EP2815821A1 - Procédé et dispositif de nettoyage de métal contenant des particules formant une poudre par élimination d'un composé fixé aux particules - Google Patents

Procédé et dispositif de nettoyage de métal contenant des particules formant une poudre par élimination d'un composé fixé aux particules Download PDF

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Publication number
EP2815821A1
EP2815821A1 EP13305813.1A EP13305813A EP2815821A1 EP 2815821 A1 EP2815821 A1 EP 2815821A1 EP 13305813 A EP13305813 A EP 13305813A EP 2815821 A1 EP2815821 A1 EP 2815821A1
Authority
EP
European Patent Office
Prior art keywords
particles
container
solvent
composition
compound
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.)
Withdrawn
Application number
EP13305813.1A
Other languages
German (de)
English (en)
Inventor
Christelle Favre
Philippe Vaxelaire
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.)
Heraeus Deutschland GmbH and Co KG
Original Assignee
Heraeus Materials Technology GmbH and Co KG
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 Heraeus Materials Technology GmbH and Co KG filed Critical Heraeus Materials Technology GmbH and Co KG
Priority to EP13305813.1A priority Critical patent/EP2815821A1/fr
Publication of EP2815821A1 publication Critical patent/EP2815821A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B5/00—Washing granular, powdered or lumpy materials; Wet separating
    • B03B5/28—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
    • B03B5/30—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
    • B03B5/32—Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions using centrifugal force
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04B—CENTRIFUGES
    • B04B1/00—Centrifuges with rotary bowls provided with solid jackets for separating predominantly liquid mixtures with or without solid particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04B—CENTRIFUGES
    • B04B5/00—Other centrifuges
    • B04B5/10—Centrifuges combined with other apparatus, e.g. electrostatic separators; Sets or systems of several centrifuges
    • 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
    • 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
    • B22F2202/00—Treatment under specific physical conditions
    • B22F2202/17—Treatment under specific physical conditions use of centrifugal or vortex forces

