EP0269612B1 - Procédé pour la fabrication d'articles - Google Patents
Procédé pour la fabrication d'articles Download PDFInfo
- Publication number
- EP0269612B1 EP0269612B1 EP19870890270 EP87890270A EP0269612B1 EP 0269612 B1 EP0269612 B1 EP 0269612B1 EP 19870890270 EP19870890270 EP 19870890270 EP 87890270 A EP87890270 A EP 87890270A EP 0269612 B1 EP0269612 B1 EP 0269612B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- metal
- alloy
- particles
- process according
- oxygen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000000034 method Methods 0.000 title claims description 43
- 238000004519 manufacturing process Methods 0.000 title description 6
- 229910052751 metal Inorganic materials 0.000 claims description 73
- 239000002184 metal Substances 0.000 claims description 73
- 239000002245 particle Substances 0.000 claims description 46
- 239000000843 powder Substances 0.000 claims description 42
- 229910045601 alloy Inorganic materials 0.000 claims description 39
- 239000000956 alloy Substances 0.000 claims description 39
- 238000005245 sintering Methods 0.000 claims description 30
- 239000001301 oxygen Substances 0.000 claims description 25
- 229910052760 oxygen Inorganic materials 0.000 claims description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 23
- 239000000654 additive Substances 0.000 claims description 21
- 150000002739 metals Chemical class 0.000 claims description 17
- 230000000996 additive effect Effects 0.000 claims description 14
- 150000002927 oxygen compounds Chemical class 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 229910000997 High-speed steel Inorganic materials 0.000 claims description 6
- 150000002736 metal compounds Chemical class 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 230000001788 irregular Effects 0.000 claims description 3
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 238000009692 water atomization Methods 0.000 claims description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 2
- 125000005595 acetylacetonate group Chemical group 0.000 claims description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 2
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 2
- 125000001485 cycloalkadienyl group Chemical group 0.000 claims description 2
- 125000002188 cycloheptatrienyl group Chemical group C1(=CC=CC=CC1)* 0.000 claims description 2
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 150000003891 oxalate salts Chemical class 0.000 claims description 2
- 230000036961 partial effect Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000005056 compaction Methods 0.000 claims 3
- -1 cyclooctadienyl Chemical group 0.000 claims 2
- 230000001747 exhibiting effect Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 238000007906 compression Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 230000006835 compression Effects 0.000 description 8
- 238000000465 moulding Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- FSJSYDFBTIVUFD-SUKNRPLKSA-N (z)-4-hydroxypent-3-en-2-one;oxovanadium Chemical compound [V]=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FSJSYDFBTIVUFD-SUKNRPLKSA-N 0.000 description 4
- 239000002775 capsule Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- FAQSSRBQWPBYQC-UZUXQKAQSA-N dioxomolybdenum;(z)-4-hydroxypent-3-en-2-one;(e)-4-hydroxypent-3-en-2-one Chemical compound O=[Mo]=O.C\C(O)=C\C(C)=O.C\C(O)=C/C(C)=O FAQSSRBQWPBYQC-UZUXQKAQSA-N 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005496 tempering Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001347 Stellite Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000000304 alkynyl group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- AHICWQREWHDHHF-UHFFFAOYSA-N chromium;cobalt;iron;manganese;methane;molybdenum;nickel;silicon;tungsten Chemical compound C.[Si].[Cr].[Mn].[Fe].[Co].[Ni].[Mo].[W] AHICWQREWHDHHF-UHFFFAOYSA-N 0.000 description 1
- XEHUIDSUOAGHBW-UHFFFAOYSA-N chromium;pentane-2,4-dione Chemical compound [Cr].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O XEHUIDSUOAGHBW-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006735 deficit Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012048 reactive intermediate Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
Definitions
- the invention relates to a method for the powder-metallurgical production of moldings for tools, machine parts, articles of daily use with metals or metal alloys, powder-fine particles of the alloy components and / or master alloys and / or the alloy itself being mixed with at least one additive containing a metal and at least with heating to be compressed into a desired shaped body.
- Powder metallurgy is particularly well suited for the production of tools, machine parts and articles of daily use for economic reasons.
