CN104818459B - Sputtering target and its manufacturing method - Google Patents
Sputtering target and its manufacturing method Download PDFInfo
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- CN104818459B CN104818459B CN201510056784.4A CN201510056784A CN104818459B CN 104818459 B CN104818459 B CN 104818459B CN 201510056784 A CN201510056784 A CN 201510056784A CN 104818459 B CN104818459 B CN 104818459B
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- main body
- target
- bushing pipe
- liner plate
- indium
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 229910052738 indium Inorganic materials 0.000 claims abstract description 69
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 23
- 239000010936 titanium Substances 0.000 claims abstract description 22
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004411 aluminium Substances 0.000 claims abstract description 17
- 239000010935 stainless steel Substances 0.000 claims abstract description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000005266 casting Methods 0.000 claims description 25
- 230000001590 oxidative Effects 0.000 claims description 15
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- 229910052733 gallium Inorganic materials 0.000 claims description 9
- 230000003746 surface roughness Effects 0.000 claims description 8
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 230000002159 abnormal effect Effects 0.000 abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 23
- 238000004544 sputter deposition Methods 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000012535 impurity Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000010408 film Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910000846 In alloy Inorganic materials 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- -1 indium tin Chemical compound 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005488 sandblasting Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N tin hydride Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000004873 anchoring Methods 0.000 description 1
- 238000003556 assay method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000002592 echocardiography Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium(0) Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002471 indium Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 230000003595 spectral Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000005478 sputtering type Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Abstract
It is fully firmly engaged by so that the target main body of indium is constituted with by stainless steel, titanium or aluminium bushing pipe or liner plate, abnormal generation when preventing from being sputtered.The double-layer structure for the target main body that the bushing pipe or liner plate that the sputtering target of the present invention is made of any material of stainless steel, titanium or aluminium are constituted with indium is constituted, and it is 95% or more to make the bonding rate between the bushing pipe measured by ultrasonic examination or liner plate and target main body.
Description
Technical field
The present invention relates to one kind in the surface of bushing pipe (backing tube) or liner plate (backing plate), engagement master
The sputtering target and its manufacturing method to be formed by the target main body that indium is constituted, in particular, proposing a kind of when by sputtering direction
When substrate forms film, it can prevent from extremely occurring caused by the decline due to the refrigerating function of the target main body based on bushing pipe etc.
Technology.
Background technology
It is being in progress in recent years in the exploitation of the increase with the demand to solar power generation, and solar cell,
In general, carrying out in order to improve configured according to priority on substrate back electrode layer, light absorbing layer, impedance buffer layer,
Transparency conducting layer and the various researchs of the light absorpting ability of the light absorbing layer of solar cell constituted.
Here, in the formation of light absorbing layer, sometimes used as the wave with extensive covering sunlight spectral region
Long and high light absorpting ability alloy and well known CIGS classes alloy, specifically, can by by Cu, In, Ga, Se etc. form should
CIGS classes alloy carries out the substrate of glass substrate etc. by sputtering as sputtering target.
When being used to form the sputtering of such light absorbing layer etc., the engagement target main body on the liner plate of writing board shape has been used
And the magnetron sputtering of the plate sputtering target formed is mainstream.But in cases in which the method is applied, due to because of magnet
It configures and causes the amount being sputtered in face different, so when being easiest to the place of sputtering until being splashed to target thickness just
End-of-life.Therefore, not used part is also very much, and service efficiency is lower.
For such case, in order to improve the utilization ratio on target surface, for example, as illustrated in Figure 1, using in circle
The cylinder type sputtering target 103 that target main body 102 is engaged on the outer circumference surface of the bushing pipe 101 of barrel shape is splashed in such cylinder type
It is sputtered under being pivoted shot at the target, which has had reached functionization.
