DE1607454A1 - Verfahren zur Herstellung von feinteiligem Metallpulver - Google Patents

Verfahren zur Herstellung von feinteiligem Metallpulver

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Publication number
DE1607454A1
DE1607454A1 DE19671607454 DE1607454A DE1607454A1 DE 1607454 A1 DE1607454 A1 DE 1607454A1 DE 19671607454 DE19671607454 DE 19671607454 DE 1607454 A DE1607454 A DE 1607454A DE 1607454 A1 DE1607454 A1 DE 1607454A1
Authority
DE
Germany
Prior art keywords
metal
organic
grinding
metal powder
less
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.)
Pending
Application number
DE19671607454
Other languages
English (en)
Inventor
Groszek Aleksander Jerzy
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.)
BP PLC
Original Assignee
BP PLC
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 BP PLC filed Critical BP PLC
Publication of DE1607454A1 publication Critical patent/DE1607454A1/de
Pending legal-status Critical Current

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    • C10M5/00—Solid or semi-solid compositions containing as the essential lubricating ingredient mineral lubricating oils or fatty oils and their use
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
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Description

Verfahren zur Herstellung von feinteiligem Metallpulver
Die Erfindung betrifft verbesserte Metallpulver, insbesondere Metallpulver mit großer Oberfläche.
Feine Metallpulver werden zur Herstellung von Metallgegenständen (durch Sintern der Pulver), als Pigmente, als Füllstoffe für Kunststoffe, als Reagentien, als Raketentreibstoffe, Hart- und Weichlötmittel usw. verwendet.
Es ist bekannt, Metallpulver auf chemischem Wege, ζ.Β* durch Kondensation der Dämpfe oder durch Ausfällung aus Lösung, herzustellen, jedoch ist festgestellt worden, daß mechanisches Mahlen im allgemeinen eine billigere Methode zur Herstellung dieser Pulver ist. Als Vortichtungen zum Mahlen eignen sich beispielsweise Planetenkugelmühlen, Abriebkugelmühlen und Kugelschwingmühlen.
Es ist ferner seit einiger Zeit bekannt, das Mahlen von Metallen in einer Mahlflüssigkeit, z.B. einer Erdölfraktion, Äthanol, Methylendichlorid oder n-Heptan usw., durchzuführen. Ferner ist die Verwendung von Mahlhilfsstoffen, z.B. Fettsäuren und ihren Metallsalzen, beispielsweise Stearinsäure und Aluminiumstearat, bekannt. Nähere Einzelheiten hierüber finden sich in "Ultrafine Particles" von W.E. Kuhn, heraus-
909836/0740
gegeben von Wiley 1963. Es wird angegeben, daß ein Mahlhilf sstoff die Aufgabe hat, Agglomerierung der gemahlenen Teilchen während des Mahlens zu verhindern.
Die nach bekannten Verfahren hergestellten Metallpulver haben jedoch die Nachteile einer kleinen Oberfläche und geringer Schmierwirkung.
Gegenstand der Erfindung sind feinteilige Metallpulver, die eine große Oberfläche und hohe Reaktionsfähigkeit haben und als Festschmiermittel wirksam sind.
Gemäß der Erfindung wird ein feinteiliges Pulver hergestellt durch Mahlen eines Metalls in Gegenwart einer organischen Halbflüssigkeit und eines organischen Zusatzstoffes, der die Schmierfähigkeit und die Hochdruckeigenschaften verbessert und eines oder mehrere der Elemente Schwefel, Chlor, Phosphor und Stickstoff enthält.
Als organische Mahlflüssigkeiten eignen sich Flüssigkeiten, die unter 50O0C destillieren, eine Viskosität von weniger
ο Oberflächenspannung als 600 cS bei 37|8 C und eine sriefe«**^^«; von weniger als 72 Dyn/cm bei 250O, vorzugsweise von 10 bis 40 Dyn/cm bei 250C haben. Bei einer bevorzugten Ausführungsform der Erfindung dient als Mahlflüssigkeit ein Kohlenwasserstoff, insbesondere beispielsweise n-Heptan, Isooctan, Cyclohexan, Toluol, Hexadecan oder eine durch Destillation von Erdöl erhaltene Kohlenwasserstofffraktion.
