GB2259309A - Ceramic particles - Google Patents

Ceramic particles Download PDF

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Publication number
GB2259309A
GB2259309A GB9119239A GB9119239A GB2259309A GB 2259309 A GB2259309 A GB 2259309A GB 9119239 A GB9119239 A GB 9119239A GB 9119239 A GB9119239 A GB 9119239A GB 2259309 A GB2259309 A GB 2259309A
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GB
United Kingdom
Prior art keywords
melt
ceramic particles
aluminium
metal
dispersion
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Withdrawn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
GB9119239A
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GB9119239D0 (en
Inventor
Peter Davies
James Leslie Frederick Kellie
John Vivian Wood
John Richard Charlton
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.)
London and Scandinavian Metallurgical Co Ltd
Original Assignee
London and Scandinavian Metallurgical Co Ltd
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 London and Scandinavian Metallurgical Co Ltd filed Critical London and Scandinavian Metallurgical Co Ltd
Priority to GB9119239A priority Critical patent/GB2259309A/en
Publication of GB9119239D0 publication Critical patent/GB9119239D0/en
Publication of GB2259309A publication Critical patent/GB2259309A/en
Withdrawn legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides whether added as such or formed in situ
    • C22C32/0047Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14Methods for preparing oxides or hydroxides in general
    • C01B13/145After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/06Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00Boron; Compounds thereof
    • C01B35/02Boron; Borides
    • C01B35/04Metal borides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

The invention provides a method of making a concentrated supply of ceramic particles which are readily wettable when added to an aluminium-based melt. The method companies forming a dispersion of ceramic particles (preferably titanium diboride) in a metal melt (preferably aliuminium) such that the ceramic particles are thoroughly wetted by the melt, solidifying the melt, and extracting metal from the solidified dispersion (preferably by caustic soda treatment where the melt comprises aluminium). The resulting supply of ceramic particles can then be dispersed in an aluminium-based melt under easily producible conditions (generally under ambient atmosphere, and at less than 1000 degrees C), with full wetting of the particles. The preferred method of producing the initial dispersion is by an in situ reaction of titanium and boron, which are preferably formed by reaction of aluminium in the melt with salts containing boron (preferably KBF4) and titanium (preferably K2TiF6).

