EP0633083B1 - Poudre métallique pour la réalisation de pièces par compression et frittage et procédé d'obtention de cette poudre - Google Patents
Poudre métallique pour la réalisation de pièces par compression et frittage et procédé d'obtention de cette poudre Download PDFInfo
- Publication number
- EP0633083B1 EP0633083B1 EP94420188A EP94420188A EP0633083B1 EP 0633083 B1 EP0633083 B1 EP 0633083B1 EP 94420188 A EP94420188 A EP 94420188A EP 94420188 A EP94420188 A EP 94420188A EP 0633083 B1 EP0633083 B1 EP 0633083B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- granules
- metallic powder
- gelatin
- powder
- particles
- 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
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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/35—Iron
Definitions
- the metal powder which is the subject of the invention relates to the production of parts by compression and sintering from stainless steels, other metals or alloys stainless or refractory and alloy steel, intended for the production of parts quality.
- metal powders by spraying a metal or alloy liquid by means of a gas jet which can be, for example, a neutral gas such as argon or nitrogen or any suitable gas.
- a gas jet which can be, for example, a neutral gas such as argon or nitrogen or any suitable gas. This gives powders having a much lower oxide content than powders obtained by spraying water and which thus have substantially the same purity as the starting metal.
- the elementary particles of these powders have a substantially shaped spherical but in the state is not easily shaped.
- these powders allow, after compression and sintering, to obtain by compression of parts having an apparent density at least equal to that allow to obtain the usual angular powders.
- the raw part obtained from spherical particles has a mechanical resistance often insufficient to allow its manipulation and in particular its ejection from the mold, then transfer to the sintering furnace, without chipping or cracking.
- Patent application GB 2 228 744 describes a similar method for joining together elements of alloys such as graphite, phosphorus or others with a base metal. According to this method, a mixture of an acrylic acid ester is used as binder with a methacrylic acid ester and an unsaturated polymerizable acid.
- the aim is to avoid the segregation of finer or lighter particles such as graphite or others compared to a base metal, such as iron, by bonding these particles between them.
- a paste is made by mixing metallic powder, lubricant of the stearate type, of cellulose gum and water, this paste is injected into a cold compaction mold, optionally drying and carrying out an operation of debinding - sintering of the raw parts obtained.
- Such operations require wet pulp injection equipment which are similar to those of plastic injection molding and are different from cold powder compaction equipment.
- the metal powder according to the invention consists of a set of granules each comprising a group of elementary metallic particles of shape spherical agglomerated with gelatin at a content of at least 0.5% of the weight of metallic powder.
- the spherical particles are advantageously obtained by a spraying process, by means of a gas which can be air or a neutral or reducing gas such as N 2 , H 2 , NH 3 , Ar, or other, of a metal or liquid alloy.
- a gas which can be air or a neutral or reducing gas such as N 2 , H 2 , NH 3 , Ar, or other, of a metal or liquid alloy.
- the main metals or alloys that can be used are, for example, stainless steels, stainless or refractory metals or alloys or alloy steels with high mechanical characteristics.
- the dimensions of these particles and those of the granules are chosen mainly according to the dimensions and characteristics in particular of density of the molded parts that it is to realise.
- each granule contains a sufficient number of spherical particles agglomerated by the gelatin. he these granules must also be able to correctly fill the mold in its every corner. However, a certain number of granules can be formed isolated elementary particles coated with gelatin without affecting the quality of the final product obtained.
- a maximum diameter "d 1 " of the elementary spherical particles and a maximum width "d 2 " of the granules obtained are determined. It is found that the powder according to the invention must preferably have a ratio of d 2 / d 1 ⁇ 3 so that the cold-pressure molded parts reach sufficient mechanical strength.
- this ratio d 2 / d 1 can reach at least 4 or more.
- a maximum width "d 2 " of the granules of 300 microns constitutes a lower limit.
- the gelatin content should be determined based on the average size of the elementary spherical particles which are agglomerated by gelatin. This content also depends on the jelly strength of the gelatin. This jelly force is expressed in Bloom (standardized unit) and can vary between 50 and 250 blooms depending on the gelatin used.
- the granules of which the elementary spherical particles are agglomerated by means of gelatin, do not stick to the walls of the molds, even when the latter heat up to temperatures of 100 ° C or higher, lubrication by a small amount of Zn stearate or other suitable lubricant can be used.
