CN104425416A - Stacked wiring film and manufacturing method thereof, and Ni alloy sputtering target material - Google Patents
Stacked wiring film and manufacturing method thereof, and Ni alloy sputtering target material Download PDFInfo
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- CN104425416A CN104425416A CN201410459218.3A CN201410459218A CN104425416A CN 104425416 A CN104425416 A CN 104425416A CN 201410459218 A CN201410459218 A CN 201410459218A CN 104425416 A CN104425416 A CN 104425416A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
- H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
- H01L21/2855—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by physical means, e.g. sputtering, evaporation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02422—Non-crystalline insulating materials, e.g. glass, polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02436—Intermediate layers between substrates and deposited layers
- H01L21/02439—Materials
- H01L21/02491—Conductive materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/0257—Doping during depositing
- H01L21/02573—Conductivity type
Abstract
The invention relates to a stacked wiring film and a manufacturing method thereof, and a Ni alloy sputtering target material. The invention provides a novel stacked wiring film which can be used for stable wet-type etching and meets requirements of low reflection of electrodes or wiring film in order to improve display quality of a high-precision flat panel display element, and the invention provides a Ni alloy sputtering target material used to form a Ni alloy film of the intermediate film used to form low reflection. The stacked wiring film is provided with the following stacked structure, the intermediate film containing Ni alloy is formed on a transparent substrate or a transparent substrate provided with a transparent film, the thickness of the intermediate film being 20-100 nm, and a conductive film whose electrical resistance is lower than 150 [mu][omega]cm is directly formed on the intermediate film, and visible light reflectance measured from a transparent substrate side is lower than 20%.
Description
Technical field
The present invention relates to stacked wiring membrane that require low reflection characteristic, that use in the electrode film of such as plane display element or wiring membrane and its manufacture method and the Ni alloy sputtering target for the formation of low-reflection film.
Background technology
Above transparent glass substrate etc., be formed with the flat display apparatus such as the electrophoretype display utilized in the liquid crystal display (hereinafter referred to as " LCD "), plasm display panel (hereinafter referred to as " PDP "), Electronic Paper etc. of membrane equipment (flat-panel monitor, hereinafter referred to as " FPD "), along with large picture, fine, high-speed responsive, low resistance value required to its wiring membrane.And, in recent years, develop the touch panel of FPD implementation and operation or use the goods that FPD of the flexibility of transparent resin substrate, very thin glass substrate etc. is new.
In recent years, the wiring membrane as the thin-film transistor (hereinafter referred to as " TFT ") of the driving element of FPD needs low resistance value to realize above-mentioned high performance, as the material of main wiring film, employs Al, Cu.
At present, TFT uses Si semiconductor film, when Al, Cu and Si as main wiring material directly contact, due to the heating process in TFT manufacture, thermal diffusion occurs, sometimes makes the characteristic degradation of TFT.Therefore, the stacked wiring membrane of pure Mo, Mo alloy as barrier film being provided with excellent heat resistance between the main wiring film and the Si of semiconductor film of Al, Cu is employed.In addition, the pixel electrode connected from wiring membrane is used as the film of the indium-tin-oxide (hereinafter referred to as ITO) of nesa coating usually.
In addition, the maximization of giving the touch panel substrate picture of direct operability while seeing the picture of FPD is also developed, and the goods also carrying out touch panel operation in smart mobile phone, dull and stereotyped PC and then Desktop PC etc. are popularized.The position probing electrode of this touch panel also uses the ito film of nesa coating usually.
In recent years, for the touch panel that can carry out the electrostatic capacity type of multiple spot detection, become the common name diamond configuration of the ito film being configured with quadrangle, the electrode, the wiring membrane that connect the ito film of quadrangle also use metal film.This metal film uses and is easy to obtain the stacked film with the Mo alloy of the contact of ito film, Mo alloy and Al.
As thermal endurance, corrosion resistance, low-resistance metal film with the excellent adhesion of substrate, present applicant has proposed V, the Nb containing 3 ~ 50 atom % in Mo and then be added with the metal film of Ni, Cu.(patent documentation 1)
On the other hand, in order to protect the surface of the main wiring film of low-resistance Cu, propose the stacked wiring membrane covered with Ni-Cu alloy.(such as patent documentation 2, patent documentation 3)
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2004-140319 publication
Patent documentation 2: Japanese Unexamined Patent Publication 2011-52304 publication
Patent documentation 3: Japanese Unexamined Patent Publication 2006-310814 publication
Summary of the invention
the problem that invention will solve
In recent years, for become main flow full HD substitute, the large-scale 4K-TV with 4 times of pixels, be the smart mobile phone of the closely operating display frame of several about 10cm in distance viewpoint, high-precision refinement just advances.With this high-precision refinement, the new problem that the reflection of the incident light produced by metal film makes display quality reduce becomes obviousization.Therefore, the requirement that metal film has an antiradar reflectivity characteristic new like this (hereinafter referred to as " low reflection ") raises sharp.
In addition, the Al film used in the wiring membrane of plane display element is the metal of the high reflectance in visible region with more than 90%.In addition, the Cu film used in the wiring membrane of same plane display element has the reflectivity of 70% in visible region, has the high reflectance of be equal to Ag film more than 95% in the long wavelength region of more than 600nm.