In addition, above-mentioned plate and cylinder type any type of sputtering target, typically mainly passes through melt-casting method
Casting indium target main body and manufactured.For example, in patent document 1, it is proposed that " a kind of manufacturing method of sputtering target,
It is characterized in that, after by forming the film of indium, indium alloy, tin or tin alloy on liner plate, be perfused on the film indium,
Indium alloy, tin or tin alloy are cast, to be formed as one with liner plate ".
But in the case where the bushing pipe or liner plate engaged with indium target main body is made of copper, made by using indium tin
Bushing pipe or liner plate and target main body can be made mutual to be based on melting copper admittedly in indium tin for the solder for completing with the engagement of target main body
Such as it is engaged with 90% or more relatively high bonding rate.In addition, it is by following ultrasonic examinations to be somebody's turn to do " bonding rate "
Come what is measured.
On the other hand, the case where bushing pipe or liner plate are also made of in the metal material other than copper stainless steel or titanium, aluminium
Under, in particular, when the indium metal liquid that such as 200 DEG C or so are perfused into the casting space of mold for being internally provided with bushing pipe or liner plate
When casting target main body, indium cannot be fused to admittedly due to stainless steel at low temperature etc., wetability is very poor, and leads to bushing pipe or liner plate
It is engaged with low bonding rate with target main body.
Moreover, such low bonding rate of sputtering target is when being sputtered, such as can exist based on flowing to bushing pipe or liner plate
Inner passage liquid circulation and the refrigerating function that causes target main body declines, the generation for thus causing sputtering abnormal it is hidden
Suffer from.
Here, in patent document 2, in order to improve the zygosity between bushing pipe and target main body, it is " Ni-based to record use
The content of adhesive layer ".More specifically, describing " makes indium melt, and is cast to from crucible around support tube at 190 DEG C
Pre-warmed steel mold in, at this point, the foot of steel mold is connect by sealing element with support tube...., in order to improve indium
And the combination of support tube, support tube have indium solder in advance, and have Ni-based adhesive layer ".
Existing technical literature
Patent document
Patent document 1:Japanese Patent Publication 63-44820 bulletins
Patent document 2:Japanese Unexamined Patent Publication 2012-172265 bulletins
However, before the formation of target main body, it is provided with as described in patent document 2 on the surface of bushing pipe or liner plate
In the case of the basal layer be made of nickel, admittedly the nickel being fused in indium largely remains in as impurity in target main body, existing makes the sun
The worry that energy battery performance deteriorates.In this way, in the case where the surface of bushing pipe or liner plate is provided with nickel basal layer, what is produced splashes
It shoots at the target as including three layers or more of structure of bushing pipe or liner plate, nickel basal layer and target main body.
In addition, before target cast, only on the surface of bushing pipe etc., only form as described in patent document 1 that
In the case of the basal layer of the indium film of sample, due to when casting target main body, by being so that bushing pipe is heated to indium fusing point or more
Purpose and the preheating carried out, to make the surface oxidation of bushing pipe for being provided with indium film etc., so bushing pipe etc. to indium metal
The wetability of liquid reduces, as a result, the bonding rate with target main body such as bushing pipe cannot be effectively improved.Specifically, preheating
When bushing pipe temperature be 170~180 DEG C.
Invention content
The present invention is this as project possessed by the prior art to solve the problems, such as, it is intended that providing a kind of sputtering target
And its manufacturing method, wherein sputtering target in a manner of not mixing a large amount of impurity in the target main body of indium, by make target main body with
The bushing pipe or liner plate being made of stainless steel or titanium, aluminium fully firmly engage, abnormal generation when can prevent from being sputtered.
What the bushing pipe or liner plate that the sputtering target of the present invention is made of any one of stainless steel, titanium or aluminium material were constituted with indium
The double-layer structure of target main body is constituted, and makes the bushing pipe measured by ultrasonic examination or the liner plate be with the intersubjective bonding rate of target
95% or more.
