WO2000012247A1 - Process for debinding and sintering metal injection molded parts made with an aqueous binder - Google Patents
Process for debinding and sintering metal injection molded parts made with an aqueous binder Download PDFInfo
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- WO2000012247A1 WO2000012247A1 PCT/US1999/018753 US9918753W WO0012247A1 WO 2000012247 A1 WO2000012247 A1 WO 2000012247A1 US 9918753 W US9918753 W US 9918753W WO 0012247 A1 WO0012247 A1 WO 0012247A1
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- Prior art keywords
- article
- debinding
- binder
- stainless steel
- sintering
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- 239000011230 binding agent Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000005245 sintering Methods 0.000 title claims abstract description 32
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 23
- 239000002184 metal Substances 0.000 title claims abstract description 23
- 230000008569 process Effects 0.000 title claims description 28
- 238000002347 injection Methods 0.000 title claims description 7
- 239000007924 injection Substances 0.000 title claims description 7
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000001746 injection moulding Methods 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 150000004676 glycans Chemical class 0.000 claims description 6
- 229920001282 polysaccharide Polymers 0.000 claims description 6
- 239000005017 polysaccharide Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 229920001817 Agar Polymers 0.000 abstract description 15
- 239000008272 agar Substances 0.000 abstract description 15
- 229910001256 stainless steel alloy Inorganic materials 0.000 abstract description 11
- 229910045601 alloy Inorganic materials 0.000 description 14
- 239000000956 alloy Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000001513 hot isostatic pressing Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
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- 229910000734 martensite Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000004881 precipitation hardening Methods 0.000 description 2
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- 238000000638 solvent extraction Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- VLCLHFYFMCKBRP-UHFFFAOYSA-N tricalcium;diborate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]B([O-])[O-].[O-]B([O-])[O-] VLCLHFYFMCKBRP-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229920000936 Agarose Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000003052 fractional factorial design Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012633 leachable Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000002991 molded plastic Substances 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- This invention relates to a process for debinding and sintering 17-4PH stainless steel and components thereof from metal injection molded powder. More particularly, the invention is directed to a debinding and sintering schedule that attains mechanical properties comparable to cast and wrought 17-4PH components for aerospace and other structural applications. Such components are made by the net shape process of metal injection molding using an aqueous based feedstock binder.
- Stainless steel alloys in the precipitation hardening (PH) class have found ubiquitous application in the aerospace and other high technology industries because of their wide range of mechanical properties. Yield strengths range from 75 to 205 ksi, ultimate strengths from 125 to 220 ksi and elongations from 1 to
- Common alloys include the martensitic 15-5PH , semi-austenitic 17-7PH, and austenitic A-286.
- the martensitic alloy, 17-4PH has the nominal composition of 17Cr-4Ni-4Cu-2Si-Fe(balance) and has widespread application in aerospace applications.
- Stainless steels are typically available in cast or wrought forms but are also available as a powder metallurgy (PM) product.
- PM processing of stainless steel includes press and sinter and metal-injection-molding (MIM). Press and sinter results in a compact of only 80 to 85% dense in the sintered condition and is limited to simple geometric shapes such as cylinders. Additional processing such as hot isostatic pressing (HIP) can bring densities to near 100% of theoretical density.
- HIP hot isostatic pressing
- Metal-injection-molding is recognized as a premier forming method for complex shapes, affording significant advantages over other forming methods due to its capability of rapidly producing net shape, complex parts in high volume.
- MLM comprised the step of mixing metal powder with a dispersant and a thermoplastic organic binder of variable composition.
- the molten powder/binder mixture was heated during the injection molding process and injected into a relatively cold mold. After solidification, the part was ejected in a manner similar to injection-molded plastic parts. Subsequently, the binder was removed and the part was densified by a high temperature heat treatment. There were a number of critical stages in this process including the initial mixing of the powder and binder, the injection of the mixture into the mold, and the removal of the organic matrix material.
- One of the main disadvantages of the initial MEM process is the removal of the organic vehicle.
- Solvent extraction causes difficulties because the remainder still needs to be removed at elevated temperatures, resulting in the formation of porosity throughout the part which allows removal of the remaining organic material.
- part slumping can pose problems, especially for the larger particle sizes if the green density/strength is not high enough.
