CN106460160B - W-Ti sputtering targets - Google Patents
W-Ti sputtering targets Download PDFInfo
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- CN106460160B CN106460160B CN201580021546.8A CN201580021546A CN106460160B CN 106460160 B CN106460160 B CN 106460160B CN 201580021546 A CN201580021546 A CN 201580021546A CN 106460160 B CN106460160 B CN 106460160B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The W Ti sputtering targets of the present invention have following composition：The Fe in Ti and the range of 25 mass ppm or more and 100 mass ppm or less in range containing 5 mass % or more and 20 mass % or less, and surplus is made of W and inevitable impurity, many places in target surface measure Fe concentration, and the maximum value of the Fe concentration measured is set as Femax, the minimum value of Fe concentration is set as FeminIn the case of, meet (Femax‑Femin)/(Femax+FeminThis relational expression of)≤0.25.
Description
Technical field
The present invention relates between a kind of convex block and grounding electrode for example used when installing semiconductor element, as preventing
The diffusion preventing layer of mutual elements diffusion forms the W-Ti sputtering targets of W-Ti films.
This application claims based on October 8th, 2014 in the priority of the patent application 2014-207343 of Japanese publication,
And its content is applied at this.
Background technology
In the past, when semiconductor chip being installed to substrate, such as Au convex blocks or scolding tin are formed on Al electrodes or Cu electrodes
Convex block etc..
Here, for example being resulted in the case where Al electrodes and Au convex blocks are in direct contact because Al is spread each other with Au
The intermetallic compound of Al and Au may be such that resistance rising or adhesiveness declines.Also, such as in Cu electrodes and solder bump
In the case of being in direct contact, the intermetallic compound of Cu and Sn is resulted in because the Sn in Cu and scolding tin is spread each other, it may
Resistance rising or adhesiveness can be made to decline.
Thus, for example using W-Ti sputtering targets disclosed in patent document 1,2, as anti-between grounding electrode and convex block
Only the diffusion preventing layer of mutual elements diffusion forms W-Ti films.
In addition, the W-Ti sputtering targets described in patent document 1,2 are manufactured by powder sintering respectively.
Here, when forming W-Ti films as diffusion preventing layer between grounding electrode and convex block, in the entire of grounding electrode
Face forms the W-Ti films for forming convex block after W-Ti films, and not forming the region of convex block by etching removal.But due to erosion
It is very slow to carve speed, therefore there is a problem of that the production efficiency of the W-Ti films is poor.
Therefore, the W-Ti sputtering targets using micro addition Fe are disclosed in patent document 3, to make to be formed by W-Ti films
In contain Fe, and the technology of etching speed can be improved.
Patent document 1：No. 2606946 bulletins of Japanese Patent No.
Patent document 2：Japanese Unexamined Patent Publication 05-295531 bulletins
Patent document 3：No. 4747368 bulletins of Japanese Patent No.
However, as described above by the micro addition Fe in W-Ti films and its etching speed is improved, but in W-Ti
In the case that the Fe concentration of film generates deviation, etching speed localized variation in W-Ti films can be led to, so as to carry out
Uniform etching.
Therefore, expect that a kind of deviation that can form Fe concentration is smaller and the W-Ti sputterings of the uniform W-Ti films of etching speed
Target.
Invention content
The present invention has been made in view of the above-described circumstances, and an object thereof is to provide a kind of deviation that can form Fe concentration compared with
The W-Ti sputtering targets of the uniform W-Ti films of small and etching speed.
In order to solve the above problems, the W-Ti sputtering targets as the mode of the present invention are characterized in that, have such as the following group
At：Ti and 25 mass ppm or more and 100 mass ppm in range containing 5 mass % or more and 20 mass % or less is below
Fe in range, and surplus is made of W and inevitable impurity, many places in target surface measure Fe concentration, and will be measured
The maximum value of Fe concentration be set as Femax, the minimum value of Fe concentration is set as FeminIn the case of, meet following relational expression：
(Femax-Femin)/(Femax+Femin)≤0.25。
In the W-Ti sputtering targets of the thus configured present invention, due to containing 25 mass ppm or more and 100 mass ppm or less
In the range of Fe, therefore the etching speed for being formed by W-Ti films can be improved.
