CN1250766C - Method for producing composite material and composite material produced thereby - Google Patents

Method for producing composite material and composite material produced thereby Download PDF

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Publication number
CN1250766C
CN1250766C CNB018001831A CN01800183A CN1250766C CN 1250766 C CN1250766 C CN 1250766C CN B018001831 A CNB018001831 A CN B018001831A CN 01800183 A CN01800183 A CN 01800183A CN 1250766 C CN1250766 C CN 1250766C
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Prior art keywords
base material
aluminium
composite material
dispersing
block object
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CN1362998A (en
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久保田高史
渡边弘
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0005—Separation of the coating from the substrate
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a manufacturing method for a composite material comprising two or more metals or nonmetals and compounds thereof and, more particularly, to a manufacturing method in which a dispersion material can be dispersed very homogeneously into a base material of the composite material independently of the composition of the composite material. The present invention is characterized in that in a manufacturing method for a composite material in which a metal or a nonmetal or a compound thereof is used as abase material, and at least one kind of metals or nonmetals or compounds thereof different from the base material is dispersed as a dispersion material, a raw material for base material comprising a metal or a nonmetal or a compound thereof constituting the base material and at least one raw material for dispersion material comprising metals or nonmetals or compounds thereof constituting the dispersion material are evaporated simultaneously or alternately, and the evaporated particles are deposited on a substrate to form a bulk body.

Description

Make the method for matrix material and the matrix material that this method is made
Technical field
The present invention relates to a kind of manufacturing and comprise two or more metals or nonmetal and their method of matrix material of compound, particularly, the present invention relates to dispersing material is evenly dispersed in the composite material base very much, and suitability does not rely on the manufacture method of matrix material.
Background technology
Comprise that the metal or nonmetal or their matrix material of compound are widely used in various uses, as be used for the structured material of automotive component, aircraft components etc., electrode materials, be used for film forming target material etc.Metal by will being different from base material or nonmetal or their compound are dispersed in the base material, and the control material performance makes material possess the performance that is fit to each purposes, makes matrix material.Used herein term " nonmetal " comprises hydrogen, boron, carbon, silicon, nitrogen, phosphorus etc., as generalized concept the time, also comprises being called semimetallic antimony, bismuth etc.
Make the method for above-mentioned matrix material, known have composite casting and a powder metallurgic method.In composite casting, the metal that is used as base material is a semi-molten state, pours in the metal of semi-melting as the non-metallic particle of dispersing material, and vigorous stirring forces non-metallic particle to be dispersed in the base material.As if using and making matrix material as the bad non-metallic particle of the molten metal wettability of base material, this method is effective.Adopt this method, make matrix material, separate with base material in order to prevent non-metallic material in semi-molten state.Yet, in composite casting, because semi-molten state is in the state that is called jelly, the defective as hole takes place easily in the shaping prod that makes, cause gas entrainment therein, thereby reduce the density of material.
The typical case of powder metallurgic method representative has hot pressing and hot isostatic pressing method (HIP), in this method, as the metal-powder of base material with as the non-metal powder of dispersing material, mixes with predetermined proportion, carries out sintering after the shaping, makes matrix material.In this method, to the metal of easy oxidation, because raw material is a powder, the oxygen concn in the matrix material that makes is higher, therefore is difficult to control the character of matrix material sometimes.In the powder metallurgic method, because the restriction that exists in powder control and combination treatment is difficult to dispersing material is evenly dispersed in the base material sometimes.
Except composite casting and powder metallurgic method, generally also adopt melt casting.Yet, be metal at base material and dispersing material, be respectively the situation of low melting point metal and hot spots metal, for example, adopt the vacuum fusion method just to be difficult to make such metal-metal matrix material.
Now as an example, describe the matrix material that adopts conventional manufacture method to make in detail with the sputtering target material.In recent years, when forming the circuit of liquid-crystal display or semiconductor integrated circuit, adopt the wiring technique of the target material sputtering method that uses matrix material always.When forming circuit by sputter, using the low-resistance aluminium film of high thermal resistance usually, here is to be that the matrix material of base material forms the aluminium film as the sputtering target material with aluminium.
To the aluminium film as the circuit of liquid-crystal display or semiconductor integrated circuit, for example, in the matrix material as target material, aluminium is base material, and carbon and IVa family metal such as titanium are dispersed in wherein.This is because if when using this matrix material that aluminium constitutes as target material, can form high thermal resistance and low-resistance circuit, can prevent the line interruption that stress causes.Owing to this reason, generally the matrix material that need constitute with aluminium is as target material, and it is formed can form the film that meets the line characteristic requirement.And, require the defective of target material such as hole and space few, the density height is seldom carried the gas that forms impurity secretly.
