US20060101945A1 - Method for producing a hard metal stock - Google Patents

Method for producing a hard metal stock Download PDF

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Publication number
US20060101945A1
US20060101945A1 US10/544,997 US54499705A US2006101945A1 US 20060101945 A1 US20060101945 A1 US 20060101945A1 US 54499705 A US54499705 A US 54499705A US 2006101945 A1 US2006101945 A1 US 2006101945A1
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US
United States
Prior art keywords
hard metal
slurry
wet slurry
wet
minutes
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.)
Abandoned
Application number
US10/544,997
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English (en)
Inventor
Andreas Lackner
Gerhard Knunz
Christian Muller
Karl Beiser
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ceratizit Austria GmbH
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Ceratizit Austria GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Ceratizit Austria GmbH filed Critical Ceratizit Austria GmbH
Publication of US20060101945A1 publication Critical patent/US20060101945A1/en
Abandoned legal-status Critical Current

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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • 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
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the invention relates to a process for producing a hard metal batch by drying a wet slurry produced by wet-milling the hard material and binder metal fractions to the desired grain size, using water as liquid phase, with or without fractions of a pressing aid.
  • Shaped parts formed from hard metal alloys are produced by pressing and sintering a hard metal batch.
  • the hard metal batch contains the hard material and binder metal fractions desired in the finished hard metal alloy in finely distributed form, with or without the use of a pressing aid.
  • the fine-particle starting powders with a mean grain size in the range of a few ⁇ m, and in some cases even smaller are converted into granule form, i.e. into as ideal a spherical shape as possible, with a granule size of approximately 140 ⁇ m. This improves the flow properties of the hard metal batch, which in particular significantly simplifies the uniform filling of the press moulds for production of shaped parts of complex shape.
  • the granules are produced by spray-drying the desired hard metal batch in a spray-drying installation.
  • a process of this type using water as liquid phase is described, for example, in Austrian utility model AT U 4.929.
  • a drawback of a process of this type is that it is relatively expensive.
  • Good flow properties of the hard metal batch are not necessarily required for many shaping processes for further processing of a hard metal batch. These include, for example, the production of simple shaped parts by hydrostatic compacting or extrusion, but also the production of complex small shaped parts by powder injection molding.
  • the object of the present invention is to provide a process for producing the hard metal batch for hard metal shaped parts whose production does not require good flow properties on the part of the hard metal batch which is significantly less expensive than previously known processes.
  • this is achieved by virtue of the fact that the wet slurry is applied to a moving carrier belt with a solids content of from 75% by weight to 95% by weight and a layer thickness of from 0.2 mm to 2 mm and as it passes through a drying zone is heated, over the course of in total 1 minute to 7 minutes, to a maximum temperature within a range from >100° C. to 150° C., the time which it takes for the wet slurry to be heated to over 100° C. being within a range from 15 seconds to 2 minutes, and that the hard metal batch which has been dried in this manner is cooled to room temperature and if necessary comminuted.
  • a pressing aid for further processing of the hard metal batch, in particular by extrusion, it may be expedient for a pressing aid to be admixed to the wet slurry before it is dried. If this pressing aid is a water-insoluble pressing aid based on wax, such as for example paraffin, it is admixed to the wet slurry in the form of an emulsion which is produced with the aid of an emulsifier and the addition of water.
  • the process according to the invention despite the use of water as liquid phase and despite the drying in air at elevated temperatures, surprisingly allows the production of hard metal batches with an extremely low oxygen content.
  • the oxygen content is under certain circumstances even lower than in hard metal batches which are produced in accordance with the prior art and in which the wet slurry is prepared using organic solvents, such as acetone, followed by drying in vacuo.
  • the maximum drying temperature and the drying time are matched to the layer thickness of the wet slurry applied. The greater the layer thickness, the higher the maximum drying temperature and the longer the drying time required.
  • an antioxidant for example based on amino compounds, e.g. aminoxethylate or resorcinol, to be added to the water prior to milling for producing the wet slurry, with the result that an excessive oxygen content in the dried batch is prevented even with these oxidation-sensitive hard metal batches.
  • amino compounds e.g. aminoxethylate or resorcinol
  • the process according to the invention works particularly advantageously if the wet slurry is applied to the carrier belt in a layer thickness of from 0.5 mm to 1 mm, since the total time taken to pass through the drying zone can then be shortened to 1.5 minutes to 6 minutes, and the time taken for the wet slurry to be heated to over 100° C. can be restricted to a range from 30 seconds to 60 seconds. This minimizes the oxygen uptake by the hard metal batch.
  • wet slurry prefferably be heated to the desired temperature first of all by hot air and then additionally by radiant heat, resulting in particularly rapid removal of the moisture from the wet slurry.
  • the radiant heat is in this case advantageously generated by infrared radiators.