Organische Zusatzstoffe, diedie Tragfähigkeit verbessern, sind bekannt und werden weitgehend in Schmiermitteln verwendet. Sie haben die Aufgabe, die verschleißmindernden Eigenschaften und/oder die Höchstdruckeigenschaften der Schmiermittel zu verbessern. Wenn zwei geschmierte bewegte Flächen unter leichter Belastung aufeinander gleiten, sind sie durch einen elastisch-hydrodynamischen Ölfilm getrennt. Mit zunehmender Belastung wird die Dicke des Ölfilms geringer. Wenn die Ölfilmdicke die Dimensionen der Oberflächenrauhigkeit erreicht, wird der Film von Unebenheiten der Oberfläche durchdrungen.· In diesem Bereich setzt die Wirkung der ver-
909836/0746 BAD original
sehleißmindernden Zusätze ein, die die festigkeit des Ölfilms verbessern und dadurch die Berührung zwischen den Metallen verringern. Bei weiterem Anstieg der Belastung fällt der größte Teil des Ölfilms zusammen, und die verschleiß— verhindernden Zusätze genügen nicht mehr zum Schutz der Oberfläche. Höchstdruckzusätze werden in diesem Bereich wirksam, indem sie mit den Metalloberflächen zu einer anorganischen Eisenverbindung reagieren, die ein Fressen der aufeinander gleitenden Metallfächen nicht zulassen.
Der Ausdruck "Zusätze, die die Tragfähigkeit und Druckaufnahmefähigkeit verbessern", nachstehend kurz als "Hochdruckzusätze" bezeichnet, umfaßt sowohl verschleißverhindernde Zusätze-als auch Höchstdruckzusätze.
Für die Zwecke der Erfindung eignen sich Hochdruckzusätze, die eines oder mehrere der folgenden Elemente enthalten: Chlor, Schwefel, Phosphor und Stickstoff. Beispiele geeigneter Hochdruckzusätze sind organische chlorhaltige Verbindungen, z.B. die niedrigmolekularen chlorierten Kohlenwasserstoffe, vorzugsweise solche mit 1-4 C-Atomen, z.B. tetrachlorkohlenstoff, Chlorbenzylester von Alkylxanthinsä-uren und Thiosäuren, z.B. Thiocarbonsäure und chlorierte Kohlenwasserstoffwaohse·
Als Hochdruckzusätze eignen sich ferner die covalenten schwefelhaltigen Verbindungen, z.B. Diphenolpolysulfide, beispielsweise Di-(4-hydroxyphenol)polysulfid, Alkyl- und Arylthioäther, Alkyl- und Arylthiocarbonate und -thiocarbamate, schwefelsubstituierte Carbonsäureester, z*B. Essigsäureester, die in α-Stellung durch Schwefel substituiert sind, geschwefelte Polymere, z.B. geschwefelte Copolymere von Butadien-1,3 und Styrol, das Reaktionsprodukt von Schwefel und Polyalkylenglykolen, Alkyldisulfide, z.B. Di-n-butyldisulfid- und Di(2-äthylhexyl)disulfid, und Biaryldisulfide, z.B. Dibenzyldisulfid und Di-(aminobenzyl)disulfid.
Weitere geeignete. Hochdruckzusätze sind die phosphorsulfurisierten organischen Verbindungen« Typische organische Materialien, die phosphorsulfurisiert werden können, sind
909836/07A6 . B
I bU
- 4 -
saueretoffhaltIge Wachse, chlorierte Phenole, wacheartige Ester, cyclische Ketone, hydriertes Spermazetöl, Ester von ungesättigten Säuren, z.B. Glykol- und Glyceryloleate, und Abietinsäureester.
Weitere geeignete Hochdruckzusätze sind die organischen Verbindungen, die Phosphat- oder Thiophosphatgruppen enthalten, z.B. triaromatische Phosphate, beispielsweise Trikresylphosphat, Trialkylphosphate, z.B. Trifebutylphosphat, und Metalldialkyldithiophosphate, z.B. die Zinkdialkyldithiophosphate. Metanorganische Verbindungen, z.B. Organozinndithiosphosphate und BIeinaphthenat, können ebenfalls als Hoohdruokzusätze verwendet werden.