With prior art, although can use aluminium as base material, carbon and IVa family metal are made a kind of matrix material as dispersing material, and the matrix material of making is difficult to meet the requirement of the target material that forms circuit.Particularly, make the above-mentioned target material that aluminium constitutes even adopt composite casting, powder metallurgic method or melt casting, the homogeneity that carbon and IVa family metal are dispersed in the aluminium base is also restricted, the matrix material that the result makes can not effectively also be used as target material, satisfies the circuit that the actual track characteristic requires with stable formation.For using matrix material, need have the to a certain degree block object of volume (bulk body) as target material.But, if adopt conventional manufacture method to be formed for the matrix material of block object, will produce subsurface defect such as hole, therefore the density of block object can descend.Gas and other impurity also can enter this material under many situations.So,, still be difficult to stably form circuit by sputter even the block object that adopts ordinary method to make can be used as target material.
By the example of this target material as can be known, adopt the ordinary method of making matrix material dispersing material can be distributed in the base material, but its dispersity is not enough, in block object, can produces subsurface defect and carry impurity secretly.Therefore, there is the improved defective of many need in Chang Yong matrix material.Except that as the target material, manufacturing is used for the matrix material situation of other purposes, as the structured material or the electrode materials of usefulness such as automotive component, aircraft components, be difficult to usually make with conventional manufacture method and form different matrix materials.
At above-mentioned situation, carried out the present invention, therefore, an object of the present invention is to provide to make and comprise two or more metals or nonmetal and their method of matrix material of compound, in this method, dispersing material is evenly dispersed in the base material of matrix material very much, compares with conventional manufacture method, and the suitability of this method does not generally rely on the composition with matrix material.
Summary of the invention
For addressing the above problem, the inventor studies energetically, will concentrate on the film forming gas phase oriented growth of shape technology.As a result, finished and made the method for matrix material, and can not make this matrix material with conventional manufacture method.
At first, first invention that the inventor provides is a method of making matrix material, this method uses metal or nonmetal or their compound as base material, at least a metal that is different from base material or nonmetal or their compound are dispersed in the base material as dispersing material, in this method, form metal nonmetal or they these base materials of compound raw material and form metal or nonmetal or they these dispersing materials of compound at least a raw material simultaneously or alternatively vaporised, form block object in the particle deposition substrate that evaporation and condensation becomes.
In this first invention, the raw material that forms the raw material of base material and form dispersing material is by being called the particle that physical vaporous deposition (PVD method) forms evaporation, and the particle deposition of evaporation forms block object on ground.According to first invention, can deposit with the form of evaporating particle owing to form the raw material of base material and the raw material of formation dispersing material, different with the manufacture method of routine, dispersing material can be evenly dispersed in the base material very much, therefore, produce various matrix materials easily and irrelevant with feedstock property.That is to say the matrix material that easily to make refractory metal and low melting point metal formation.
This first the invention in, better be to use sputtering method or vacuum deposition method in the physical vaporous deposition.Reason is in these methods, is to produce the particle of evaporation with higher speed by each raw material, is easy to be formed with the block object of pre-determined volume.Sputtering method or vacuum deposition method are applied to first when invention, because raw material is at inert atmosphere such as argon gas or evaporate under vacuum condition, even can use the raw material of easy oxidation.So, can control the oxygen level that enters the block object that makes, avoid entering of gas and other impurity as far as possible.And, can make the block object of the matrix material that does not almost have subsurface defect.
In this first invention, the raw material of base material and the raw material of dispersing material can be simultaneously or alternatively vaporised.Raw material evaporate simultaneously with sedimentary situation under, the raw material of base material and the deposition of the raw material of dispersing material after evaporation are chaotic.Even in the situation of raw material alternatively vaporised,, can produce the matrix material that is dispersed on the dispersing material macroscopic view in the base material as long as the settled layer of the settled layer of base material and dispersing material is controlled at the order of magnitude of dust.In first invention, consider in the short period to form block object, should adopt sputtering method to evaporate raw material.
Secondly, as second invention, the inventor has invented the method for making a kind of matrix material, this matrix material uses metal or nonmetal or their compound as base material, at least a metal that is different from base material or nonmetal or their compound are dispersed in the base material as dispersing material, in this method, be used to evaporate the metal that forms base material nonmetal or they compound or form the metal of dispersing material or nonmetal or their raw material of compound at hydrocarbon gas, evaporate in any atmosphere of oxygen and nitrogen, the particle deposition of evaporation forms block object on ground.