- Their advantage is that, starting from metal powders, a porous body is produced by mechanical pressing, which is then compressed to the final shape during a so-called sintering.
- Sintering is generally understood to mean the caking of powder particles under the action of heat in an oven. In many cases, the air-filled pores originally present in the powder compact are removed. This process is very badly affected by the oxygen content of the powder. The oxygen content on the surface of the powder particles in particular has a sinter-inhibiting effect and leads to porosities and inadequate mechanical properties.
- GB-PS 2 084 612 describes e.g. a method for producing a workpiece from gas-atomized powder with low oxygen content, which is characterized in that the powder is ground. The ground powder is then mixed with a pressing aid, pressed to a shaped body, sintered and hot isostatically compressed. The disadvantage of this process is still the use of the expensive gas-atomized powder, which can only be ground with great effort into a uniformly compressible fine powder.
- Water atomized powders have the advantage that they have irregular shapes and can therefore be pressed well into preform bodies. However, they have the disadvantage that they contain a relatively large amount of oxide (700 to 1500 ppm) or are surrounded by an oxide layer which hinders the sintering process and causes porosity.
- a process for the production of sintered blanks for rolling or forging by a powder metallurgical process, in particular the evaporation of alloy components during a tempering and sintering process of the metal powder is known from DE-A-2 461 736.
- an additive containing a metal from the group of alkali metals and alkaline earth metals is added to a mechanically produced powder and the mixture is left at a temperature which is higher than the decomposition temperature of the additive to soften the powder grain material.
- the mixture is then compacted and sintered.
- the alkali metal-containing additive should be broken down under the influence of heat to form a uniform solid solution in the form of the alkali metal or in the form of an oxide on the surface of the metal particles.
- this surface layer improves the sliding properties of the powder particles to one another and leads to a dense green blank
- an azeotropic mixture is formed, for example with zinc, which prevents evaporation losses and accelerates the sintering process.
- the object of the invention is to design a method of the type mentioned in such a way that a shaped body is obtained in a labor and energy-saving manner, the sintering properties of which are optimal and whose porosity is minimal.
- this is achieved in that surface oxygen-containing particles or powders are brought into contact with at least one compound of at least one metal as an additive, which, at temperatures of 50 to 800 ° C., has at least one alloy-specific or alloy-compatible metal and / or releases a substoichiometric oxygen compound of such a metal with respect to oxygen, after which the final compression of the particles into the shaped body takes place at least with heating or with sintering with at least partial dissolution (breaking up) of the surface oxygen layer of the powder grains.
- This makes it possible to produce moldings that have practically no porosity and excellent mechanical properties. Sintering at low temperatures is also possible, i.e.
- the additives used according to the invention have the effect that the ease of sintering of the shaped body components is increased; the additives bring about an improvement in diffusion at the particle boundaries, so that the achievable sintered composite is improved.
- the additives used according to the invention When heated as a result of decomposition, the additives used according to the invention release metal atoms or metal oxygen compounds whose oxygen content is substoichiometric, that is to say which contain oxygen in deficit, and which combine with the oxygen of oxides or oxide layers present on the particles or tear these layers apart. This creates metallic contact between the particles so that they can optimally sinter together. At the same time, the oxygen torn from the oxide compound reacts more easily to CO or CO2 with the carbon contained in the structure. The resulting metallic contact leaves a decrease in the sintering temperature. Obtained from preforms with 700 to 1500 ppm O2 moldings with max. 50 to 100 ppm O2.
- the densities of sintered bodies achieved to date from about 99.5% to 99.8% based on the The maximum achievable density is increased and the densities of moldings produced by the process according to the invention are more than 99.8%.
- the temperatures for the compression of the preforms are somewhat below the temperatures currently customary for the respective metals of the alloys. In the method according to the invention, the use of temperatures about 5 to 10 ° lower is possible, which makes the sintering process much more manageable compared to temperature fluctuations in the sintering furnace; sintering is currently taking place just below the melting point of the respective eutectic compounds.