Description

Ceramic Particles This invention relates to making a concentrated supply of ceramic particles which are readily wettable when added to an aluminium-based melt, such as a melt of aluminium or of an aluminium alloy.
A considerable amount of work has been carried out on incorporating ceramic particles into metals to improve their mechanical properties such as stiffness, and to improve their performance at elevated temperatures. It is important that in the resulting metal matrix composite material the ceramic particles are fully wetted by the matrix metal, since otherwise the mechanical properties such as strength will be impaired.
U.S. Patent Specification No. 3037857 (assigned to Union Carbide) teaches making an aluminium-based metal matrix composite by adding pre-formed particles of a boride such as titanium diboride to aluminium or an aluminium alloy. For relatively low boride particle loadings this may be accomplished by adding them to an aluminium melt. However, U.S. 3037857 teaches making the addition at 1200 degrees C in a vacuum or under an argon atmosphere. The preferred method taught in U.S. 3037857, to obtain higher particle loadings, is to dry-blend powders of the boride and of the aluminium-based metal matrix cold, compact the blend at high pressure, and then heat to between 1000 and 1150 degrees C. For both techniques taught in U.S. 3037857, having to provide the conditions required considerably increases the cost of operating the process.Further, the surfaces of pre-formed ceramic particles formed by known techniques are contaminated, especially when the particles have been subjected to a comminution process, and neither technique taught in U.S. 3037857 can be relied upon to achieve full ceramic particle wetting regardless of the contaminants on the particle surfaces. U.S. 3037857 illustrates the difficulties which are experienced when trying to achieve adequate wetting of the ceramic particles when incorporating pre-formed ceramic particles into a matrix metal melt.
An alternative way of incorporating ceramic particles into a metal matrix melt is to form the ceramic particles by an in situ chemical reaction within the melt; see, for example, European Patent Specification No.
EP 0113249 A (Alcan International), and the specification of our U.K.
patent application No , filed on 9th September, 1991 and entitled "Metal Matrix Alloys". However, for some purposes it is desirable to achieve a level of ceramic particle loading which is greater than is achievable by such means.
According to the present invention, there is provided a method of making a concentrated supply of ceramic particles which are wettable when added to an aluminium-based melt, the method comprising forming a dispersion of ceramic particles in a metal melt such that the ceramic particles are thoroughly wetted by the melt, solidifying the melt, and extracting metal from the solidified dispersion, whereby to increase the concentration of ceramic particles in the dispersion.
We prefer that the metal melt in which the dispersion of ceramic particles is formed is an aluminium-based melt, such as a melt of an aluminium alloy or, preferably, aluminium. In such cases, the preferred method of performing the step of extracting metal from the solidified dispersion comprises alkali-leaching it to extract aluminium, preferably with an aqueous solution comprising caustic soda.
We have found that, as soon as sufficient metal is extracted from the solidified dispersion that the remaining product is of particulate form, then that product can be highly concentrated in ceramic particles. For example, where the matrix metal is aluminium and the ceramic particles are of titanium diboride, the resulting product at that stage contains only about 10% by weight aluminium. However, we generally prefer that substantially all of the metal should be extracted from the solidified dispersion.
For most applications, it is preferable that the ceramic particles should be sufficiently fine that the majority of the ceramic particles are of mass equivalent to spheres which are less than 1 micron in diameter; that is readily achievable using the following teachings. However, in some applications, e.g. where the particles are to provide abrasion resistance, the ceramic particles may usefully be coarser.
Although generally not the best method, formation of the initial dispersion of ceramic particles in a metal melt may be carried out by introducing pre-formed ceramic particles into the metal melt. As will be appreciated from the prior art discussion above, care will be needed in sourcing the ceramic particles, and considerable care will have to be taken to provide conditions to ensure that the ceramic particles are fully wetted by the metal melt. Nevertheless, in some circumstances it may worthwhile for a bulk producer to make the necessary arrangements, so that customers producing final metal matrix composites are relieved of individually having to make such arrangements.
In general, we greatly prefer that the dispersion of ceramic particles in the metal melt should be formed by reacting, within the metal melt, precursors for the ceramic particles.
The ceramic particles used in the method of the present invention may be any suitable ceramic particles such as one or more of the refractory oxides, silicides, borides, nitrides or carbides, for example. We generally prefer that the ceramic particles should be substantially insoluble in, and unreactive with, the metal melt in which they are dispersed in the method of the invention. It is not necessary for the ceramic particles to be of the same chemical composition; mixtures of different types of ceramic particles may be used. Nor is it necessary for them to be chemically pure; their metal constituents may be mixed (tungsten titanium carbide, for example) and/or their non-metal constituents may be mixed (titanium carbonitride, for example). The ceramic particles may be of any suitable shape, such as granular, tabular, acicular or fibrous, for example.