- the invention also relates to the process for preparing a metal powder based on of elementary spherical particles suitable for cold forming by compression then sintering.
- an agglomeration is carried out in granules of the particles elementary spherical.
- the amount of water used being in the range of two to five times the amount of gelatin and the temperature of the water being 40 to 80 ° C.
- the amount of gelatin to be used work depends on the size of the elementary spherical particles and also on the strength in gelatin jelly.
- the mixture of elementary particles and gelatin solution the time necessary to obtain the wetting of the particles metal and during cooling the gradual formation of a gel.
- Granules are thus formed, the drying of which is continued until elimination, preferably as complete as possible, water.
- We end the operation preferably, by a final calibration which allows to individualize the granules by separating from each other and also giving them relatively dimensions regular.
- the amount of gelatin contained in the granules is at least 0.5% of the weight of the metallic powder obtained.
- the fines can be separated by a suitable opening sieve. It is noted that if the maximum diameter "d 1 " of the elementary spherical particles and the width "d 2 " of the granules obtained after drying are in a ratio d 2 / d 1 at least equal to 3 and, preferably, equal to or greater than 4, parts can be obtained by cold compression in a mold whose raw mechanical strength is much higher than in the case of the same powder with spherical particles not agglomerated into granules.
- a lubricant such as zinc stearate.
- this lubricant and the gelatin are removed by preheating the part. raw compressed at a temperature generally between 300 and 500 ° C.
- Preheating can be carried out in air or in the presence of a neutral or reducing gas such as Ar, H 2 , NH 3 or the like. After complete elimination of the gelatin and of the lubricant, if any, sintering is carried out at a temperature appropriate to the material to obtain the desired densification.
- a neutral or reducing gas such as Ar, H 2 , NH 3 or the like.
- the examples below describe, without limitation, the characteristics of the metallic powder agglomerated into granules based on spherical particles elementary suitable for cold compression forming and subsequent sintering the invention.
- the examples also describe, without limitation also, a mode for producing such an agglomerated powder and an embodiment of this powder for making parts by compression in a mold then sintering.
- Example 1 - This example relates to the process according to the invention for preparation of a metallic powder agglomerated into granules from spherical particles elementary which has the properties according to the invention of aptitude for forming by cold compression and sintering.
- Spherical particles obtained in known manner are used atomization by a neutral gas of a stainless steel bath whose composition corresponds to grade 316 defined by the ASTM standard.
- a batch is prepared by sieving of these particles, the particle diameter of which is not more than 106 microns.
- An aqueous solution based on deionized water containing by weight 30% is prepared a gelatin whose jelly strength is 50 blooms. We heat the solution between 50 and 70 ° C to completely dissolve the gelatin.
- a mixture is produced containing 95% of 316 steel particles of not more than 106 microns in diameter and 5% aqueous solution, or 1.5% by weight of gelatin. We must make an intimate mixture in order to wet the entire surface of the elementary particles.
- Granules are thus obtained.
- the drying of these by cold or hot air is continued then a second sieving is carried out in order to separate the granules from each other of the others and to calibrate them by passing through a 500 micron mesh screen.
- Granules are thus obtained whose dimensional ratio is at least 4.7 compared to the maximum diameter of metallic particles.
- These dried granules are made up of agglomerated spherical metallic particles, firmly linked between them by gelatin films, certain granules can however be constituted by isolated elementary particles coated with gelatin.
- the powder thus agglomerated into granules is capable of forming by cold compression in a mold of parts having raw mechanical strength much higher than that obtained with the starting metal particles.
- Adding a small amount of a lubricant to the agglomerated powder in granules such as zinc stearate further facilitates forming.
- the release is also facilitated by the fact that the solidified gelatin does not stick to the walls of the molds when these are heated.
- the agglomerated powder in granules according to the invention is produced, added with about 0.75% by weight of zinc stearate a series of test tubes cold compression tensile in a mold according to standard ASTM B312 under two different compression ratios of 314 and 422 MPa.
- a comparative test is made on the same grade of stainless steel 316 using spherical particles having a maximum diameter of not more than 150 microns.
