifth target temperature of 1210 ° C. to 1305 ° C. at a temperature rising rate of 10 ° C./min to 80 ° C./min.
- the 5th target temperature is set to 1300 degreeC.
- the fifth target temperature is kept isothermal for 1 to 10 minutes.
- the temperature of the tungsten carbide powder 205 in the mold 200 is raised to the sixth target temperature of 1310 ° C. to 1405 ° C. at a temperature rising rate of 10 ° C./min to 80 ° C./min.
- the 6th target temperature is set to 1400 degreeC.
- the sixth target temperature is kept isothermal for 1 to 10 minutes.
- the temperature of the tungsten carbide powder 205 in the mold 200 is raised to the 7th final target temperature of 1410 ° C. to 2000 ° C. at a temperature rising rate of 10 ° C./min to 80 ° C./min.
- the seventh final target temperature is set at 1500 ° C.
- the seventh final target temperature is kept isothermal for 1 to 10 minutes.
- the cooling step cools the inside of the chamber 110 while maintaining the pressure applied to the tungsten carbide powder 205 in the mold 200 after reaching the final target temperature and isothermal holding time.
- the tungsten carbide sintered body may be demolded from the mold 200, and the tungsten carbide sintered body manufactured through the above-described process is formed as shown in FIG. 4.
- a large current in a low voltage pulse flows into a gap between particles of tungsten carbide powder by the current applied through the upper and lower electrodes 211 and 212, and is caused by the high energy of the discharge plasma generated instantaneously by the spark discharge phenomenon.
- the sintered body is formed by heat diffusion and electric field diffusion and pressure and electric energy due to thermal diffusion and electric field diffusion and the electrical resistance of the mold 200.
- the pulsed current activating method is a direct heating method in which a current flows directly into a specimen of tungsten carbide through the punches 215 and 216. At the same time, a current is applied to the mold 200 and heat is also generated inside the specimen. Due to the low temperature difference, relatively low temperature and short sintering time, the thermal activation reaction generated during the sintering process can be minimized. In particular, when tungsten carbide powder is sintered, it is possible to increase the density and finer the grain size of 99.5% or more, which is suitable for the friction stir welding tool.
- a large sintered body having a large area of 50 to 150 mm in diameter and 25 to 30 mm in thickness can be manufactured.
- Tungsten carbide sintered body manufactured through such manufacturing process can be sintered without sintering materials such as cobalt in a single process without post-treatment process compared with conventional HP, HIP and atmospheric sintering methods, and also has a relative density of 99.5% or more and Microstructure control is possible.
- the sintered body manufacturing method according to the present invention can be produced 20 times or more in diameter, 20 times or more thicker than the conventional sintering method (HP, HIP, atmospheric pressure sintering), and even a large-size sintered body has a high strength with uniform physical properties It can be seen that the tungsten carbide sintered body having high wear resistance and high density (relative density 99.5% or more) can be produced.
- FIG. 4 is a state in which the surface of the prepared tungsten carbide sintered body is corroded by Murakami corrosion method after surface polishing. As can be seen from Figure 4 it can be seen that when tungsten carbide sintered spherical tungsten carbide has a plate shape.
- 5 and 6 illustrate a sintered body prepared by the discharge plasma sintering apparatus before the shape processing to a width of 65.5 mm and a thickness of 30 mm.
- FIG. 8 is a photograph taken after a test process in which the tungsten carbide tool of FIG. 5 is mounted on an FSW device and moved to a friction state on a SS400 (tensile strength 400 MPa grade) steel plate.
- a SS400 tensile strength 400 MPa grade
- the center of the SS400 (tensile strength 400MPa) steel plate supported at the center is shown a deeply tapered groove by frictional movement of the tungsten carbide tool along the left and right longitudinal direction, which can be used for welding. You can check it.
- FIG. 9 is a photograph taken before and after the mounting test for the tungsten carbide-cobalt tool that is currently distributed in Korea as a result of testing at a lower level than the tool mounting test conditions manufactured in the present invention SS400 (tensile strength 400MPa) steel In the case of a steel plate, the progress is not made, and the tool is destroyed at the same time as the progress insertion.
- SS400 tensile strength 400MPa
- FIG. 10 shows the shape after the test procedure of the tungsten carbide tool of FIG. 7 that has been mounted and tested using an actual FSW device.
