WO2005120749A1 - Sintered metal parts and method for the manufacturing thereof - Google Patents

Sintered metal parts and method for the manufacturing thereof Download PDF

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Publication number
WO2005120749A1
WO2005120749A1 PCT/SE2005/000908 SE2005000908W WO2005120749A1 WO 2005120749 A1 WO2005120749 A1 WO 2005120749A1 SE 2005000908 W SE2005000908 W SE 2005000908W WO 2005120749 A1 WO2005120749 A1 WO 2005120749A1
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Prior art keywords
powder
sintered
mpa
powder metallurgical
compacted
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PCT/SE2005/000908
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French (fr)
Inventor
Anders Bergmark
Koki Kanno
Original Assignee
Höganäs Ab
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Application filed by Höganäs Ab filed Critical Höganäs Ab
Priority to MXPA06014234A priority Critical patent/MXPA06014234A/en
Priority to AU2005252150A priority patent/AU2005252150B2/en
Priority to CA002570236A priority patent/CA2570236A1/en
Priority to BRPI0512041-1A priority patent/BRPI0512041A/en
Priority to JP2007516433A priority patent/JP4825200B2/en
Priority to EP05752520A priority patent/EP1771268A1/en
Priority to UAA200700314A priority patent/UA85245C2/en
Publication of WO2005120749A1 publication Critical patent/WO2005120749A1/en

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy
    • C22C33/0257Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/02Making ferrous alloys by powder metallurgy
    • C22C33/0207Using a mixture of prealloyed powders or a master alloy
    • C22C33/0228Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/16Both compacting and sintering in successive or repeated steps
    • B22F3/164Partial deformation or calibration
    • B22F2003/166Surface calibration, blasting, burnishing, sizing, coining
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment

