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WO1997048651A2 - Procede de fabrication de materiaux ultrafins comprenant des metaux, des ceramiques et des diamants - Google Patents

Procede de fabrication de materiaux ultrafins comprenant des metaux, des ceramiques et des diamants Download PDF

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Publication number
WO1997048651A2
WO1997048651A2 PCT/US1997/010633 US9710633W WO9748651A2 WO 1997048651 A2 WO1997048651 A2 WO 1997048651A2 US 9710633 W US9710633 W US 9710633W WO 9748651 A2 WO9748651 A2 WO 9748651A2
Authority
WO
WIPO (PCT)
Prior art keywords
ultrafine
materials
precursor material
silicon
laser
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.)
Ceased
Application number
PCT/US1997/010633
Other languages
English (en)
Other versions
WO1997048651A3 (fr
Inventor
Shengzhong Liu
Pravin Mistry
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.)
QQC Inc
Original Assignee
QQC Inc
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 QQC Inc filed Critical QQC Inc
Publication of WO1997048651A2 publication Critical patent/WO1997048651A2/fr
Publication of WO1997048651A3 publication Critical patent/WO1997048651A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/25—Diamond
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/25—Diamond
    • C01B32/26—Preparation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • This invention relates to silicon carbide powders. More particularly, this invention relates to the low-cost production of ultrafine silicon and diamond materials by directing energy at reactants in a vacuum chamber. The synthesized materials are optionally stabilized by a cooling medium.
  • ultrafine materials typically about 1 -1000 nm in grain diameter
  • Applications of ultrafine materials generally include treating military wastes, air cleaning, military personnel protection against chemical weapons, joining materials and bonding materials.
  • Properties (characteristics) of ultrafine materials include large surface area (e.g., relative to volume), high reactivity, low melting point, and utility as
  • ultrafine materials for many applications.
  • the large surface area is a critical property for chemical and physical adsorption, catalysis and many chemical reactions. Greatly enhanced chemical reactivity has been demonstrated with ultrafine materials.
  • Ultrafine materials such as silicon, silicon carbine, or diamonds have great utility as corrosion-resistant, wear-resistant, erosion-resistant, and heat-resistant articles or coatings. Their potential uses are considerable However, production costs related to the manufacture of such materials remain prohibitive.
  • Patent No. 4,681 ,861 issued July 21 , 1987 for SILICON CARBIDE
  • a further object of the present invention is to provide a technique for producing ultrafine silicon materials at a low cost.
  • Still a further object of the present invention is to provide a technique for producing ultrafine silicon carbide materials at a low cost.
  • An additional object of the present invention is to provide a technique for producing ultrafine diamond materials at a low cost.
  • Yet a further object of the present invention is to provide a technique for producing ultrafine silicon carbide-diamond composite materials at low cost.
  • Still an additional object of the present invention is to provide a technique for making ultrafine SiC materials and SiC-diamond materials with a C0 2 laser from silane or ethylene precursors or from precursors containing both silane and ethylene. These materials have considerable
  • SiC is very hard and light in weight and has excellent resistance to wear, corrosion and erosion. It is also stable at high temperatures, and thus is particularly suitable for engine and exhaust systems, as a barrier coating, and as a surface treatment technique including ion implantation, carburising, and siliconising.
  • the steps for producing these materials include: (1) introducing at lest one precursor material having a high absorption coefficient into a reaction system; (2) providing at lest one energy source to rapidly dissociate and ionize said precursor material so as to produce an ultrafine material; and (3) cooling the ultrafine materials to prevent agglomeration.
  • Figure 1 is a diagrammatic view of the apparatus for employing the general method of the present invention
  • Figure 2 is a flowchart illustrating a preferred set of steps to be taken in the production of ultrafine silicon materials
  • Figure 3 is a flowchart illustrating the first preferred set of steps to be taken in the production of ultrafine silicon carbide materials
  • Figure 4 is a flowchart illustrating the second preferred set of steps to be taken in the production of ultrafine silicon carbide materials
  • Figure 5 is a flowchart illustrating the third preferred set of steps to be taken in the production of ultrafine silicon carbide materials
  • Figure 6 is a flowchart illustrating the first preferred set of steps to be taken in the production of ultrafine diamond materials
  • Figure 7 is a flowchart illustrating the second preferred set of steps to be taken in the production of ultrafine diamond materials
  • Figure 8 is a flowchart illustrating the third preferred set of steps to be taken in the production of ultrafine diamond materials
  • Figure 9 is a flowchart illustrating the first preferred set of steps
  • Figure 10 is a flowchart illustrating the second preferred set of
  • the method of making ultrafine materials including metals, ceramics, and diamonds generally involves a series of steps including (1 ) introducing at least one precursor material having a high absorption coefficient into a reaction system; (2) providing at lest one energy source to rapidly dissociate and ionize said precursor material so as to produce an ultrafine material; and (3) cooling the ultrafine materials to prevent agglomeration. Variations of these general steps may be employed to produce different ultrafine materials, as set forth below, however a suggested apparatus for accomplishing the general steps of the preferred method
