CN109996903A - The manufacturing method of physical vapor deposition target structure and sputtering target structure and physical vapor deposition film and layer structure - Google Patents
The manufacturing method of physical vapor deposition target structure and sputtering target structure and physical vapor deposition film and layer structure Download PDFInfo
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- CN109996903A CN109996903A CN201780072744.6A CN201780072744A CN109996903A CN 109996903 A CN109996903 A CN 109996903A CN 201780072744 A CN201780072744 A CN 201780072744A CN 109996903 A CN109996903 A CN 109996903A
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- vapor deposition
- physical vapor
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- film
- substrate
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Abstract
A kind of physical vapor deposition target structure is provided, wherein, the deterioration of substrate caused by oxidation is few when forming physics evaporation film, it is few in the defect that the joint portion of physical vapor deposition film and substrate generates, physical vapor deposition film and the lattice of substrate are good, in turn, rotten few caused by the hydration of its own or the physical vapor deposition film formed.Physical vapor deposition uses target structure to include Mg, M (M is trivalent metallic element) and O as main component, Mg and M and is scaled MgO and M respectively2O3Molar ratio after such oxide is 70:30~10:90.
Description
Technical field
The present invention relates to the manufacturers of physical vapor deposition target structure and sputtering target structure and physical vapor deposition film and layer structure
Method.
Background technique
In recent years, as improve magnetic recording system packing density magnetic recording element, magnetic tunnel-junction (MTJ) element by
Concern.MTJ element has structure, i.e. ferromagnetic layer/tunnel barrier layer/iron using two ferromagnetic layer clamping tunnel barrier layers
The three-decker of magnet layer.Existing tunnel barrier layer has used Al oxidation film (the amorphous AlO with amorphous structurexFilm)
Or the crystallinity MgO membrane of (001) planar orientation.But amorphous AlOxFilm due to the engagement resistance with ferromagnetic layer is high, with it is ferromagnetic
The interface roughness of body layer is big, characteristic deviation is big, tunnel magneto resistance ratio (TMR ratio) is small, thus is unsuitable for the tunnel gesture of MTJ element
Barrier layer.On the other hand, there is the ferromagnet of bcc crystal structure for Fe or FeCo etc., crystallinity MgO membrane is due to tunnel resistor
(TR) small, TMR is suitable for the tunnel barrier layer of MTJ element than big.Therefore, expect performance raising, the MTJ member of MTJ element
Part miniaturization, the packing density of magnetic recording system for having MTJ element further increase.But MgO is easy to happen hydration, because
This reacts sometimes with the moisture etc. in atmosphere in Surface Creation hydroxide, worries crystallinity MgO membrane or is used to form
The MgO sputtering target structure of the film occurs rotten.
A kind of spinel structure MgAl for being added in crystallinity MgO membrane and having Al is described in patent document 12O4Film.About
Spinel structure MgAl2O4Film, discovery: TR is than amorphous AlOxFilm reduces an order of magnitude or more；Available bigger TMR ratio；It is right
In the full heusler alloy of ferromagnetic Co base or CoFe alloy, lattice is good compared with crystallinity MgO membrane, therefore being capable of shape
At the few extension tunnel knot of defect, the tunnel barrier layer as MTJ element is highly expected.
Existing technical literature
Patent document
Patent document 1: Japanese Patent No. 5586028
Summary of the invention
Problems to be solved by the invention
Herein, the spinel structure MgAl recorded in patent document 12O4The manufacturing method of film is as described below.That is, by splashing
It penetrates in the ferromagnetic layer of substrate after lamination Mg film and Al film, implements plasma oxidation processing, alternatively, sputtering MgAl2Alloy
And MgAl is formed in the ferromagnetic layer of substrate2After alloy film, implement plasma oxidation, thus metal film or alloy film are by oxygen
Change, crystallization, forms spinel structure MgAl2O4Film.
The spinel structure MgAl recorded in patent document 12O4The manufacturing method of film is due to forming metal film or alloy film
Implement plasma oxidation processing, therefore deterioration caused by the oxidation of the ferromagnetic layer of worry substrate afterwards.In addition, along with metal
The oxidation of film or alloy film, crystallization need oxygen atom to enter the metal in metal film or alloy film and metal film or alloy film
The rearrangement of atom is worried to generate defect.Therefore, from spinel structure MgAl2O4The removal of the defect of film or extension tunnel knot is not filled
Point, the limit of the densification of the miniaturization and magnetic recording system of MTJ element is worrying.
1st and the 2nd mode of the invention is designed to provide a kind of physical vapor deposition target structure and sputtering target structure,
In, the deterioration of substrate caused by oxidation is few when forming physics evaporation film, lacks what the joint portion of physical vapor deposition film and substrate generated
Fall into few, the lattice of physical vapor deposition film and substrate is good, and in turn, the hydrability of its own or the physical vapor deposition film formed is low,
It is rotten few caused by hydration.3rd mode of the invention is designed to provide a kind of physical vapor deposition film, wherein caused by aoxidizing
The deterioration of substrate is few, few in the defect generated with the joint portion of substrate, good with the lattice of substrate, in turn, caused by hydration
It is rotten few.4th mode of the invention is designed to provide a kind of layer of structure, wherein and the deterioration of the substrate caused by aoxidizing is few,
Few in the defect that the joint portion of physical vapor deposition film and substrate generates, the lattice of physical vapor deposition film and substrate is good, Jin Ershui
It is rotten few caused by closing, therefore TMR ratio improves, it can be expected that miniaturization.