This second invention is based on physical vaporous deposition (PVD method) or chemical Vapor deposition process (CVD method).To the atmosphere used of evaporation raw material, can select any in hydrocarbon gas, oxygen and the nitrogen, make that carbide, nitride or oxide compound are evenly dispersed in the base material as dispersing material very much in the matrix material that produces.For the evaporation raw material that is used to evaporate in second invention, adopt sputtering method in the physical vaporous deposition and the activation sedimentation in vacuum deposition method or the chemical deposition preferably.
To the restriction that has nothing concrete of the composition of the hydrocarbon gas that uses in second invention, as long as this gas can resolve into carbon and hydrogen when sputter or deposition.Methane, ethane and acetylene gas are arranged preferably.In second invention, the atmosphere to the evaporation raw material is used can also comprise rare gas element such as argon gas, thus the vaporization efficiency of control raw material.
In second invention, can use to comprise the metal that forms base material or nonmetal or their the evaporation raw material of compound, perhaps use to remove to comprise also to comprise the metal that forms dispersing material or nonmetal or their the evaporation raw material of compound the formation base material.For example, use the evaporation raw material that comprises the copper that is used to form base material and be used to form the silicon of dispersing material, adopt sputtering method to produce evaporating particle in nitrogen and be deposited on the ground, silicon and nitrogen reacted to each other and produced stable silicon nitride this moment.So in the matrix material of manufacturing, silicon nitride is a dispersing material, is evenly dispersed in very much in the copper as base material.Equally, use to comprise the copper that is used to form base material and as the evaporation raw material of the aluminium of dispersing material, adopt sputtering method to produce evaporating particle in oxygen and be deposited on the ground, aluminium and oxygen react to each other at this moment, produce stable aluminum oxide.So in the matrix material of manufacturing, aluminum oxide is a dispersing material, is evenly dispersed in very much in the copper as base material.
According to second invention, can make the matrix material that conventional manufacture method can not be made, in this matrix material, even the wettability of dispersing material and base material is very poor, dispersing material also can be evenly dispersed in the base material very much.Atmosphere by the control raw materials evaporate is used can limit the impurity that enters the biglyyest, produces the block object that does not almost have subsurface defect.In second invention, consider in the short period to form block object, should adopt sputtering method evaporation raw material.
Matrix material by above-mentioned first invention of the present invention and the acquisition of the manufacture method of second invention is the block object of formation of deposits on ground.The general object of this block body image held like that get not so difficultly, this is different with the material that is called film.After block object separated from ground, this block object had volume to a certain degree, got thereby can its former state hold.The block object of first invention of the present invention who separates from ground and second inventive method manufacturing just can just be used for various uses, for example as target material.
Among the present invention, block object by first invention of the present invention and the acquisition of the manufacture method of second invention, can also melt with the raw material of the metal that forms base material or nonmetal or its compound, mix and cast form, control the concentration of dispersing material by this process.In the manufacture method of first and second invention, the matrix material of the block object that obtains structurally is an ideal, because dispersing material is evenly dispersed in the base material very much.Yet these two kinds of manufacture method all are based on gas phase oriented growth method, if will obtain the block object of large volume, manufacturing time can be very long, and be difficult to obtain complex-shaped block object.Therefore, the block object that these two kinds of methods are obtained again with the raw material as base material melt, mixing and cast form, control the concentration of dispersing material, make the matrix material of relatively large shape object like this.If when casting, use the mould of predetermined shape, just make the matrix material of complicated shape easily.
By melting, mix also cast form, meeting is the same with conventional manufacture method, dispersing material and the isolating phenomenon of base material may occur with first invention and second invention block object that obtains and the raw material that is used for base material.Yet in first invention of the present invention and second invention, the state that the block body forms is that base material and dispersing material disperse very carefully each other, and promptly in the state of the block object of formation, dispersing material has very high wettability to base material.So, even should the bulk object and the raw material of base material melt together, dispersing material can not separate with base material yet.Therefore, with the fusing of this bulk object and base material raw material, mix and the state of the matrix material that casting obtains, be that dispersing material is evenly dispersed in the base material very much.Make matrix material if melt this bulk object and base material raw material in such a way, when forming this bulk object, should control the dispersing material amount or the base material material quantity of adding in advance, the composition of the final matrix material that obtains of so easy control.
According to the composition of matrix material, can determine to melt the proper temperature of block object and base material raw material.Generally be that fusing point to vaporization temperature scope at block object melts.On effect, temperature controllable makes block object become abundant mobile state, and the material of base material raw material and block object is uniform mixing each other.To carrying out the restriction that has nothing special of fused atmosphere.To wherein the base material or the matrix material of the easy oxidation of dispersing material, should melt in vacuum environment or in rare gas element such as ar gas environment.And, when casting, should cast under the condition of cure rapidly in fusing with after mixing.This is that the crystalline structure of matrix material is just tiny because if casting under the condition of cure rapidly, and dispersing material just can be tiny and be evenly dispersed in the base material.