- particles obtained with water atomization optionally with an addition of up to max. 50% of gas atomized and / or ground particles, a metal, an alloy or pre-alloy with an irregular shape and size are used. Together with the irregularly shaped water-atomized particles, other particles can also be used, and a preform can be produced well and precisely due to the possible plastic deformation of the particles. Due to the addition of the additive, it is possible that particles or powders containing surface oxygen are also used. To form the preform body, it is expedient if the particles are subjected to a preform body formation after the addition of the additive with the application of pressure and / or temperature. The additive contributes to the cohesion of the particles.
- a durable preform and a structure with a good structure are obtained when the particles are combined with the metal by mixing, in particular Stir, be brought into contact, preferably the entire surface of the particles being contacted, in particular wetted, with the compound of the metal.
- the particles can be intimately bonded over their entire surface during sintering. Mixing can take place in known mixing devices.
- the compound of the metal is brought into contact with the particles in a solid or fluid state at room temperature or in a state dissolved in a solvent.
- An addition of a gaseous compound of a metal to the particles can be carried out as well as an admixture of powdery particles of a compound of a metal to the particles to be sintered.
- the solvent of the compound of the metal is expediently evaporated off before the preform is formed.
- the heating directly adjoins the preform formation or the evaporation of the solvent for the final compression.
- the sintering process or the compression to form the shaped body follows the production of the preform directly following the admixing of the connection of a metal or the evaporation of the solvent that may be necessary without any further intermediate step; further reactive intermediate steps are also not required, which makes the procedure simple.
- particles of tool steels are advantageously used ledeburitic cold work steels, high temperature or sintered alloys based on Ni and / or Co or the like. used. After sintering, the particles form the corresponding steels or alloys with a standardized composition.
- the released metal (s) or the oxygen compound (s) which is substoichiometric with respect to oxygen comprises metals or oxygen compounds of metals from the group Fe, Co, Ni, Cr , Mo, W, Ta, Nb, V, Ti Zr, Hf, Al, Si.
- the process becomes particularly simple with good results if, preferably in an organic solvent, dissolved complex, addition and / or coordination compounds of at least one alloy-specific or alloy-compatible metal, preferably with zero valence, are used.
- Such compounds of metals release the metal or the oxygen-sub-stoichiometric metal compound at a relatively low temperature, and the connection residues leave the heated preform body relatively unhindered even before the compression process begins. It is expedient if the residues of the compound of the metal after release of the metal or the oxygen compound which is substoichiometric with respect to oxygen in the course of the temperature increase before reaching the compression temperature from the preform body, for example be removed by applying a vacuum.
- the procedure according to the invention is carried out as follows: Particles of at least one metal or a metal alloy are mixed with at least one compound of an alloy-specific or alloy-compatible metal which, when heated, releases a metal or a compound of the metal which is substoichiometric with respect to oxygen.
- the particles can be water-atomized metal powder, which to a certain extent, preferably 50%, is also gas-atomized or produced in another way or may contain pretreated powders. These particles are intimately mixed with the dissolved compound, for example by stirring, the particles being well wetted; after evaporation of the solvent, a layer of the compound should be deposited in molecular thickness on the particles. The particles are then pressed under pressure to form a preform.
- the preform is pressed in a press mold, which is also the sintered mold, and has a density of 80%.
- This preform is then heated to the compression temperature without further treatment, the connection being disassembled when heated.
- the metals released remain in the structure and the connection residues, in particular organic components, leave the preform body.
- the sintering temperature is reached, there is only the alloy structure that is sintered, since the organic components are selected such that they have left the structure before the main shrinkage process and have already released the reactive metal atoms and sub-stoichiometric oxygen compounds.
- Evaporation of the solvent is carried out by means of a vacuum or vacuum, if appropriate using protective gas, as is heating of the preform and compression or sintering.
- one or more compounds of one or more metals can be added to the particles to be compressed, which each give off one or more metal (s) or one or more oxygen substoichiometric oxygen compound (s) of a metal when heated.
- the particles to be compacted also have substances which improve the compression or sintering properties, for example, before, after or simultaneously with the addition of the compound of a metal. Paraffin or others can be added.