Means for solving the problems
(1) the 1st mode of the invention is related to a kind of physical vapor deposition target structure, which is characterized in that it includes Mg, M (M 3
Valence metallic element) and O as main component, Mg and M be scaled MgO and M respectively2O3Molar ratio after such oxide is 70:
30~10:90.
Make physical vapor deposition target structure as main component in substrate using comprising Mg, M (M is trivalent metallic element) and O
The physical vapor deposition film for having carried out physical vapor deposition supplies required oxygen (O) from physical vapor deposition target structure, therefore does not need to form a film
Oxidation processes afterwards.Therefore, the deterioration of the substrate caused by aoxidizing is few.In addition, it is not necessary that the oxidation of metal film or alloy film, crystal
Change, therefore, the defect generated at the joint portion of physical vapor deposition film and substrate can be reduced.In addition, being changed respectively by using Mg and M
Calculating is MgO and M2O3The physical vapor deposition target structure that molar ratio after such oxide is 70:30~10:90 is enterprising in substrate
Row physical vapor deposition is capable of forming the physical vapor deposition film good with the lattice of substrate.Further, since physical vapor deposition target structure
It is not MgO with physical vapor deposition film, thus it is rotten few caused by hydration, and resistance to hydrability equistability is excellent.
(2) the 2nd mode of the invention is related to a kind of physical vapor deposition target structure, which is characterized in that it includes Mg, M (M 3
Valence metallic element) and O as main component, physical vapor deposition target structure includes the crystal phase with spinel structure.
Make physical vapor deposition target structure as main component in substrate using comprising Mg, M (M is trivalent metallic element) and O
The physical vapor deposition film for having carried out physical vapor deposition supplies required oxygen (O) from physical vapor deposition target structure, therefore does not need to form a film
Oxidation processes afterwards.Therefore, the deterioration of the substrate caused by aoxidizing is few.In addition, it is not necessary that the oxidation of metal film or alloy film, crystal
Change, therefore, the defect generated at the joint portion of physical vapor deposition film and substrate can be reduced.In addition, by using comprising having point
The physical vapor deposition of the crystal phase of spinel structure carries out physical vapor deposition with target structure in substrate, is capable of forming the Lattice Matching with substrate
The good physical vapor deposition film of property.Further, since physical vapor deposition target structure and physical vapor deposition film are not MgO, thus caused by hydration
Rotten few, resistance to hydrability equistability is excellent.
(3) in the 1st or the 2nd mode of the invention, M is preferably selected from a kind or 2 kinds in the group being made of Al and Ga.It is logical
It crosses and carries out physics steaming in substrate with target structure for a kind or 2 kinds of the physical vapor deposition in the group being made of Al and Ga using M
Plating, is capable of forming and the physically better evaporation film of the lattice of substrate.
(4) in the 1st or the 2nd mode of the invention, light transmittance when making with a thickness of 2mm is preferably 60% or less.As packet
Make the purposes of composition as main component containing Mg, M (especially Al) and O, it is known that the window of electrical equipment, manufacture container
Material, but physical vapor deposition do not need window material with target structure as light permeability.Therefore, by making physical vapor deposition target structure structure
Light transmittance when as with a thickness of 2mm is 60% hereinafter, can be easier and physical vapor deposition target structure be manufactured at low cost.
(5) in the 1st or the 2nd mode of the invention, dielectric loss under 10GHz be preferably 45000GHz in terms of fQ value with
On.The dielectric loss of physical vapor deposition target structure under 10GHz is calculated as 45000GHz or more with fQ value and reflects physical vapor deposition
It is few with the defect of target structure, inevitable impurity.Physical vapor deposition is carried out with target structure by using this physical vapor deposition, it can
Form that defect, inevitable impurity is less, physical vapor deposition film more evenly.
(6) in the 1st or the 2nd mode of the invention, whiteness is preferably 30 or more.Whiteness reflects physics for 30 or more
The inevitable impurity of vapor deposition target structure, defect are few.Physical vapor deposition is carried out with target structure by using this physical vapor deposition,
It is capable of forming that inevitable impurity, defect be less, physical vapor deposition film more evenly.
(7) in the 1st or the 2nd mode of the invention, physical vapor deposition is suitable for sputtering target structure with target structure.
(8) the 3rd mode of the invention is related to a kind of manufacturing method of physical vapor deposition film, which is characterized in that its using the 1st or
The physical vapor deposition target structure of 2nd mode physical vapor deposition in substrate goes out physical vapor deposition film.
Using the physical vapor deposition target structure of the 1st or the 2nd mode physical vapor deposition film that physical vapor deposition goes out in substrate from object
Oxygen (O) required for vapor deposition is supplied with target structure is managed, therefore does not need the oxidation processes after film forming.Therefore, caused base is aoxidized
The deterioration at bottom is few.In addition, it is not necessary that the oxidation of metal film or alloy film, crystallization, therefore, can reduce physical vapor deposition film with
The defect that the joint portion of substrate generates.In addition, being scaled MgO and M respectively by using Mg and M2O3Rubbing after such oxide
You are than being that 70:30~10:90 or the physical vapor deposition comprising the crystal phase with spinel structure are carried out in substrate with target structure
Physical vapor deposition is capable of forming the physical vapor deposition film good with the lattice of substrate.Further, since physical vapor deposition film is not MgO,
Rotten few caused by being thus hydrated, resistance to hydrability equistability is excellent.