To block object according to first invention and second invention formation, and by melting, mix and cast the matrix material of block object and the acquisition of base material raw material, again by rolling or its crystalline structure of thermal treatment control.The matrix material that makes at last can have the performance that is applicable to its purposes.Control its crystalline structure by rolling or thermal treatment, can obtain to have the purposes of being suitable for performance such as high-intensity matrix material.Can adopt rolling and thermal treatment this moment, perhaps only adopts wherein a kind of.
Make in the method for matrix material according to first invention and second invention, deposit on the ground that the particle of evaporation rotates more fortunately.Use is with the ground of predetermined constant speed of rotation rotation, and evaporating particle can be deposited on all surfaces of rotation ground equably, therefore, compares with the situation of deposition evaporating particle on static ground, can form and form and all more uniform block object of thickness.
And the ground of deposition evaporating particle is preferably by constituting with the base material identical materials.In this case, sedimentary particle just deposits on ground under the identical situation of structure, therefore obtains uniform crystalline structure easily.By melting, mix and cast the situation of block object and base material raw material manufacturing matrix material, if the substrate of preparation block body and function is identical with its contained base material, then should need not just to peel off and can melt by the bulk object from ground, simplified manufacture method.
Make the method for matrix material with the present invention, can make the matrix material that is fit for various uses, the suitability of this method does not generally rely on its composition, dispersing material can be evenly dispersed in the base material very much, limited entering of impurity, can make does not have the block of subsurface defect such as hole composite material.So, adopt on the matrix material reality that manufacture method of the present invention obtains applicable to various uses, be especially suitable for use as structured material, the electrode materials of automotive component, aircraft components etc. or be used for film forming target material.
And, adopt manufacture method of the present invention, as base material, carbon is as dispersing material with aluminium, and the matrix material of acquisition is particularly suitable as target material.As mentioned above, the aluminium film can effectively be used as the circuit of liquid-crystal display or semiconductor integrated circuit.Can use in the known technology to be called the target material of inlaying, in this material, when adopt that sputtering method will form be carbon containing aluminium film the time, the chip of carbon or silicon directly is embedded in the aluminum metallic material as sputter material (the open No.2-292821 of Japanese Patent).Yet the target material that this class is inlayed has pointed out that the problem that exists is the ununiformity formed of the film that forms and dust can occur, so such target material fails to be used for forming the aluminium film in fact always.And the matrix material that method constructed in accordance obtains, carbon is tiny and divide equably in the aluminium as base material.So,, can stablize and form high thermal resistance and low-resistance circuit if use such matrix material as the target material that forms circuit.
The accompanying drawing summary
Fig. 1 is sputtering method forms block object situation on static ground a synoptic diagram;
Fig. 2 is vacuum deposition method forms block object situation on static ground a synoptic diagram;
Fig. 3 is sputtering method forms block object situation on the rotation ground a synoptic diagram;
Fig. 4 is sputtering method and vacuum deposition method form block object situation on the rotation ground a synoptic diagram;
Fig. 5 is through the cross section microphotograph of the matrix material of water cooling casting among the embodiment 1;
Fig. 6 adopts sputtering method feeding the synoptic diagram that forms block object situation under the appropriate hydrocarbon gas situation on static ground;
Fig. 7 adopts sedimentation feeding the synoptic diagram that forms block object situation under the appropriate hydrocarbon gas situation on static ground.
Implement best mode of the present invention
Some better embodiments that the present invention makes composite process are described below.First embodiment relates to the manufacture method of aforementioned first invention, and second embodiment relates to the manufacture method of aforementioned second invention.
First embodiment: in the manufacture method that first embodiment relates to, adopt sputtering method or vacuum deposition method, the raw material of evaporation base material and the raw material of dispersing material form block object.Fig. 1 is to the synoptic diagram that Figure 4 shows that the various manufacture method of first embodiment.
In the method shown in Figure 1, use raw metal as base material, nonmetal raw material evaporates these raw materials as dispersing material by sputtering method, and it is deposited on the static ground plate.Static ground plate 2 is installed in the chamber 1, places metal target 4 that is used for base material and the nonmetal target 5 that is used for dispersing material on each ground 3, and these two targets are facing to static ground 2.Static ground 2 and target 4 and 5 are connected to the power supply (not shown).Static ground 2 also can be formed by the metal that is used for base material.Although the metal target 4 that is used for base material and nonmetal target 5 these two targets that are used for dispersing material of being to use shown in Figure 1 according to the composition of final matrix material, can suitably provide a plurality of targets.