  • FIG. 1 shows an outline diagram of a belt drying installation for carrying out the production process according to the invention.
  • the milling bodies used were 2000 kg of hard metal beads with a diameter of 9 mm.
  • the rotational speed of the attritor was 78 rpm, and the wet slurry was circulated at a pumping rate of 1000 l/hour.
  • the temperature of the wet slurry during milling was kept constant at approximately 40° C.
  • the fully milled wet slurry had a viscosity of 4000 mPas at a shear rate of 5.18 [1/s].
  • a belt drying installation which operates in air and at standard pressure as shown in FIG. 1 was used to dry the wet slurry produced in this manner.
  • the belt drying installation shown in FIG. 1 comprises a 3 m long, revolving conveyor belt - 1 -.
  • a feed device - 2 - for applying the wet slurry - 3 - to the conveyor belt - 1 - in different layer thicknesses is provided at the start of the conveyor belt - 1 -.
  • This feed device is followed by a drying zone - 4 -.
  • the wet slurry - 3 - which has been applied in layer form is heated in a first passage zone - 5 - by means of a hot air blower - 6 -.
  • the pre-dried wet slurry is heated to the desired maximum temperature within a range from >100° C. to 150° C. by means of infrared radiators.
  • the dried hard metal batch drops into a collection vessel - 8 -.
  • the belt drying installation was operated at a belt velocity of 1 m/min, and the wet slurry - 3 - was applied to the conveyor belt - 1 - in a thickness of 0.8 mm.
  • the total passage time through the drying zone - 4 - was 3 minutes, with the following temperature sequence: after 20 seconds: 40° C. after 52 seconds: 50° C. after 84 seconds: 60° C. after 150 seconds: 95° C. after 165 seconds: 102° C. after 180 seconds: 110° C.
  • the applied wet slurry - 3 - was heated to a temperature of approximately 60° C. by the hot air blower - 6 -, with the result that the majority of the water was evaporated.
  • the time of the second passage zone - 7 -, in which the wet slurry was at a temperature of more than 100° C. was restricted to approximately 15 seconds in order to achieve the required maximum permissible residual moisture content in the dried hard metal batch.
  • the dried hard metal batch was cooled to room temperature over the course of 20 seconds.
  • the oxygen content of the hard metal batch dried in this manner was 0.53% by weight, and the residual moisture content was 0.13% by weight.
  • the dried hard metal batch was broken up in a hammer mill, to a particle size of approximately 0.4 mm, mixed with a plasticizer in the standard way and extruded to form a hard metal rod with a diameter of 16 mm. This rod was then sintered for 80 minutes at 1410° C. and then recompacted at 70 bar.
  • Example 2 For comparison purposes, two further hard metal batches of the same composition as in Example 1 were produced.
  • Example 3 the hard metal batch was produced by vacuum drying with organic solvent.
  • the hard metal alloys produced from these hard metal batches were then compared with one another.
  • Example 2 To produce this hard metal batch, the same raw materials in the same ratio and the same quantities as in Example 1 were milled with 160 l of water, under otherwise identical conditions, in an attritor.
  • a spray tower with a cylindrical section 6 m high with a diameter of 4 m was used to dry the wet slurry produced in this manner.
  • the spray tower was designed for countercurrent operation in accordance with the fountain principle.
  • the gas used to dry the wet slurry was air which was fed to the spray tower at 4000 m 3 /hour.
  • the wet slurry was fed to the spray tower via a spray lance with a single-flurry nozzle having an outlet opening with a diameter of 1.12 mm, at a pressure of 15 bar.
  • the air outlet temperature was set to a constant level of 88° C., which under the given conditions was achieved by an air entry temperature of 145° C.
  • the spray-dried hard metal granules produced in this way had an oxygen content of 0.52% by weight and a moisture content of 0.15% by weight.
  • the hard metal granules produced in this way were mixed with a plasticizer in the standard way and extruded to form a hard metal rod with a diameter of 16 mm.
  • This rod was then sintered for 80 minutes at 1410° C. and then recompacted at 70 bar.
  • the metallurgical assessment revealed a hard metal quality having the following properties: Density: 14.85 g/cm 3 Hardness HV30: 2030 daN/mm 2 Magnetic saturation: 112 ⁇ 10 ⁇ 3 T m 3 /kg Coercive force: 491 Oe.
  • the temperature of the acetone/powder mixture during the milling was kept constant at approximately 35° C.
  • the fully milled suspension had a viscosity of ⁇ 200 mPa at a shear rate of 5.18 [1/s].
  • a vacuum drier of conventional design was used to dry this hard metal suspension produced in this way.
  • the heat was supplied via hot water in a double jacket. Moreover, vacuum was applied to the suspension, so that the acetone evaporated. In addition, this vacuum drier was equipped with a slowly rotating stirring mechanism.
  • the hard metal batch produced in this way had an oxygen content of 0.48% by weight.
  • the hard metal batch produced in this manner was pressed through a screen then mixed with a plasticizer in the standard way and extruded to form a hard metal rod with a diameter of 16 mm. This rod was then sintered for 80 minutes at 1400° C. and then recompacted at 70 bar.
  • the metallurgical assessment revealed a hard metal quality with the following properties: Density: 14.83 g/cm 3 Hardness HV30: 2032 daN/mm 2 Magnetic saturation: 113 ⁇ 10 ⁇ 3 T m 3 /kg Coercive force: 488 Oe.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Powder Metallurgy (AREA)
US10/544,997 2003-02-10 2004-02-09 Method for producing a hard metal stock Abandoned US20060101945A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
ATGM64/2003 2003-02-10
AT0006403U AT6486U1 (de) 2003-02-10 2003-02-10 Verfahren zur herstellung eines hartmetallansatzes
PCT/AT2004/000041 WO2004070069A1 (de) 2003-02-10 2004-02-09 Verfahren zur herstellung eines hartmetallansatzes