  • the apparatus of Figure 1 includes a reaction system 12 (which may be an enclosure), a source for one or more reactants 14, an energy source 16, a cooling media 18, and a vacuum system or similar system 20 for creating a vacuum within the system 12 as may be desired for the particular reaction at hand.
  • the energy source 16 may be a laser of the C0 2 or excimer type.
  • an inert gas may be introduced for: (a) transferring
  • the method of the present invention may be undertaken in an enclosure, in a vacuum, or in an ambient environment.
  • Laser energy may be used, and as two of the preferred components of the precursors, silane and ethylene, are known to be among the most effective absorbents for C0 2 (10.6 ⁇ m) laser energy, this type of laser is preferred, although other lasers are usable as required for most effectively energizing the selected precursor, the latter being determined by the sought-after product. Accordingly, and for example, it is possible to synthesize ultrafine SiC powders and SiC-diamond composites with C0 2 laser energy. Furthermore, by adjusting the silane:ethylene ratio, one may get SiC powder, or SiC-diamond composites with different compositions.
  • a single preferred process is disclosed for producing ultrafine silicon materials. The steps of this process are set forth in Figure 2. At
  • Step 30 silane is introduced into an enclosure preferably having a vacuum formed therein, afterwhich energy, preferably in the form of a laser beam produced by a C0 2 laser, is directed to the silane at Step 32 to produce an ultrafine material The produced material is allowed to cool at Step 34.
  • energy preferably in the form of a laser beam produced by a C0 2 laser
  • a silane- and ethylene-containing precursor material is introduced into an enclosure preferably having a vacuum formed therein at Step 40 Thereafter, energy in the form of a laser beam produced by a laser such as a C0 2 laser is directed to the precursor material to produce an ultrafine product at Step 42 At Step 44 the produced material is allowed to cool
  • a first material containing toluene is introduced into the enclosure and a second precursor material containing silane is introduced into the enclosure preferably having a vacuum formed therein, both of these introductions occurring at Step 50
  • the carbon to silicon ratio is about 1.
  • the source for dissociation and tonization of the toluene is preferably a KrF
  • the energy source for dissociation and tonization of the silane is preferably a C0 2 laser These energy sources are directed to the precursors at Step 52.
  • the produced material is allowed to cool at Step 54.
  • the silicon to carbon ratio is about 1.
  • benzene is introduced as the precursor material into an enclosure preferably having a vacuum therein at Step 90. Thereafter, energy, preferably in the form of a beam produced by a KrF excimer laser, is directed to the precursor material at Step 92 to produce an ultrafine material. Finally, the produced ultrafine material is allowed to cool at Step 94.
  • Ultrafine Silicon Carbide-Diamond Composite Materials Two preferred processes are disclosed for producing ultrafine silicon carbide-diamond materials. The steps of these processes are set forth in Figures 9 and 10. With respect to the process as set forth in Figure 9, a precursor
  • the carbon-to-silicon ratio is preferably greater than 1.
  • energy preferably produced by a C0 2 laser, is directed to the precursor material to produce an ultrafine material at Step 102.
  • the produced material is thereafter allowed to cool
  • Step 104 With respect to the process as set forth in Figure 10, a first precursor material containing silicon is ablated from a silicon substrate
  • the first precursor material is a compound (e.g. Si wafer) at Step 110. Thereafter, the first precursor material is a compound (e.g. Si wafer) at Step 110. Thereafter, the first precursor material is a compound (e.g. Si wafer) at Step 110. Thereafter, the first precursor material is a compound (e.g. Si wafer) at Step 110. Thereafter, the first precursor material is
  • the energy source for ablating the silicon substrate is preferably an excimer laser.
  • the carbon to silicon ratio is greater than 1. This example does not require a vacuum.
  • silicon-containing and carbon-containing powder materials may be used to replace silane and ethylene.
  • Other lasers, radiation sources such as microwave, RF, etc. may be used to replace the C0 2 laser. Cooling, such as via inert gas, liquid nitrogen, water, etc. may be necessary to stabilize ultrafine powder materials.
  • nitrogen-containing materials may be used as precursor materials.
  • boranes and other boron- containing materials may be used as precursor materials. Selection energy source so that the precursor material can effectively absorb the radiation for creating rapid reactions to produce ultrafine materials. For example, radiation by C0 2 laser can be effectively absorbed by ammonium and boranes for creating rapid reactions to produce the ultrafine materials.
  • a laser preferably an
  • SiC or SiC-diamond composite may be produced very effectively.
  • silicon e.g. Si wafers
  • More lasers may be used to ablate silicon and excite gases for the reactions.
  • Another possible method is to use multiple energy sources or lasers. For example, one laser is absorbed strongly by one material and another laser is efficiently absorbed by another precursor, the combination produces the desired material, e.g. SiC, efficiently.
  • silane absorbs C0 2 laser radiation very efficiently and benzene and toluene strongly absorbs 248 nm radiation of KrF based excimer laser. If silane and toluene are used as precursors and C0 2 and KrF lasers used for energy sources, SiC or SiC-diamond composite may be produced very effectively.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Nanotechnology (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