In chamber 1, feed rare gas element such as argon gas, control this gaseous tension to preset value.Afterwards, between metal target 4 that is used for base material and the static ground 2 and be used for applying voltage between the nonmetal target 5 of dispersing material and the static ground 2, cause sputtering phenomenon, like this, be used for the metal of base material and be used for the nonmetal of dispersing material being deposited on static ground 2 then with regard to evaporation.Apply voltage, on target 4 and 5, cause sputtering phenomenon simultaneously, also can apply voltage, alternately cause sputtering phenomenon.Although, can use high-frequency sputtering system or magnetron sputtering system being DC2-utmost point sputtering system shown in Fig. 1.
Carry out the sputter of a preset time in this manner, on static ground 2, just formed block object 6.Form after the predetermined block object,, take off block object 6 from ground 2 by static ground 2 is ground or etching.Like this, the common block object of this piece can be used for various uses as structured material, electrode materials or target material.Although this block object just can use without handling, control its crystalline structure if desired, can be rolled or thermal treatment after use.
Can also not take off block object 6 from static ground 2, with block object 6 and static ground 2 with the substrate metal heat fused of preparation separately.By the control substrate metal amount of preparation separately, can determine the composition of the final matrix material that obtains artificially, i.e. the concentration of dispersing material wherein.These materials are heated to after but preset temperature is melted to a certain degree flow state, fully mix, and then, cast form under condition of cure rapidly like this, can make the composition with requirement and the matrix material of shape.And, if desired, can rolling or this matrix material of thermal treatment, control crystalline structure.
In the method shown in Figure 2, use raw metal as base material, nonmetal raw material evaporates these raw materials as dispersing material by vacuum deposition method, is deposited on the static ground plate.The static ground 2 of plate shape is installed in the chamber 1, places metal deposition source 8 that is used for base material and the nonmetal deposition source 9 that is used for dispersing material in each deposition crucible 7, and these two sources are facing to static ground 2. Deposition source 8 and 9 is connected to the power supply (not shown).If the structure of deposition source is the clavate source that can provide continuously, mass production matrix material effectively just.Static ground 2 also is to be formed by the metal that is used for base material.In the vacuum deposition method shown in Figure 2,,, also can suitably provide a plurality of deposition sources according to the composition of final matrix material as situation shown in Figure 1.
Chamber 1 is evacuated to predetermined pressure, produces vacuum environment.Electric current is flowed heat metal deposition source 8 that is used for base material and the nonmetal deposition source 9 that is used for dispersing material, be used for the metal of base material and be used for the nonmetal of dispersing material from deposition source 8 and 9 evaporations respectively, be deposited on the static ground 2.Carry out the deposition of certain hour in this manner, on static ground 2, form the matrix material of block object.As situation shown in Figure 1, form after the predetermined block object 6, block object 6 just can be used as single common objects and uses, perhaps itself and the metal that is used for base material are melted, mix and cast the concentration of controlling dispersing material, become and answer material again, if desired, can also be rolled or thermal treatment, control its crystalline structure this matrix material.
In conjunction with Fig. 3 and Fig. 4, the existing manufacture method of using the rotation ground of describing.Figure 3 shows that the situation of on the rotation ground, making block object by sputtering method.The cylindrical ground 10 of one rotation is installed in chamber 1, is placed metal target 4 that is used for base material and the nonmetal target 5 that is used for dispersing material on each ground 3, target is facing to rotation ground 10, and target 4 and 5 is each other in the right angle.
In this case, also be in chamber 1, to feed argon gas, apply voltage by the power supply (not shown) and carry out sputter, like this, be used for the metal of base material and be used for the nonmetal peripheral surface that is deposited on rotational circle cylindricality ground 10 of dispersing material, form block object 6 '.In such a way, use the rotation ground form block object 6 ', block object 6 ' microstructure be to be used for the metal of base material and to be used for the nonmetal of dispersing material with dust order of magnitude alternating deposit stratification.Yet, block object 6 ' on macroscopic view, what be used for the metal of base material and be used for dispersing material nonmetally has an even composition, and dispersing material is dispersed in the base material very thinly.
As situation shown in Figure 1, the block object 6 that forms on the rotation ground ' can be used as the matrix material of various uses needn't be handled, and also itself and substrate metal can be melted the concentration of controlling dispersing material together, is cast as matrix material.And, but this matrix material mat is rolling or its crystalline structure is controlled in thermal treatment.Although Figure 3 shows that the situation of using two targets, can form by matrix material as requested, provide three or more targets around the rotation ground.Only be used to the situation of using sputtering method is described in conjunction with the description of Fig. 3,, also can adopt vacuum deposition method according to the same manner, use rotation ground 10 make block object 6 ' matrix material.When adopting vacuum deposition method, as long as target among Fig. 34 and 5 usefulness deposition sources are replaced, so omit detailed description.