Definitions

  • the present invention refers to powder metallurgy and more specifically to pre-alloyed chromium powder metal parts with improved fatigue properties.
  • sintered products made by powder metallurgy are advantageous in cost over ingot steels obtained through forging and rolling steps and has wide utility as parts in e.g. motor vehicles.
  • the sintered product has pores which are inevitably formed during the course of its fabrication. These remaining pores of the sintered powder-metallurgical materials impair the mechanical properties of the materials, as compared with completely dense materials. This is a result of the pores acting as stress concentrations and also because the pores reduce the effective volume under stress.
  • strength, ductility, fatigue strength, macro-hardness etc. in iron-based powder-metallurgical materials decrease as the porosity increases.
  • Distaloy ® HP available from H ⁇ ganas AB ® , Sweden, is a steel powder possible for use in high perform- ing purposes.
  • this Distaloy ® -powder the base-powder is alloyed with nickel, which is an expensive alloying element.
  • This high performing material is therefore rather costly and there is a need for less expensive materials, which have at least as good fatigue strength.
  • One route to improve the fatigue performance of powder metallurgical steels are secondary operations.
  • shot peening Through hardening, case hardening or shot peening (or a combina- tion) are possible processes to get highest possible fatigue resistance of a component. Shot peening is normally performed in order to utilize the beneficial influence of compressive residual stresses in the surface. Pores open to the surface are weak points in powder metallurgical materials. These pores are at least partly neutralized by introduction of surface compression residual stresses.
  • Shot peening of compacted parts is disclosed in e.g. the US patent 6 171 546. According to this patent the shot peening is followed by a final sintering step.
  • An iron- based powder containing i. a. nickel is used as starting material.
  • nickel is expensive.
  • Other disadvantages with nickel containing powders are dusting problems which may occur during the processing of the powder, and which may cause allergic reactions also in minor amounts . The use of nickel should thus be avoided.
  • the US patent application 2004/0177719 relates to a method including shot peening.
  • this application discloses a method, wherein a portion of the surface of a compacted part is subjected to shot peening after sintering. According to this application a densifying process involving powder forging or sizing is necessary in order improve the prop- erties of the final compacted part.
  • An object of the present invention is to provide a cost effective process for the preparation of powder metallurgical components with high fatigue strength without any steps for achieving core densification . Another object is to provide a process involving powder materials, which are free from nickel.
  • components having high fatigue strength can be obtained by shot peening of sintered components prepared from iron based powders distinguished by low levels of chromium and molybdenum.
  • the powders used in the present invention are pre-alloyed iron-base powders comprising low amounts of chromium and molybdenum.
  • a preferred amount is 1.3-3.5% by weight of chromium and 0.15-0.7% by weight of molybdenum.
  • the pow- der may also contain small amounts, 0.09 to 0.3% by weight, of manganese and inevitable impurities.
  • Such powders are known from the US patent 6 348 080 and WO 03/106079.
  • the base powder is further mixed with graphite to obtain the desired strength in the material.
  • the amount of graphite which is mixed with the iron-base powder is 0.1- 1.0%, preferably 0.15-0.85%.
  • the powder mixture is compacted in a die to produce a green body.
  • the compaction pressure is at least 600 MPa, preferably at least 700 MPa and more preferably 800 MPa.
  • the compaction can be performed by cold compaction or warm compaction. After the compaction the obtained green part is sintered at a sintering temperature above 1100°C, preferably above 1220°C.
  • the sintering atmosphere is preferably a mix of nitrogen and hydrogen.
  • a normal cooling rate in the sintering process is 0.8°C/s, a range between 0.5°C/s and 1.0°C/s is preferred.
  • the sintered density is preferably above 7.15 g/cm 3 , more preferably above 7.3 g/cm 3 .
  • the obtained microstructure in the as-sinterd material is mainly fine- pearlitic with a lower chromium and molybdenum content and martensitic or lower bainitic for slightly higher chromium and molybdenum content .
  • the degree of shot peening as defined by Almen A intensity is preferably between 0.20 and 0.37 mm.
  • Secondary operations e.g. through hardening and case hardening, can be performed before the shot peening in order to improve the properties even more.
  • the material is mainly martensitic and the fatigue limit is raised by shotpeening.
  • the martensite in the surface which is formed during case hardening is believed to form compres- sive stresses, which is beneficial for the fatigue limit.
  • Sinterhardening is an alternative process which is applied in the sintering process. Sinterhardening uses forced cooling at the end of the sintering process of the components which results in a hardened structure.
  • the fatigue tests have been performed on notched specimen with a stress concentration factor, K t , of 1.38 and on un-notched specimen.
  • the tests show a greater increase in bending fatigue limit when shot peening notched specimen than when the shot peening is performed on un-notched specimen.
  • the expression "notched” in this context refers to a specimen or component having a stress concentration factor above 1.3.
  • the invention is illustrated by the following non- limiting examples .
  • Example 1 Two pre-alloyed base-powders, Astaloy ® CrL and Astaloy ® CrM, and one diffusion-alloyed base powder, Distaloy ® HP, are included in the study.
  • Distaloy ® HP is diffusion- alloyed with Ni and Cu and pre-alloyed with Mo. The three materials included in this study are shown in Table 1.
  • the microstructure of Astaloy CrL with sintered carbon below 0.6% and cooling rate about 0.8°C/s is upper bainite. Increased carbon above 0.74% changes the microstruc- ture to fine pearlite.
  • Microstructure analysis of 1120°C sintered Astaloy CrM materials and cooling rate 0.8°C/s and with sintered carbon levels between 0.32% and 0.49% show a dense upper bainitic microstructure.
  • Dense upper bainite has the same characteristics as regular upper bainite, i.e. an irregular mix of ferrite and cementite . The differences are the smaller distances between carbides and sizes of the carbides. Increased sintered carbon shifts the microstruc- ture to a mix of martensite and lower bainite.
  • Table 3 shows influence of compaction pressure and carbon level for cold compacted Astaloy CrL. All materials were sintered at 1120°C for 30 min. in 90/10 N 2 /H 2 .
  • table 3 a summary of plane bending fatigue performance of Astaloy CrL at two compaction pressures and two levels of additional graphite. Std. dev. ⁇ 5 indicates that the scatter is small and the MPIF standard 56 evaluation of standard deviation cannot be applied. The specimen in table 3 are un-notched. Table 3
  • Influence of sintering temperature on the fatigue performance with un-notched specimen is shown in Table 4.
  • the microstructures of the materials in table 4 are characterized by mainly upper bainite (1120°C 0.58%C) and fine pearlite (1120°C, 0.77%C and 1250°C, 0.74%C).
  • the materials are sintered at 1280°C for 30 min in H 2 . Cooling rate is 0.8°C/s.
  • the shot peening is performed to obtain an Almen A inten- sity of 0.32 mm.
  • Estimated plane bending fatigue performance of as sintered and as-sintered plus shot peened samples is shown in table 5.