The surface roughness of the bushing pipe or liner plate and the engagement surface of target main body of the sputtering target of the present invention, that is, JIS
The arithmetic average roughness Ra of B0601 defineds is preferably 4.0 μm or more.
In addition, herein, target main body can also also contain at least one selected from Ni, Fe, Cr, Ti, Al, Si, and each
Content is 10wtppm hereinafter, alternatively, it is also possible to also contain at least one selected from Cu, Ga, and each content is
10000wtppm or less.
In addition, the manufacturing method of the sputtering target of the present invention, by casting, the target main body that will be made of indium is basic via indium
Layer, is joined on the surface of the bushing pipe or liner plate that are made of any one of stainless steel, titanium or aluminium material, to manufacture sputtering target,
At this point, indium basal layer is formed on the surface of bushing pipe or liner plate, it is right under non-oxidizing atmosphere later before the casting for carrying out target main body
The bushing pipe or liner plate for being attached with indium basal layer are preheated.
Described in the manufacturing method carries out in the state of being configured with bushing pipe or liner plate preferably in the casting mold of target main body
Preheating, and be more than during preheating, but also tieed up always during the casting for being pre-heated to target main body from this terminates
Hold non-oxidizing atmosphere.
In addition in the method, target main body can also also contain selected from least one of Ni, Fe, Cr, Ti, Al, Si, and
Each content is 10wtppm or less.
Sputtering target according to the present invention, due to by making any material by stainless steel, titanium or aluminium constitute bushing pipe or
Liner plate is 95% or more with the bonding rate of indium target main body, thus when being sputtered with its implementation, by being fully close to target main body
Bushing pipe or liner plate, the cooling of target main body can be effectively performed, therefore can help to realize the good sputtering that is not abnormal.
The manufacturing method of sputtering target according to the present invention, due to being made of any material of stainless steel, titanium or aluminium
The surface of bushing pipe or liner plate forms indium basal layer, before the casting of target main body, by being carried out to this under non-oxidizing atmosphere
The preheating of bushing pipe or liner plate, to inhibit bushing pipe or liner plate indium basal layer oxidation, so can greatly improve therewith
Bonding rate between the target main body of the indium cast afterwards.
Description of the drawings
Fig. 1 is the summary stereogram for an example for indicating cylinder type sputtering target.
Specific implementation mode
Hereinafter, embodiments of the present invention are described in detail.
Sputtering target involved by an embodiment of the invention has:By any material structure of stainless steel, titanium or aluminium
At, be, for example, cylindric bushing pipe or discoid liner plate;And it is joined to the outer circumference surface or discoid of cylindric bushing pipe
On the surface of liner plate and using indium as the target main body of main material.
In addition, herein, being made as illustrated in Figure 1 by being that cylindric bushing pipe 101 and target main body 102 is constituted
When cylinder type sputtering target 103, it can provide and make above-mentioned rotary-type sputtering target, can be improved compared with plate sputtering target using effect
Rate.
The sputtering target is bushing pipe or liner plate and target main body, the mutually different double-layer structure of principal component, in these bushing pipes or
There is no the layers being made of the other materials of nickel etc. between liner plate and target main body.
Here, bushing pipe or liner plate, especially constitute cylinder type sputtering target bushing pipe, as present embodiment sputtering target that
There are many sample, the case where being made of stainless steel, titanium or aluminium, therefore, using be difficult to be fused to admittedly to form target main body indium in stainless steel,
The property of titanium or aluminium can reduce impurity present in target main body.
In this case, when forming target main body, when by being perfused into the mold configured with above-mentioned bushing pipe or liner plate
200 DEG C or so of molten indium and when being allowed to hardening by cooling and being cast, will be as described above, the gold such as stainless steel or titanium, aluminium
Belong to material hardly to melt admittedly with indium in a low temperature of 200 DEG C or so, lack due to the wetability between the metal material and indium,
Indium fully cannot be engaged firmly with the bushing pipe or liner plate being configured in mold, the bonding rate between bushing pipe or liner plate and target main body
It is lower.