On the other hand, in order to protect these wiring membranes and stacked Mo film, Mo alloy film have about 60% reflectivity.Even if these metal films are through the manufacturing process of plane display element, reflectivity does not also change substantially, therefore, in the display unit of particularly fine, metal film be reflected as the main cause that display quality is reduced.In the display unit of high-precision refinement as described above, require electrode, the wiring membrane of less than 30% of the half degree such as Mo film such lower reflection.
Above, so far, develop the wiring membrane employing various material, stacked wiring membrane, be conceived in these patent documentations of result as wiring membrane, tectal barrier, protective value and being studied.And, in these patent documentations, about the characteristic that the low reflection needed for the display unit in order to tackle fine is from now on new like this, do not carry out any research.
In addition, according to the research of the present inventor, to be formed disclosed in above-mentioned patent documentation 2, patent documentation 3 the tectal stacked wiring membrane comprising Ni alloy carry out Wet-type etching time, the tectal etching also confirming to comprise Ni alloy in real estate becomes uneven, be easy to inequality occurs, wiring width produces other such problems of deviation.
The object of the invention is to, there is provided can carry out stable Wet-type etching and needed for the display quality can tackling the plane display element in order to improve fine, that require, the novel stacked wiring membrane of the low reflection of electrode or wiring membrane, and be provided for forming the Ni alloy sputtering target as the Ni alloy film of the intermediate coat of low reflection.
for the scheme of dealing with problems
The present inventor, in view of above-mentioned problem, in the manufacturing process of plane display element, touch panel, on the basis of stable Wet-type etching, in order to obtain low reflection characteristic new like this, have studied various alloy film and stacked film.Found that: by the transparent substrate or the transparency carrier upper strata stacked package being formed with hyaline membrane containing the intermediate coat of Ni alloy and conducting film, thus the stacked wiring membrane of low reflection can be obtained, thus complete the present invention.
Namely, the present invention is a kind of invention of stacked wiring membrane, described stacked wiring membrane has following layers stack structure: on the transparent substrate or the transparency carrier being formed with hyaline membrane is formed with the thickness comprising Ni alloy is the intermediate coat of 20 ~ 100nm, directly on this intermediate coat, be formed with the conducting film that resistivity is 150 μ below Ω cm, the visible reflectance measured from aforementioned transparent substrate side is less than 20%.
Aforesaid conductive film is preferably to be selected from element in Al, Cu, Mo, Ni, Ag as main component, and its thickness is 10 ~ 500nm.
Preferably, in aforementioned intermediate coat, be selected from more than one element in Cu, Mn, Mo and Fe to count 15 ~ 60 atom %, remainder is made up of Ni and inevitable impurity.
In addition, preferably, aforementioned intermediate coat contains the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom % and the total amount of Cu and Mo is 15 ~ 50 atom %, and remainder is made up of Ni and inevitable impurity.
In addition, it is further preferred that in aforementioned intermediate coat, Mn be 1 ~ 25 atom %, Mo be 3 ~ 30 atom % and the total amount of Mn and Mo be 15 ~ 50 atom %, remainder by Ni and inevitably impurity form.
In addition, further preferably, aforementioned intermediate coat contains the Mn of 1 ~ 25 atom %, the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, the Fe of 0 ~ 5 atom %, and remainder is made up of Ni and inevitable impurity.
In addition, the present invention is a kind of invention of Ni alloy sputtering target, described Ni alloy sputtering target is the Ni alloy sputtering target for the formation of aforementioned intermediate coat, it contains to amount to more than one the element be selected from Cu, Mn, Mo and Fe counting 15 ~ 60 atom %, remainder is made up of Ni and inevitable impurity, and Curie point is below normal temperature.
Preferably, aforementioned Ni alloy sputtering target contains the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, and the total amount of Cu and Mo is 15 ~ 50 atom %.
In addition, it is further preferred that aforementioned Ni alloy sputtering target contains the Mn of 1 ~ 25 atom %, the Mo of 3 ~ 30 atom %, and the total amount of Mn and Mo is 15 ~ 50 atom %.
In addition, further preferably, aforementioned Ni alloy sputtering target contains the Mn of 1 ~ 25 atom %, the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, the Fe of 0 ~ 5 atom %.
Aforementioned intermediate coat containing 20 ~ 60 volume % be selected from the atmosphere of at least one in oxygen and nitrogen under, use above-mentioned Ni alloy sputtering target to be formed by sputtering method.
the effect of invention
Stacked wiring membrane of the present invention is due in the manufacturing process of plane display element, touch panel, on the basis of stable Wet-type etching, also can realize existing electrode, low reflectivity that wiring membrane cannot obtain, so the display quality of such as FPD etc. can be improved.Therefore, the technology become that the FPD as more fine is received publicity, such as 4K-TV, smart mobile phone or dull and stereotyped PC etc. information terminal of future generation, using the FPD of the flexibility of transparent resin substrate useful.This is because, particularly the low reflectionization of metal film is extremely important in these goods.
Accompanying drawing explanation
Fig. 1 is the schematic cross-section of the application examples that stacked wiring membrane of the present invention is shown.
description of reference numerals
1 transparency carrier
2 intermediate coats
3 conducting films
Embodiment
The application examples of stacked wiring membrane of the present invention is shown in Fig. 1.Stacked wiring membrane of the present invention such as can by forming intermediate coat 2, this intermediate coat 2 forming conducting film 3 and obtains on transparency carrier 1.It should be noted that, in Fig. 1, conducting film 3 is set to homogenous material, result can coordinate the heating-up temperature in required resistance value, manufacturing process, atmosphere ground stacked, also can suitably select.