(9) the 4th mode of the invention is related to the manufacturing method of a kind of layer of structure, which is characterized in that it uses of the invention
The physical vapor deposition target structure of 1st or the 2nd mode physical vapor deposition in substrate goes out physical vapor deposition film, is formed on physical vapor deposition film
Ferromagnetic layer, substrate are ferromagnetic layer, and physical vapor deposition film is tunnel barrier layer.
The physical vapor deposition film of physical vapor deposition is carried out in substrate with target structure using the physical vapor deposition of the 1st or the 2nd mode
Required oxygen (O) is supplied from physical vapor deposition target structure, therefore does not need the oxidation processes after film forming.Therefore, substrate is because of oxygen
Deterioration caused by changing is few.In addition, it is not necessary that therefore the oxidation of metal film or alloy film, crystallization can be reduced in physical vapor deposition
The defect that the joint portion of film and substrate generates.In addition, being scaled MgO and M respectively by using Mg and M2O3After such oxide
Molar ratio be that 70:30~10:90 or the physical vapor deposition comprising the crystal phase with spinel structure carry out physics with target structure
Vapor deposition, is capable of forming the physical vapor deposition film good with the lattice of substrate.If substrate is ferromagnetic layer, physical vapor deposition film is tunnel
Road barrier layer then forms the layer structure using 2 ferromagnetic layer clamping tunnel barrier layers.This layer of structure due to TMR ratio improve, because
This can manufacture the magnetic tunnel junction element of miniaturization compared with the past.Further, since physical vapor deposition film is not MgO, thus it is hydrated
Caused is rotten few, and resistance to hydrability equistability is excellent.
Specific embodiment
Physical vapor deposition of the invention can be used resistive heating evaporation with target structure, sputtering method, e-beam evaporation, divide
Physical vapor deposition well known to beamlet epitaxy, ion plating vapour deposition method, laser ablation method etc., hereinafter, as a reality of the invention
Mode is applied, the sputtering target structure for sputtering method is illustrated.It should be noted that present embodiment described below is not
The contents of the present invention recorded in claim are undeservedly limited, and whole constitute illustrated in present embodiment is used as this hair
Bright solution it is not necessary to.
(1) target structure is sputtered
The sputtering target structure of present embodiment includes Mg, M (M is trivalent metallic element) and O as main component.In addition to master
It wants other than ingredient, sputtering target structure also may include accessory ingredient.To comprising Mg, M (M be trivalent metallic element) and O conduct mainly at
The sputtered film that the sputtering target structure divided is sputtered and formed supplies required oxygen (O) from sputtering target structure, therefore does not need
Oxidation processes after film forming.Therefore, the deterioration of the substrate caused by aoxidizing is few.In addition, it is not necessary that the oxidation of metal film or alloy film,
Therefore crystallization can reduce the defect generated at the joint portion of sputtered film and substrate.Further, since sputtering target structure and splashing
Penetrating film is not MgO, thus rotten few caused by hydration, and resistance to hydrability equistability is excellent.
The Mg and M for including in sputtering target structure are scaled MgO and M respectively2O3Molar ratio after such oxide is preferably
70:30~10:90, more preferably 65:35~20:80, further preferably 60:40~30:70, particularly preferably 55:45~
40:60.It is scaled MgO and M respectively by adjusting the Mg and M for including in sputtering target structure2O3Mole after such oxide
Than crystal phase, the lattice constant of sputtered film can be controlled.Therefore, it is capable of forming the sputtered film good with the lattice of substrate.
Sputtering target structure preferably comprises the crystal phase with spinel structure.By to including the crystal phase with spinel structure
Sputtering target structure sputtered, be capable of forming the sputtered film good with the lattice of substrate.
The M for including in sputtering target structure is preferably selected from a kind or 2 kinds in the group being made of Al and Ga.By being choosing to M
1 kind or 2 kinds of sputtering target structure in the group of free Al and Ga composition is sputtered, and the lattice with substrate is capable of forming
Better sputtered film.
The light transmittance of sputtering target structure when making with a thickness of 2mm is preferably 60% or less, more preferably 45% or less.As
Make the purposes of composition as main component comprising Mg, M (especially Al) and O, it is known that the window of electrical equipment, manufacture container
Material, but sputter the permeability that target structure does not need light as window material.By making light transmittance above range, can it is easier and
Manufacture sputtering target structure at low cost.
The inevitable impurity of sputtering target structure is at least 0.5 mass %, is preferably 0.1 mass % or less, more preferable
For 0.01 mass % or less.It is sputtered, is capable of forming inevitable by the sputtering target structure few to inevitable impurity
Impurity, defect is less, sputtered film more evenly.
The dielectric loss of sputtering target structure under 10GHz is preferably 45000GHz or more in terms of fQ value, is more preferably
50000GHz or more, further preferably 70000GHz or more, particularly preferably 80000GHz or more.The fQ value of dielectric loss
Defect, the inevitable impurity for reflecting sputtering target structure greatly are few.It, can by being sputtered to such sputtering target structure
Form that defect, inevitable impurity is less, sputtered film more evenly.It should be noted that dielectric loss by tan δ or its fall
Several quality factor Q values (=1/tan δ) indicates, changes because of frequency, therefore also product, that is, fQ of conventional frequency f and Q value
Value indicates.The more big then dielectric loss of fQ value is smaller.