Such bushing pipe or liner plate and target main body are being supplied to the sputtering target of low bonding rate engagement for substrate
In the case of the sputtering that film is formed, even if for cooled target main body, supplied to the channel for the inside for being set to bushing pipe or liner plate
The cooling of target main body can not be effectively performed due to the reason of bonding rate low with target main body in cooling water, so that sputtering
Exception.
In order to cope with the problem, in the present invention, above-mentioned bushing pipe or liner plate are set as leading to the intersubjective bonding rate of target
Cross ultrasonic examination and measure 95% or more of value.As a result, in sputtering, since bushing pipe or liner plate are effectively cooled down and are filled with it
Divide the target main body being firmly bonded, therefore can prevent due to the insufficient abnormal generation of the cooling of target main body.
Here, when measuring the bonding rate between bushing pipe or liner plate and target main body, using ultrasonic flaw-detecting machine, in plane
In the case of target along longitudinal direction and laterally, in addition in the case of cylinder type target along long dimension direction (axis direction) and circumferencial direction,
Entire interface is scanned according to the spacing of regulation respectively, and in the face for finding out the defective part as the part not being bonded fully
After product Ad, according to the area At of the area Ad of the defective part and interface entirety, energy will be by formula:Pa=100 × (At-Ad)/At
The value Pa (%) acquired is set as bonding rate.
In addition, herein, as the impurity for the target main body being mainly made of indium, Ni, Fe, Cr, Ti, Al, Si, target can be enumerated
As long as its content of each of these elements contains in 10wtppm or less in main body.It is more due to containing in target main body
In the case of above-mentioned impurity, the conversion ratio for the solar cell made using sputtering target is low, therefore preferably impurity is less.Cause
This, the impurity contained by target main body more preferably add up to 100wtppm hereinafter, particularly preferably 80wtppm hereinafter, further, more preferably
50wtppm or less.However, due to the inscape that Cu, Ga are CIGS solar cells, so while as impurity by except,
But in embodiments of the present invention, at least one selected from these Cu, Ga can be contained 10000wtppm or less respectively.
When manufacturing above-described sputtering target, for example, first, before the formation of target main body, by stainless steel, titanium or aluminium
The outer surface of the cylindric bushing pipe of composition forms indium basal layer by plating or spraying plating etc..In addition, from further increasing and indium
Bonding rate from the viewpoint of, preferably before forming this indium basal layer, sandblasting etc. is imposed to the outer surface of bushing pipe, keeps this outer
The surface roughness Ra on surface reaches 4.0 μm or more.
Secondly, the bushing pipe for being attached with indium basal layer is configured in such a way that its outer surface is exposed in cylindric casting space
In the specified position in mold, and make in mold full of the indifferent gas as nitrogen or argon or helium or other rare gas elements
On the basis of the non-oxidizing atmosphere of body, bushing pipe is implemented to preheat.As a result, by producing non-oxide ring when implementing to preheat
Border can inhibit the progress of the oxidation of the indium basal layer formed in the outer surface of bushing pipe.Here, " non-oxidizing atmosphere " refers to filling
Oxygen concentration in gas is in 0.5vol% states below.In addition, herein, liner temperature when preheating can be 170~
180℃。
Later, by 200 DEG C or so of indium metal liquid of perfusion molten condition in the casting space to mold, such as pass through
Make molten metal hardening by cooling in casting space by the cooling equipment etc. being configured at around mold, in the excircle of bushing pipe
Side casts target main body.
Here, do not aoxidized by the indium basal layer of bushing pipe outer surface, to target main body via indium basal layer firmly
It is joined on the outer surface of bushing pipe, for example, the sputtering target that their bonding rate is 95% or more can be manufactured.In addition, for being formed
The indium of target main body can use the raw material of 4N.In addition, due to the constitution element that Cu, Ga are CIGS, so can also contain respectively
10000wtppm or less.