On décrit un procédé permettant de fabriquer des matériaux ultrafins comprenant des métaux, des céramiques et des diamants. Les étapes générales de production desdits matériaux sont les suivantes: (1) on introduit au moins un matériau précurseur à coefficient d'absorption élevé dans un système de réaction; (2) on fournit au moins une source d'énergie afin de rapidement dissocier et ioniser ledit matériau précurseur de manière qu'il produise un matériau ultrafin; et (3) on refroidit les matériaux ultrafins afin d'empêcher qu'ils s'agglomèrent.
PCT/US1997/010633 1996-06-20 1997-06-20 Procede de fabrication de materiaux ultrafins comprenant des metaux, des ceramiques et des diamants Ceased WO1997048651A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US67177896A 1996-06-20 1996-06-20
US08/671,778 1996-06-20

Publications (2)

Publication Number Publication Date
WO1997048651A2 true WO1997048651A2 (fr) 1997-12-24
WO1997048651A3 WO1997048651A3 (fr) 1998-05-14

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PCT/US1997/010633 Ceased WO1997048651A2 (fr) 1996-06-20 1997-06-20 Procede de fabrication de materiaux ultrafins comprenant des metaux, des ceramiques et des diamants

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117623780A (zh) * 2023-12-08 2024-03-01 清华大学 碳化硅模板诱导煤基金刚石/碳化硅涂层与复合材料及其制备方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59206042A (ja) * 1983-05-07 1984-11-21 Sumitomo Electric Ind Ltd 微粉末の製造方法及び製造装置
JPS6397225A (ja) * 1986-10-13 1988-04-27 Nkk Corp 超微粒子の製造方法
JPS6395102A (ja) * 1986-10-13 1988-04-26 Nkk Corp 超微粒子の製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117623780A (zh) * 2023-12-08 2024-03-01 清华大学 碳化硅模板诱导煤基金刚石/碳化硅涂层与复合材料及其制备方法
CN117623780B (zh) * 2023-12-08 2025-10-17 清华大学 碳化硅模板诱导煤基金刚石/碳化硅涂层与复合材料及其制备方法

Also Published As

Publication number Publication date
WO1997048651A3 (fr) 1998-05-14

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