One of important feature of the present invention is following aspect: as at the such transparency carrier of such as glass substrate or be such as formed with the intermediate coat that the transparency carrier of the hyaline membranes such as transparent resin film is formed, adopt Ni alloy, its thickness is set to 20 ~ 100nm.In addition, in the present invention, on above-mentioned intermediate coat, directly form the conducting film that resistivity is 150 μ below Ω cm, form stepped construction.And another important feature of the present invention is following aspect: the visible reflectance measured from transparent substrate side is less than 20%.Below, each feature of the present invention is described in detail.
It should be noted that, in the following description, " reflectivity " refers to the average reflectance of the scope of the wavelength 360 ~ 740nm of visible region.
The intermediate coat as Ni alloy in stacked wiring membrane of the present invention passes through containing more than one the element be selected from such as Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Cu in Ni, thus can obtain the semi-permeable painted intermediate coat of low reflection.
In addition, in stacked wiring membrane of the present invention, by the thickness of intermediate coat is set to more than 20nm, can obtain suppressing light through, prevented the low reflection characteristic of the reflection of light by the conducting film on upper strata.In addition, by the thickness of intermediate coat is set to below 100nm, can film formation time be shortened, be conducive to the raising of productivity ratio.In addition, in order to obtain the reflectivity of less than 10%, preferably the thickness of intermediate coat is set to 40 ~ 70nm.
At least one that be selected from oxygen and nitrogen of intermediate coat in stacked wiring membrane of the present invention preferably containing 20 ~ 60 atom % in Ni alloy.Its reason is because make intermediate coat for being easy to light absorbing semi-permeable coloring film, reduces visible reflectance.In the present invention, by the content of oxygen contained in intermediate coat, nitrogen is set to 20 more than atom %, is formed as the semi-permeable coloring film that inhibit metallic luster, is conducive to the reduction of visible reflectance.In addition, in the present invention, by the content of oxygen contained in intermediate coat, nitrogen is set to 60 below atom %, be conducive to maintaining the adaptation with transparency carrier, conducting film.
The resistivity of the direct conducting film formed on intermediate coat in stacked wiring membrane of the present invention is expected low as much as possible, is set to 150 μ below the Ω cm be equal to ito film.
The present invention, by being formed stacked above-mentioned intermediate coat and conducting film with the thickness of the best, can be formed as the stacked wiring membrane with lower reflection characteristic.As conducting film, preferably to be selected from element in such as Al, Cu, Mo, Ni, Ag as main component.This can consider the temperature of the heating process in required resistance value, manufacturing process, atmosphere, suitably select with the adaptation, barrier etc. of other oxide-films, diaphragm.It should be noted that, in the present invention, so-called " main component " refers to, the element be selected from Al, Cu, Mo, Ni, Ag containing 50 more than atom % in conducting film.
Wherein, the resistance value of Al low and be applicable to time, stacked through heating process with the ito film as nesa coating, at the oxide of Interface debond Al, sometimes electrical contact reduce.Therefore, also the coverlay formed between the conducting film of Al and ito film using the Mo of the contact excellence with ito film as main component can comprised.
In addition, the resistance value of Cu is also low and when being applicable to, the oxidative resistance of Cu is low, therefore can to cover as the coverlay of main component in order to Ni and comprise on the conducting film of Cu.
When Al, Cu of being used as above-mentioned low-resistance conducting film useful, for the problem of oxidative resistance, can pass through conducting film and deal with using Mo, Ni as the coverlay of main component is stacked.On the other hand, in the purposes that required resistance value can be higher, also can use using the high Mo of thermal endurance as the conducting film of main component, using the Ni of weatherability excellence as the conducting film of main component with individual layer.In addition, having with Cu using Ag as the conducting film of main component is the low resistance value of equal extent, and compared with Cu oxidative resistance, excellent moisture resistance, therefore for these requirements, also can use conducting film using Ag as main component with individual layer.
The thickness of conducting film is preferably 10 ~ 500nm.In the present invention, by the thickness of conducting film is set to more than 10nm, the continuity of conducting film can be maintained, be easy to obtain low reflection, in addition, relatively diminish pro rata in the impact of conducting film surface electronic scattering, be conducive to suppressing resistance value to increase.In addition, in the present invention, by the thickness of conducting film is set to below 500nm, can film formation time be shortened, and the generation of the warpage caused by membrane stress when being applied to transparent film substrate etc. can be suppressed.
In addition, the photopermeability of conducting film is different according to selected material, and the thickness of conducting film, in order to obtain stable low reflection characteristic, is more preferably set to more than the 50nm reduced through light by result.In addition, in order to conducting film film surface make the impact of electron scattering relatively reduce pro rata, relax resistance value increase, obtain stable resistance value, more preferably the thickness of conducting film is set to more than 100nm.
In addition, preferably, intermediate coat is formed as being selected from more than one element in Cu, Mn, Mo and Fe, remainder by Ni and the inevitable Ni alloy that forms of impurity to amount to containing 15 ~ 60 atom %.