The whiteness of sputtering target structure is preferably 30 or more, is more preferably 50 or more, is more preferably 60 or more, special
Preferably 65 or more.It is few that whiteness height reflects the inevitable impurity of sputtering target structure, defect.By to this sputtering target
Component is sputtered, and is capable of forming that defect, inevitable impurity is less, sputtered film more evenly.It should be noted that white
Degree uses the L* of CIE1976 (L*, a*, b*).Whiteness is indicated closer to 100 closer to white.
The surface roughness of sputtering target structure is preferably 5 μm or less, more preferably 2 μm or less, be more preferably 1 μm with
Under.Sputter target structure surface roughness is smaller, i.e. surface is more smooth, then can more equably to sputter the surface of target structure into
Row sputtering, is capable of forming that defect is less, sputtered film more evenly.
The thickness and diameter for sputtering target structure can be changed to desired thickness and diameter according to sputtering equipment, as one
Example, can enumerate thickness 2.0mm or less.
The material for sputtering target structure is not particularly limited as long as uniformly and as long as densification, is preferably made of sintered body.It can also be with
It is easy by the manufacturing methods of other solids such as melting and solidification and manufacture uniform and fine and close sputtering target structure at low cost.
The relative density of sintered body is preferably 95 mass % or more, more preferably 98 mass % or more, is more preferably
99 mass % or more, particularly preferably 99.5 mass % or more.The relative density of sintered body is higher, then it is finer and close to sputter target structure
And uniformly, it is capable of forming that defect is less, sputtered film more evenly.
The three-point bending strength of sintered body is preferably 230MPa or more, more preferably 250MPa or more, is more preferably
300MPa or more, particularly preferably 320MPa or more.The bending strength of sintered body is higher, then it is finer and close and equal to sputter target structure
It is even, it is capable of forming that defect is less, sputtered film more evenly.It should be noted that the measuring method of three-point bending strength uses JIS
R1601。
Using use circle to convert particle area Heywood conversion diameter as partial size when, crystalline substance about composition sintered body
The average grain diameter of grain, as long as can make sintered body uniformly and it is fine and close as long as be not particularly limited, preferably 1~100 μm, more preferably
2~80 μm, further preferably 2~60 μm, particularly preferably 2~50 μm.By to uniform and fine and close sputtering target structure into
Row sputtering, is capable of forming that defect is less, sputtered film more evenly.
About the D90/D10 for the crystal grain for constituting sintered body, do not limited especially as long as sintered body can be made uniform and is fine and close
System, preferably 4 or less, more preferably 3 or less, further preferably 2.5 or less, particularly preferably 2.3 or less.By to uniform
And fine and close sputtering target structure is sputtered, and is capable of forming that defect is less, sputtered film more evenly.
It should be noted that finding out the partial size of 200 crystal grain about average grain diameter, use particle diameter distribution (number benchmark)
50% value (D50).D10, D90 equally use the value of 10% value of particle diameter distribution (number benchmark), 90%.
(2) manufacturing method of target structure is sputtered
The manufacturing method of the sputtering target structure of present embodiment includes following processes: weigh, mixed raw material powder and obtain
The raw material mixed processes of slurry；Granulation is dried to slurry and obtains the drying-granulating process of pelletizing；Pelletizing is formed
And obtain the molding procedure of formed body；Formed body is sintered and obtains the sintering process of sintered body；Outside to sintered body
Shape, which is processed, obtains the sharp processing process of sputtering target structure.Hereinafter, being carried out to the manufacturing method of sputtering target structure more detailed
Thin explanation.
(2-1) raw material mixed processes
As the raw material of sputtering target structure, MgO, M can be used2O3The powder of (M is trivalent metallic element).M is preferably selected
1 kind or 2 kinds in the group of free Al and Ga composition.Raw material includes MgO and M2O3It, as needed can be into one as main component
Step includes accessory ingredient.The purity of raw material powder is preferably high, at least 99.5 mass % or more, preferably 99.9 mass % or more,
More preferably 99.99 mass % or more, further preferably 99.999 mass % or more.By using the raw material powder of purity is high
End can obtain the few sputtering target structure of inevitable impurity.By being sputtered to the sputtering target structure, it is capable of forming not
Evitable impurity, defect be less, sputtered film more evenly.
When using the Heywood conversion diameter to be converted with circle to particle area, the average grain diameter (D50) of raw material powder is more
It is small, then it is sintered and is more promoted, obtain more uniform and fine and close sputtering target structure, therefore at least 100 μm or less, preferably 1 μm
Below, it is more preferably 0.5 μm or less.
The raw material of sputtering target structure is not limited to MgO, M2O3Carbonate, nitrate etc. also can be used in such oxide
Become the compound of oxide in manufacturing process.
Weigh raw material powder.Mg and M are scaled MgO and M respectively2O3Molar ratio after such oxide is preferably 70:30
~10:90, more preferably 65:35~20:80, further preferably 60:40~30:70, particularly preferably 55:45~40:60.
By adjusting the molar ratio of Mg and M, crystal phase, the lattice constant of sputtered film can be controlled.Therefore, it is capable of forming the lattice with substrate
The good sputtered film of matching.