- Agglomeration with gelatin is carried out with the same concentrations of gelatin and the same sieving conditions as above, the diameter of the granules obtained not exceeding 500 microns.
- the dimensional ratio between granules and spherical particles is therefore reduced to 3.3.
- Example 2 A metallic powder is produced by the process described in Example 1 agglomerated into granules from stainless steel type 904 L which contains in% by weight: Cr 20; Ni 25; Mo 4.5; Cu 2: remains Fe.
- the starting material contains spherical particles with a diameter not greater than 106 microns. Agglomeration is carried out in the same way as in the case of steel 316 described in Example 1, the final calibration of the granules being carried out by through a 500 micron mesh screen, the dimensional ratio between granules and spherical particles therefore being 4.7.
- a corrosion test, carried out at room temperature, in 1% sulfuric solution does not show any attack after 48 hours.
Landscapes
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
Claims (11)
- Poudre métallique, apte au frittage après formage par compression à froid caractérisée en ce qu'elle est constituée par un ensemble de granules comprenant chacun un groupe de particules élémentaires de forme sphérique agglomérées par de la gélatine à une teneur d'au moins 0,5 % du poids de la poudre métallique.
- Poudre métallique suivant revendication 1 caractérisée en ce que le diamètre maximal d1 des particules élémentaires sphériques et la largeur maximale d2 des granules sont dans un rapport d2/d1 ≥3.
- Poudre métallique suivant revendication 2 caractérisée en ce que le rapport d2/d1 est ≥4.
- Poudre métallique suivant l'une des revendications 1 à 3 caractérisée en ce que la teneur des granules en gélatine est de 1 à 5 % du poids de la poudre métallique.
- Poudre métallique suivant l'une des revendications 1 à 4 caractérisée en ce qu'elle est en un acier inoxydable ou allié.
- Poudre métallique suivant l'une des revendications 1 à 4 caractérisée en ce qu'elle est en un métal ou alliage inoxydable ou réfractaire.
- Procédé de préparation d'une poudre métallique apte au frittage après formage par compression à froid caractérisé en ce qu'on part de particules métalliques élémentaires de forme sphérique à laquelle on mélange une solution aqueuse de gélatine afin de mouiller toute la surface des particules sphériques puis en ce qu'après un début de formation d'un gel donnant au mélange une consistance pâteuse, on fragmente cette pâte de façon à obtenir des granules comprenant chacun un groupe de particules élémentaires dont on achève ensuite le séchage, la teneur en gélatine des granules étant d'au moins 0,5 % en poids de la poudre métallique.
- Procédé suivant revendication 7 caractérisé en ce que la teneur en gélatine est de 1 à 5 % en poids de la poudre métallique.
- Procédé suivant revendication 7 ou 8 caractérisé en ce qu'on effectue la fragmentation de la pâte par passage à travers au moins un tamis de façon à obtenir après séchage des granules ayant une largeur d2 telle que le rapport entre cette largeur d2 et le diamètre maximal d1 des particules sphériques soit au moins égal à 3.
- Procédé suivant revendication 9 caractérisé en ce que le rapport d2/d1 est au moins égal à 4.