In addition, herein, since indium basal layer is main body integrated with target in casting, so the sputtering target thus manufactured becomes
For any one of the stainless steel, titanium or the aluminium that form bushing pipe or liner plate material with target main body and the bilayer of the indium based on indium basal layer
Structure.
In such manufacturing method, as described above, by before casting target main body, bushing pipe or liner plate and target
On the engagement surface that main body engages, formed using indium as the basal layer of principal component, so as to improve indium to bushing pipe or liner plate table
The wetability in face, and improve the engaging force between bushing pipe or liner plate and target main body.On the surface of bushing pipe or liner plate, such as can be with
Indium basal layer is arranged in the film-form that thickness is 1 μm~100 μm or so.
And in this case, indium is similarly by the principal component of basal layer and target main body, thus will not be just like patent
The nickel of gene basis layer caused by method described in document 2 sputters the hidden of abnormal generation caused by being largely mixed into target main body
Suffer from.
In addition, the engagement surface engaged with target main body in the surface of bushing pipe or liner plate, sandblasting is based on by carrying out in advance
Deng surface treatment, preferably it is coarse turn to arithmetic mean roughness Ra be 4.0 μm or more.It as a result, can be based on bushing pipe or liner plate
Anchoring effect at the bumps on the surface being roughened, greatly improves the bond strength between bushing pipe or liner plate and target main body.From
From the point of view of this viewpoint, the roughness Ra of the engagement surface of bushing pipe or liner plate is more preferably 5 μm or more, further preferably 6 μm with
On, especially more preferably 7 μm or more.In addition, the no special appropriate upper limit value of the roughness Ra of engagement surface, but have 20
μm or so be sufficient.
Herein, it from the viewpoint of the oxidation for more efficiently inhibiting indium basal layer, is preferably pre-heated to from above-mentioned
During the casting of target main body terminates, the above-mentioned non-oxidizing atmosphere around bushing pipe is maintained always.In addition in this case, can aspirate
Nitrogen or inert gas simultaneously make mold inner pressure relief, while indium metal liquid is perfused to casting space.
In addition it is illustrated as described previously for the manufacturing method of cylinder type sputtering target, however for plane
Sputtering target substantially clearly can also be manufactured according to same sequence.
The sputtering target so manufactured can be suitably used in the manufacture of the light absorbing layer of CIGS based thin film solar cells.
Embodiment
Then, due to having manufactured experimently the sputtering target of the present invention, and its characteristic is had rated, therefore illustrated as follows.
The target of embodiment 1 is manufactured by following method.Surface roughness Ra is being set as to 4.0 μm of SUS304 systems
Bushing pipe (outer diameter φ 133mm, internal diameter φ 125mm, length 640mm) outer surface be previously formed indium basal layer after, by the bushing pipe
It is configured in the mold of SUS304, is preheated under the non-oxidizing atmosphere based on nitrogen, later, continued to non-oxide
Environment is constant, in the indium of purity 4N having been melted and the indium metal perfusion to the cylindric casting space of the mold that is formed,
Make its hardening by cooling there, manufactures the sputtering target that target main body of sening as an envoy to is engaged with bushing pipe.In addition, target outer diameter is φ in casting
161mm is cut to φ 157mm by lathe, and final shape (outer diameter φ 157mm, internal diameter φ 133mm, length is made
600mm)。
The target of embodiment 2, other than being preheated under the non-oxidizing atmosphere full of argon, the target with embodiment 1
It manufactures in the same way.The target of embodiment 3 other than making the surface roughness Ra of bushing pipe be 8 μm, with the target of embodiment 1 with
Same method manufacture.The target of embodiment 4 other than making the surface roughness Ra of bushing pipe be 10 μm, with the target of embodiment 1 with
Same method manufacture.The target of embodiment 5 is other than making the material of bushing pipe be titanium, in the same way with the target of embodiment 1
Manufacture.The target of embodiment 6 manufactures other than making the material of bushing pipe be aluminium with the target of embodiment 1 in the same way.