Abstract

The invention relates to a method consisting of the steps of providing a pre-alloyed iron-based metal powder comprising at least 1.3-3.5% chromium, 0.15-0.7% molybdenum, manganese and unavoidable impurities, mixing said powder with 0.1-1.0% graphite, compacting the obtained mixture at a pressure of at least 600 MPa, sintering the compacted part in a single step at a temperature above 1100°C, shot-peening the part and after sintering optionally hardening the component. The invention also relates to a powder metallurgical part and use of a low chromium prealloyed powder for preparing notched sintered parts having a bending fatigue limit of at least 340 MPa at a sintered density of 7.15 g/cm3, preferably at least 400 MPa at a sintered density of 7.3 g/cm3.

Description

SINTERED METAL PARTS AND METHOD FOR THE MANUFACTURING THEREOF
FIELD OF THE INVENTION
The present invention refers to powder metallurgy and more specifically to pre-alloyed chromium powder metal parts with improved fatigue properties.
BACKGROUND OF THE INVENTION
In general, sintered products made by powder metallurgy are advantageous in cost over ingot steels obtained through forging and rolling steps and has wide utility as parts in e.g. motor vehicles. However, the sintered product has pores which are inevitably formed during the course of its fabrication. These remaining pores of the sintered powder-metallurgical materials impair the mechanical properties of the materials, as compared with completely dense materials. This is a result of the pores acting as stress concentrations and also because the pores reduce the effective volume under stress. Thus, strength, ductility, fatigue strength, macro-hardness etc. in iron-based powder-metallurgical materials decrease as the porosity increases.
Despite their comparatively low fatigue strength , iron- based powder-metallurgical materials are, to a certain extent, used in components requiring high fatigue strength. Distaloy® HP, available from Hδganas AB®, Sweden, is a steel powder possible for use in high perform- ing purposes. In this Distaloy®-powder the base-powder is alloyed with nickel, which is an expensive alloying element. This high performing material is therefore rather costly and there is a need for less expensive materials, which have at least as good fatigue strength. One route to improve the fatigue performance of powder metallurgical steels are secondary operations. Through hardening, case hardening or shot peening (or a combina- tion) are possible processes to get highest possible fatigue resistance of a component. Shot peening is normally performed in order to utilize the beneficial influence of compressive residual stresses in the surface. Pores open to the surface are weak points in powder metallurgical materials. These pores are at least partly neutralized by introduction of surface compression residual stresses.
Shot peening of compacted parts is disclosed in e.g. the US patent 6 171 546. According to this patent the shot peening is followed by a final sintering step. An iron- based powder containing i. a. nickel is used as starting material. As indicated above there is an increasing demand for powders, which do not contain nickel, as nickel is expensive. Other disadvantages with nickel containing powders are dusting problems which may occur during the processing of the powder, and which may cause allergic reactions also in minor amounts . The use of nickel should thus be avoided. Also the US patent application 2004/0177719 relates to a method including shot peening. More specifically, this application discloses a method, wherein a portion of the surface of a compacted part is subjected to shot peening after sintering. According to this application a densifying process involving powder forging or sizing is necessary in order improve the prop- erties of the final compacted part.
An object of the present invention is to provide a cost effective process for the preparation of powder metallurgical components with high fatigue strength without any steps for achieving core densification . Another object is to provide a process involving powder materials, which are free from nickel. SUMMARY OF THE INVENTION
It has unexpectedly been found that components having high fatigue strength can be obtained by shot peening of sintered components prepared from iron based powders distinguished by low levels of chromium and molybdenum.
DETAILED DESCRIPTION OF THE INVENTION
The powders used in the present invention are pre-alloyed iron-base powders comprising low amounts of chromium and molybdenum. A preferred amount is 1.3-3.5% by weight of chromium and 0.15-0.7% by weight of molybdenum. The pow- der may also contain small amounts, 0.09 to 0.3% by weight, of manganese and inevitable impurities. Such powders are known from the US patent 6 348 080 and WO 03/106079.
The base powder is further mixed with graphite to obtain the desired strength in the material. The amount of graphite which is mixed with the iron-base powder is 0.1- 1.0%, preferably 0.15-0.85%. The powder mixture is compacted in a die to produce a green body. The compaction pressure is at least 600 MPa, preferably at least 700 MPa and more preferably 800 MPa. The compaction can be performed by cold compaction or warm compaction. After the compaction the obtained green part is sintered at a sintering temperature above 1100°C, preferably above 1220°C. The sintering atmosphere is preferably a mix of nitrogen and hydrogen. A normal cooling rate in the sintering process is 0.8°C/s, a range between 0.5°C/s and 1.0°C/s is preferred. The sintered density is preferably above 7.15 g/cm3, more preferably above 7.3 g/cm3. The obtained microstructure in the as-sinterd material is mainly fine- pearlitic with a lower chromium and molybdenum content and martensitic or lower bainitic for slightly higher chromium and molybdenum content .