Moreover, many places in target surface measure Fe concentration, the maximum value (Fe of the Fe concentration measuredmax) and Fe concentration
Minimum value (Femin) meet above-mentioned relation formula, therefore the deviation of the Fe concentration in target surface is inhibited.It is dense therefore, it is possible to form Fe
The deviation of degree is smaller and the uniform W-Ti films of etching speed.
As described above, according to smaller the present invention can provide a kind of deviation that can form Fe concentration and etching speed is uniform
The W-Ti sputtering targets of W-Ti films.
Description of the drawings
Fig. 1 is the flow chart for the manufacturing method for indicating the W-Ti sputtering targets involved by one embodiment of the present invention.
Fig. 2 is the definition graph of the Fe concentration in the target surface for indicate the rounded W-Ti sputtering targets of target surface to locate.
Fig. 3 is the definition graph of the Fe concentration in the target surface for indicate the rectangular W-Ti sputtering targets of target surface to locate.
Fig. 4 is the definition graph for illustrating to measure the position for the etching speed for being formed in the W-Ti films on substrate in embodiment.
Specific implementation mode
Hereinafter, refer to the attached drawing illustrates the W-Ti sputtering targets as embodiments of the present invention.
W-Ti sputtering targets involved by present embodiment pass through for example in order to engage liquid crystal drive IC to COF bands
It sputters between the Au convex blocks being formed on liquid crystal drive IC and Al weld pads portion (grounding electrode) and forms W- as diffusion preventing layer
It is used when Ti films.
W-Ti sputtering targets involved by present embodiment have following composition：Containing 5 mass % or more and 20 mass % with
Under range in Ti and the Fe in the range of 25 mass ppm or more and 100 mass ppm or less, and surplus is by W and inevitable
Impurity constitute.
Moreover, many places in target surface measure Fe concentration, and the maximum value of the Fe concentration measured is set as Femax, by Fe
The minimum value of concentration is set as FeminIn the case of, meet following relationship：
(Femax-Femin)/(Femax+Femin)≤0.25
Hereinafter, the reasons why being formed to predetermined component as above illustrates.
＜ Ti：5 mass % or more and 20 mass % or less ＞
In the case that Ti contents in W-Ti sputtering targets are less than 5 mass %, it may make to be formed by W-Ti films and ground connection
The adhesiveness of electrode declines.On the other hand, in the case that the Ti contents in W-Ti sputtering targets are more than 20 mass %, institute can be caused
The resistance of the W-Ti films of formation rises, and the element of composition convex block possibly can not be substantially prevented from by being formed by W-Ti films
(being Au in present embodiment) and element (being Al in present embodiment) mutual diffusion for constituting grounding electrode.
Therefore, in the present embodiment, by the content of the Ti in W-Ti sputtering targets regulation more than 5 mass % and 20 matter
In the range for measuring % or less.In addition, the lower limit of the content of Ti is preferably set to 7 mass % or more, be more preferably set as 9 mass % with
On.Also, the upper limit of the content of Ti is preferably set to 15 mass % hereinafter, being more preferably set as 13 mass % or less.
＜ Fe：25 mass ppm or more and 100 mass ppm or less ＞
In the case that the content of Fe in W-Ti sputtering targets is less than 25 mass ppm, it may be unable to fully improve being formed
W-Ti films etching speed.It on the other hand, can in the case that the content of the Fe in W-Ti sputtering targets is more than 100 mass ppm
The element (being Au in present embodiment) that composition convex block can not be substantially prevented from by being formed by W-Ti films is electric with composition ground connection
The mutual diffusion of the element (being Al in present embodiment) of pole.
Therefore, in present embodiment, the content of the Fe in W-Ti sputtering targets is provided more than 25 mass ppm and 100 matter
In the range for measuring ppm or less.