The weatherability of Ni is excellent, on the other hand, also not easily etched utilizing in the etchant of the liquid of normally used Al, Cu in FPD etc., and dry-etching patience is also high, therefore for being not easily processed as the element of wiring membrane.Cu, Mn, Mo, Fe are the element had by containing the effect improving the Wet-type etching using liquid in Ni.This effect increases along with addition.In FPD, mainly based on the etchant of Al, Cu, carry out the etching of the conducting film using Mo, Ni, Ag as main body.Therefore, when considering the etching with the etchant of Al, Cu, the content of Cu, Mn, Mo and Fe is preferably set to 15 more than atom % to amount to.
On the other hand, when the content of Cu, Mn, Mo and Fe is to amount to more than 60 atom %, the weatherability that Ni is original had significantly reduces.Therefore, in the present invention, preferably the content of Cu, Mn, Mo and Fe is set to 15 ~ 60 atom % to amount to.
In addition, when the improvement effect based on the etching of the Cu contained in intermediate coat is 10 more than atom %, become clear and definite.On the other hand, when the content of Cu is more than 40 atom %, when importing oxygen, the reflectivity of low reflection characteristic, particularly short wavelength side becomes and is difficult to reduce.Therefore, in the present invention, preferably the content of the Cu of intermediate coat is set to 10 ~ 40 atom %.Be more preferably 10 ~ 25 atom %.
In addition, the Mn contained in intermediate coat is the element that the improvement effect of etching in Cu, Mn, Mo and Fe is the highest, and is easy to be combined with oxygen, nitrogen, therefore for easily intermediate coat being formed as the element of semi-permeable coloring film.Improvement effect based on the etching of Mn embodies when 1 more than atom %, and the effect being formed as the semi-permeable coloring film being conducive to low reflection characteristic becomes clear and definite when 6 more than atom %.
On the other hand, when Mn is more than 25 atom %, time such as, in intermediate coat containing nitrogen, the adaptation of intermediate coat reduces sometimes.Therefore, in the present invention, preferably the content of the Mn of intermediate coat is set to 1 ~ 25 atom %.Be more preferably 6 ~ 20 atom %.
Improvement effect based on the etching of the Mo contained in intermediate coat embodies when 3 more than atom %.In addition, the improvement effect based on the low reflection characteristic of Mo is the highest in Cu, Mn, Mo and Fe, and its effect becomes clear and definite when 5 more than atom %, along with its effect of increase of content increases.But when the content of Mo is more than 30 atom %, the moisture-proof sometimes as one of weatherability reduces, be therefore preferably 30 below atom %.
In addition, time simultaneously containing Mo and Cu, when the content of Mo is more than 20 atom %, larger variation can be there is along with the thickness of intermediate coat to the wavelength reflection in visible region, therefore, become and be difficult to obtain stable low reflection characteristic.Its reason is still not clear, but considers following impact: Cu and Mo on equilibrium state diagram for being easy to the combination of the element be separated, so simultaneously containing more amount time, intermediate coat becomes irregular.
In addition, time simultaneously containing Mo and Cu, when the content of Mo is more than 20 atom %, select Cu as conducting film and stacked with intermediate coat time, the etching inequality when etchant being easy to generations Cu etches.
According to above situation, in the present invention, preferably with Cu by intermediate coat be set to 3 ~ 20 atom % containing the content of Mo sometimes and the total amount of Cu and Mo is set to 15 ~ 50 atom % simultaneously.More preferably Mo is 5 ~ 15 atom %.
In addition, time in intermediate coat simultaneously containing Mn and Mo, preferably the content of Mo is set to 30 below atom %.This is because, when the content of Mo is more than 30 atom %, above-mentioned such moisture-proof reduces sometimes.
In the present invention, in order to etch with the etchant of Cu, Al, the content of Mn and Mo of intermediate coat is preferably 15 more than atom % to amount to.In addition, when the total amount of Mn and Mo of intermediate coat is more than 50 atom %, oxidative resistance, moisture-proof reduce sometimes.
According to above situation, in the present invention, the total amount of Mn and Mo of intermediate coat is more preferably the scope of 15 ~ 50 atom %.
In addition, in order to coincidently stably obtain the characteristic of low reflection with above-mentioned etching, the Mn more preferably containing 1 ~ 25 atom % in the Ni alloy of intermediate coat, the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, the Fe of 0 ~ 5 atom %.
In addition, according to the material of the conducting film stacked with intermediate coat, sometimes meet etching with Mn, Cu.In above-mentioned situation, Mo can be used as the displacements such as Ti, Zr, Hf, V, Nb, Ta, Cr, W, Co of other transition metal.
In addition, Fe is the element that can improve etching.When the Fe contained in intermediate coat is more than 5 atom %, according to the thickness of intermediate coat, reflectivity is increased, bring the impact to be magnetic etc. simultaneously.When the stacked wiring membrane of FPD etc. has magnetic characteristic, sometimes produce noise due to electromagnetic induction when flowing through electric current etc., intermediate coat is expected as far as possible for non magnetic.Therefore, in the present invention, the Fe contained in intermediate coat preferably only contains with the scope of 5 below atom % when the improvement effect deficiency of the etching based on above-mentioned element.Be more preferably 3 below atom %.
As the method forming above-mentioned intermediate coat, the sputtering method using Ni alloy sputtering target is best.Sputtering method is one of physical vapor deposition, compared with other vacuum evaporations, ion plating, for can film forming be stably large-area method, and is the effective ways of the thin layer that can obtain the few excellence of component fluctuation.