In accordance with a preferred embodiment of the invention, the ceramic particles comprise titanium boride, preferably titanium diboride. In practising this embodiment we prefer that the metal melt is an aluminium-based melt; and: (a) a boron-containing salt (preferably potassium borofluoride, KBF4) is reacted with aluminium within the melt to produce boron, which then reacts with titanium within the melt; and/or (b) a titanium-containing salt (e.g. potassium fluorotitanate, preferably potassium hexafluorotitanate, K2TiF6) is reacted with aluminium within the melt to produce titanium, which then reacts with boron within the melt.
These procedures are generally as employed in the grain refiner art for making titanium-boron-aluminium grain refiners. Preferably, both (a) and (b) apply; in such cases the boron-containing and titanium-containing salts are preferably added as a mixture (generally in stoichiometric proportions) at a controlled rate. However, (a) may apply without (b) (e.g. where the metal melt is an aluminium-titanium alloy); and (b) may apply without (a) (e.g. where the metal melt is an aluminium-boron alloy). We recommend that the reaction temperature be kept below 1000 degrees C, and that the reaction should be carried in an electric induction furnace.
We have found that a concentrated supply of ceramic particles made in accordance with the teachings of the invention can surprisingly easily be incorporated into an aluminium-based melt with full wetting of the ceramic particles. In particular we have found it possible to achieve such incorporation with aluminium-based melts which are at substantially less than 1000 degrees C, and also when the incorporation is carried out in air.
We expect that it will be possible to incorporate a concentrated supply of ceramic particles made in accordance with the invention with similar ease into other melts (e.g. magnesium-based melts), also with full wetting of the ceramic particles.
A concentrated supply of ceramic particles made in accordance with the invention may also be used to make a metal matrix composite, by forming a mixture comprising a supply of suitable matrix metal (such as aluminium or an aluminium alloy, for example, or any other metal which when molten will wet the ceramic particles) and the concentrated supply of ceramic particles, and subjecting the mixture to a suitable powder metallurgical process. Use of such a procedure can attain relatively high ceramic particle loadings, in the resulting metal matrix composite, such as from 15 up to about 60 weight percent. Because of the good wettability of the ceramic particles, the resulting metal matrix composite can be expected to have good mechanical properties such as strength.
In order that the invention may be more fully understood, an embodiment in the accordance therewith will now be described in the following Example, with reference to the single Figure of the accompanying drawing, which shows a micrograph formed by a scanning electron microscope, at a magnification of 7000, of the titanium diboride particles produced in the Example.
Example Approximately 20 kg of aluminium was melted in a carbon bonded silicon carbide crucible by induction heating. At a starting temperature of 660 degrees C an intimate mixture of K2TiF6 and KBF4 was fed into the aluminium while stirring the aluminium by induction. The K2TiF6 and KBF4 salts were in the stoichiometric ratio required to produce titanium diboride, TiB2, ceramic particles. The exothermic heat of reaction caused the temperature of the melt to rise but was kept below 1000 degrees C.
Sufficient salt was reacted to produce a melt of aluminium with approximately 8 wt.% TiB2. Potassium aluminium fluoride produced as a by-product of the reaction was removed from the surface of the melt. The resulting dispersion of titanium diboride particles in aluminium was then cast to billet. Most of these TiB2 particles are below one micron in diameter, as seen under an optical microscope.
A 100 g piece taken from the billet was placed in a glass beaker, and about 1 1 of 17 percent aqueous caustic soda solution at about 20 degrees C was added to it. The resulting mixture was heated to about 60 degrees C and maintained under agitation until substantially all of the aluminium had been extracted, after about one hour. The residue was allowed to settle, washed by decantation in distilled water and dried.
A sample of the resulting TiB2 particles is shown in the Figure, from which it can be seen that the particles are of generally tabular (i.e. plate-like) shape, typically having a diameter of about 2.5 microns or less and a thickness of about 0.1 micron. Thus, the majority are equivalent in mass to spherical particles of less than 1 micron in diameter; this accords with what was observed under the optical microscope prior to extraction of the aluminium.
1 g of the extracted TiB2 particles was then added to the surface of a melt of 100 g of aluminium held at 730 degrees C in a alumina crucible.
The surface of the aluminium melt was cleaned, by skimming it, immediately prior to adding the TiB2 particles, and the melt was gently stirred during the addition. As soon as they were added to the melt surface, the TiB2 particles were seen to be wetted by the melt, and they then sank into it.
When the same quantity of TiB2 particles supplied by Rhone-Poulenc Chemicals Limited and having an average particle size of 11.8 microns was added in the same manner to an aluminium melt which had been heated and skimmed in the same way and was similarly stirred during the addition, the majority of the particles remained on the melt surface and were pushed to the side of the crucible. Thus, they were clearly not wetted by the melt.