Zu den geeigneten stickstoffhaltigen Verbindungen gehören Phosphors? midate, z.B. die in der britischen Patentschrift 899.101 beschriebenen, Nitrobenzole, Nitronaphthalint,
AMiinphosphate, Tetraalkylammoniumphosphate und -thiophosphate, und Ehodanin und Rhodaninderivate.
Alle Verbindungen, die die Tragfähigkeit und Druokaufnahmefähigkeit von Schmiermitteln verbessern, können für die Zweoke der Erfindung verwendet werden. Wenn die org/anische Mahlflüssigkeit ebenfalls ein Hochdruckzusatz ist, z.B. Tetrachlorkohlenstoff, brauoht kein weiterer Hochdruckzusatz zugesetzt zu werden.
Beliebige Metalle oder Legierungen, die gemahlaa werden können, eignen sich für die Zwecke der Erfindung. Bevorzugt als Metalle werden Eisen einschließlich Flußstahl und Gußeisen, und Aluminium. Weitere geeignete Metalle sind die Übergangsmetalle, z.B. Nickel, Kobalt, Chrom und Titan, Kupfer und Kupferlegierungen, wie Messing.
Bei einer bevorzugten Ausführungsform der Erfindung wird eine mit hoher Geschwindigkeit arbeitende Kugeisohwingmühle verwendet. Die Mahlkugeln bestehen vorzugsweise aus gehärtetem Stahl* Das Mahlen wird vorzugsweise durchgeführt, bis das gebildete Metallpulver eine Oberfläche von wenigstens
909836/0746
BAD GTu^
2 m /g und vorzugsweise ein Schüttgewioht nach dem Einrütteln von weniger als 1 g/onr hat«
Bs wird angenommen, daß die Hochdruokzusätze an der Oberfläche der Metallteilchen adsorbiert werden und daß in gewissen !"allen eine Schicht aus chemisch umgesetztem Material auf der Metalloberfläche während des Mahlens gebildet wird. Beispielsweise kann Tetrachlorkohlenstoff mit der Oberfläche von Teilchen von feingemahlenem Eisen übt er Bildung von Eisenchloriden usw. reagieren.
Allgemein ist der Hochdruckzusatz um so wirksamer in der Bildung der feinteiligen Metallpulver gemäß der Erfindung, je besser seine Hochdruckeigenschaften sind. Hochdruokzusätze können jedoch bei Verwendung mit verschiedenen Metallen unterschiedliche Wirksamkeit haben, und es ist zweckmäßig, bei der Wahl des Hochdruckzusatzes das zu mahlende Metall zu berücksichtigen.
Es wurde überraschenderweise gefunden, daß die gemäß der Erfindung hergestellten Metallteilchen gute Hochdruckeigenschaften , d.lu Schmierfähigkeit und Druckaufnahmefähigkeit, aufweisen. Aufgrund dieser Eigenschaften eigenen sich die Pulver für die Herstellung von verstärkten, selbstschmierenden Kunst st off lagern, z.B«. für Nylonlager, die mit Eisen gefüllt sindo Aufgrund der Natur der Metalloberflächen eignen sich die erfindungsgemäßen Pulver besonders als !Füllstoffe , für Kunststoffe im allgemeinen oder als Pigmente, Eefcalysatoren usw..
Es wurde ferner überraschenderweise gefunden, daß die feinteiligen Metallpulver gemäß der Erfindung als Verdickungsmittel für Schmierfette verwendet werden können. Zur Herstellung eines Schmierfettes kann das feinteilige Metall einfach in ein Grundöl eingerührt werden, oder es können beliebige Verfahren zur Herstellung von Schmierfetten angewendet werden, die in der deutschen P at ent sehrif t., .*.,..»« (Patentanmeldung B 89074 XV o/23o) der Anmelderin beschrieben sind.