- a commercially available water-atomized high-speed steel powder with the material number 1.3343 and an oxygen content of 710 ppm was intimately mixed with 0.3% by weight of vanadyl acetylacetonate and with mineral spirits in a planetary mill. Then 1.5 wt .-% paraffin was added as a pressing or sintering aid and distributed homogeneously. After the solvent had been evaporated off, the powder was mechanically pressed into shaped bodies in a die at 5000 bar and then sintered under vacuum. The sintering conditions were 1235 ° C with a holding time of 30 minutes. The sintered density of the shaped body was 8.12 g / cm 3. The flexural strength was over 2000 N / mm2. The oxygen content was 20 ppm. The comparative body sintered without the additive according to the invention could only achieve a density of 8.00 g / cm 3 and a 20% lower bending strength.
- a commercially available water-atomized high-speed steel powder with the material number 1.3215 was added with 0.5% cobalt acetylacetonate, 1% molybdenyl acetylacetonate and mixed with benzene in a planetary mill and then dried in a desiccator.
- the mechanical pressing was carried out at 5500 bar.
- the size of the moldings was 5 x 5 x 45 mm. Vacuum sintering of the pressed moldings took place at 1250 ° C., the holding time was 1 hour.
- the density of the sintered body, to which the additives according to the invention were fed, could be increased by 0.15 g / cm3 compared to the comparison body produced without additives.
- the flexural strength of the molded article produced according to the invention was 25% higher than that of the comparative article.
- a commercially available water-atomized high-speed steel powder with the material number 1.3343 was mixed according to the invention with 0.5% by weight molybdenyl acetylacetonate, 0.5% by weight vanadyl acetylacetonate and 0.3% by weight aluminum acetylacetonate and benzene. After the solvent had been evaporated off, the dry powder was pressed in a mechanical press at 5000 bar to form inserts with the ISO designation SPGN 120308. The green compacts were sintered at 1240 ° C. and in vacuo for 30 min. The carbon content of the sintered alloy after sintering was 0.91% by weight and the oxygen content was 20 ppm. The residual porosity was less than 0.1% by volume. The comparison body sintered without additives showed a lower carbon content and a residual porosity of 0.7% by volume. A wear test using the grinding wheel method gave the following results in specific weight loss (%):
- the cutting inserts according to the invention showed a significant improvement in wear behavior.
- a mixture of a high-speed steel powder with the material number 1.3343 consisting of 50% water atomized and 50% gas atomized parts was produced and investigated in accordance with the conditions of Example 3.
- the following tool life was determined in the machining test at a cutting speed of 40 m / min, a cutting depth of 2 mm and a feed of 0.23 mm / rev on a tempering steel with material number 1.6582 and a hardness of 230 HB 30:
- Water-atomized powder based on cobalt (stellite 6) was mixed with 1% by weight of vanadyl acetylacetonate, 0.1 % By weight of aluminum acetylacetonate and 0.1% by weight of chromium acetylacetonate dissolved in acetone mixed in a stirrer.
- the dried powder was pressed into molds in a die at 6000 bar and sintered in a vacuum oven at 1290 ° C. with a holding time of 60 min.
- the residual porosity of the sintered body provided with the additive according to the invention was less than 0.1% by volume, while the comparison body produced without additive had a residual porosity of 12.1%.
- Water-atomized powder with the material number 1.2379 was mixed according to the invention with 0.3% by weight molybdenyl acetylacetonate, 1% by weight vanadyl acetylacetonate and benzene in a planetary mill and then dried under vacuum and mechanically pressed to give shaped bodies.
- the sintering took place at 1210 ° C. and a holding time of 1 hour.
- the residual porosity was below 0.2 vol%.
- the comparison body produced without additives showed a residual porosity of 3.8% by volume.