The formation of intermediate coat can be used Ni alloy sputtering target, be obtained by reactive sputtering method.Now, for the atmosphere of sputtering, except the non-active gas that is generally used for sputter gas and Ar, formed by sputtering method containing being selected from the atmosphere of at least one party in oxygen and nitrogen of 20 ~ 60 volume %.
For Ni alloy sputtering target of the present invention, in order to form above-mentioned intermediate coat, contain with more than one the element be selected from Cu, Mn, Mo and Fe counting 15 ~ 60 atom %, remainder is made up of Ni and inevitable impurity, and Curie point is set to below normal temperature.
In addition, there is following problem: because the Ni contained in intermediate coat is magnetic material at normal temperatures, so in FPD purposes in normally used magnetic controlled tube sputtering apparatus, sputtering target material absorbs the magnetic flux of magnetic loop, is difficult to efficiency and carries out stable sputtering well.Therefore, in the present invention, under the normal temperature using Ni alloy sputtering target, by non magnetic, namely Curie point be set to below normal temperature.It should be noted that, in the present invention, " Curie point is below normal temperature " refers to, is the situation of 0 when measuring saturation magnetization under normal temperature (25 DEG C).
When adding Mn in Ni, Curie point reduces until the region of Mn solid solution and addition about 15 atom %.On the other hand, when the addition of the Mn in Ni exceedes about 20 atom %, Curie point uprises, during more than 25 atom %, due to abnormal mutually and show Compound Phase, Curie point is higher than pure Ni, and Ni alloy sputtering target becomes fragile, and becomes to be difficult to carry out the such problem of stable machining and also to become obvious.
In addition, Mn is the element being easy to oxidation than Ni, when adding Mn in Ni, is easy to form oxide at the interface with glass substrate, nesa coating etc., also has the effect can improving adaptation further.Therefore, when adding Mn in the present invention, preferably its addition is set to 1 ~ 25 atom %.More preferably the addition of Mn is 6 ~ 20 atom %.
When adding Cu in Ni, Curie point reduces, and on the other hand, as described above, when the addition of Cu is more than 40 atom %, when importing oxygen in intermediate coat, the reflectivity of low reflection characteristic, particularly short wavelength side becomes and is difficult to reduce.Therefore, in the present invention, preferably the addition of Cu is set to 10 ~ 40 atom %.Be more preferably 10 ~ 25 atom %.In addition, the total amount of Cu and Mo is preferably set to 15 ~ 50 atom %.
For the effect making to reduce as the Curie point of the Ni of magnetic material, the Mo as nonmagnetic elements is the highest, and when adding the Mo of about 8 more than atom % in Ni, Curie point becomes below normal temperature.In addition, when the addition of the Mo that unmagnetize effect is high increases, there is the effect improved with the adaptation of glass substrate, nesa coating, on the other hand, the reductions such as weatherability.Therefore, in the present invention, preferably the addition of Mo is set to 3 ~ 20 atom %.Be more preferably 5 ~ 15 atom %.In addition, the total amount of Mn and Mo is preferably set to 15 ~ 50 atom %.
The improvement effect of the etching of Mn, Fe is high.But when the Fe as magnetic material adds in Ni, Curie point significantly raises.In addition, Fe's is few with the solid solution region of Cu, and is easy to be formed the compound with Mo, when excessively adding, makes sputtering target material brittle.Therefore, in the present invention, preferably meet non magnetic and etching at sputtering target material, do not occur to add Fe in brittle scope, its addition is 5 below atom %.Be more preferably 3 below atom %.
According to above situation, the Mn of Ni alloy sputtering target of the present invention more preferably containing 1 ~ 25 atom %, the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, the Fe of 0 ~ 5 atom %.
For Ni alloy sputtering target of the present invention, as the element added in magnetic material and Ni, selection Curie point is the element of below normal temperature, such as can obtain as follows: make lysed blank, after being formed as tabular by plastic working, be cut into given size by machining, thus obtain.
But the composition that the addition for Mn is many, comprise the composition of Mo and Fe, be easy to show Compound Phase in Ni alloy sputtering target, it is tired that plastic working sometimes becomes difficulty.Under such circumstances, preferably select to add to as the element in the Ni of magnetic material, pressure sintering is carried out to the Ni alloy powder that Curie point is below normal temperature.Particularly stacked wiring membrane of the present invention owing to using, so in order to stably manufacture Ni alloy sputtering target of the present invention, most preferably carry out pressure sintering to Ni alloy powder in the FPD field using large-scale transparency carrier.
Curie point is that the Ni alloy powder of below normal temperature can be the atomization of the Ni alloy of final composition by Use Adjustment and easily obtain.In addition, lysed blank pulverizing can also be made Ni alloy powder.In addition, can also apply and manufacture various Ni alloy powder, be mixed the method being final composition.
In addition, in the present invention, be the Ni alloy powder of more than 5 μm by use average grain diameter, the increase of the impurity in gained Ni alloy sputtering target can be suppressed.In addition, in the present invention, be the Ni alloy powder of less than 300 μm by use average grain diameter, highdensity sintered body can be obtained.
It should be noted that, in the present invention, so-called average grain diameter utilizes the ball equivalent diameter based on specifying, using the light scattering method of laser in JIS Z 8901, represents with the D50 of cumulative particle size distribution.