*■· Ό ·■*
Beispiel
Eisenpulver wurde in einer Kugelsohwingmühle "Megapaet · Mark I" (Hersteller Bilamec Limited) 3 Stunden gemahlen. In dieser Mühle bestehen die Mahlräume aus Stahlzylindern von 38 mm Innendurchmesser und 38 cm Länge. Sie sind mit gehärteten Stahlkugeln von 6,35 mm 0 fast gefüllt. Die Mühle ist mit einem Elektromotor von 1/8 HP versehen, und die Schwingung kann von 1-4 mm eingestellt werden. Im Betrieb wurde jeder Zylinder vollständig mit n-Heptan gefüllt, in dem ein Hochdruckzusatz gelöst war, worauf die Stahlkugeln und 10-30 g Eisenpulver, dessen Teilchen ein Sieb einer Masohen— weite vonTY-295 /^/zugesetzt wurden. Hierauf blieben etwa 150-250 ml n-Heptan in jedem Zylinder. Die Enden wurden dann mit Metallkappen verschlossen, die mit Gummidichtungen versehen waren, worauf gemahlen wurde. Nach dem Mahlen wurden die Kugeln von der Aufschlämmung aus Eisenpulver und n-Heptan.sowie Hochdruckzusatz abgesiebt, und das behandelte Eisenpulver wurde durch Filtration, Waschen und Trocknen gewonnen.
Die Oberflächen und Schüttgewichte, die unter Verwendung verschiedener Zusatzstoffe erhalten wurden, sind nachstehend in Tabelle I angegeben.
Versuch Ho chdruckzus at ζ ά Zusatzmenge 1,0 1,0 I» luLver ge Im Pulver ge des Eis« Jhe Schütt-
Nr· in n-Heptan Dibenzy^ulfid in Grew.-# 2,0 2,0 fundener S, fundenes Cl m2/gerS)
η von n-Heptan phosphorsulfurisier- 0,5 0,5 Gew«-$ des in Gew.-# des 2 m" Einrütteln.
1 β plus Z us at as tes Terpen „ Pulvers !Silvers : 5 g/em3 #
2 Tetrachlorkohlen - η η 0,5 - - 1,35
stoff 0,5 H-Laurylphosphor- _ 30 mm
3 -.amidat 7
4 1,0 Zinkdithiophosphat - 0,03 3 0,39
5 2,0 - - 2 0,40
tf-k 6 0,5 0,66 - 3 -
\JLJ
O 		7 1,0 0,14 - 2 0,40
co
CX) 		8 2,0 0,07 2 -
u>
cn ι		 9 Di-tert-butyldisulfid 0,5 0,22 - 2 -
f—\ 10 η η 0,13 - 2 0,52
CJ 11 u n 0,16 - 7
cn 12 0,24 5
13 0,5 - 7 0,30
14 0,16 - 0,34
3 «■
15
—
* Das Sohüttgewicht wurde wie folgt gemessen: Ein Teil des feinteiligen Metalls wurde in einen Meßzylinder gefüllt und eingerüttelt, "bis das gemessene Tolumen konstant war, worauf die Pulvermenge gewogen wurde.
Die Werte in dieser Tabelle zeigen, daß mit Tetrachlorkohlenstoff die größte Oberfläche beim Mahlen von Eisenpulver gemäß der Erfindung erzielt wird. Ferner ist ersichtlich, daß mit bestimmten Konzentrationen der Hochdruckzusätze eine optimale Vergrößerung der Oberfläche erhalten wird.
Nickel-jMolybdän- und Chrompulver wurden ebenfalls in n-Heptan in Gegenwart von Tetrachlorkohlenstoff gemahlen. Die Ergebnisse sind nachstehend in Tabelle II angegeben.
Metall
Hochdruckzusatz in n-Heptan
Zusatzmenge in Gew.-^ von n-Heptan plus Zusatz
B.E.T.Oberfläche
des Pulvers
in m2/g
Sohüttgewicht nach Einrütteln
1.ITi
2.Ni
3.Ni μ 4.Mo « 5.Cr μ
6.ungemah- u lenes Ni
7.ungemah- " lenes Gr
Tetrachlorkohlenstoff
1 2
100 ** 1 1
2
4
4
0,34
0,44 0,34 3,5
3,87
** Die Mahlflüssigkeit bestand ausschließlich aus Tetrachlorkohlenstoff,
Die Tragfähigkeit der Pulver wurde gemessen, indem Dispersionen der Pulver in einem Grundöl in einem VierkugeVgerät geprüft wurden. Die Ergebnisse sind nachstehend in Tabelle III angegeben«
90 9 8 36/0746
Tabelle III
Grundöl Im öl dispergierter Peststoff- Verschleiß, Peststoff menge im öl, gemessen am
Gew.-fo Durchmesser der Anschliff-Fläche Belastung 115 kg 30 Minuten
1. Medizini
sches
Paraffinöl		 "oleophiler" Graphit* - 5 Pestfressen in
weniger als
1 Minute
2. dto. 11 oleophiles" MoS2** 5 4,0 mm in 1 Min.