Sputtering method and two kinds of methods of vacuum deposition method of being to use shown in Figure 4, the situation of manufacturing block composite material on the rotation ground.The right cylinder ground 10 of rotation is installed in chamber 1, is placed the sputtering target 4 that is used for base material on ground 3, place the nonmetal deposition source 9 that is used for dispersing material in deposition crucible 7, they all face toward rotation ground 10, each other in the right angle.
In this case, feed argon gas, control its pressure to preset value, the metal that is used for base material by sputter vaporization, on the other hand, the heating of can electric current flowing be used for the nonmetal of dispersing material, the temperature the when vapour pressure that reaches nonmetallic substance up to its temperature is higher than chamber 1 internal pressure, and evaporation is used for the nonmetal of dispersing material.As a result, the nonmetal peripheral surface that is deposited on rotation ground 10 that is used for the metal of base material and is used for dispersing material, form block object 6 '.Formed block composite material 6 ', its structure identical with the described structure of Fig. 3 just also can according to described the same manner of Fig. 1 just handle block object 6 ', it illustrates omission.
Some embodiment of first embodiment are described below.
Embodiment 1
Sputtering method is adopted in embodiment 1 representative, uses rotation ground shown in Figure 3 to make the situation of aluminium carbon composite.Preparation is with aluminium (purity: the metal target of using as base material and with carbon (purity: these two kinds of materials of nonmetal target of using as dispersing material 99.9%) 99.999%).These two long 127mm of target, wide 279.4mm, thick 10mm.As sputtering equipment, can use the equipment of 3-negative electrode magnetron sputtering type, use two in three negative electrodes.Make the rotation ground of the octagon column bodily form, its manufacture method is that the long limit with eight stainless steel plates (each long 279mm, wide 80mm) is connected to each other.Reeling on the side of this rotation ground, (measure: 99.999%), aluminium and carbon just are deposited on this aluminium foil the thick aluminium foil of 12 μ m.
Sputtering condition is as follows: at indoor feeding argon gas, sputtering pressure is 0.87Pa, and the electric power that applies is 12kw (24.8W/cm to the aluminium target 2), be 4kw (8.3W/cm to the carbon target 2), the speed of rotation of rotation ground is 30rpm.Carry out 30 hours sputter, form the thick block object of 0.6mm in the side of rotation ground.In the cross section structure of the block object that forms, be thickness be about the aluminium lamination of 0.3 μ m and carbon-coating that thickness is about 0.01 μ m stacked, thickness forms rate transition one-tenth by film.Chemical analysis shows that carbon concentration is 2.6% (weight) (5.6% (atomic wts)) in the block object.
Under vacuum condition, with the aluminium of block object and preparation separately (purity: fusing together 99.999%), control the composition of aluminium carbon like this, making carbon concentration is 0.7% (weight), uses water-cooled copper mold to cast.Examine under a microscope the matrix material of cast form.The result confirms that in aluminium base, its form is Al-C (Al to carbon with about 1mm particle size dispersion 4C 3) phase.Figure 5 shows that Al-C (Al in the aluminium carbon composite that obtains among the embodiment 1 4C 3) the observations of dispersion state.Among Fig. 5, black is partly represented Al-C (Al 4C 3) phase.
Aluminium carbon (0.7% (the weight)) matrix material that forms by above-mentioned casting uses this target material to form the aluminium film as the target material of sputter.The condition that forms the aluminium film is as follows: use the DC magnetron sputtering apparatus, sputtering pressure is 0.333Pa (2.5mTorr), and the electric power that applies is 3watt/cm 2Under these conditions, on glass substrate, formed the film of about 3000 dust thickness.Form about 100 seconds of about 3000 dust thickness film required times.After having formed the film of 3000 dusts, change glass substrate, form film again.Repeat the film forming operation of shape, use a sputtering target material, can be carried out to membrane process over a long time continuously.The situation of hillock appears in the film that observation forms on the film that forms for the first time, through sputter in about 20 hours altogether time the and through on the film that forms about 40 hours the time altogether, and this hillock is represented resistive properties.After hillock refers to that 300 ℃ of thermal treatments have the glass substrate certain hour of film under vacuum herein, the ridge that produces on the film surface.The result confirms, seldom occurs hillock on each film, and irrelevant with sputter total time.Also measured the resistance of each film.The result confirms that resistivity is about 5 μ Ω cm under top condition.These results show that liquid-crystal display and semiconductor integrated circuit are had good link performance.So find, if the matrix material that embodiment 1 obtains as the raw material of sputtering target material, can be stablized the film of preparation characteristic good.