Publications (1)

Publication Number Publication Date
US20060101945A1 true US20060101945A1 (en) 2006-05-18

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Family Applications (1)

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US10/544,997 Abandoned US20060101945A1 (en) 2003-02-10 2004-02-09 Method for producing a hard metal stock

Country Status (9)

Country Link
US (1) US20060101945A1 (de)
EP (1) EP1592817B1 (de)
KR (1) KR20050111738A (de)
AT (2) AT6486U1 (de)
CA (1) CA2515379A1 (de)
DE (1) DE502004000663D1 (de)
DK (1) DK1592817T3 (de)
ES (1) ES2263136T3 (de)
WO (1) WO2004070069A1 (de)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080289495A1 (en) * 2007-05-21 2008-11-27 Peter Eisenberger System and Method for Removing Carbon Dioxide From an Atmosphere and Global Thermostat Using the Same
US20110041688A1 (en) * 2007-05-21 2011-02-24 Peter Eisenberger Carbon Dioxide Capture/Regeneration Structures and Techniques
US8500860B2 (en) 2007-05-21 2013-08-06 Peter Eisenberger Carbon dioxide capture/regeneration method using effluent gas
US8500855B2 (en) 2010-04-30 2013-08-06 Peter Eisenberger System and method for carbon dioxide capture and sequestration
US9028592B2 (en) 2010-04-30 2015-05-12 Peter Eisenberger System and method for carbon dioxide capture and sequestration from relatively high concentration CO2 mixtures
US9427726B2 (en) 2011-10-13 2016-08-30 Georgia Tech Research Corporation Vapor phase methods of forming supported highly branched polyamines
US9908080B2 (en) 2007-05-21 2018-03-06 Peter Eisenberger System and method for removing carbon dioxide from an atmosphere and global thermostat using the same
US9925488B2 (en) 2010-04-30 2018-03-27 Peter Eisenberger Rotating multi-monolith bed movement system for removing CO2 from the atmosphere
US11059024B2 (en) 2012-10-25 2021-07-13 Georgia Tech Research Corporation Supported poly(allyl)amine and derivatives for CO2 capture from flue gas or ultra-dilute gas streams such as ambient air or admixtures thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108907092B (zh) * 2018-06-29 2020-08-28 安徽大卫模具有限公司 一种消失模精准烘干装置

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2928725A (en) * 1955-05-20 1960-03-15 British Titan Products Preparation of ferrous sulfate monohydrate suspensions
US4354964A (en) * 1979-11-12 1982-10-19 Thorn Emi Limited Cermet materials
US4397889A (en) * 1982-04-05 1983-08-09 Gte Products Corporation Process for producing refractory powder
US4478888A (en) * 1982-04-05 1984-10-23 Gte Products Corporation Process for producing refractory powder
US5922978A (en) * 1998-03-27 1999-07-13 Omg Americas, Inc. Method of preparing pressable powders of a transition metal carbide, iron group metal or mixtures thereof
US20030061906A1 (en) * 2001-03-29 2003-04-03 Gerhard Knunz Method for producing hard metal granulate
US20030075012A1 (en) * 2001-03-29 2003-04-24 Gerhard Knunz Method of producing hard metal grade powder

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2928725A (en) * 1955-05-20 1960-03-15 British Titan Products Preparation of ferrous sulfate monohydrate suspensions
US4354964A (en) * 1979-11-12 1982-10-19 Thorn Emi Limited Cermet materials
US4397889A (en) * 1982-04-05 1983-08-09 Gte Products Corporation Process for producing refractory powder
US4478888A (en) * 1982-04-05 1984-10-23 Gte Products Corporation Process for producing refractory powder
US5922978A (en) * 1998-03-27 1999-07-13 Omg Americas, Inc. Method of preparing pressable powders of a transition metal carbide, iron group metal or mixtures thereof
US20030061906A1 (en) * 2001-03-29 2003-04-03 Gerhard Knunz Method for producing hard metal granulate
US20030075012A1 (en) * 2001-03-29 2003-04-24 Gerhard Knunz Method of producing hard metal grade powder