The target of embodiment 7, on the liner plate of aluminum, after having implemented based process same as Example 1, setting is internal
The frame of size 130mm × 510mm is put into the closed-loop operation case after having replaced nitrogen, after being heated, in identical closed behaviour
Make the indium metal liquid that input heating has been melted in case, is cooled down, later the work in-process heart, target size machining to 127mm
× 508mm × 5mmt, makes target.Embodiment 8,9,10 is added to Cu, Ga to indium in addition to having used according to concentration recorded in table 1
In raw material except, manufactured in the same way with the target of embodiment 1.
On the other hand, the target of comparative example 1, other than having used nickel basal layer instead of indium basal layer, the target with embodiment 1
It manufactures in the same way.Comparative example 2 is not in addition to being under non-oxidizing atmosphere but is preheated in an atmosphere and casts it
Outside, it is manufactured in the same way with the target of embodiment 1.Comparative example 3 in addition to being preheated and being cast under atmospheric environment, and
It is to be manufactured in the same way with the target of embodiment 1 except 3 μm to make the roughness Ra of liner surface.Comparative example 4 is in addition in air
It is preheated and is cast under environment, and the Ra of liner surface is made to be except 1 μm, in the same way with the target of embodiment 1
Manufacture.Comparative example 5 in nitrogen in addition to being preheated, later in by mold to directly starting to cast it after atmosphere opening
Outside, it is made in the same way with the target of embodiment 1.
Ultrasonic wave spy is carried out using engineering company of Hitachi ultrasonic flaw-detecting machine FSLINE for each target so made
Wound, the assay method based on the foregoing description measure the bonding rate Pa between bushing pipe or liner plate and target main body.In further detail,
Cylindric indium target is arranged in flaw detector sink, after being scanned with 1mm spacing in long dimension direction, in a circumferential direction
Target is set to rotate in a manner of becoming 1mm spacing, the cycle that repetition is scanned in long dimension direction again measures complete cycle.
The detector that 10MHz is used in measurement, is measured with gain decibel value 30dB.In addition, in general, in ultrasonic examination
In, due to that can be changed according to the obtained echo of device, detector, determination of the environment used, make has zero defect in advance
Specific standard sample, is measured.Specifically, outputing the φ from the liner inner surface side of cylindric indium target until reaching target
The hole of 1mm is chosen to be defective part (part not being bonded fully), is detected a flaw according to the condition that can be differentiated.Bonding rate Pa
According to above-mentioned formula, pass through bond area (the area At of interface entirety is acquired by subtracting the area Ad of defective part) divided by interface
Whole area At, calculates multiplied by with 100.
In addition, using above-mentioned each target, sputtered with following sputtering conditions, has investigated the generation of breakdown.Here, it uses
The average value (secondary/h) of 2h after pre-sputtering.
Sputter gas:Ar
Sputtering pressure:0.5Pa
Sputter gas flow:50SCCM
Sputter temperature:R.T. (no heating)
Access Sputtering power density:1.3W/cm2
Pre-sputtering:1h under these conditions
The results are shown in Table 1 for these.
【Table 1】
From the result of table 1 it will be apparent that, when the embodiment 1,2 that will be preheated and cast under non-oxidizing atmosphere with than
When being compared compared with example 2, the bonding rate that the embodiment for preheating and casting has been carried out under non-oxidizing atmosphere is higher.In addition, root
According to the comparison of embodiment 1,3,4 it is found that the surface roughness of bushing pipe is rougher can be bonded more preferably.In comparative example 1 known to although
It is middle to have used layer based on nickel instead of indium basal layer, but nickel has been diffused into target.When comparative example 2 and 5 is compared,
Known to when being preheated by being more than, when casting is also to be carried out under non-oxidizing atmosphere, and bonding rate can be got higher.In addition, according to reality
Apply example 8,9,10, it is known that can obtain same bonding rate if even if containing Cu, Ga as CIGS inscapes.