- the tool in comparison with the tungsten carbide-cobalt tool of FIG. 9, which is currently distributed, the tool is broken or worn without the shape at the same time as the existing commercial tool.
- the tool shaped by the manufactured sintered body having a relative density of 99.8% or more it can be confirmed that the wear or fracture of the probe or the shoulder part does not occur after the friction stir welding test.
- Figure 11 is a graph showing the weight change of the tool of Figure 7 processed during the mounting test, it can be seen that the change in weight after the friction stir welding test more than 50m to 0.177g hardly wear.
- FIG. 12 As a result of analyzing the components for the sintered body produced according to the manufacturing method of the present invention is shown in FIG. As can be seen from FIG. 12, no impurities were observed other than the WC component, and no W 2 C component was found.
- the upper surface of 30mm height and 25mm, 15mm, and 5mm positions corresponding to the positions of 25mm, 15mm, and 5mm are cut along the thickness direction to measure hardness and fracture toughness
- Table 2 One result is shown in Table 2 below.
- the relative density is about 94% when the sintered body is manufactured by continuously raising the temperature rising rate to the final target temperature at a temperature rising rate set within the range of 30 to 70 °C per minute,
- the hardness was about 2200 kg / mm 2 and the fracture toughness was measured as 6 Mpa ⁇ m 1/2 . From these results, when forming a large diameter thick sintered compact having a diameter of 60 mm or more and a thickness of 30 mm or more for a tool, it is preferable to apply the multistage temperature rising pattern shown in Table 1 above.
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Abstract
Description
단계별 목표온도(℃) | 0 | 550~650 | 900~1005 | 1010~1105 | 1100~1205 | 1210~1305 | 1310~1405 | 1410~1600 |
승온(℃/min) | 0 | 60~150 | 30~80 | 10~80 | 10~80 | 10~80 | 10~80 | 10~80 |
유지(min) | 0 | 1~10 | 1~10 | 1~10 | 1~10 | 1~10 | 1~10 | 1~10 |
절단 위치(position) | 상대밀도(%) | 경도(kg/mm2)Hv30 | 파괴인성(Mpa·m1/2) |
표면(30mm) | 99.8 | 2484.9 | 4.30 |
25mm | 99.8 | 2474.6 | 4.96 |
15mm | 99.8 | 2686.4 | 5.29 |
5mm | 99.8 | 2573.4 | 4.82 |
Claims (6)
- 가. 텅스텐 카바이드(WC) 분말을 그라파이트 소재로 된 몰드 내에 충진하는 충진단계와;나. 상기 텅스텐 카바이드 분말이 충진된 상기 몰드를 방전 플라즈마 소결 장치의 챔버 내에 장착하는 장착단계와;다. 상기 챔버 내부를 진공화하는 진공화단계와;라. 상기 몰드 내의 상기 텅스텐 카바이드 분말에 일정한 압력을 유지하면서 설정된 승온패턴에 따라 승온시키면서 최종 목표온도에 도달할 때 까지 성형하는 성형단계와;마. 상기 성형단계 이후 상기 몰드 내에 가압된 압력을 유지하면서 상기 챔버 내부를 냉각하는 냉각단계;를 포함하는 것을 특징으로 하는 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법.
- 제1항에 있어서, 상기 성형단계의 상기 최종 목표온도는 1410 내지 2000℃인 것을 특징으로 하는 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법.
- 제2항에 있어서, 상기 충진단계에서 상기 텅스텐 카바이드 분말은 입자크기 10nm 내지 100㎛이며, 상기 텅스텐 카바이드 분말을 상기 몰드 내에 충진하고 성형 프레스를 이용하여 1400 내지 1600kgf의 압력으로 예비 가압을 하고 5 내지 15분간 유지시키는 예비가압과정을 포함하는 것을 특징으로 하는 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법.