It has now unexpectedly been found that a remarkable in- crease in the bending fatigue limit can be obtained by shot peening the sintered low chromium powder materials. Especially remarkable increase is obtained for notched parts, where an increase of more than 50% and even more than 70% can be obtained as can be seen from the follow- ing examples. The degree of shot peening as defined by Almen A intensity, is preferably between 0.20 and 0.37 mm.
Secondary operations e.g. through hardening and case hardening, can be performed before the shot peening in order to improve the properties even more. Thus, after through hardening followed by tempering the material is mainly martensitic and the fatigue limit is raised by shotpeening. The martensite in the surface which is formed during case hardening is believed to form compres- sive stresses, which is beneficial for the fatigue limit.
Sinterhardening is an alternative process which is applied in the sintering process. Sinterhardening uses forced cooling at the end of the sintering process of the components which results in a hardened structure.
The fatigue tests have been performed on notched specimen with a stress concentration factor, Kt, of 1.38 and on un-notched specimen. The tests show a greater increase in bending fatigue limit when shot peening notched specimen than when the shot peening is performed on un-notched specimen. The expression "notched" in this context refers to a specimen or component having a stress concentration factor above 1.3. The invention is illustrated by the following non- limiting examples .
Example 1 Two pre-alloyed base-powders, Astaloy® CrL and Astaloy® CrM, and one diffusion-alloyed base powder, Distaloy® HP, are included in the study. Distaloy® HP is diffusion- alloyed with Ni and Cu and pre-alloyed with Mo. The three materials included in this study are shown in Table 1.
Table 1
Figure imgf000006_0001
Detailed information on process parameters, density and carbon levels will be given below. In table 2 plane bend- ing fatigue performance of un-notched specimen is shown for different alloys which are sintered 30 min in 90/10 2/H2 with cooling rate about 0.8C/sec. Fatigue tests on un-notched specimens are performed using 5 mm IS03928 samples with chamfered edges. The tests are made in four- point plane bending at load ratio R=-l. The staircase method is used with 13 - 18 samples in the staircase and 2 million cycles as run-out limit. Evaluation of the staircase (50% probability fatigue limit and standard deviation) is made according to the MPIF 56 standard. Test frequency is 27 - 30 Hz. Table 2
Figure imgf000007_0001
The microstructure of Astaloy CrL with sintered carbon below 0.6% and cooling rate about 0.8°C/s is upper bainite. Increased carbon above 0.74% changes the microstruc- ture to fine pearlite.
Microstructure analysis of 1120°C sintered Astaloy CrM materials and cooling rate 0.8°C/s and with sintered carbon levels between 0.32% and 0.49% show a dense upper bainitic microstructure. Dense upper bainite has the same characteristics as regular upper bainite, i.e. an irregular mix of ferrite and cementite . The differences are the smaller distances between carbides and sizes of the carbides. Increased sintered carbon shifts the microstruc- ture to a mix of martensite and lower bainite.
Table 3 shows influence of compaction pressure and carbon level for cold compacted Astaloy CrL. All materials were sintered at 1120°C for 30 min. in 90/10 N2/H2. In table 3 a summary of plane bending fatigue performance of Astaloy CrL at two compaction pressures and two levels of additional graphite. Std. dev. <5 indicates that the scatter is small and the MPIF standard 56 evaluation of standard deviation cannot be applied. The specimen in table 3 are un-notched. Table 3
Figure imgf000008_0001
Influence of sintering temperature on the fatigue performance with un-notched specimen is shown in Table 4. The microstructures of the materials in table 4 are characterized by mainly upper bainite (1120°C 0.58%C) and fine pearlite (1120°C, 0.77%C and 1250°C, 0.74%C).
Table 4
Figure imgf000008_0002
Example 2
Influence of shot peening and the combination of heat treatment and shot peening has been investigated on Astaloy CrL 3 mm edge-notched specimens. The notch is included in the press tool and no machining is performed. The stress concentration factor in bending is obtained by FEM to Kt=1.38. Test frequency is 27-30 Hz.
The materials are sintered at 1280°C for 30 min in H2. Cooling rate is 0.8°C/s.
The shot peening is performed to obtain an Almen A inten- sity of 0.32 mm. Estimated plane bending fatigue performance of as sintered and as-sintered plus shot peened samples is shown in table 5.
Table 5
Figure imgf000009_0001
In table 6 an estimated plane bending fatigue performance of through hardened tempered and shot peened samples is shown. Through hardening is performed with an austeniti- zation temperature at 880°C. The cooling rate after aus- tenitization is made at 8°C/s. Finally the specimen are tempered at 250°C for 1 hour .
Table 6
Figure imgf000009_0002
From the tables 5 and 6 it can be found that by shot peening the materials containing chromium and molybdenum a great increase of the bending fatigue limit is achieved.