Mixed raw material powder and obtain slurry.About mixed method, as long as can not have as long as mixed raw material powder equably
Especially limitation, such as preferred wet ball mill.In the case where wet ball mill, raw material powder, decentralized medium and ball are put into
In container and mixed (wet mixed).The organic solvents such as water or ethyl alcohol, methanol can be used in decentralized medium.About raw material
With the mass ratio of decentralized medium, it is not particularly limited as long as it can equably mix raw material powder, is usually mostly 15:
85~75:25.In order to equably mix raw material powder, dispersing agent can be further added.As long as dispersing agent is in aftermentioned degreasing
Or it decomposes in sintering process and is just not particularly limited without remaining.About incorporation time, as long as can be by raw material powder equably
Mixing is just not particularly limited, and preferably 10 hours or more.If raw material powder is not uniformly mixed, sputtering target structure can be sent out
Raw composition, density unevenness, intensity are easily reduced.In addition, being easy to happen in sputtering if being sputtered to this sputtering target structure
Paradoxical discharge, and then defect easy to form is more, non-uniform sputtered film.
Raw material mixed processes may further include following processes: after raw material powder is mixed, slurry is dried and
Obtain the drying process of xeraphium；Xeraphium is heat-treated obtain raw material part or all by composite oxides structure
At heat treatment powder heat treatment procedure；It is put into container and goes forward side by side with by the methanol and alumina balls that are heat-treated powder, decentralized medium
Row case of wet attrition and obtain the pulverizing process of slurry.By heat treatment, the reaction of raw material powder is carried out, therefore, in follow-up sintering
Sputtering target structure obtained in process is easy comprising the crystal phase with spinel structure.About the partial size of heat treatment powder, due to holding
Easily promote the sintering of follow-up sintering process, therefore preferably smaller.Therefore, pulverizing process can take a step forward combination in case of wet attrition
Dry grinding.
(2-2) drying-granulating process
Slurry obtained in raw material mixed processes is dry, granulation obtains being suitable for molding pelletizing.Slurry can be dry
Shaping assistant is added as needed before dry.Shaping assistant is not particularly limited, and usually uses polyvinyl alcohol (PVA), poly- second mostly
Glycol (PEG), Selosol, alkane etc..Drying means is not particularly limited, such as preferred rotary evaporator, spray drying
Machine.The purity of pelletizing is preferably high, at least 99.5 mass %, more preferably 99.9 mass %, further preferably 99.99 matter
Measure % or more.
(2-3) molding procedure
Pelletizing is formed, the formed body of regulation shape is obtained.About forming method, can will use mold it is uniaxial at
Forming method well known to type, CIP (isostatic cool pressing) molding etc. carries out alone or in combination.About briquetting pressure, as long as can obtain
It is just not particularly limited to good formed body, it is often preferred that 100MPa or more.It should be noted that in aftermentioned sintering process
In the case that middle progress HP (hot uniaxial compression) sintering or HIP (hot isostatic pressing) are sintered, molding procedure or reduction also can be omitted
Briquetting pressure.
(2-4) sintering process
Formed body is sintered and obtains sintered body.By sintering, the manufacturing method letter of other solids can also be passed through
Just uniform and fine and close sputtering target structure and is at low cost manufactured.It, can be by normal pressure-sintered, HP sintering, HIP about sintering method
Sintering method well known to sintering etc. carries out alone or in combination.About sintering temperature, without spy as long as it can obtain sintered body
Do not limit, if 1800 DEG C hereinafter, can then be carried out under air atmosphere it is normal pressure-sintered, therefore it is preferred that.HP sintering, HIP are sintered energy
It is enough to obtain highdensity sintered body in the case where being lower than normal pressure-sintered sintering temperature.In addition, including dispersing agent or molding in pelletizing
In the case where auxiliary agent, in order to decompose, remove by them, degreasing is preferably carried out before sintering.Skimming temp is not particularly limited, excellent
Dispersing agent and shaping assistant is selected to be decomposed completely, the temperature that removes and heating rate.It should be noted that about sputtering target structure
Manufacturing method other solids such as melting and solidification also can be used as long as uniform and fine and close sputtering target structure can be manufactured
Manufacturing method.
(2-5) sharp processing process
Sintered body is processed into desired shape, obtains sputtering target structure.The method of sharp processing can be used cutting,
Method well known to grinding, grinding etc..Sputtering target structure is bonded with backboard, is supplied to sputtering as sputtering target.
(3) application of target structure is sputtered
The application examples of sputtering target structure as present embodiment, clamps tunnel barrier using 2 ferromagnetic layers to having
The layer structure of layer, the i.e. MTJ element of substrate ferromagnetic layer/tunnel barrier layer/upper ferromagnetic body layer three-decker are illustrated.
MTJ element is formed on substrate.Spinelle MgAl can be used for example in substrate2O4Monocrystalline, Si monocrystalline, GaAs monocrystalline
Or thermal oxide Si.On the surface of the substrate, the buffer layer being for example made of MgO can be formed as needed.