The pressure sintering used when obtaining Ni alloy sputtering target of the present invention can adopt high temperature insostatic pressing (HIP) (hereinafter referred to as " HIP "), hot pressing, preferably 800 ~ 1250 DEG C, 10 ~ 200MPa, to carry out under the condition of 1 ~ 10 hour.The selective dependency of these conditions is in the device carrying out pressure sintering.Such as HIP is easy to application under the condition of cryogenic high pressure, and hot pressing is easy to application under the condition of high-temperature low-pressure.In the present invention, carry out under being preferably used in low temperature sintering and can suppress the diffusion of Ni alloy and under high pressure carry out sintering and the HIP of highdensity sintered body can be obtained.
When sintering temperature is lower than 800 DEG C, sintering is difficult to advance, and is difficult to obtain highdensity sintered body.On the other hand, when sintering temperature is more than 1250 DEG C, performance liquid phase, or the crystal growth of sintered body becomes obvious, is difficult to the tissue obtaining fine uniform structure.By sintering in the scope of 800 ~ 1250 DEG C, highdensity Ni alloy sputtering target easily can be obtained.
In addition, when plus-pressure during sintering is less than 10MPa, sintering is difficult to advance, and cannot obtain highdensity sintered body.On the other hand, when pressure is more than 200MPa, the problem that the device that existence can tolerate is restricted.
In addition, sintering time is less than 1 constantly little, is difficult to sinter fully, is difficult to obtain highdensity sintered body.On the other hand, the sintering time more than 10 hours is preferably avoided from the viewpoint manufacturing efficiency.
Utilize HIP, hot pressing is when carrying out pressure sintering, expect to be filled into by Ni alloy powder after in pressurizing vessel, pressurization mould, it is degassed that limit heating edge carries out decompression.Reduce pressure in the degassed scope being desirably in heating-up temperature 100 ~ 600 DEG C, carry out under the decompression lower than atmospheric pressure (101.3kPa).This is because, the oxygen of gained sintered body can be reduced further, the formation of the thick oxide hindering machining property can be suppressed, highly purified sputtering target material can be obtained.
In addition, the element of Ni alloy sputtering target of the present invention preferably except Ni and Mn, Cu, Mo and Fe is few as best one can.When impurity except these elements is many, the resistance value that resultant layer folds wiring membrane sometimes increases, or reacts with other laminate films according to the kind of element thus make the characteristic degradation such as adaptation, weatherability.Particularly the oxygen of gas componant, nitrogen generate thick oxide, nitride in sputtering target material, hinder machining property.Therefore, the purity of Ni alloy sputtering target of the present invention is preferably more than 99.9 quality %, and impurity is preferably below 1000 quality ppm, is more preferably below 300 quality ppm.
[embodiment 1]
First, in order to form the Ni-Cu-Mo alloy film as intermediate coat, being that the mode of Ni-15%Cu-8%Mo weighs with atomic ratio measuring, in vacuum melting stove, making blank by melting casting.By carrying out machining to this blank, make the Ni alloy sputtering target of diameter 100mm, thickness 5mm.
Make gained Ni alloy sputtering target near SmCo magnet, results verification its be not attached to magnet.In addition, a part for the blank obtained in above-mentioned is dropped in the housing that magnetic characteristic measures, use the vibration sample type magnetometer (model number: VSM-5) of Riken Densi K. K., under normal temperature (25 DEG C), measure magnetic characteristic, results verification its be non magnetic.
In addition, in order to be formed as the Al film of the conducting film be layered on intermediate coat, Ag film, Cu film and Mo film, prepare the sputtering target material of Al, Ag, Cu and Mo of diameter 100mm, thickness 5mm.Al sputtering target material uses the product of Sumitomo Chemical Co, and Ag sputtering target material uses the product of Furuya metal Co., Ltd..In addition, the Cu sputtering target material for the formation of the Cu film as conducting film passes through to cut out making the raw material of the oxygen-free copper (OFC) made from Hitachi Cable Ltd.'s (at present: Hitachi Metal Co., Ltd.).In addition, for the formation of the Mo sputtering target material of the Mo film as conducting film by having carried out cutting out making in the raw material of pressure sintering from by the Mo powder of purity 4N.
Each sputtering target material of above-mentioned preparation is soldered on backing plate made of copper, is installed on ULVAC, the sputter equipment (model number: CS-200) of Inc..Then, in glass substrate (the goods numbering: EagleXG) the upper film forming the thickness shown in table 1 and form, makes each sample of 25mm × 50mm.It should be noted that, the sputter gas composition [Ar+O shown in table 1
2] comprise in Ar in the atmosphere of the oxygen of 50 volume % and formed.In addition, conducting film uses Ar gas to be formed directly on intermediate coat.
For each sample of gained, the result measuring reflectivity and resistivity is shown in table 1.It should be noted that, the mensuration of reflectivity uses Konica Minolta, and the spectral photometric colour measuring meter (model number: CM2500d) of Inc. measures respectively from glass substrate side and the reflectivity from conducting film side.In addition, the mensuration of resistivity uses the resistivity of film resiativity meter (model number: MCP-T400) mensuration from conducting film side of Mitsubishi Petrochemical Co., Ltd's system (at present: DIA INSTRUMENTS CO., LTD.).