- MLM offers certain advantages for high volume automation of net shape, complex parts.
- aqueous-based binders contain either polyethylene glycols, PNA copolymers, or COOH-containing polymers.
- BASF has developed a polyacetal- based system that is molded at moderately high temperatures, after which the binder is removed by a heat treatment with gaseous formic or nitric acid. The acid treatment keeps the debind temperature low to exclude the formation of a liquid phase and thus distortion of the green part due to viscous flow.
- the gaseous catalyst does not penetrate the polymer, and the decomposition takes place only at the interface of the gas and binder, thereby preventing the formation of internal defects.
- water serves the role of the fluid medium in the aqueous injection molding process, comprising roughly 50 volume% of the composition, and agar provides the "setting" function for the molded part.
- the agar sets up a gel network with open channels in the part, allowing easy removal of the water by evaporation.
- the Hens et al system requires a solvent debind to attain similar open channels in the part.
- the agar is eventually removed thermally; however, it comprises less than 5 volume fraction of the total formation, and debind times are rapid compared to wax/polymeric debind systems. This is an advantage over the Hens et al system.
- This agar-based aqueous binder is especially applicable for the production of stainless steel components using MLM. Due to the easy removal of the aqueous-based binder and its relatively low level of carbon, as compared to wax or polymeric binder systems, sintering schedules can be developed which impart little or no additional carbon to stainless steel alloys such as 316L, 410L and 17- 4PH. Excessive amounts of carbon, typically above about 0.07wt% for 17-4PH, for example, seriously compromise the mechanical properties and corrosion resistance of stainless steels. Moreover, the agar-based binder and its associated carbon are removed in a simple one-step, air debinding process consisting of relatively short debind times of approximately 1/2 to 2 hours.
- wax or polymer based binders require several step debinding processes in which each debind step often takes many more hours. Accordingly, the short air debind times of the agar-based 17-4PH alloy are economically advantageous.
- the present invention relates to a debinding and sintering process for an article of manufacture made from a metal powder and an aqueous binder in an injection molding process comprising the steps of raising the temperature of an air atmosphere to a value sufficient to decompose the polysaccharide in the aqueous binder, and then sintering at elevated temperatures in a hydrogen atmosphere to reduce oxidation formed on the article during the debinding step.
- This invention is also directed to an injection molding process for a metal powder comprising the following steps: a) injecting a mixture comprising
- the invention further provides a critical air debinding step prior to sintering which results in high densification and minimization of carbon in 17-4PH stainless steel alloy.
- the air debinding step is not limited to 17-4PH or other stainless steels. Rather, it is applicable to all metal powders utilizing the agar-based aqueous binder system.
- this invention also discloses other sintering parameters such as peak sintering temperature and hold time, which in conjunction with the air debinding step, are important in producing injection molded 17-4PH alloy components having mechanical properties comparable to cast or wrought processed material.
- Fig. 1 are Paretto and Main Effects plots from the Statistical Software Package MINITAB which show that of the five factors tested, debinding in an air atmosphere is the most significant factor in minimizing carbon.
- Fig. 2 are similar plots which show that air debinding is significant in maximizing density in excess of 99%.
- Fig. 3 are similar plots which show that debinding in an air atmosphere is significant in maximizing tensile elongation in an unHIPed 17-4PH stainless steel alloy heat treated to the HI 025 condition.
- Fig. 4 is a photograph of a 507 jet engine diffuser vane produced using the agar based feedstock in a 17-4PH stainless steel alloy.
- Example 1 This example describes the criticality of an air debinding step prior to sintering in order to prevent excessive carbon in the 17-4PH stainless steel alloy.
- 17-4PH feedstock was compounded using argon atomized 17-4PH stainless steel powder of minus 20 micrometer size purchased from Ultrafine Metals, Inc.
- the 17-4PH powder was mixed with agar (S-100, Frutarom Meer Corp), water, and calcium borate to have the composition (in wt%) of 92.5% 17-4PH, 1.7 % agar, 5.7 % water, and 0.1% calcium borate.
- Compounding was performed in a sigma blender that was heated to 88°C for 45 minutes, after which the temperature was reduced to 77°C, and mixing continued for another 45 minutes.
- the material was allowed to cool to room temperature, it was shredded using a food processor (Kitchen Aid KSM90) and sieved using a #5 sieve to remove any large and fine shards.