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8500859B2 (en) 2007-05-21 2013-08-06 Peter Eisenberger Carbon dioxide capture/regeneration method using vertical elevator and storage
US9555365B2 (en) 2007-05-21 2017-01-31 Peter Eisenberger System and method for removing carbon dioxide from an atmosphere and global thermostat using the same
US20110041688A1 (en) * 2007-05-21 2011-02-24 Peter Eisenberger Carbon Dioxide Capture/Regeneration Structures and Techniques
US8163066B2 (en) 2007-05-21 2012-04-24 Peter Eisenberger Carbon dioxide capture/regeneration structures and techniques
US8500860B2 (en) 2007-05-21 2013-08-06 Peter Eisenberger Carbon dioxide capture/regeneration method using effluent gas
US9908080B2 (en) 2007-05-21 2018-03-06 Peter Eisenberger System and method for removing carbon dioxide from an atmosphere and global thermostat using the same
US20100319537A1 (en) * 2007-05-21 2010-12-23 Peter Eisenberger System and Method for Removing Carbon Dioxide from an Atmosphere and Global Thermostat Using the Same
US8500857B2 (en) 2007-05-21 2013-08-06 Peter Eisenberger Carbon dioxide capture/regeneration method using gas mixture
US8696801B2 (en) 2007-05-21 2014-04-15 Peter Eisenberger Carbon dioxide capture/regeneration apparatus
US8500858B2 (en) 2007-05-21 2013-08-06 Peter Eisenberger Carbon dioxide capture/regeneration method using vertical elevator
US8500861B2 (en) 2007-05-21 2013-08-06 Peter Eisenberger Carbon dioxide capture/regeneration method using co-generation
US8894747B2 (en) 2007-05-21 2014-11-25 Peter Eisenberger System and method for removing carbon dioxide from an atmosphere and global thermostat using the same
US20080289495A1 (en) * 2007-05-21 2008-11-27 Peter Eisenberger System and Method for Removing Carbon Dioxide From an Atmosphere and Global Thermostat Using the Same
US9227153B2 (en) 2007-05-21 2016-01-05 Peter Eisenberger Carbon dioxide capture/regeneration method using monolith
US9028592B2 (en) 2010-04-30 2015-05-12 Peter Eisenberger System and method for carbon dioxide capture and sequestration from relatively high concentration CO2 mixtures
US9433896B2 (en) 2010-04-30 2016-09-06 Peter Eisenberger System and method for carbon dioxide capture and sequestration
US9630143B2 (en) 2010-04-30 2017-04-25 Peter Eisenberger System and method for carbon dioxide capture and sequestration utilizing an improved substrate structure
US9878286B2 (en) 2010-04-30 2018-01-30 Peter Eisenberger System and method for carbon dioxide capture and sequestration
US8500855B2 (en) 2010-04-30 2013-08-06 Peter Eisenberger System and method for carbon dioxide capture and sequestration
US9925488B2 (en) 2010-04-30 2018-03-27 Peter Eisenberger Rotating multi-monolith bed movement system for removing CO2 from the atmosphere
US9975087B2 (en) 2010-04-30 2018-05-22 Peter Eisenberger System and method for carbon dioxide capture and sequestration from relatively high concentration CO2 mixtures
US10413866B2 (en) 2010-04-30 2019-09-17 Peter Eisenberger System and method for carbon dioxide capture and sequestration
US10512880B2 (en) 2010-04-30 2019-12-24 Peter Eisenberger Rotating multi-monolith bed movement system for removing CO2 from the atmosphere
US9427726B2 (en) 2011-10-13 2016-08-30 Georgia Tech Research Corporation Vapor phase methods of forming supported highly branched polyamines
US11059024B2 (en) 2012-10-25 2021-07-13 Georgia Tech Research Corporation Supported poly(allyl)amine and derivatives for CO2 capture from flue gas or ultra-dilute gas streams such as ambient air or admixtures thereof

Also Published As

Publication number Publication date
DK1592817T3 (da) 2006-09-25
WO2004070069A1 (de) 2004-08-19
ATE328127T1 (de) 2006-06-15
KR20050111738A (ko) 2005-11-28
EP1592817B1 (de) 2006-05-31
DE502004000663D1 (de) 2006-07-06
EP1592817A1 (de) 2005-11-09
ES2263136T3 (es) 2006-12-01
AT6486U1 (de) 2003-11-25
CA2515379A1 (en) 2004-08-19

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