[table 1]
As described in Table 1, can confirm, as the stacked wiring membrane of the example of the present invention intermediate coat comprising Ni alloy formed in the sputter gas comprising Ar and oxygen being formed with conducting film, there is the low reflectivity that the reflectivity measured from transparent glass substrate side is less than 10%.In addition, use as conducting film the resistivity of the conducting film of the stacked wiring membrane of the example of the present invention of Cu, Al, Ag, Mo, Ni alloy to be 150 μ below Ω cm, can low resistance be confirmed as.
In addition, for being the sample of 50nm by the intermediate coat film forming in stacked wiring membrane of the present invention, use the x-ray photoelectron light-dividing device (ESCA) (model number: AXIS-HS) of KRATOS ANALYTICAL Inc., measure the oxygen concentration in intermediate coat.As a result, the oxygen containing 46 atom %, confirms there is Cu by analysis diagram
2o, MoO
3, the part confirming Addition ofelements becomes oxide and is present in intermediate coat.
[embodiment 2]
Then, in order to make by taking atomic ratio measuring as the Ni alloy sputtering target that Ni-10%Mn-25%Cu-10%Mo-3%Fe is formed, first, the Ni alloy powder that the purity making above-mentioned composition by gas atomization is 99.9%, average grain diameter is 65 μm.
Make gained Ni alloy powder near SmCo magnet, results verification its be not attached to magnet.In addition, a part for gained Ni alloy powder is dropped in the powder housing of magnetic characteristic mensuration, use the vibration sample type magnetometer (model number: VSM-5) of Riken Densi K. K., under normal temperature (25 DEG C), measure magnetic characteristic, results verification its be non magnetic.
Then, the Ni alloy powder obtained in above-mentioned is filled into internal diameter 133mm, height 30mm, thickness 3mm mild steel container in, heat 10 hours at 450 DEG C, carry out de-gas treatment, then mild steel container is sealed, utilize HIP device, 1000 DEG C, 148MPa, to sinter under the condition of 5 hours.
After this mild steel container is cooled, take out from HIP device, by machining removing mild steel container, obtain the Ni alloy sputtering target of diameter 100mm, thickness 5mm.In addition, test film is cut out from remainder.
Measured the relative density of gained test film by Archimedes method, results verification its be 99.9%.It should be noted that, in the present invention, so-called relative density refers to, using the bulk density measured by Archimedes method divided by as the solid density obtained according to the weighted average that forms the element simple substance calculated with the mass ratio that the ratio of components of sputtering target material obtains by cover layer of the present invention, income value is multiplied by 100 and the value that obtains.
Then, the inductively coupled plasma apparatus for analyzing luminosity (ICP) (model number: ICPV-1017) of Shimadzu Scisakusho Ltd is used to carry out the quantitative analysis of the metallic element of gained test film, measure oxygen quantitative by non-dispersive type infrared absorption, the purity of the total of the assay value of results verification Ni, Mn, Cu, Mo, Fe is 99.9%, oxygen concentration is 500 quality ppm.
Operate similarly to Example 1 and the Ni alloy sputtering target obtained in above-mentioned is soldered on backing plate made of copper, be then installed on ULVAC, the sputter equipment (model number: CS-200) of Inc..Then, in glass substrate (the goods numbering: include in the atmosphere of the oxygen of 50 volume % the Ni alloy film formed as intermediate coat EagleXG) in Ar of 25mm × 50mm.In addition, use Ar gas that the conducting film be directly formed on above-mentioned intermediate coat is carried out film forming, make each sample according to the formation shown in table 2.In addition, the Ni alloy of the sample No.39 ~ No.43 shown in table 2, the conducting film of No.45 and No.48 uses by taking atomic ratio measuring as the Ni alloy that Ni-10%Mn-25%Cu-10%Mo-3%Fe is formed.
The evaluation of each sample adopts method similarly to Example 1 to measure reflectivity and resistivity.The results are shown in table 2.
[table 2]
As shown in sample No.11, No.12, the No.19 of the comparative example shown in as table 2, confirm the Film Thickness Ratio 20nm of the intermediate coat formed by the oxygen containing Ni alloy of bag thin time, the low reflectivity of less than 20% cannot be obtained.
On the other hand, the reflectivity being laminated with the stacked wiring membrane of intermediate coat within the scope of the invention and conducting film is less than 20%, can confirm that low reflection characteristic is excellent.In addition, the resistivity as the conducting film using the stacked wiring membrane of the example of the present invention of Mo, Cu, Al, Ni alloy in conducting film is 150 μ below Ω cm, can confirm as low resistance.
The thickness of the intermediate coat that reflectivity reduces most is different according to the material of conducting film, and known thickness is near 50nm.Herein, when the thickness of the intermediate coat comprising Ni alloy can be confirmed to be fixed on 50nm, if the thickness of conducting film is more than 10nm, then can obtain the low reflection characteristic of less than 15%.
Then, the evaluation of etching is carried out.For the sample of sample No.44 and No.45, use the Al etchant of Kanto Kagaku K. K. to etch, result does not also produce inequality, can etch well.In addition, for the sample of sample No.48, use the Cu etchant of Kanto Kagaku K. K. to etch, result does not also produce residue, can etch well.
[embodiment 3]
Substrate shown in table 3 forms intermediate coat, then directly on this intermediate coat, forms conducting film and obtain the sample of stacked wiring membrane.It should be noted that, when forming intermediate coat, use Ar or in Ar, be mixed with the sputter gas film forming on substrate being the gas concentration of regulation by mass flow controller adjustment oxygen or nitrogen.In addition, conducting film uses Ar gas directly film forming on intermediate coat.