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Claims (16)
- Procédé pour la fabrication par métallurgie des poudres de corps de forme pour des outils, des pièces de machines, des objets usuels comportant des métaux ou des alliages métalliques, des particules en poudre fine des composants de l'alliage et/ou des préalliages et/ou de l'alliage même étant mélangées avec au moins un produit d'addition contenant un métal et compressées, au minimum sous chauffage, pour arriver au corps de forme désiré, tandis que des particules ou de la poudre renfermant de l'oxygène en surface sont amenées en contact avec au minimum un composé d'au moins un métal comme produit d'addition, lequel composé, à des températures de 50 à 800°C, libère au moins un métal propre à l'alliage ou compatible avec celui-ci et/ou un composé substoechiométrique par rapport à l'oxygène d'un tel métal,après quoi, au minimum sous chauffage ou par frittage, avec décomposition (rupture) partielle au moins de la couche d'oxygène superficielle des grains de poudre, a lieu la compression finale des particules pour arriver au corps de forme.
- Procédé selon la revendication 1, caractérisé en ce que les particules, après addition du produit d'addition, sous charge de pression ou de température, sont soumises à un préformage du corps de forme.
- Procédé selon la revendication 1 ou 2, caractérisé en ce que l'on met en oeuvre au moins en partie des poudres qui sont préparées par pulvérisation dans l'eau.
- Procédé selon l'une des revendications 1 à 3, caractérisé en ce que les particules sont amenées au contact avec le composé du métal par mélange, mélange liquide notamment, toute la surface des particules étant de préférence mise en contact, imprégnée en particulier, avec le composé du métal.
- Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le composé du métal est amené en contact avec les particules à l'état soit solide soit liquide à la température ambiante ou à l'état dissous dans un solvant.
- Procédé selon la revendication 5, caractérisé en ce que le solvant du composé du métal est concentré avant le préformage du corps de forme.
- Procédé selon l'une des revendications 1 à 6, caractérisé en ce que le chauffage pour la compression finale fait directement suite au préformage du corps de forme ou à la concentration du solvant.
- Procédé selon l'une des revendications 1 à 7, caractérisé en ce que le métal ou les métaux libéré(s) ou le(s) composé(s) oxygéné(s) substoechiométrique(s) par rapport à l'oxygène d'un métal ou de métaux ou les composés oxygénés de métaux sont du groupe Fe, Co, Ni, Cr, Mo, W, Ta, Nb,V,Ti, Zr, Hf, Al, Si.
- Procédé selon l'une des revendications 1 à 8, caractérisé en ce que l'on utilise des particules obtenues par pulvérisation dans l'eau, comportant éventuellement un apport jusqu'à 50% max. de particules obtenues par pulvérisation dans un gaz et/ou broyées, d'un métal, d'un alliage ou d'un préalliage, avec des particules de forme et de taille irrégulières.
- Procédé selon l'une des revendications 1 à 9, caractérisé en ce que l'on utilise des particules d'aciers à outils, aciers à coupe rapide notamment, d'aciers ledeburitiques pour travail à froid, d'alliages à haute température ou frittés à base de Ni et/ou de Co ou analogues.
- Procédé selon l'une des revendications 1 à 10, caractérisé en ce que l'on utilise, dissous de préférence dans un solvant organique, des composés complexes, d'addition et/ ou de coordination, d'au moins un métal propre à l'alliage ou compatible avec celui-ci, de valence nulle de préférence.
- Procédé selon l'une des revendications 1 à 11, caractérisé en ce que l'on utilise, le cas échéant exclusivement, des composés présentant des groupes carbonyles, des oxalates par exemple, de métaux propres à l'alliage ou compatibles avec celui-ci.
- Procédé selon l'une des revendications 1 à 12, caractérisé en ce que l'on utilise, le cas échéant exclusivement, des (cyclo)alkyles, des (cyclo)alkényles ou alkinyles, par exemple de l'alkyle C₁-C₅, de l'allyle, du cycloalkadiènyle, du cyclopentadiènyle, du cycloheptatriènyle, du cyclooctadiènyle, de métaux propres à l'alliage ou compatibles avec celui-ci.
- Procédé selon l'une des revendications 1 à 3, caractérisé en ce que l'on utilise, dissous de préférence dans des solvants organiques, des acétylacétonates des métaux propres à l'alliage ou compatibles avec celui-ci, de Co, Ni, Cr, Mo et/ou V de préférence.