Definitions

  • the present invention relates to a process and a device for cleaning metal-containing particles forming a powder by removing a compound attached to the particles.
  • the invention can in particular be applied for cleaning metal-containing particles contaminated by oil.
  • This invention relates to the production means of these ultrafine solder powders.
  • powder herein designates here particles having an average diameter of less than 25 ⁇ m.
  • Ultrafine solder powder is produced by dispersing melted metal-containing alloy in a dispersing media.
  • an ingot made of said alloy is provided in a fluid compound.
  • Said ingot is heated to a temperature above the melting temperature of the alloy.
  • a mixture of two fluid phases is thus created: a first fluid phase consisting of the fluid compound and the second fluid phase consisting of the melted alloy.
  • Said mixture is then subjected to shearing strain so as to create an emulsion of melted alloy droplets in the fluid compound.
  • the droplets are then solidified so as to form metal-containing particles that may be used as a solder powder.
  • Oil is a medium usually used to melt metal or alloy and get high dispersion performance.
  • the powder is intended to be mixed with a flux so as to form a solder cream, which is deposited on circuit boards so as to form solder bumps in order to connect electronic components.
  • the cleanliness of the powder is an issue since the presence of a contamination such as oil is likely to deteriorate the quality of the electrical connection.
  • a continuous cleaning process involving the circulation of the particles within a solvent flow and the retention of the cleaned particles by a filter cannot be carried out to clean such a fine powder.
  • the powder since the powder is very dense, it can hardly be rendered fluid enough to be compatible with a solvent flow.
  • Document EP 1 396 551 describes a device for cleaning oil-adhered particles that comprises an agitation tank and a centrifugal apparatus coupled to the agitation tank by a conveying apparatus.
  • the particles are first agitated with a solvent in the agitation tank, then transferred, via the conveying apparatus, to the centrifugal apparatus where the mixture is centrifuged.
  • the centrifugal apparatus includes a central screw intended to separate the particles from the solvent, the particles being directed downwards while the solvent and oil are directed upwards.
  • the particles have to be transferred to the agitation tank in order to be mixed with fresh solvent and then conveyed again to the centrifugal apparatus for the centrifugation step.
  • the cleaning step should be compatible with an industrial process.
  • Such process should also be as short as possible and allow treating large amounts of particles at the same time.
  • a goal of the invention is also to provide a device for carrying out such a process.
  • Said device should allow a shorter cleaning and an easier maintenance (especially washing) that known devices.
  • Said device should also allow repeating the cleaning steps in a simple way, as long as the desired cleanliness has not been obtained.
  • Such device should be of dimensions compatible with an industrial process and should be operated using minimal manpower.
  • An object of the invention is a process for cleaning metal-containing particles, said particles forming a powder, by removing a compound attached to the particles, comprising the following steps:
  • metal-containing particle is meant here a particle that comprises at least one metal; such a particle may be formed of an alloy of two or more metals.
  • the metal-containing particle is made of a solder alloy usable in microelectronics.
  • Step (b) may comprise stirring the composition in the container before centrifuging step (c).
  • ultrasonic treatment of the composition is carried out during stirring.
  • the container is rotated at a rotational speed that is less than the rotational speed of centrifugation step (d).
  • the process may further comprise repeating steps (e) to (g) at least once.
  • the process comprises, after the last fluid phase removal step, the further steps of:
  • the stirred composition may be transferred into a column-shaped container and steps (i) and (j) are carried out in said column-shaped container.
  • An ultrasonic treatment may be carried out during said further stirring step.
  • the average size of the particles is preferably less than 25 micrometer.
  • a further object of the invention is a device for carrying out such a process.
  • Said device comprises:
  • said device further comprises an ultrasonic vibrator extending at least partially into the container.
  • Said device may further comprise a column-shaped container coupled to the rotatable container by a conveying pipe adapted to transfer a composition comprising the solvent and the particles suspended in said solvent from the rotatable container to the column-shaped container.
  • a further object of the invention is a process of manufacturing a powder made of metal-containing particles.
  • Said process comprises:
  • the fluid compound comprises oil.
  • the particles to be cleaned are provided with a compound attached thereto.
  • this compound may have been attached during the manufacturing process of the particles.
  • the compound comprises said medium.
  • the compound may consist of a single component or of a mixture of different components.
  • Examples of compounds that may be attached to the metal-containing particles comprise: residues of organic oils (e.g. synthetic oil, polyolefin oil, vegetable oil such as castor oil), residues of mineral oils (e.g. silicone oil), organic acids, polymer resins, amines, organometallic compounds, metal oxides.
  • organic oils e.g. synthetic oil, polyolefin oil, vegetable oil such as castor oil
  • mineral oils e.g. silicone oil
  • organic acids e.g. synthetic oil, polyolefin oil, vegetable oil such as castor oil
  • organic acids e.g. synthetic oil, polyolefin oil, vegetable oil such as castor oil
  • mineral oils e.g. silicone oil
  • the compound to be removed from the particles is typically oil.
  • solvent is meant herein a fluid wherein a given amount of the compound to be removed from the metal-containing particles can be dissolved at room temperature (25°C).
  • the solubility of the compound in the solvent at room temperature is at least 10 g/l, i.e. it is possible to dissolve at least 10 g of the compound in 1 I of solvent.
  • organic solvents such as non-polar solvents (e.g. pentane, hexane, cyclohexane, benzene, toluene, xylene) or polar solvents (e.g. dimethylformamide (DMF), dimethylsulfoxide (DMSO), acetone, isopropanol), halogenated solvents (e.g. trichloroethane
  • acetone, isopropanol and halogenated solvents can be used as a solvent for castor oil residues.
  • a device for carrying out at least the first steps of the cleaning process is shown in Figure 1 .
  • Said device comprises a container 1 that is intended to receive a composition comprising the particles to be cleaned and a solvent for the compound to be removed.
  • the container has a general symmetry of revolution around a vertical axis X.
  • the container 1 has a bowl shape.