According to the above situation, it is known that by being preheated under non-oxidizing atmosphere, the oxidation of indium basal layer can be inhibited,
And it greatly improves and the bonding rate of the indium target main body cast later.
The explanation of reference numeral
101 bushing pipes
102 target main bodys
103 cylinder type sputtering targets
Claims (6)
1. a kind of manufacturing method of sputtering target, wherein
By casting, the target main body that will be made of indium is joined to via indium basal layer by any one of stainless steel, titanium or aluminium material
Texture at bushing pipe or liner plate surface on, to manufacture sputtering target,
Indium basal layer is formed on the surface of bushing pipe or liner plate, later, before the casting for implementing target main body, under non-oxidizing atmosphere
The bushing pipe or liner plate that are attached with indium basal layer are preheated,
The preheating is carried out in the state of being configured with bushing pipe or liner plate in the casting mold of target main body, and from the preheating
Start to the casting of target main body to terminate, maintain non-oxidizing atmosphere always,
It is surface-treated in advance on the surface of bushing pipe or liner plate, makes the engagement between target main body of the bushing pipe or liner plate
The surface roughness Ra on surface is 4.0 μm or more.
2. the manufacturing method of sputtering target according to claim 1, wherein
The target main body also contains at least one selected from Ni, Fe, Cr, Ti, Al, Si, and each content be 10wtppm with
Under.
3. a kind of sputtering target is the sputtering target manufactured by the manufacturing method of sputtering target described in claim 1,
Pair for the target main body that the bushing pipe or liner plate that the sputtering target is made of any material of stainless steel, titanium or aluminium are constituted with indium
Layer structure is constituted, make the bonding rate between the bushing pipe measured by ultrasonic examination or liner plate and target main body for 95% with
On, it is 4.0 μm or more to make the surface roughness Ra of the engagement surface between target main body of the bushing pipe or liner plate.
4. sputtering target according to claim 3, wherein the target main body also contains selected from Ni, Fe, Cr, Ti, Al, Si
At least one, and each content is 10wtppm or less.
5. sputtering target according to claim 3, wherein the target main body also contains at least one selected from Cu, Ga, and
Each content is 10000wtppm or less.
6. sputtering target according to claim 4, wherein the target main body also contains at least one selected from Cu, Ga, and
Each content is 10000wtppm or less.
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JP2014019511A JP6305083B2 (en) | 2014-02-04 | 2014-02-04 | Sputtering target and manufacturing method thereof |
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JPH11236664A (en) * | 1998-02-24 | 1999-08-31 | Mitsui Chem Inc | Backing plate of target for sputtering |
CN102644053A (en) * | 2011-02-22 | 2012-08-22 | 贺利氏材料工艺有限及两合公司 | Tube-shaped sputtering target |
CN103124805A (en) * | 2011-06-08 | 2013-05-29 | 株式会社半导体能源研究所 | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
JP2013253298A (en) * | 2012-06-08 | 2013-12-19 | Ulvac Japan Ltd | Method and apparatus for producing target unit |
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH11236664A (en) * | 1998-02-24 | 1999-08-31 | Mitsui Chem Inc | Backing plate of target for sputtering |
CN102644053A (en) * | 2011-02-22 | 2012-08-22 | 贺利氏材料工艺有限及两合公司 | Tube-shaped sputtering target |
CN103124805A (en) * | 2011-06-08 | 2013-05-29 | 株式会社半导体能源研究所 | Sputtering target, method for manufacturing sputtering target, and method for forming thin film |
JP2013253298A (en) * | 2012-06-08 | 2013-12-19 | Ulvac Japan Ltd | Method and apparatus for producing target unit |
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