In addition, the lower limit of the content of Fe is preferably set to 30 mass ppm or more, it is further preferably set as 35 mass ppm or more.
Also, the upper limit of the content of Fe is preferably set to 75 mass ppm hereinafter, being further preferably set as 50 mass ppm or less.
＜ (Femax-Femin)/(Femax+FeminThe ＞ of)≤0.25
In the case where forming W-Ti films using the W-Ti sputtering targets of present embodiment, each atom is from W-Ti sputtering targets
Entire target surface sputters out and forms film.
Here, maximum value (the Fe of Fe concentration that many places in target surface measure Fe concentration and measuredmax) and Fe concentration
Minimum value (Femin) meet above-mentioned relation formula in the case of, the deviation of Fe concentration becomes smaller in target surface.Therefore, it is splashed using the W-Ti
The deviation of the Fe concentration of W-Ti films shot at the target and formed also becomes smaller, and etching speed becomes uniform.
In addition, (Femax-Femin)/(Femax+Femin) 0.2 is preferably set to hereinafter, being more preferably set as 0.15 or less.In addition
(Femax-Femin)/(Femax+Femin) more lower better, but extremely reduce (Femax-Femin)/(Femax+Femin) cost can be caused
Increase.Therefore, (Femax-Femin)/(Femax+Femin) can be 0.005 or more.
Here, in present embodiment, in the case where the target surface of W-Ti sputtering targets is rounded, as shown in Fig. 2, in round
The heart (1) and outer peripheral portion (2), (3), (4), (5) this 5 points by round center and on 2 mutually orthogonal straight lines measure
Fe concentration, and find out the maximum value (Fe of above-mentioned Fe concentrationmax) with the minimum value (Fe of Fe concentrationmin).Outer peripheral portion (2), (3),
(4), (5) for example can be from the position that the periphery of target is about 10mm to central side.
Also, in the case where the target surface of W-Ti sputtering targets is rectangular, as shown in figure 3, in the orthogonal intersection point of diagonal line (1)
And the corner (2) on each diagonal line, (3), (4), (5) this 5 points measurement Fe concentration, and find out the maximum value of above-mentioned Fe concentration
(Femax) with the minimum value (Fe of Fe concentrationmin).Corner (2), (3), (4), (5) for example can be
The position of 10mm.
The measurement site number of Fe concentration can be 5 points or more and 20 points or less.In this case, measurement site can be with
It is the point that pinwheel point, the intersection point from straight line and target outer peripheral edge by its center are about 10mm to central side.
Then, with reference to the flow chart of figure 1 to manufacture present embodiment involved by W-Ti sputtering targets an embodiment into
Row explanation.
As shown in Figure 1, the manufacturing method of the W-Ti sputtering targets involved by present embodiment has：Co-grinding process S01,
Co-grinding carries out the raw material powder of dispensing with defined dosage；Sintering circuit S02 heats the raw material powder of co-grinding and burns
Knot；And manufacturing procedure S03, obtained sintered body is processed.
First, as raw material powder, prepare Ti powder, W powder and Fe powder.Here, as Ti powder, it is preferable to use purity
It it is 1 μm or more and 40 μm of powder below for 99.999 mass % or more, average grain diameter.Also, as W powder, it is preferable to use
Purity is 99.999 mass % or more, average grain diameter is 0.5 μm or more and 20 μm of powder below.In addition, as Fe powder, it is excellent
It is 99.999 mass % or more to select using purity, average grain diameter is 75 μm or more and 150 μm of powder below.
＜ co-grinding process S01 ＞
These raw material powder are weighed, them is made to become containing in 5 mass % or more and the 20 following ranges of mass %
Fe in Ti and 25 mass ppm or more and the 100 following ranges of mass ppm, and the group that surplus is made of W and inevitable impurity
At, and the co-grinding raw material powder.In present embodiment, the raw material powder weighed is mixed with ball mill, followed by hard
Alloy ball carries out co-grinding by grater device.
It is 10 μm or less to be ground into average grain diameter by co-grinding process S01, Fe powder.