Substrate ferromagnetic layer (substrate), tunnel barrier layer and upper ferromagnetic body layer are sequentially formed on substrate.Substrate is ferromagnetic
Body layer, tunnel barrier layer and upper ferromagnetic body layer respectively can for example, by successively sputter the full heusler alloy of Co base (for example,
Co2FeAl0.5Si0.5), the sputtering target structure of present embodiment and CoFe alloy be (for example, Co75Fe25Alloy) it is formed.By splashing
The tunnel barrier layer (sputtered film) penetrating the sputtering target structure of present embodiment and being formed supplies required oxygen from sputtering target structure
(O), therefore the oxidation processes after film forming are not needed.Therefore, the deterioration of the substrate ferromagnetic layer caused by aoxidizing is few.In addition, tunnel
Barrier layer does not need oxidation, crystallization, therefore, can reduce in the generation of the joint portion of tunnel barrier layer and substrate ferromagnetic layer
Defect.In addition, tunnel barrier layer and the substrate ferromagnetic layer that is made of the full heusler alloy of Co base and being made of CoFe alloy
The lattice of upper ferromagnetic body layer is good.Therefore, there is substrate ferromagnetic layer/tunnel barrier layer/upper ferromagnetic body layer MTJ
TMR ratio can be improved in element, it is thus possible to manufacture small-sized MTJ element compared with the past.The magnetic recording system for having the MTJ element
Packing density can be further increased.In addition, tunnel barrier layer is not due to being MgO, rotten few, resistance to hydration caused by hydration
Property equistability is excellent.
The purposes of the sputtering target structure of present embodiment is not limited to sputtering method, and those skilled in the art can easily be understood that energy
It is enough in such as resistive heating evaporation, e-beam evaporation, molecular beam epitaxy, ion plating vapour deposition method, laser ablation method
Well known physical vapor deposition.
Embodiment
Hereinafter, the embodiment of the present invention is described in detail.
(1) manufacture of target structure is sputtered
(1-1) embodiment 1
As raw material, 0.2 μm of average grain diameter, 0.15 μ of powder and average grain diameter of the MgO of 99.98 mass % of purity are used
M, the Al of 99.99 mass % of purity2O3Powder.According to MgO and Al2O3Molar ratio be 50:50 mode weighed.?
Decentralized medium methanol, raw material powder and nylon ball are put into resin balling mill container, mixing (wet mixed) 15 hours obtains
Slurry.(drying process) is dried to slurry using rotary evaporator, by obtained xeraphium in air atmosphere, 1000 DEG C
Under be heat-treated (heat treatment procedure), obtain heat treatment powder.For being heat-treated powder, after carrying out dry grinding, to resin system
Decentralized medium methanol, heat treatment powder and alumina balls through dry grinding are added in balling mill container, carries out case of wet attrition and (crushes
Process), obtain slurry (raw material mixed processes).Slurry is dried using rotary evaporator, obtained xeraphium is broken
Broken, granulation, obtains pelletizing (drying-granulating process).
Pelletizing is subjected to HP sintering at Ar atmosphere, 1500 DEG C, pressure 20MPa, obtains HP sintered body.HP sintered body exists
Further progress HIP is sintered under Ar atmosphere, 1400 DEG C~1550 DEG C of temperature region, pressure 100MPa, obtains HIP sintered body
(sintering process).HIP sintered body is reduced by the sintering under non-active gas atmosphere, therefore, oxygen-containing atmosphere, 1500 DEG C,
5 hours oxidation processes are carried out under normal pressure, obtain sintered body.Sintered body is processed into desired shape (sharp processing process), will
Obtained sample is for evaluation.
(1-2) embodiment 2,3
Make MgO:Al2O3Molar ratio be that 40:60,30:70 utilize process production same as Example 1 in addition to this
Sample, for evaluation.
(1-3) embodiment 4
Using raw material powder same as Example 1, according to MgO:Al2O3Molar ratio be 20:80 mode claimed
Amount.Wet mixed same as Example 1 is carried out, slurry (raw material mixed processes) are obtained.Slurry is done using rotary evaporator
It is dry, obtain xeraphium.Xeraphium is crushed without heat treatment, is granulated, and pelletizing (drying-granulating process) is obtained.It will make
After grain powder is formed at pressure 100MPa (molding procedure), it is sintered 3 hours, is sintered under air atmosphere, 1750 DEG C, normal pressure
Body (sintering process).Sintered body is processed into desired shape (sharp processing process), by obtained sample for evaluation.
(1-4) embodiment 5~7
Make MgO:Al2O3Molar ratio be 10:90,60:40,70:30 utilize work same as Example 4 in addition to this
Sequence makes sample, for evaluation.
(1-5) embodiment 8
Using raw material powder same as Example 1, according to MgO:Al2O3Molar ratio be 50:50 mode claimed
Amount.Wet mixed same as Example 1 is carried out, slurry is obtained.It is using rotary evaporator that slurry is dry, obtain xeraphium.
Xeraphium is heat-treated at air atmosphere, 1000 DEG C, obtains heat treatment powder.Heat treatment powder is directly made without broken
For pelletizing.For pelletizing, HP sintering same as Example 1, HIP sintering are carried out, sintered body is obtained.Sintered body is processed into
Desired shape, by obtained sample for evaluation.
(1-6) embodiment 9
Make MgO:Al2O3Molar ratio be 30:70, in addition to this, process same as Example 4 is utilized to make sample, supplied
Evaluation.