- Procédé suivant l'une des revendications 7 à 10 caractérisé en ce que la poudre métallique est un acier allié ou inoxydable ou un métal ou alliage inoxydable ou réfractaire.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9308535 | 1993-07-06 | ||
FR9308535A FR2707191B1 (fr) | 1993-07-06 | 1993-07-06 | Poudre métallique pour la réalisation de pièces par compression et frittage et procédé d'obtention de cette poudre. |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0633083A1 EP0633083A1 (fr) | 1995-01-11 |
EP0633083B1 true EP0633083B1 (fr) | 2001-09-12 |
Family
ID=9449157
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94420188A Expired - Lifetime EP0633083B1 (fr) | 1993-07-06 | 1994-07-04 | Poudre métallique pour la réalisation de pièces par compression et frittage et procédé d'obtention de cette poudre |
Country Status (10)
Country | Link |
---|---|
US (1) | US5460641A (fr) |
EP (1) | EP0633083B1 (fr) |
JP (1) | JP3325390B2 (fr) |
KR (1) | KR960013531A (fr) |
AT (1) | ATE205430T1 (fr) |
CA (1) | CA2127344A1 (fr) |
DE (1) | DE69428236T2 (fr) |
DK (1) | DK0633083T3 (fr) |
ES (1) | ES2162849T3 (fr) |
FR (1) | FR2707191B1 (fr) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SE511834C2 (sv) | 1998-01-13 | 1999-12-06 | Valtubes Sa | Heltäta produkter framställda genom enaxlig höghastighetspressning av metallpulver |
SE518986C2 (sv) * | 2000-04-28 | 2002-12-17 | Metals Process Systems | Metod vid sintring av kolstål med utnyttjande av bindemedel som kolkälla |
US6585795B2 (en) * | 2000-08-07 | 2003-07-01 | Ira L. Friedman | Compaction of powder metal |
US6537489B2 (en) | 2000-11-09 | 2003-03-25 | Höganäs Ab | High density products and method for the preparation thereof |
SE0102102D0 (sv) * | 2001-06-13 | 2001-06-13 | Hoeganaes Ab | High density stainless steel products and method for the preparation thereof |
SE0201825D0 (sv) * | 2002-06-14 | 2002-06-14 | Hoeganaes Ab | Warm compaction of steel powders |
CA2534472A1 (fr) * | 2003-09-03 | 2005-03-17 | Apex Advanced Technologies, Llc | Composition a utiliser dans le domaine de la metallurgie des poudres |
US7470307B2 (en) * | 2005-03-29 | 2008-12-30 | Climax Engineered Materials, Llc | Metal powders and methods for producing the same |
US7604679B2 (en) * | 2005-11-04 | 2009-10-20 | Sumitomo Metal Mining Co., Ltd. | Fine nickel powder and process for producing the same |
DE102014113425A1 (de) * | 2014-09-17 | 2016-03-17 | Fachhochschule Münster | Verfahren zum Beschichten eines Gegenstands |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4006838A (en) * | 1974-11-25 | 1977-02-08 | Western Industries, Inc. | Brazing alloy and brazing paste for gas container joints |
FR2469233B1 (fr) * | 1979-11-14 | 1982-06-18 | Creusot Loire | |
US4787934A (en) * | 1988-01-04 | 1988-11-29 | Gte Products Corporation | Hydrometallurgical process for producing spherical maraging steel powders utilizing spherical powder and elemental oxidizable species |
DE4027887A1 (de) * | 1990-09-03 | 1992-03-05 | Stoess & Co Gelatine | Koerniges agglomerat und verfahren zu seiner herstellung |
US5126104A (en) * | 1991-06-06 | 1992-06-30 | Gte Products Corporation | Method of making powder for thermal spray application |
-
1993
- 1993-07-06 FR FR9308535A patent/FR2707191B1/fr not_active Expired - Fee Related
-
1994
- 1994-06-29 JP JP17023794A patent/JP3325390B2/ja not_active Expired - Fee Related
- 1994-07-04 DK DK94420188T patent/DK0633083T3/da active
- 1994-07-04 ES ES94420188T patent/ES2162849T3/es not_active Expired - Lifetime
- 1994-07-04 CA CA002127344A patent/CA2127344A1/fr not_active Abandoned
- 1994-07-04 EP EP94420188A patent/EP0633083B1/fr not_active Expired - Lifetime
- 1994-07-04 DE DE69428236T patent/DE69428236T2/de not_active Expired - Lifetime
- 1994-07-04 AT AT94420188T patent/ATE205430T1/de not_active IP Right Cessation
- 1994-07-06 KR KR1019940016267A patent/KR960013531A/ko not_active Application Discontinuation
- 1994-07-06 US US08/268,117 patent/US5460641A/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
FR2707191A1 (fr) | 1995-01-13 |
DK0633083T3 (da) | 2002-01-14 |
JPH0754002A (ja) | 1995-02-28 |
DE69428236D1 (de) | 2001-10-18 |
JP3325390B2 (ja) | 2002-09-17 |
FR2707191B1 (fr) | 1995-09-01 |
US5460641A (en) | 1995-10-24 |
EP0633083A1 (fr) | 1995-01-11 |
ATE205430T1 (de) | 2001-09-15 |
DE69428236T2 (de) | 2002-06-27 |
CA2127344A1 (fr) | 1995-01-07 |
ES2162849T3 (es) | 2002-01-16 |
KR960013531A (ko) | 1996-05-22 |
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