＜ sintering circuit S02 ＞
Then, to the raw material powder (mixed powder) of co-grinding as above in vacuum or inert gas atmosphere or in reducing atmosphere
It is sintered.In sintering circuit S02, it is that 10 μm of Fe powder below are uniformly spread in W to be ground into average grain diameter.
Here, the sintering temperature in sintering circuit is preferably according to the fusing point Tm settings of W-Ti alloys to be manufactured.
In sintering circuit S02, as sintering method, normal pressure-sintered, hot pressing, hip moulding can be applied.
In present embodiment, to graphite molding jig filling raw material powder (mixed powder), by by pressure be set as 10MPa or more and
60MPa or less, the vacuum hotpressing that temperature is set as to 1000 DEG C or more and 1500 DEG C are sintered.
＜ manufacturing procedure S03 ＞
Machining or grinding are implemented to the sintered body obtained in sintering circuit S02, to be processed into regulation shape
The sputtering target of shape.
By process as above, the W-Ti sputtering targets as present embodiment are produced.About the W-Ti sputtering targets, In is made
For scolding tin, it is bonded on Cu or SUS (stainless steel) or the backing plate being made of other metals (such as Mo) and uses.
According to the W-Ti sputtering targets as constructed as above as present embodiment, due to containing 25 mass ppm or more and 100 matter
The Fe in ppm or less ranges is measured, therefore the etching speed for being formed by W-Ti films can be improved.
Moreover, many places in target surface measure Fe concentration, and the maximum value (Fe of the Fe concentration measuredmax) and Fe concentration
Minimum value (Femin) meet (Femax-Femin)/(Femax+FeminThis relational expression of)≤0.25, therefore the Fe concentration in target surface
Deviation be inhibited.Deviation therefore, it is possible to form Fe concentration is smaller and the uniform W-Ti films of etching speed.
Also, in present embodiment, by co-grinding Ti powder, W powder and Fe powder, the grain of the Fe powder before sintering
Diameter becomes 10 μm hereinafter, therefore in sintering, Fe particles can be made equably to be spread in the W as parent phase, and can make Fe
It is evenly dispersed into entire sintered body.The grain size of Fe powder before sintering be preferably 5 μm hereinafter, more preferably 2 μm hereinafter, but simultaneously
It is without being limited thereto.Also, the grain size of the Fe powder before being sintered is the smaller the better, but the grain size for extremely reducing the Fe powder before sintering can be led
Cause the increase of cost.Therefore, the grain size of the Fe powder before sintering can be 0.1 μm or more.
In addition, in the case where directly accounting for the fine Fe powder of whole 50% or more using 50 μm of particles below,
It needs to be regarded as danger to operate, but in present embodiment, is 75 μm or more and 150 μm Fe powder below by average grain diameter
End is mixed together crushings with other raw material powder (Ti powder, W powder), so that grain size is set as 10 μm hereinafter, Fe powder in addition
Ratio is sufficiently low, therefore easy to operate.
More than, embodiments of the present invention are illustrated, but the present invention is not limited thereto, are not departing from the present invention's
It can be suitably changed in the range of technological thought.
For example, in present embodiment, to being illustrated in the way of grater device co-grinding raw material powder, but simultaneously
It is without being limited thereto, other methods co-grinding raw material powder can also be passed through.
In addition, the method as co-grinding raw material powder, can enumerate planetary ball mill, vibrator etc..
As the inevitable impurity in W-Ti sputtering targets, Na, K, Ca, Ni, Cr, Mn etc. can be enumerated.These can not keep away
The impurity exempted from preferably amounts to 0.01 mass % hereinafter, but it is not limited to this.
Embodiment
Hereinafter, being said to the result of the evaluation test of the function and effect of evaluation W-Ti sputtering targets according to the present invention
It is bright.
＜ example ＞ of the present invention
As raw material powder, preparing purity is 99.999 mass % and average grain diameter is 15 μm Ti powder, purity is
The Fe powder that W powder and purity are 99.999 mass % and average grain diameter is 100 μm that 99.999 mass % and average grain diameter are 1 μm
End, and Ti powder, Fe powder and W powder are weighed in the way of as shown in Table 1 form.