(1-7) embodiment 10
Carry out raw material mixed processes same as Example 1 (including drying process, heat treatment procedure and pulverizing process) and
Drying-granulating process, obtains pelletizing.Pelletizing carries out 5 hours oxidation processes under oxygen-containing atmosphere, 1700 DEG C, normal pressure.Through oxygen
Change the powder of processing without broken and directly as pelletizing, carries out sintering process same as Example 1 (HP sintering, HIP
Sintering and oxidation processes) and sharp processing process, by obtained sample for evaluation.
(2) evaluation method
For obtained sample, the evaluation of following items is carried out.
(2-1) relative density
The density of sample can for example be found out by Archimedes method.The relative density of sample can be close by the sample surveyed
It spends and (theoretical density of crystal phase for constituting sample is integrated with the product of volume ratio relative to the theoretical density under sample composition
Value) ratio indicate.
(2-2) constitutes phase, Spinel volume ratio, Spinel lattice constant, Spinel composition
The volume ratio of the crystal phase (constituting phase), the Spinel constituted that constitute sample and the lattice constant of Spinel can
To be found out by X ray diffracting spectrum.Spread out about the X-ray for using XRD device (D8ADVANCE of Bruker AXS manufacture) to obtain
Map is penetrated, the volume ratio and lattice of Spinel are calculated using Rietveld analysis software (Bruker AXS TOPAS)
Constant.In addition, finding out forming for Spinel: Mg by lattice constantxAl2-2xO3-2xX.
(2-3) average grain diameter, D90/D10
The partial size for constituting the crystal grain of sample can carry out image analysis by the crystal grain in the mirror ultrafinish face to sample to ask
Out.That is, the partial size of crystal grain uses the Heywood conversion diameter to be converted with circle to the area of the crystal grain in mirror ultrafinish face.About
Average grain diameter finds out the partial size of 200 crystal grain, uses 50% value (D50) of particle diameter distribution (number benchmark).D10, D90 are same
Sample uses the value of 10% value of particle diameter distribution, 90%.
(2-4) whiteness
The whiteness of sample uses the L* of CIE 1976 (L*, a*, b*).The value of whiteness indicates to get over closer to 100
Close to white.Using colour difference meter (Japan electricity decorations industry manufacture ZE6000), thickness 2mm is measured by bounce technique (JIS Z-8722)
Sample, use calculated value.
(2-5) light transmittance
About the light transmittance of sample, thickness is measured using spectrophotometer (V-670 of JASCO manufacture), using integrating sphere
The total light transmittance of the sample of 2mm uses the average transmittance of 400~800nm of wavelength.
(2-6) dielectric loss
The dielectric loss of sample can be found out by waveguide tube method.About quality factor Q value, sample is set to waveguide
In, it is measured using Network Analyzer (Agilent Technologies 8720ES) with measuring frequency 10GHz.Herein, make
For the index of dielectric loss, product, that is, fQ value (GHz) of measurement frequency f (GHz) and Q value is used.The more big then dielectric damage of fQ value
It consumes smaller.
(2-7) intensity
The intensity of sample uses three-point bending strength (JIS R1601).
The detection of (2-8) film forming
Obtained sample is bonded with Cu backboard with In, is set to sputtering equipment as sputtering target (ULVAC manufactures CSL)
It is interior, the presence or absence of paradoxical discharge in observation sputtering.
(2-9) inevitable impurity
About the concentration for the inevitable impurity for including in sample, inductively coupled plasma body (ICP) analysis is carried out.
(3) evaluation result
Evaluation result is shown in table 1.
(3-1) Examples 1 to 3
In Examples 1 to 3, relative density is the high density of 99.6~99.8 mass %.In addition, about phase is constituted, point is brilliant
The volume ratio of stone phase is 100%, and the composition of Spinel reflects the MgO and Al of raw material2O3Molar ratio 50:50~30:
70, x=0.5~0.3 (Mg0.5~0.3Al1~1.4O2~2.4).It is thought that because promoting original by the heat treatment procedure before being granulated
The reaction at feed powder end.The average grain diameter (D50) of sintered body is 2.1~2.4 μm, and D90/D10 is 2.4~3.6.Whiteness be 66~
It 75, is white, light transmittance is 40~45%.In addition, fQ value is 74000~89000GHz, is low-loss, bending strength is
320~345MPa, the sufficient intensity of target structure is sputtered to be used as.Paradoxical discharge in sputtering is few, is able to carry out good film forming.
(3-2) embodiment 4~7
In embodiment 4~7, relative density is the high density of 99.5~100 mass %.In addition, about phase, spinelle is constituted
The volume ratio of phase is low, is 16~88%, in addition observes Al in embodiment 4,52O3Phase is observed in embodiment 6,7
MgO phase.The group of Spinel becomes x=0.48~0.5 (Mg0.48~0.5Al1.04~1O2.04~2).The average grain diameter (D50) of sintered body
It is 5.2~6.5 μm, is greater than Examples 1 to 3.It is thought that grain growth has occurred because sintering temperature is high.D90/D10 is
2.2~3.2.Whiteness is 77~82, is white, and light transmittance is 27~36%, is lower than Examples 1 to 3.FQ value is 88000
It~107000GHz, is low-loss, bending strength is 340~385MPa, is as the sputtering sufficient intensity of target structure.In sputtering
Paradoxical discharge it is few, be able to carry out good film forming.