- the shredded feed-stock was dried to a desired solids level by exposing a loose bed of material to the atmosphere. Solids loadings were determined using a moisture balance (Ohaus Corp.).
- Injection molding of the feedstock into tensile specimens was next performed. This was accomplished on a 55 ton Cincinnati Milacron injection molding machine at 85°C using a fill pressure of 200 psi and a mold pressure of 100 psi by forming the feedstock into an epoxy tensile bar mold.
- Such parts after injection molding but before sintering, are referred to as "green" parts.
- the tensile bars were next divided into sixteen batches and run in a 5 factor-2 level fractional factorial design of experiment (DOE), which was analyzed by MINITAB statistical software.
- DOE 5 factor-2 level fractional factorial design of experiment
- the five factors used as inputs and their levels are summarized in Table I.
- the output value for the analysis is the carbon level, with low levels being the desired result.
- a total of sixteen experimental debind/sintering runs were performed in a laboratory tube furnace.
- Fig. 1 shows the Main Effects and Paretto chart from the MINITAB statistical software.
- factors appearing to the right of the dotted line are considered statistically significant, while those to the left are statistically insignificant.
- the Paretto chart clearly indicates that debinding in an air atmosphere as opposed to a hydrogen atmosphere results in a dramatic minimization of carbon.
- the Paretto chart indicates that the sintering time also plays a role in carbon reduction. The magnitude of the effects is shown in the
- Example 2 This example describes the criticality of an air debinding step prior to sintering for 17-4PH stainless steel alloy in order to achieve densities in excess of 99% after sintering.
- Samples were prepared and analyzed using MINITAB, as described in Example 1.
- the Paretto and Main Effects plots using final density as an output are shown in Fig. 2.
- the Paretto chart indicates that the debinding atmosphere is the only significant factor for obtaining maximum density within the factors and levels analyzed in this 16 run experiment. Examination of the main effects plots shows that the air debind produces a maximum of >98% density, while a hydrogen debind shows only a 90% density.
- Example 3 This example describes the criticality of an air debinding step prior to sintering in order to achieve tensile elongations in the range of 9% after sintering in 17-4PH stainless steel alloy heat treated to the HI 025 condition.
- Samples were prepared and analyzed using MINITAB, as described in Example 1.
- the Paretto and Main Effects plots using tensile elongation as an output are shown in Fig. 3.
- the Paretto chart indicates that the debinding atmosphere is the only significant factor for obtaining maximum tensile elongation within the factors and levels analyzed in this 16 run experiment. Examination of the Main Effects plots shows that the air debind results in a maximum of >10% tensile elongation, while debinding in a hydrogen atmosphere produces only a 2% elongation.
- Example 4 This example shows that a sintering run using the optimized parameters from the 16 level DOE described in Example 1 will result in as-sintered, HI 025 treated MIM 17-4PH material having tensile properties comparable to HI 025 treated 17-4PH produced conventionally by either cast or wrought processing.
- the tensile properties for material produced by these three methods are listed in Table II.
- the MLM 17-4PH alloy test bars of this example represent the average of three tests. Wrought and cast minimums listed in Table II are from the Aerospace Structural Metals Handbook.
- This example shows the beneficial effect of using a HIP treatment after sintering but before austenization and aging.
- Nine test bars fabricated as in Example 4 were HTPed using the standard industrial HIP cycle of 15 ksi argon pressure at 1162°C for 4 hours after sintering. The samples were then austenitized and given the HI 025 treatment described previously.
- the tensile results are listed in Table III along with BROWSE data for cast and wrought processed 17-4PH in the HI 025 condition.
- Table III includes the average minus three sigma values that are an indication of variability in properties from sample to sample. For aerospace applications, average minus 3 sigma values are used for qualification. The tensile elongation average minus 3 sigma values are significantly higher for the HJPed MLM specimens than for the cast specimens.
- FIG. 4 shows a photograph of a 507 diff ⁇ ser vane for an Allied Signal jet engine.
- the vane was made in a manner similar to the tensile bars of Example 1.
- the epoxy mold employed was that of the diffuser vane instead of the tensile bar mold.