In the Ti powder of weighing, Fe powder and W powder, the hard alloy system for being about 5mm with diameter by W powder and Fe powder
Ball puts into grater device (MA1D of NIPPON COKE＆ENGINEERING CO., LTD.) together, and with rotating speed 300ppm
Condition implement 1 hour co-grinding under an ar atmosphere.In addition, when being pulverized and mixed, the impurity from container is mixed in order to prevent
Enter, in the inside of the mixing vessel of the grater, implements the liner of W foils.Here, the input weight of hard alloy ball is set
It is about 10 times of the input weight of W powder and Fe powder.
The W powder and Fe powder and Ti powder of co-grinding are mixed by rotary mill device, to obtain
Mixed-powder.Here, using the mixed-powder before the observation sintering of EPMA devices, and it is true by the surface analysis image of characteristic X-ray
Determine Fe particles, and confirmed its grain size.The particle diameter is shown in table 1.The Fe particles detected all have less than 10 μm
Grain size.
Obtained mixed-powder is filled into graphite molding jig, in pressure：15MPa, temperature：1200 DEG C, keep 3 hours items
By vacuum hotpressing under part, to make hot pressed sintering body, and obtained hot pressed sintering body is machined, is produced
With diameter：152.4mm, thickness：The W-Ti sputtering targets of the example of the present invention of 6mm.
＜ comparative examples ＞
As raw material powder, preparing purity is 99.999 mass % and average grain diameter is 15 μm Ti powder, purity is
The Fe powder that W powder and purity are 99.999 mass % and average grain diameter is 100 μm that 99.999 mass % and average grain diameter are 1 μm
End, and Ti powder, Fe powder and W powder are weighed in the way of as being formed shown in table 1.
It is mixed by the Ti powder, Fe powder and W powder of rotary mill device weighing, to obtain mixed powder
End.That is, in comparative example, the crushing of raw material powder is not carried out.Here, using the mixed-powder before the observation sintering of EPMA devices, pass through
The surface analysis image of characteristic X-ray determines Fe particles, and confirmed its grain size.It is shown in Table 1 the grain size.The Fe particles detected
Substantially have grain size of the value as maximum value shown in table 1.
Obtained mixed-powder is filled into graphite molding jig, in pressure：15MPa, temperature：1200 DEG C, kept for 3 hours
Under the conditions of carry out vacuum hotpressing, to make hot pressed sintering body.Obtained hot pressed sintering body is machined, tool has been produced
There is diameter：152.4mm, thickness：The W-Ti sputtering targets of the comparative example of 6mm.
Fe concentration ＞ in ＜ target surfaces
In the case where the target surface of obtained W-Ti sputtering targets is round (circular), as shown in Fig. 2, from round center (1)
And the position (2) for being about 10mm apart from periphery by center and on 2 mutually orthogonal straight lines, (3), (4), this 5 points of (5)
Composition analysis sample is acquired using the drill bit of hard alloy.
Also, in the case where the target surface of obtained W-Ti sputtering targets is rectangle (square target), as shown in figure 3, from diagonal line
Position (2) that on the intersection point (1) of intersection and each diagonal line is about 10mm apart from corner, (3), (4), this 5 points of (5) using hard
The drill bit of matter alloy acquires composition analysis sample.
The Fe concentration of these samples is analyzed by ICP emission spectrometry methods.It is shown in Table 2 measurement result.
The formation ＞ of ＜ W-Ti films
Then, the W-Ti sputtering targets of aforementioned present invention example and comparative example are welded to anaerobic backing plate made of copper, are installed
To sputter equipment (Co., Ltd. Aifake SIH-450H), and spatter film forming is implemented under the following conditions.