(3-3) embodiment 8
In embodiment 8, relative density is the high density of 99.8 mass %, and the volume ratio of Spinel is 100%, point is brilliant
The group of stone phase becomes x=0.5 (Mg0.5AlO2).Whiteness is 30, is black, light transmittance 1%.In addition, fQ value is
48000GHz。
(3-4) embodiment 9
In embodiment 9, relative density is 96.5 mass %, and Spinel volume ratio is 100%, the composition of Spinel
For x=0.5 (Mg0.5AlO2).The average grain diameter (D50) of sintered body is 1.6 μm, D90/D10 2.6.Whiteness is 98, is white
Color, light transmittance 1%, fQ value are 48000GHz.
(3-5) embodiment 10
In embodiment 10, relative density is the high density of 99.8 mass %, and the volume ratio of Spinel is 100%, point
The group of spar phase becomes x=0.5 (Mg0.5AlO2).The average grain diameter (D50) of sintered body is big, is 12 μm.
(3-6) inevitable impurity
The concentration of the inevitable impurity of Examples 1 to 10 is several ppm~Determination Limit value or less.
It should be noted that as described above, present embodiment is described in detail, but those skilled in the art can hold
It is readily understood, various deformation is carried out in the case where new item and effect of the invention can not departed from substantially.Therefore, this change
Shape example is integrally incorporated in the scope of the present invention.For example, in the description, difference identical with more broadly or meaning at least once
The term that term is recorded together can be replaced the different term in any part of specification.In addition, physical vapor deposition target
The compositions such as component, physical vapor deposition film and layer structure and operation are not limited to the case where illustrating in present embodiment, can carry out various
Deformation.
Claims (9)
1. a kind of physical vapor deposition target structure, which is characterized in that it includes Mg, M and O as main component, and wherein M is trivalent gold
Belong to element,
The Mg and M are scaled MgO and M respectively2O3Molar ratio after such oxide is 70:30~10:90.
2. a kind of physical vapor deposition target structure, which is characterized in that it includes Mg, M and O as main component, and wherein M is trivalent gold
Belong to element,
Physical vapor deposition target structure includes the crystal phase with spinel structure.
3. physical vapor deposition target structure as claimed in claim 1 or 2, which is characterized in that the M is selected from being made of Al and Ga
Group in a kind or 2 kinds.
4. physical vapor deposition target structure according to any one of claims 1 to 3, which is characterized in that when making with a thickness of 2mm
Light transmittance is 60% or less.
5. physical vapor deposition target structure as described in any one of claims 1 to 4, which is characterized in that the dielectric damage under 10GHz
Consumption is calculated as 45000GHz or more with fQ value.
6. such as physical vapor deposition target structure according to any one of claims 1 to 5, which is characterized in that whiteness is 30 or more.
7. a kind of sputtering target structure, which is characterized in that it is by physical vapor deposition according to any one of claims 1 to 6 target structure
Part is constituted.
8. a kind of manufacturing method of physical vapor deposition film, which is characterized in that it uses object described in any one of claim 1~6
Reason vapor deposition target structure physical vapor deposition in substrate goes out physical vapor deposition film.
9. the manufacturing method of a kind of layer of structure, which is characterized in that it is steamed using physics described in any one of claim 1~6
Plating target structure physical vapor deposition in substrate goes out physical vapor deposition film,
Ferromagnetic layer is formed on the physical vapor deposition film,
The substrate is ferromagnetic layer, and the physical vapor deposition film is tunnel barrier layer.
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| JP2016-229214 | 2016-11-25 | ||
| JP2016229214 | 2016-11-25 | ||
| PCT/JP2017/041030 WO2018096992A1 (en) | 2016-11-25 | 2017-11-15 | Physical vapor-deposition target member and sputtering target member, and physical vapor-deposition film and layer structure manufacturing method |
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| CN109996903A true CN109996903A (en) | 2019-07-09 |
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| JP (1) | JPWO2018096992A1 (en) |
| KR (1) | KR20190085948A (en) |
| CN (1) | CN109996903A (en) |
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| WO2019187324A1 (en) * | 2018-03-30 | 2019-10-03 | Ｊｘ金属株式会社 | Mgal2o4 sintered body, sputtering target using sintered body, and method for producing mgal2o4 sintered body |
| JP6832437B2 (en) * | 2018-09-13 | 2021-02-24 | Ｊｘ金属株式会社 | MgO sintered body sputtering target |
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| JPS5928936B2 (en) | 1978-12-23 | 1984-07-17 | オムロン株式会社 | Photoelectric switch |
| WO2010119928A1 (en) | 2009-04-16 | 2010-10-21 | 独立行政法人物質・材料研究機構 | Ferromagnetic tunnel junction structure, and magnetoresistive effect element and spintronics device each comprising same |
| JP2011202268A (en) * | 2010-03-04 | 2011-10-13 | Mitsubishi Materials Corp | Vapor deposition material for forming thin film, thin film sheet having the thin film and laminated sheet |
| WO2012056808A1 (en) * | 2010-10-25 | 2012-05-03 | 日本碍子株式会社 | Ceramic material, member for semiconductor manufacturing device, sputtering target member, and manufacturing method for ceramic material |
| WO2012173108A1 (en) * | 2011-06-15 | 2012-12-20 | 住友電気工業株式会社 | Electrically conductive oxide and method for producing same, and oxide semiconductor film |
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| DE112017005990T5 (en) | 2019-08-08 |
| KR20190085948A (en) | 2019-07-19 |
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