- Example 7 This example illustrates that low carbon levels can be achieved in samples having various cross sectional thicknesses. Alloy 17-4PH was prepared as described in Example 1 , except that five step samples were molded instead of tensile bars. The five step samples are designed to test the variation of properties with respect to thickness and consist of five sections, each having a greater thickness than the preceding section. Table IV lists the carbon, oxygen and nitrogen values from a five step sample in which thickness varied from 0.882 inches to 0.048 inches. The table reveals carbon levels below 0.04 wt% even for the thickest section of sample.
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- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
- Sealing Material Composition (AREA)
Abstract
Description
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Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002342176A CA2342176A1 (en) | 1998-08-27 | 1999-08-19 | Process for debinding and sintering metal injection molded parts made with an aqueous binder |
AU54911/99A AU5491199A (en) | 1998-08-27 | 1999-08-19 | Process for debinding and sintering metal injection molded parts made with an aqueous binder |
JP2000567331A JP2002523629A (en) | 1998-08-27 | 1999-08-19 | Debinding and sintering method for metal injection molded parts made using aqueous binder |
DE69916633T DE69916633D1 (en) | 1998-08-27 | 1999-08-19 | METHOD FOR BINDING AND SINTERING INJECTION MOLDED OBJECTS MADE WITH AN AQUEOUS BINDING AGENT |
EP99941217A EP1113893B1 (en) | 1998-08-27 | 1999-08-19 | Process for debinding and sintering metal injection molded parts made with an aqueous binder |
AT99941217T ATE264725T1 (en) | 1998-08-27 | 1999-08-19 | METHOD FOR DEBONDING AND SINTERING INJECTION-MOLDED OBJECTS PRODUCED WITH AN AQUEOUS BINDER |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/141,444 | 1998-08-27 | ||
US09/141,444 US5985208A (en) | 1998-08-27 | 1998-08-27 | Process for debinding and sintering metal injection molded parts made with an aqueous binder |
Publications (1)
Publication Number | Publication Date |
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WO2000012247A1 true WO2000012247A1 (en) | 2000-03-09 |
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ID=22495723
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/US1999/018753 WO2000012247A1 (en) | 1998-08-27 | 1999-08-19 | Process for debinding and sintering metal injection molded parts made with an aqueous binder |
Country Status (9)
Country | Link |
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US (1) | US5985208A (en) |
EP (1) | EP1113893B1 (en) |
JP (1) | JP2002523629A (en) |
CN (1) | CN1325331A (en) |
AT (1) | ATE264725T1 (en) |
AU (1) | AU5491199A (en) |
CA (1) | CA2342176A1 (en) |
DE (1) | DE69916633D1 (en) |
WO (1) | WO2000012247A1 (en) |
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- 1999-08-19 CA CA002342176A patent/CA2342176A1/en not_active Abandoned
- 1999-08-19 JP JP2000567331A patent/JP2002523629A/en not_active Withdrawn
- 1999-08-19 CN CN99812761.2A patent/CN1325331A/en active Pending
- 1999-08-19 AU AU54911/99A patent/AU5491199A/en not_active Abandoned
- 1999-08-19 AT AT99941217T patent/ATE264725T1/en not_active IP Right Cessation
- 1999-08-19 EP EP99941217A patent/EP1113893B1/en not_active Expired - Lifetime
- 1999-08-19 DE DE69916633T patent/DE69916633D1/en not_active Expired - Lifetime
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EP0503966A2 (en) * | 1991-03-14 | 1992-09-16 | Fujitsu Limited | Process for production of sintered body |
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JP2003027105A (en) * | 2001-04-25 | 2003-01-29 | Extrude Hone Corp | Binder composition |
JP2012107026A (en) * | 2001-08-14 | 2012-06-07 | Medipost Co Ltd | Composition for treating articular cartilage damage |
Also Published As
Publication number | Publication date |
---|---|
ATE264725T1 (en) | 2004-05-15 |
CN1325331A (en) | 2001-12-05 |
CA2342176A1 (en) | 2000-03-09 |
EP1113893A1 (en) | 2001-07-11 |
JP2002523629A (en) | 2002-07-30 |
DE69916633D1 (en) | 2004-05-27 |
US5985208A (en) | 1999-11-16 |
EP1113893B1 (en) | 2004-04-21 |
AU5491199A (en) | 2000-03-21 |
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