3- tt Eisenpulver in
n-Heptan gemahlen,
kein Zusatz		 10 0,99 mm in
50 Minuten
4. tt Eisen Nr. 2 10 Pestfressen in
weniger als
1 Minute
5. H EisenNr. 11 10 l,08 mm in
30 Minuten
6. t! 2,21 mm in
30 Minuten
Siehe deutsche Patentschrift.......
(Patentanmeldung B 89 077 IVa/l2i)
Siehe deutsche Patentschrift
(Patentanmeldung B 89 075 IVa/l2n)
Die Werte dieser Tabelle zeigen, daß das behandelte Eisen dem "oleophilen" Molybdändisulfid, das ausgezeichnete "Höchstdruckfestigkeit" hat, hinsichtlich der Tragfähigkeit und Druckaufnahmefähigkeit gleichwertig ist.
Die Hochdruckfestigkeit eines erfindungsgemäß hergestellten und in einem Grundöl BG 160/95 dispergierten Eisenpulvers wurde in einem Vierkugelprüfgerät ermittelt. Dieses Grundöl hat eine Redwood I-Viskosität von l60 Sekunden bei 60°C und einen Viskositätsindex von 95· Die Ergebnisse sind nachstehend in Tabelle IV genannt.
909836/0746
Tabelle IV
Grundöl 1. BG l6O/95 2. BG l6o/95
Im öl dispergierter Feststoff - Eisen Nr. 2 Peststoffmenge im öl, Gew.-%
Durchmesser der Anschlifffläche
Belastung 15 kg, 60 Minuten Belastung 115 kg, 50 Minuten Mittlere Hertz-Belastung
O ,80 mm 0, 76 mm
2 ,64 mm 1, 5 mm
22 ,6 .28, 7
909836/0746

Claims (6)

Patentansprüche
1.) Verfahren zur Herstellung von feinteiligem Metallpulver durch Mahlen eines Metalls in einer organischen Flüssigkeit, dadurch gekennzeichnet, daß' man als organische Mahlflüssigkeit solche mit einem Siedepunkt unter 5OO°C, einer Viskosität von weniger als 600 cS bei 380C und einer Oberflächenspannung von weniger als 72 Dyn/cm bei 25°C und mit einem Gehalt an die Belastbarkeit verbessernden, eines oder mehrere der Elemente Schwefel, Phosphor, Chlor und Stickstoff enthaltenden Schmiermittel-Zusatzstoffen verwendet . ">
2.) Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man als Mahlflüssigkeit Kohlenwasserstoffe verwendet.
3.) Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß man als Zusatzstoffe niedrigmolekulare chlorierte Kohlenwasserstoffe, phosphorsulfurierte organische Verbindungen, organische Schwefelverbindungen, organische Phosphate und Thiophosphate oder Phosphoramidate verwendet .
4.) Verfahren nach Anspruch 1 bis J, dadurch gekennzeichnet, daß man das Metall in einer Kugelschwingmühle bis zu einer Oberfläche des Metallpulvers von mindestens 2 m /g und einem Schüttgewicht von weniger als 1 g/cnr mahlt.
5.) Verfahren nach Anspruch 1 bis 4, dadurch gekennzeichnet, daß man die die Belastbarkeit verbessernden Zusätze in einer dem Gewicht des Metalles entsprechenden oder geringeren Menge verwendet,
6.) Verwendung der Metallpulver nach Anspruch 1 bis 5 als Pestschmiermittel.
909#36/0746
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FR2701271B1 (fr) * 1993-02-05 1995-04-28 Michel Fontaine Produit remétallisant lubrifiant destiné notamment à des moteurs thermiques de véhicules.
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US3409549A (en) * 1965-10-22 1968-11-05 Freeman Michael Walter Compositions and articles including non-pyrophoric microparticles

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FR2003424B1 (de) 1974-05-24
SE331942B (de) 1971-01-18
GB1198445A (en) 1970-07-15
US3532623A (en) 1970-10-06
NL6903600A (de) 1969-09-09
NL6710818A (de) 1968-02-06
GB1255172A (en) 1971-12-01
AT299559B (de) 1972-06-26

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