- 제3항에 있어서, 상기 장착단계에서상기 몰드 내에 전계를 인가하기 위한 상기 챔버 내의 상부전극과 상기 몰드 내에 상방향에서 진입되는 상부 펀치 사이에는 그레파이트 소재로 된 복수 개의 상부 스페이서가 상기 상부 펀치를 향할 수록 외경이 작게 형성된 것이 적용되고, 상기 챔버 내의 하부전극과 상기 몰드 내에 하방향에서 진입되는 하부 펀치 사이에는 그레파이트 소재로 된 복수 개의 하부 스페이서가 상기 하부 펀치를 향할수록 외경이 작게 형성되어 있고,상기 상부 스페이서는 상기 상부전극으로부터 상기 상부 펀치 방향으로 원형상으로 형성된 제1상부 스페이서와, 제2 상부 스페이서 및 제3상부 스페이서가 마련되어 있고,상기 하부 스페이서는 상기 챔버 내의 하부전극으로부터 몰드 방향으로 원형상으로 형성된 제1하부 스페이서와, 제2 하부 스페이서 및 제3하부 스페이서가 마련되어 있으며,상기 제1 상부 스페이서 및 상기 제1하부 스페이서는 직경이 350mm, 두께가 30mm이고, 상기 제2 상부 스페이서 및 상기 제2하부 스페이서는 직경이 300mm, 두께가 60mm이고, 상기 제3 상부 스페이서 및 상기 제3하부 스페이서는 직경이 100 내지 200mm, 두께가 15 내지 30mm인 것이 적용된 것을 특징으로 하는 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법.
- 제4항에 있어서, 상기 진공화단계는상기 챔버 내부에서 상기 텅스텐 카바이드 분말의 산화 및 불순물로 인한 오염을 억제하기 위해 6Pa 내지 1X10-3 Pa로 상기 챔버 내부를 진공화하고,상기 성형단계는 상기 텅스텐 카바이드 분말이 충진된 상기 몰드 내부를 30 내지 100MPa의 압력으로 유지하는 것을 특징으로 하는 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법.
- 제5항에 있어서, 상기 성형단계는라-1. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 60℃/min 내지 150℃/min의 승온속도로 1차 목표온도까지 1차 승온하는 단계와;라-2. 상기 1차 목표온도를 1 내지 10분동안 유지하는 단계와;라-3. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 30℃/min 내지 80℃/min의 승온속도로 2차 목표온도까지 2차 승온하는 단계와;라-4. 상기 2차 목표온도를 1 내지 10분 동안 유지하는 단계와;라-5. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 10℃/min 내지 80℃/min의 승온속도로 3차 목표온도까지 3차 승온하는 단계와;라-6. 상기 3차 목표온도를 1 내지 10분동안 유지하는 단계와;라-7. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 10℃/min 내지 80℃/min의 승온속도로 4차 목표온도까지 4차 승온하는 단계와;라-8. 상기 4차 목표온도를 1 내지 10분동안 유지하는 단계와;라-9. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 10℃/min 내지 80℃/min의 승온속도로 5차 목표온도까지 5차 승온하는 단계와;라-10. 상기 5차 목표온도를 1 내지 10분동안 유지하는 단계와;라-11. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 10℃/min 내지 80℃/min의 승온속도로 6차 목표온도까지 6차 승온하는 단계와;라-12. 상기 6차 목표온도를 1 내지 10분동안 유지하는 단계와;라-13. 상기 몰드내의 상기 텅스텐 카바이드 분말에 대해 10℃/min 내지 80℃/min의 승온속도로 7차 최종 목표온도까지 7차 승온하는 단계와;라-14. 상기 7차 최종 목표온도를 1 내지 10분동안 유지하는 단계;를 포함하고,상기 1차 목표온도는 550℃ 내지 650℃이고, 상기 2차 목표온도는 900℃ 내지 1005℃이고, 상기 3차 목표온도는 1010℃ 내지 1105℃이고, 상기 4차 목표온도는 1110℃ 내지 1205℃이고, 상기 5차 목표온도는 1210℃ 내지 1305℃이고, 상기 6차 목표온도는 1310℃ 내지 1405℃이고, 상기 7차 최종목표온도는 1410℃ 내지 2000℃인 것을 특징으로 하는 마찰교반 접합툴용 텅스텐 카바이드 소결체 제조 방법.
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KR101311480B1 (ko) | 2013-11-13 |
US20140191443A1 (en) | 2014-07-10 |
KR20130015396A (ko) | 2013-02-14 |
US9580361B2 (en) | 2017-02-28 |
JP5866009B2 (ja) | 2016-02-17 |
JP2014527124A (ja) | 2014-10-09 |
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