Comparative example 1
Comparative example 1 uses composite casting.2 kilograms aluminium (purity: 99.999%) extremely about 700 ℃ of carbon crucible internal heating.After the aluminium fusing, be cooled to about 640 ℃, make aluminium be in semi-molten state (solid-liquid coexisting state).In this state, adding 15 gram mean particle sizes in molten aluminium is the carbon dust of 150 μ m, carries out vigorous stirring with an agitator.Afterwards, in water-cooled copper mold, cast.The aluminium ingot that obtains is a plate shape, and 200mm length * 200mm is wide * and 20mm is thick.Measure corresponding to the carbon concentration in the copper mold bottom surface aluminium ingot part.Carbon concentration is 0.003-0.008% (weight) as a result, and carbon does not almost disperse.This aluminium ingot of visual inspection shows the top of carbon segregation at aluminium ingot.Can suppose its reason be in composite casting, almost do not have between aluminium and the carbon wetting, so carbon is what to separate with aluminium, and because the proportion of aluminium and carbon poor, above carbon floats over.
Second embodiment: in the manufacture method of second embodiment, the raw material that is used for evaporating evaporates in the mixed atmosphere of arbitrary gas of hydrocarbon gas, oxygen and nitrogen and rare gas element such as argon gas, the particle deposition of evaporation forms block object on ground.Fig. 6 and shown in Figure 7 be the synoptic diagram of second embodiment manufacture method of the present invention.Figure 6 shows that the situation that adopts sputtering method, Figure 7 shows that the situation that adopts sedimentation.
As shown in Figure 6, in the situation that adopts sputtering method, static ground plate 2 is installed in the chamber 1, places on ground 3 by substrate metal and the nonmetal target that is used to evaporate 11 that forms of dispersing material, and target is facing to static ground 2.Static ground 2 and the target 11 that is used to evaporate are connected to a power supply 12.Make static ground 2 by the metal that is used for base material.Although, can use high-frequency sputtering system and magnetron sputtering system being the extremely golden sputtering system of DC2-shown in Fig. 6.
There is the import 13 and the outlet 14 of atmosphere gas chamber 1.From atmosphere gas import 13, feed the atmosphere gas inlet chamber 1 that hydrocarbon mixture gas such as acetylene and rare gas element such as argon gas make.
Atmosphere pressures applies predetermined voltage to preset value in the watch-keeping cubicle 1, causes sputtering phenomenon, like this, is used for the metal of base material and is used for the nonmetal of dispersing material evaporating from the target 11 that is used to evaporate.At this moment, hydrocarbon gas such as the acetylene that feeds in the chamber 1 resolves into carbon and hydrogen.For example, carbon and the nonmetal block object 6 that on static ground, forms that enters together that is used for the evaporated metal of base material and is used for dispersing material.Also can be that the metal of carbon and the evaporation that is used for base material and be used for the nonmetal reaction of dispersing material produces stable carbide, enters with the carbide form in the block object 6 of formation on static ground 2.This moment control feeds the amount of hydrocarbon gas in the atmosphere gas of chamber 1, or the voltage that applies during the control sputter, like this, can suitably determine the carbon concentration in the matrix material of block object 6 forms.
Below, the situation of employing sedimentation shown in Figure 7 is described.Among Fig. 7, in static ground plate 2 installation rooms 1, deposition source 15 is formed by the metal that is used for base material, places to be used for the nonmetal of dispersing material in disperseing crucible 7, all faces toward static ground 2.Deposition source 15 is connected to (not shown) on the power supply.As first embodiment, if the clavate source is provided continuously, this deposition source 15 is the mass production matrix material effectively.Static ground 2 also can be formed by the metal that is used for base material.
There is the import 13 and the outlet 14 of atmosphere gas chamber 1.From atmosphere gas import 13, the atmosphere gas that feeding hydrocarbon mixture gas such as acetylene and rare gas element such as argon gas make is towards inlet chamber 1.Subsequently, the pressure of watch-keeping cubicle 1 interior atmosphere is to preset value, by current flow heats deposition source 15.Be used for the metal of base material and be used for the nonmetal of dispersing material, after just evaporation is quickened probe electrode 16 by one, be deposited on the static ground 2 with particle form.At this moment, as situation shown in Figure 6, the hydrocarbon gas such as the acetylene that feed in the chamber 1 resolve into carbon and hydrogen, decompose carbon that produces and the nonmetal block object 6 that forms on static ground that enters together of evaporation that is used for the evaporated metal of base material and is used for dispersing material.Also can be that the metal of carbon and the evaporation that is used for base material and be used for the nonmetal reaction of dispersing material produces stable carbide, and enters with the carbide form in the block object 6 of formation on static ground 2.This moment control feeds the amount of hydrocarbon gas in the atmosphere gas of chamber 1, or the Heating temperature during the control deposition, can suitably determine the carbon concentration in the matrix material of block object 6 forms.