  • horizontal refers to the plane of the ground of the installation where the cleaning device is installed
  • vertical referring to the direction orthogonal to said horizontal plane
  • the container 1 is adapted to be subjected to rotation around its vertical axis, from low rotational speed up to speed suitable for centrifugation of the composition.
  • the container 1 is coupled to a centrifuge 3, in a way that is known per se.
  • the container 1 is advantageously placed in an enclosure that is closed hermetically.
  • the enclosure 10 comprises at least vertical walls 11 surrounding the container, and a cover 12 on top of the walls 11 and allowing access to the container 1, e.g. for maintenance or washing purposes.
  • the cover 12 may advantageously be crossed by a feed pipe 13 that is intended to introduce solvent (if the particles are already in the container) or a suspension comprising particles to be cleaned and solvent into the container.
  • the cover 12 may also be employed as a support for devices that may be used to clean the particles.
  • the device further comprises at least one stirrer 2 arranged at least partially into the container 1 so as to stir said composition.
  • the stirrer typically comprises a motor 20 that is arranged outside of the cover and a stirring component 21 linked to the motor 20 by a rod 22.
  • the stirrer is known per se and will not be described in more detail.
  • the stirrer 2 may be supported by the cover 12.
  • the motor 20 may be arranged above the cover 12 while the rod 22 crosses the cover 12, such that the stirring component 21 is immersed in the composition.
  • the metal-containing particles to be cleaned are put in the container 1, the solvent is put into the container 1 by the feed pipe 13, and the composition is stirred by the stirrer 2.
  • This stirring step has the effect of suspending the particles in the solvent and also of making the compound be at least partially released from the particles and pass into the solvent, thereby washing at least partially the particles.
  • the stirring may be assisted by an ultrasonic treatment that improves the efficiency in removing the compound from the particles.
  • an ultrasonic vibrator 4 is at least partially immersed in the composition during operation of the stirrer 2.
  • the ultrasonic vibrator 4 may be supported by the cover 12.
  • the container may be rotated at a low speed, i.e. a speed that is less than the centrifuging speed, e.g. between 20 and 200 rpm.
  • This rotation at low speed allows homogeneous washing by subjecting the whole powder to the stirrer effect.
  • the stirring step can be omitted if a suspension of the particles within the solvent is directly introduced in the container 1.
  • a first centrifuging step is carried out.
  • the cover 12 supporting the stirrer 2, the feed pipe 13 and optionally the ultrasonic vibrator 4 is removed and replaced by a cover 12' supporting a take-off pipe 13', as shown in Figure 2 .
  • the container 1 is then rotated at high speed by the centrifuge 3.
  • the acceleration is between 300 and 3000 g.
  • the sediment phase S accumulates on the walls of the container 1, whereas the fluid phase F is at least partially extracted by the take-off pipe 13'.
  • the removal of the fluid phase may be carried out during and/or after the centrifugation step.
  • the sequence consisting of stirring and centrifuging the composition is carried out at least twice to improve the cleaning of the particles.
  • the container 1 may also be rotated at a low speed during this stirring step.
  • the cover 12 is removed and replaced by the cover 12', and the container 1 is rotated at the centrifugation speed so as to provide a sediment phase comprising the particles and a fluid phase comprising the solvent and the compound.
  • the stirring steps are carried out in the same container than the centrifuging steps, which avoids conveying the mixture of the particles and the solvent between different devices to carry out the cleaning.
  • This sequence of stirring and centrifuging steps may be implemented as many times as necessary.
  • At least part of the fluid phase is removed from the container 1 and the sediment phase consisting of the cleaned particles can be retrieved.
  • the particles have to be suspended again in a solvent in view of subsequent treatments, e.g. in view in their transfer to another device wherein the cleaning process will be completed.
  • the mixture consisting of the solvent and the suspended particles can be transferred to a column-shape container 5.
  • said container 5 has the general form of a column, i.e. it has an elongated shape extending vertically; for example, the column is a cylinder having a vertical revolution axis.
  • the container 5 may be made of glass. It can thus be easily cleaned and one can easily observe the sedimentation step and determine when sedimentation is completed.
  • the column-shaped container 5 is closed at both ends.
  • the upper end is closed by a cover 51.
  • This cover 51 is crossed by a stirrer 6, a feed pipe 52 for the mixture of the particles and the solvent transferred from the container 1, a feed pipe 53 for fresh solvent, a take-off pipe 54 to remove used solvent for the container 5 and optionally by an ultrasonic vibrator 7.
  • the feed pipe 52 is advantageously coupled to the container 1 by a conveying pipe (not shown) so as to transfer directly the particles in suspension in the solvent from the container 1 to the container 5.
  • the bottom end of the container 5 comprises a collection valve 50.
  • the collection valve 50 is closed.
  • the collection valve 50 is opened when the cleaning is finished, in order to release the cleaned particles from the column-shaped container 5.
  • the mixture is again stirred by the stirrer 6 and, optionally, by the ultrasonic vibrator 7.
  • the sediment phase is thus on the bottom of the column-shaped container 5, the fluid phase being above the sediment phase.
  • the take-off pipe 54 is then lowered down until the sediment phase-fluid phase interface, and the fluid phase is pumped.
  • the collection valve 50 is opened and the clean particles within the solvent are collected.
  • the last cleaning step carried out in the column-shaped container 5 is quicker since there remains only a little amount of compound attached to the particles.
  • said last cleaning step can be carried out in a few hours, whereas it would take several days if the initial amount of the compound was attached to the particles.
  • Another advantage of transferring the cleaned particles in the column-shaped container 5 to complete the cleaning is that this second container is cleaner that the first container 1.
  • the treatment in the column-shaped container allows a separation of the particles according to their mass: during the stirring or the beginning of the sedimentation, coarser particle quickly fall on the bottom of the column, whereas lighter particles stay on the top a longer time. It is thus possible to pump out the lighter (finer) or the heavier (coarser) particles to reach the requested particles size distribution.
  • the above-described cleaning process may advantageously be carried out after a manufacturing process of a powder formed of metal-containing particles, comprising:

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  • Cleaning By Liquid Or Steam (AREA)
EP13305813.1A 2013-06-17 2013-06-17 Procédé et dispositif de nettoyage de métal contenant des particules formant une poudre par élimination d'un composé fixé aux particules Withdrawn EP2815821A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP13305813.1A EP2815821A1 (fr) 2013-06-17 2013-06-17 Procédé et dispositif de nettoyage de métal contenant des particules formant une poudre par élimination d'un composé fixé aux particules

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP13305813.1A EP2815821A1 (fr) 2013-06-17 2013-06-17 Procédé et dispositif de nettoyage de métal contenant des particules formant une poudre par élimination d'un composé fixé aux particules

Publications (1)

Publication Number Publication Date
EP2815821A1 true EP2815821A1 (fr) 2014-12-24

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EP13305813.1A Withdrawn EP2815821A1 (fr) 2013-06-17 2013-06-17 Procédé et dispositif de nettoyage de métal contenant des particules formant une poudre par élimination d'un composé fixé aux particules

Country Status (1)

Country Link
EP (1) EP2815821A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106391331A (zh) * 2016-11-07 2017-02-15 品第信息科技（上海）有限公司 一种热熔材料提纯方法及装置
CN106540821A (zh) * 2016-10-31 2017-03-29 广西大学 一种用于清洗回收铝合金的设备

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4019232A1 (de) * 1990-06-15 1991-12-19 Akad Wissenschaften Ddr Verfahren zur aufbereitung oelverschmutzter, feinteiliger metallischer rueckstaende
WO1992022620A1 (fr) * 1991-06-12 1992-12-23 Rig Technology Limited Depollution de materiaux contamines par des hydrocarbures
WO1993002221A2 (fr) * 1991-07-15 1993-02-04 Minnesota Mining And Manufacturing Company Procede de production de particules fines a partir d'un metal a bas point de fusion
WO2000000313A2 (fr) 1998-06-29 2000-01-06 Schulze Juergen Dispositif et procede de fabrication sans pression de metal d'apport de brasage tendre en poudre
US20030177865A1 (en) * 2002-03-19 2003-09-25 Takao Ono Process of producing metal powders
EP1396551A1 (fr) 2001-05-30 2004-03-10 Nippon Steel Corporation Dispositif et procede de traitement de particules souillees d'huile
US7608461B1 (en) * 2005-09-16 2009-10-27 Sandia Corporation Surface engineered nanoparticles for improved surface enhanced Raman scattering applications and method for preparing same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4019232A1 (de) * 1990-06-15 1991-12-19 Akad Wissenschaften Ddr Verfahren zur aufbereitung oelverschmutzter, feinteiliger metallischer rueckstaende
WO1992022620A1 (fr) * 1991-06-12 1992-12-23 Rig Technology Limited Depollution de materiaux contamines par des hydrocarbures
WO1993002221A2 (fr) * 1991-07-15 1993-02-04 Minnesota Mining And Manufacturing Company Procede de production de particules fines a partir d'un metal a bas point de fusion
WO2000000313A2 (fr) 1998-06-29 2000-01-06 Schulze Juergen Dispositif et procede de fabrication sans pression de metal d'apport de brasage tendre en poudre
EP1396551A1 (fr) 2001-05-30 2004-03-10 Nippon Steel Corporation Dispositif et procede de traitement de particules souillees d'huile
US20030177865A1 (en) * 2002-03-19 2003-09-25 Takao Ono Process of producing metal powders
US7608461B1 (en) * 2005-09-16 2009-10-27 Sandia Corporation Surface engineered nanoparticles for improved surface enhanced Raman scattering applications and method for preparing same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106540821A (zh) * 2016-10-31 2017-03-29 广西大学 一种用于清洗回收铝合金的设备
CN106540821B (zh) * 2016-10-31 2019-07-12 广西大学 一种用于清洗回收铝合金的设备
CN106391331A (zh) * 2016-11-07 2017-02-15 品第信息科技（上海）有限公司 一种热熔材料提纯方法及装置

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