Claims

1. A method for producing powder metallurgical parts with improved fatigue strength comprising the steps of: - providing a pre-alloyed iron-based metal powder comprising at least 1.3-3.5% by weight of chromium, 0.15- 0.7% by weight of molybdenum,
- mixing said powder with 0.1-1.0% by weight of graphite,
- compacting the obtained mixture at a pressure of at least 600 MPa,
- sintering the compacted part in a single step at a temperature above 1100°C,
- shot-peening the part.
2. A method according to claim 1 wherein the increase of the fatigue strength is at least 50%.
3. The method according to claim 1 or 2, wherein the compacted and sintered part is subjected to hardening and tempering prior to shot peening.
4. A powder metallurgical part manufactured according to any one of the claims 1-3 having a mainly pearlitic microstructure, preferably mainly fine pearlitic micro- structure
5. A powder metallurgical part manufactured according to any one of the claims 1-3 having a martensitic and lower bainitic microstructure.
6. The powder metallurgical part manufactured according to any one of the claims 1-3 having a mainly tempered martensitic microstructure.
7. The powder metallurgical part according to any one of the claims 1-6 , having a bending fatigue limit of at least 340 MPa at a sintered density of 7.15 g/cm3, pref- erably at least 400 MPa at a sintered density of 7.3 g/cm3.
8. Use of a low chromium prealloyed powder for preparing notched sintered parts having a bending fatigue limit of at least 340 MPa at a sintered density of 7.15 g/cm3, preferably at least 400 MPa at a sintered density of 7.3 g/cm3 characterised in that said powder is compacted, sintered and optionally tempered and annealed and is sub- jected to shot peening.
9. Use of the powder metallurgical part according to claim 10, having a stress concentration factor above 1.3,
PCT/SE2005/000908 2004-06-14 2005-06-13 Sintered metal parts and method for the manufacturing thereof WO2005120749A1 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
MXPA06014234A MXPA06014234A (en) 2004-06-14 2005-06-13 Sintered metal parts and method for the manufacturing thereof.
AU2005252150A AU2005252150B2 (en) 2004-06-14 2005-06-13 Sintered metal parts and method for the manufacturing thereof
CA002570236A CA2570236A1 (en) 2004-06-14 2005-06-13 Sintered metal parts and method for the manufacturing thereof
BRPI0512041-1A BRPI0512041A (en) 2004-06-14 2005-06-13 sintered metal parts and method of manufacture
JP2007516433A JP4825200B2 (en) 2004-06-14 2005-06-13 Powder metallurgy parts and manufacturing method thereof
EP05752520A EP1771268A1 (en) 2004-06-14 2005-06-13 Sintered metal parts and method for the manufacturing thereof
UAA200700314A UA85245C2 (en) 2004-06-14 2005-06-13 method of manufacturing parts with high fatigue resistance, part manufactured by the method (embodiments) and its use

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE0401535A SE0401535D0 (en) 2004-06-14 2004-06-14 Sintered metal parts and method of manufacturing thereof
SE0401535-0 2004-06-14

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JP (1) JP4825200B2 (en)
CN (1) CN100475389C (en)
AU (1) AU2005252150B2 (en)
BR (1) BRPI0512041A (en)
CA (1) CA2570236A1 (en)
MX (1) MXPA06014234A (en)
RU (1) RU2345867C2 (en)
SE (1) SE0401535D0 (en)
TW (1) TWI290073B (en)
UA (1) UA85245C2 (en)
WO (1) WO2005120749A1 (en)
ZA (1) ZA200610348B (en)

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RU2345867C2 (en) 2009-02-10
JP4825200B2 (en) 2011-11-30
UA85245C2 (en) 2009-01-12
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RU2007101313A (en) 2008-08-10
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