Employing forms after the predetermined block object 6 in conjunction with Fig. 6 and the described manufacture method of Fig. 7, as the described situation of first embodiment, block object 6 just can be used as common objects and uses, also it can be melted, mixes and cast with the metal that is used for base material, the concentration of control dispersing material becomes matrix material.If desired, also can be rolled or thermal treatment the control crystalline structure to this matrix material.
The embodiment that second embodiment relates to is described below.
Embodiment 2
Sputtering method shown in Figure 6 is adopted in embodiment 1 representative, makes the situation of aluminium carbon composite.Adopt the reactive behavior magnetron sputtering apparatus, use diameter to be 203.2mm, the dish-shaped aluminium of thick 10mm (purity: 99.999%) as being used for sputtering target.Used thickness is the aluminium foil (purity: 99.999%) as static ground of 10 μ m.
Indoor provide argon gas (purity: 99.999%) and acetylene gas (purity: mixed gas 99.5%), argon flow amount are 40ccm, and the acetylene gas flow is 20ccm, and sputtering pressure is controlled to be 0.4Pa.The electric power that is applied on the aluminium target is 8kw (24.7W/cm 2), the ground temperature is set at 200 ℃.
Carry out 60 minutes sputter, like this, it is thick to form 80 μ m on static ground, the block object of gross weight 6.14 grams.The concentration of carbon in the block object that gasometry forms, carbon content is 2.4% (weight) in the block object.
Under vacuum, and the aluminium of block object and preparation separately (measure: fusing together 99.999%), the composition of control aluminium carbon, making carbon concentration is 0.7% (weight), uses water-cooled copper mold to cast.Examine under a microscope the matrix material that casting forms.The result confirms, in aluminium base, its form is the Al-C (Al among the embodiment 1 as shown in Figure 5 to carbon with about 1mm particle size dispersion 4C 3) phase.
Aluminium carbon (0.7% (the weight)) matrix material that forms by above-mentioned casting forms the target material of sputter, uses this target material to form the aluminium film under the condition identical with embodiment 1.Investigate the membrane property of aluminium film, it is the same with the situation of embodiment 1 that the result shows, if use the raw material of the aluminium carbon composite of embodiment 2 acquisitions as target material, can stablize the film of preparation characteristic good.
Industrial use
As mentioned above, the method for composite constructed in accordance is made the method for composite and is compared with routine, Dispersion can be evenly dispersed in the base material of composite, therefore can make different composites, and the side The applicability of method composition general and composite is irrelevant. The composite that manufacture method of the present invention obtains can be expired Sufficient requirement to structural material and electrode material, and owing to dispersion can be evenly dispersed in the base material very much, and There are not internal flaw such as hole, so applicable to various uses. Particularly, making liquid crystal display or partly leading During circuit that the body integrated circuit is used, if as target material, can stablizing, this composite meets the requirements of film Characteristic.

Claims (8)

1. method of making aluminum series composite material, this aluminum series composite material be with aluminium as base material, carbon is dispersed in the base material as dispersing material, method is characterised in that:
The base material raw material and the dispersing material raw material that comprises above-mentioned dispersing material that will comprise aluminium or aluminum compound, while or alternatively vaporised, the particle deposition of evaporation forms block object on a ground.
2. method of making aluminum series composite material, this aluminum series composite material be with aluminium as base material, carbon is dispersed in the base material as dispersing material, method is characterised in that:
To comprise the raw material that is used to evaporate of aluminium or aluminum compound, and evaporate in hydrocarbon gas atmosphere, the particle deposition of evaporation forms block object on a ground.
3. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that described block object is melted, mixes cast form then with the aluminium that constitutes base material again, controls the concentration as the carbon of dispersing material like this.
4. the method for manufacturing aluminum series composite material as claimed in claim 3 is characterized in that described aluminum series composite material also is rolled or thermal treatment, controls crystalline structure.
5. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that described raw material evaporates by sputtering method.
6. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that the particle of described evaporation deposits on the rotation ground.
7. the method for manufacturing aluminum series composite material as claimed in claim 1 or 2 is characterized in that described ground has and base material identical materials aluminium.
8. an aluminum series composite material that is used for sputtering target adopts the method manufacturing of manufacturing aluminum series composite material as claimed in claim 3.
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