Claims (22)

Claims
1. A method of making a concentrated supply of ceramic particles which are wettable when added to an aluminium-based melt, the method comprising forming a dispersion of ceramic particles in a metal melt such that the ceramic particles are thoroughly wetted by the melt, solidifying the melt, and extracting metal from the solidified dispersion, whereby to increase the concentration of ceramic particles in the dispersion.
2. A method according to claim 1, wherein the metal melt in which the dispersion of ceramic particles is formed is an aluminium-based melt.
3. A method according to claim 2, wherein the metal melt in which the dispersion of ceramic particles is formed is a melt of aluminium metal.
4. A method according to claim 2 or claim 3, wherein the solidified dispersion is alkali-leached to extract aluminium, preferably with an aqueous solution comprising caustic soda.
5. A method according to any one of claims 1 to 4, wherein sufficient metal is extracted from the solidified dispersion that the remaining material is of particulate form.
6. A method according to claim 5, wherein substantially all of the metal is extracted from the solidified dispersion.
7. A method according to any one of claims 1 to 6, wherein the majority of the ceramic particles in the product are of mass equivalent to spheres which are less than 1 micron in diameter.
8. A method according to any one of claims 1 to 7, wherein the dispersion of ceramic particles in the metal melt is formed by reacting, within the metal melt, precursors for the ceramic particles.
9. A method according to any one of claims 1 to 8 wherein the ceramic particles comprise titanium diboride.
10. A method according to claim 9, wherein the metal melt is an aluminium-based metal, and a boron-containing salt is reacted with aluminium within the melt to produce boron, which then reacts with titanium within the melt.
11. A method according to claim 10, wherein the boron-containing salt is potassium borofluoride, KBF4.
12. A method according to any one of claims 9 to 11, wherein the metal melt is an aluminium-based melt, and a titanium-containing salt is reacted with aluminium within the melt to produce titanium, which then reacts with boron within the melt.
13. A method according to claim 12, wherein the titanium-containing salt is potassium fluorotitanate.
14. A method according to claim 13, wherein the titanium-containing salt is potassium hexafluorotitanate, K2TiF6.
15. A method according to any one of claims 9 to 14, wherein the ratio of titanium to boron is substantially stoichiometric.
16. A method of making a concentrated supply of ceramic particles, substantially as described in the foregoing Example.
17. A method according to any one of claims 1 to 16, including the additional step of dispersing the product concentrated supply of ceramic particles into an aluminium-based melt.
18. A method according to claim 17, wherein the temperature of the melt into which the product concentrated supply of ceramic particles is dispersed is less than 1000 degrees C.
19. A method according to claim 17 or claim 18, wherein the step of dispersing the product concentrated supply of ceramic particles into the aluminium-based melt is carried out in air.
20. A method according to any one of claim 1 to 16, including the additional step of forming a mixture comprising a supply of matrix metal and the product concentrated supply of ceramic particles, and subjecting the mixture to a powder metallurgical process to form a metal matrix composite.
21. A method according to claim 20, wherein the resulting metal matrix composite contains from 15 to 60 weight percent of the ceramic particles.
22. The product of any one of claims 1 to 21.
GB9119239A 1991-09-09 1991-09-09 Ceramic particles Withdrawn GB2259309A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2274467A (en) * 1993-01-26 1994-07-27 London Scandinavian Metall Metal matrix alloys
GB2288189A (en) * 1994-03-31 1995-10-11 Brunel University Of West Lond Ceramic reinforced metal-matrix composites.
GB2316092A (en) * 1996-08-08 1998-02-18 London Scandinavian Metall Metal matrix composite alloys
CN1059710C (en) * 1997-11-27 2000-12-20 宝山钢铁(集团)公司 Preparation of ceramic grain reinforced aluminium-based composite material
WO2007052174A1 (en) 2005-11-02 2007-05-10 Tubitak Process for producing a grain refining master alloy
CN100357468C (en) * 2005-04-05 2007-12-26 江苏大学 Preparation method of endogenous particle reinforced aluminium-based composite material
CN102168214A (en) * 2011-04-15 2011-08-31 江苏大学 Preparation method for light high-strength and high-tenacity aluminum-matrix composite material
US20130115370A1 (en) * 2012-05-23 2013-05-09 Shenzhen Sunxing Light Alloys Materials Co.,Ltd Process for preparing inert anode material or inert cathode coating material for aluminium electrolysis
EP2666752A1 (en) * 2012-05-23 2013-11-27 Shenzhen Sunxing Light Alloys Materials Co., Ltd Potassium cryolite for aluminum electrolysis industry and preparation method thereof
EP2669250A1 (en) * 2012-05-30 2013-12-04 Shenzhen Sunxing Light Alloys Materials Co., Ltd Preparation process of transition metal boride and uses thereof
CN106591618A (en) * 2016-12-06 2017-04-26 昆明理工大学 Preparation method of endogenous double-phase particle enhanced aluminum-based composite material
CN111020343A (en) * 2019-11-26 2020-04-17 纽维科精密制造江苏有限公司 Method for preparing high-mass-fraction particle-reinforced aluminum-based composite material by using in-situ self-generation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1103396A (en) * 1966-02-07 1968-02-14 Int Nickel Ltd Manufacture of precious metal spheres and spheroids
GB1354873A (en) * 1970-03-07 1974-06-05 Dannohl W Magnesium-containing alloys and fibre materials
EP0113249A1 (en) * 1982-12-30 1984-07-11 Alcan International Limited Metallic materials reinforced by a continuous network of a ceramic phase
WO1988007593A2 (en) * 1987-04-03 1988-10-06 Martin Marietta Corp Process for forming metal-second phase composites utilizing compound starting materials, and products thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1103396A (en) * 1966-02-07 1968-02-14 Int Nickel Ltd Manufacture of precious metal spheres and spheroids
GB1354873A (en) * 1970-03-07 1974-06-05 Dannohl W Magnesium-containing alloys and fibre materials
EP0113249A1 (en) * 1982-12-30 1984-07-11 Alcan International Limited Metallic materials reinforced by a continuous network of a ceramic phase
WO1988007593A2 (en) * 1987-04-03 1988-10-06 Martin Marietta Corp Process for forming metal-second phase composites utilizing compound starting materials, and products thereof