Substrate：The Si substrates of diameter 100mm
Final vacuum：＜ 5 × 10-5Pa
Substrate is at a distance from target：70mm
Power：Direct current 600W
Gas pressure：Ar 1.0Pa
Substrate heats：Nothing
Film thickness：300nm
The etching speed of ＜ W-Ti films evaluates ＞
In the Si substrates of the diameter 100mm so obtained, the side 20mm is cut out from the position at three positions as shown in Figure 4
Shape sample.Further, which is cut into two parts of 10mm × 20mm, the side sample of cutting is being passed through into constant temperature
Sink is set as impregnating 5 minutes in 31 volume % aquae hydrogenii dioxidis of 30 DEG C of liquid temperature.After aquae hydrogenii dioxidi taking-up, use is pure
Water fully cleans, and further dry air is utilized to dry up accompanying pure water drop, sample is made to dry.
Utilize field emission scanning electron microscope (FE-SEM：Hitachi High-Technologies
Corporation SU-70) side not impregnated in aquae hydrogenii dioxidi and dipping this both sides of side of the sample are observed, and survey
Determine the film thickness of W-Ti films.The film thickness difference for finding out the side impregnated in aquae hydrogenii dioxidi and being not impregnated with side, the film thickness difference divided by leaching
The stain time (5 minutes), the etching speed in each position of the substrate of diameter 100mm is calculated.It is shown in Table 3 the result.
[table 1]
[table 2]
The deviation of ※ Fe concentration：(Femax-Femin)/(Femax+Femin)
Femax：Fe concentration maximas in target surface
Femin：Fe concentration minimum values in target surface
[table 3]
In comparative example 1-6, as shown in table 2, the deviation for confirming the Fe concentration in target surface becomes larger.Fe concentration in target surface
Why deviation becomes larger, thus it is speculated that its reason is not carry out the crushing of raw material powder with regard to being burnt using the larger Fe particles of grain size
Knot.
In particular, in the lower comparative example of Fe concentration 2,5, Fe concentration is locally lower, and the maximum difference of Fe concentration also becomes
Greatly.
In the W-Ti films of the comparative example 11-16 formed using the W-Ti sputtering targets of comparative example 1-6, etching speed is confirmed
It spends uneven.
Also, in the W-Ti films for the comparative example 12,15 that the W-Ti sputtering targets using the lower comparative example of Fe concentration 2,5 are formed
In, locally confirming etching speed becomes very slow.
And in example 1-6 of the present invention, the deviation for confirming the Fe concentration in target surface becomes smaller.The deviation of Fe concentration in target surface
Institute become smaller, thus it is speculated that its reason be by carry out raw material powder co-grinding, thereby using the smaller Fe particles of grain size come into
Sintering is gone.
Also, in the lower higher example 3,6 of the present invention of 2,5 and Fe of example concentration of the present invention of Fe concentration, Fe concentration it is inclined
Difference is also smaller and stablizes.
In the W-Ti films of the example 11-16 of the present invention formed using the W-Ti sputtering targets of the example 1-6 of the present invention, erosion is confirmed
It is uniform to carve speed.
In particular, the W- of the example of the present invention 12,15 formed in the W-Ti sputtering targets using the lower example 2,5 of the present invention of Fe concentration
In Ti films, Fe is also reliably added in W-Ti films, and etching speed is stablized.
Also, in the W- for the example of the present invention 13,16 that the W-Ti sputtering targets using the higher example 3,6 of the present invention of Fe concentration are formed
In Ti films, the deviation of etching speed is also fully inhibited.
It is confirmed from the result of experiment identified above, according to example of the present invention, the deviation that can form Fe concentration is smaller and lose
Carve the uniform W-Ti films of speed.
Industrial availability
W-Ti sputtering targets according to the present invention, can be formed Fe concentration deviation is smaller and the uniform W-Ti of etching speed
Film.The W-Ti sputtering targets of the present invention are suitable between the convex block and grounding electrode that are for example used when installing semiconductor element, shape
At the W-Ti films of the diffusion preventing layer as the diffusion for preventing mutual element.