- Procédé selon l'une des revendications 1 à 14, caractérisé en ce que l'acétylacétonate du métal propre à l'alliage ou compatible avec celui-ci, l'acétylacétonate de Co notamment, est utilisé, rapporté au métal qu'il contient, dans des proportions de 0,05 à 0,8 % en poids, dans une proportion de 0,08 à 0,2 % en poids de préférence, des particules employées.
- Procédé selon l'une des revendications 1 à 15, caractérisé en ce que les restes du composé du métal, après libération du métal ou du composé oxygéné substoechiométrique par rapport à l'oxygène, sont lors de l'élévation de température, avant obtention de la température de compression, éliminés du préformage du corps de forme, par réalisation de vide par exemple.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT3178/86 | 1986-11-28 | ||
| AT317886A AT388124B (de) | 1986-11-28 | 1986-11-28 | Verfahren zur herstellung von formkoerpern |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0269612A2 EP0269612A2 (fr) | 1988-06-01 |
| EP0269612A3 EP0269612A3 (en) | 1989-08-09 |
| EP0269612B1 true EP0269612B1 (fr) | 1992-11-11 |
Family
ID=3546560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP19870890270 Expired - Lifetime EP0269612B1 (fr) | 1986-11-28 | 1987-11-26 | Procédé pour la fabrication d'articles |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0269612B1 (fr) |
| AT (1) | AT388124B (fr) |
| DE (1) | DE3782618D1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10224738B4 (de) * | 2001-06-05 | 2011-07-28 | DENSO CORPORATION, Aichi-pref. | Stromführendes Element für einen Gleichstrommotor bei einer Kraftstoffpumpe, Verfahren zum Herstellen von selbigem und Kraftstoffpumpe |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1180948B (de) * | 1957-04-02 | 1964-11-05 | Onera (Off Nat Aerospatiale) | Verfahren zur Herstellung eines kompressiblen, fuer pulvermetallurgische Zwecke geeigneten Pulvers aus Chrom oder einer Chromlegierung |
| DE1458360A1 (de) * | 1963-09-02 | 1969-01-09 | Deutsche Edelstahlwerke Ag | Verfahren zum Sintern und Waermebehandeln von Werkstuecken aus Metallen mit hoher Sauerstoffaffinitaet |
| GB1329246A (en) * | 1970-10-30 | 1973-09-05 | Bandstahlkombinat Veb | Process for the production of alloyed iron powder mixture |
| US4029475A (en) * | 1973-12-31 | 1977-06-14 | Kabushiki Kaisha Hamai Seisakusho | Blank for rolling and forging and method of producing same |
| US4028063A (en) * | 1974-11-11 | 1977-06-07 | Gte Laboratories Incorporated | Compacts for preparing silver-cadmium oxide alloys |
| FR2308691A1 (fr) * | 1975-04-23 | 1976-11-19 | Cime Bocuze | Nouveau procede de preparation par frittage d'alliages a base de molybdene |
| SE8105681L (sv) * | 1980-10-01 | 1982-04-02 | Uddeholms Ab | Forfarande for framstellning av foremal med forutbestemd form |
-
1986
- 1986-11-28 AT AT317886A patent/AT388124B/de not_active IP Right Cessation
-
1987
- 1987-11-26 EP EP19870890270 patent/EP0269612B1/fr not_active Expired - Lifetime
- 1987-11-26 DE DE8787890270T patent/DE3782618D1/de not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10224738B4 (de) * | 2001-06-05 | 2011-07-28 | DENSO CORPORATION, Aichi-pref. | Stromführendes Element für einen Gleichstrommotor bei einer Kraftstoffpumpe, Verfahren zum Herstellen von selbigem und Kraftstoffpumpe |
Also Published As
| Publication number | Publication date |
|---|---|
| DE3782618D1 (de) | 1992-12-17 |
| ATA317886A (de) | 1988-10-15 |
| EP0269612A3 (en) | 1989-08-09 |
| EP0269612A2 (fr) | 1988-06-01 |
| AT388124B (de) | 1989-05-10 |
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