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2274467A (en) * 1993-01-26 1994-07-27 London Scandinavian Metall Metal matrix alloys
US6099664A (en) * 1993-01-26 2000-08-08 London & Scandinavian Metallurgical Co., Ltd. Metal matrix alloys
GB2288189A (en) * 1994-03-31 1995-10-11 Brunel University Of West Lond Ceramic reinforced metal-matrix composites.
GB2316092A (en) * 1996-08-08 1998-02-18 London Scandinavian Metall Metal matrix composite alloys
CN1059710C (en) * 1997-11-27 2000-12-20 宝山钢铁(集团)公司 Preparation of ceramic grain reinforced aluminium-based composite material
CN100357468C (en) * 2005-04-05 2007-12-26 江苏大学 Preparation method of endogenous particle reinforced aluminium-based composite material
WO2007052174A1 (en) 2005-11-02 2007-05-10 Tubitak Process for producing a grain refining master alloy
CN102168214B (en) * 2011-04-15 2013-07-17 江苏大学 Preparation method for light high-strength and high-tenacity aluminum-matrix composite material
CN102168214A (en) * 2011-04-15 2011-08-31 江苏大学 Preparation method for light high-strength and high-tenacity aluminum-matrix composite material
US20130115370A1 (en) * 2012-05-23 2013-05-09 Shenzhen Sunxing Light Alloys Materials Co.,Ltd Process for preparing inert anode material or inert cathode coating material for aluminium electrolysis
EP2666752A1 (en) * 2012-05-23 2013-11-27 Shenzhen Sunxing Light Alloys Materials Co., Ltd Potassium cryolite for aluminum electrolysis industry and preparation method thereof
EP2669250A1 (en) * 2012-05-30 2013-12-04 Shenzhen Sunxing Light Alloys Materials Co., Ltd Preparation process of transition metal boride and uses thereof
CN106591618A (en) * 2016-12-06 2017-04-26 昆明理工大学 Preparation method of endogenous double-phase particle enhanced aluminum-based composite material
CN111020343A (en) * 2019-11-26 2020-04-17 纽维科精密制造江苏有限公司 Method for preparing high-mass-fraction particle-reinforced aluminum-based composite material by using in-situ self-generation method

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