Claims (1)
1. a kind of W-Ti sputtering targets, by containing average grain diameter for the raw material powder of 10 μm of Fe powder below is sintered by
It obtains, there is following composition：Ti and 25 mass ppm or more in range containing 5 mass % or more and 20 mass % or less and
Fe in the range of 100 mass ppm or less, and surplus is made of W and inevitable impurity,
Fe is diffused in the W as parent phase,
Many places in target surface, including more than 5 points of the center of target surface and outer peripheral portion measure Fe concentration, and will be measured
The maximum value of Fe concentration is set as Femax, the minimum value of Fe concentration is set as FeminIn the case of, meet following relational expression：
(Femax-Femin)/(Femax+Femin)≤0.25。
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014-207343 | 2014-10-08 | ||
| JP2014207343A JP5999161B2 (en) | 2014-10-08 | 2014-10-08 | W-Ti sputtering target |
| PCT/JP2015/077729 WO2016056441A1 (en) | 2014-10-08 | 2015-09-30 | W-ti sputtering target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106460160A CN106460160A (en) | 2017-02-22 |
| CN106460160B true CN106460160B (en) | 2018-08-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201580021546.8A Active CN106460160B (en) | 2014-10-08 | 2015-09-30 | W-Ti sputtering targets |
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| Country | Link |
|---|---|
| JP (1) | JP5999161B2 (en) |
| KR (1) | KR20160133571A (en) |
| CN (1) | CN106460160B (en) |
| TW (1) | TWI572722B (en) |
| WO (1) | WO2016056441A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6743867B2 (en) * | 2018-11-06 | 2020-08-19 | 三菱マテリアル株式会社 | W-Ti sputtering target |
| CN111155061A (en) * | 2018-11-07 | 2020-05-15 | 宁波江丰电子材料股份有限公司 | Preparation method of WTi alloy target |
| CN112111713B (en) * | 2020-09-11 | 2022-09-30 | 宁波江丰电子材料股份有限公司 | Preparation method of WTi alloy sputtering target material |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2606946B2 (en) * | 1990-03-13 | 1997-05-07 | 日立金属株式会社 | Ti-W target material and method of manufacturing the same |
| JPH05295531A (en) * | 1992-04-21 | 1993-11-09 | Toshiba Corp | Ti-w based sputtering target and its production |
| JP4747368B2 (en) * | 2007-03-05 | 2011-08-17 | 三菱マテリアル株式会社 | W-Ti target for sputtering for forming a W-Ti diffusion prevention film |
| JP5156591B2 (en) * | 2008-11-17 | 2013-03-06 | 出光興産株式会社 | Organic electroluminescence device |
| JP2011058078A (en) * | 2009-09-14 | 2011-03-24 | Toshiba Corp | SPUTTERING TARGET, Ta-W ALLOY FILM USING THE SAME, AND LIQUID CRYSTAL DISPLAY DEVICE |
| US20140360871A1 (en) * | 2012-05-22 | 2014-12-11 | Jx Nippon Mining & Metals Corporation | Fe-Pt-Ag-C-Based Sputtering Target Having C Grains Dispersed Therein, and Method for Producing Same |
| WO2014148588A1 (en) * | 2013-03-22 | 2014-09-25 | Jx日鉱日石金属株式会社 | Tungsten-sintered-body sputtering target and method for producing same |
-
2014
- 2014-10-08 JP JP2014207343A patent/JP5999161B2/en active Active
-
2015
- 2015-09-30 KR KR1020167031186A patent/KR20160133571A/en not_active Application Discontinuation
- 2015-09-30 CN CN201580021546.8A patent/CN106460160B/en active Active
- 2015-09-30 WO PCT/JP2015/077729 patent/WO2016056441A1/en active Application Filing
- 2015-10-02 TW TW104132567A patent/TWI572722B/en active
Also Published As
| Publication number | Publication date |
|---|---|
| JP2016074962A (en) | 2016-05-12 |
| JP5999161B2 (en) | 2016-09-28 |
| KR20160133571A (en) | 2016-11-22 |
| TWI572722B (en) | 2017-03-01 |
| TW201619405A (en) | 2016-06-01 |
| CN106460160A (en) | 2017-02-22 |
| WO2016056441A1 (en) | 2016-04-14 |
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