For each sample of gained, the result measuring reflectivity and resistivity is shown in table 3.It should be noted that, the mensuration of reflectivity uses Konica Minolta in the same manner as embodiment 1 and embodiment 2, and the spectral photometric colour measuring meter (model number: CM2500d) of Inc. measures reflectivity from glass substrate side with from conducting film side.In addition, the mensuration of resistivity uses the film resiativity meter (model number: MCP-T400) of Mitsubishi Petrochemical Co., Ltd's system (at present: DIAINSTRUMENTS CO., LTD.).
[table 3]
As sample No.51 ~ No.55, the No.57 ~ No.59 of example of the present invention, the stacked wiring membrane of No.61 ~ No.64 from transparent substrate side measure visible reflectance be less than 20%, can confirm to obtain low reflectivity.
In addition, as other examples of the present invention sample No.55 on the transparency carrier being formed with ito film, form intermediate coat, directly on this intermediate coat, form resistivity be the stacked wiring membrane of the conducting film of 3.7 μ Ω cm, also can confirm to obtain low reflectivity.
In addition, as as shown in the sample No.62 as other example of the present invention, the thin-film transparent substrate that the hyaline membrane of the PET as resin is formed ito film is formed with intermediate coat, to be directly formed with resistivity on this intermediate coat be the stacked wiring membrane of the conducting film of 2.4 μ below Ω cm, also can confirm to obtain low reflectivity.
Adopt the oxygen amount in the intermediate coat of the sample No.56 using Ar+10 volume % oxygen to be formed in the mensuration of method similarly to Example 1 sputter gas, the oxygen amount in result intermediate coat is 15 atom %.In addition, the oxygen amount in the intermediate coat of the sample No.57 using Ar+20 volume % oxygen to be formed in sputter gas is 24 atom %.
Use the etchant of the Al of Kanto Kagaku K. K., carry out etching test with the sample of the stacked wiring membrane of sample No.51, No.52, No.53, No.54, No.55.As a result, the whole samples as example of the present invention all do not have residue, can etch equably.
Use the etchant of the Cu of Kanto Kagaku K. K., carry out etching test with the sample of the stacked wiring membrane of sample No.55, No.59, No.62, No.63.As a result, whole sample does not all have inequality, can etch equably at short notice.
Claims (11)
1. a stacked wiring membrane, it is characterized in that, it has following layers stack structure: on the transparent substrate or the transparency carrier being formed with hyaline membrane is formed with the thickness comprising Ni alloy is the intermediate coat of 20 ~ 100nm, directly on described intermediate coat, be formed with the conducting film that resistivity is 150 μ below Ω cm
The visible reflectance measured from described transparent substrate side is less than 20%.
2. stacked wiring membrane according to claim 1, is characterized in that, described conducting film is to be selected from element in Al, Cu, Mo, Ni, Ag as main component, and thickness is 10 ~ 500nm.
3. according to stacked wiring membrane according to claim 1 or claim 2, it is characterized in that, in described intermediate coat, be selected from more than one element in Cu, Mn, Mo and Fe with count 15 ~ 60 atom %, remainder by Ni and inevitably impurity form.
4. according to stacked wiring membrane according to claim 1 or claim 2, it is characterized in that, described intermediate coat contains the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom % and the total amount of Cu and Mo is 15 ~ 50 atom %, and remainder is made up of Ni and inevitable impurity.
5. according to stacked wiring membrane according to claim 1 or claim 2, it is characterized in that, in described intermediate coat, Mn be 1 ~ 25 atom %, Mo be 3 ~ 30 atom % and the total amount of Mn and Mo be 15 ~ 50 atom %, remainder by Ni and inevitably impurity form.
6. according to stacked wiring membrane according to claim 1 or claim 2, it is characterized in that, described intermediate coat contains the Mn of 1 ~ 25 atom %, the Cu of 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, the Fe of 0 ~ 5 atom %, and remainder is made up of Ni and inevitable impurity.
7. a Ni alloy sputtering target, it is characterized in that, it is the Ni alloy sputtering target for the formation of intermediate coat according to claim 1, it contains to amount to more than one the element be selected from Cu, Mn, Mo and Fe counting 15 ~ 60 atom %, remainder is made up of Ni and inevitable impurity, and Curie point is below normal temperature.
8. Ni alloy sputtering target according to claim 7, is characterized in that, the Mo of the Cu containing 10 ~ 40 atom %, 3 ~ 20 atom %, and the total amount of Cu and Mo is 15 ~ 50 atom %.
9. Ni alloy sputtering target according to claim 7, is characterized in that, the Mo of the Mn containing 1 ~ 25 atom %, 3 ~ 30 atom %, and the total amount of Mn and Mo is 15 ~ 50 atom %.
10. Ni alloy sputtering target according to claim 7, is characterized in that, the Fe of the Cu of the Mn containing 1 ~ 25 atom %, 10 ~ 40 atom %, the Mo of 3 ~ 20 atom %, 0 ~ 5 atom %.
The manufacture method of 11. 1 kinds of stacked wiring membranes, it is characterized in that, described intermediate coat be containing 20 ~ 60 volume % be selected from the atmosphere of at least one in oxygen and nitrogen under, use the Ni alloy sputtering target described in any one of claim 7 ~ claim 10 to be formed by sputtering method.
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