JP2007113033A - METHOD FOR PRODUCING Mo TARGET MATERIAL, AND Mo TARGET MATERIAL - Google Patents
METHOD FOR PRODUCING Mo TARGET MATERIAL, AND Mo TARGET MATERIAL Download PDFInfo
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本発明は、粉末焼結法によるＭｏターゲット材の製造方法およびＭｏターゲット材に関するものである。 The present invention relates to a method for producing a Mo target material by a powder sintering method and a Mo target material.
現在、液晶ディスプレイにおける導電膜や半導体装置の電極膜等には、比較的電気抵抗の小さい高融点金属であるＭｏ等の金属薄膜が利用されている。そして、その金属薄膜を形成するための材料として、スパッタリングターゲット材が広く利用されている。 Currently, metal thin films such as Mo, which is a refractory metal having a relatively low electrical resistance, are used for conductive films in liquid crystal displays, electrode films of semiconductor devices, and the like. A sputtering target material is widely used as a material for forming the metal thin film.
高融点金属の中でも、融点が２６００℃を超えるようなＭｏは、ターゲット材を作製するのに溶解鋳造法を適用するのが困難であるため、一般的には、化学的に生成したＭｏ粉末を原料とした粉末焼結法が適用されている。例えば、Ｍｏ粉末を焼結して予備焼結体を得た後、熱間塑性加工を施して高密度の焼結体ターゲットを得る方法が提案されている（例えば、特許文献１参照）。
近年、液晶ディスプレイ基板の大型化の要求に伴い、基板へ金属薄膜を形成するためのＭｏターゲット材のスパッタ面サイズも大型化への要求があり、特に現在は、スパッタリング面の１辺が１ｍを超えるような大型品が要求されている。この大型品への対応としては、粉末焼結では寸法上の制約があるために、粉末焼結で作製した焼結体を塑性加工により大型化することが検討されている。
一方、上述した特許文献１に記載されるＭｏターゲット材の製造方法では、相対密度８５％程度の予備焼結体を、１２００〜１５００℃の熱間温度域で塑性加工を施して、相対密度９９％以上の高密度の焼結体ターゲットを得ることが開示されている。これは、予備焼結体の密度を高めるためには有効な技術であるが、一方で、Ｍｏの加圧焼結体を効率的に大型化する上では、なお課題を残している。
In recent years, with the demand for an increase in the size of a liquid crystal display substrate, there is also a demand for an increase in the size of the sputtering surface of the Mo target material for forming a metal thin film on the substrate. There is a demand for large-sized products that exceed. In order to cope with this large product, since there is a dimensional limitation in powder sintering, it has been studied to increase the size of a sintered body produced by powder sintering by plastic working.
On the other hand, in the method for producing a Mo target material described in
また、相対密度が８５％程度の予備焼結体を高温域で塑性加工すると、焼結体内に残存する空隙を起点として、塑性加工中に割れが発生する場合があるという問題もある。
他方、一般的に粉末焼結法により作製された焼結体は靭性が低いために、製造工程上、不可避の軽微な衝撃でも割れることがあるという問題もある。
本発明の目的は、Ｍｏの粉末焼結体を使用して効率的に大型のＭｏターゲット材を作製する製造方法を提供することにある。
In addition, when a pre-sintered body having a relative density of about 85% is plastically processed in a high temperature region, there is a problem that cracks may occur during the plastic processing starting from voids remaining in the sintered body.
On the other hand, since a sintered body produced by a powder sintering method generally has low toughness, there is also a problem that it may be cracked even by inevitable light impacts in the manufacturing process.
The objective of this invention is providing the manufacturing method which produces a large sized Mo target material efficiently using the powder sintered compact of Mo.
本発明者は、Ｍｏの粉末焼結体を塑性加工によって大型化する方法に関して種々検討した結果、Ｍｏ粉末を加圧焼結することによってＭｏターゲット材に要求される相対密度の焼結体を実現すると同時に、その焼結体を効率的に塑性加工するために必要な温度域を見出した。また、上記の製造方法により従来にない機械的特性を有するＭｏターゲット材を実現し、本発明に到達した。 As a result of various studies on the method of enlarging the Mo powder sintered body by plastic working, the present inventor realized a sintered body having a relative density required for the Mo target material by pressure sintering the Mo powder. At the same time, the inventors have found a temperature range necessary to efficiently plastically process the sintered body. Moreover, Mo target material which has an unprecedented mechanical characteristic was implement | achieved by said manufacturing method, and it reached | attained this invention.
すなわち、本発明は、Ｍｏ原料粉末を加圧焼結して酸素含有量５００ｐｐｍ以下、相対密度９９．０％以上の焼結体とした後、該焼結体を２００〜８００℃で塑性加工をするＭｏターゲット材の製造方法である。
また、他の本発明は、抗折力が１２００Ｎ／ｍｍ２以上で、かつ吸収エネルギーが１０００Ｎ・ｍｍ以上のＭｏターゲット材である。
好ましくは、スパッタ面のＸ線回折における主ピーク４点で規格化した（１１０）面の相対強度比Ｒ（１１０）が４０％以上であるＭｏターゲット材である。
That is, in the present invention, Mo raw material powder is pressure-sintered to obtain a sintered body having an oxygen content of 500 ppm or less and a relative density of 99.0% or more, and then the sintered body is subjected to plastic working at 200 to 800 ° C. It is a manufacturing method of Mo target material to do.
Another aspect of the present invention is a Mo target material having a bending strength of 1200 N / mm 2 or more and an absorbed energy of 1000 N · mm or more.
Preferably, it is a Mo target material in which the relative intensity ratio R (110) of the (110) plane normalized by four main peaks in the X-ray diffraction of the sputter surface is 40% or more.
本発明の製造方法によれば、Ｍｏ焼結体を効率的に塑性加工可能となるため、塑性加工によるＭｏターゲット材の大型化にあたり欠くことのできない技術となる。 According to the manufacturing method of the present invention, the Mo sintered body can be efficiently plastically processed, and thus becomes a technique indispensable for increasing the size of the Mo target material by plastic processing.
本発明の重要な特徴は、上述したようにＭｏターゲット材の製造方法として、加圧焼結によって相対密度９９％以上の焼結体を作製し、その焼結体を形状変更によって大型化するための塑性加工において最適な温度域を見出した点にある。
以下、本発明の実施の形態について説明する。
An important feature of the present invention is that, as described above, as a method for producing the Mo target material, a sintered body having a relative density of 99% or more is produced by pressure sintering, and the sintered body is enlarged by changing its shape. This is the point of finding the optimum temperature range in plastic processing.
Hereinafter, embodiments of the present invention will be described.
本発明においては、まず、Ｍｏ原料粉末を加圧焼結して、酸素含有量５００ｐｐｍ以下で、Ｍｏターゲット材として要求される相対密度９９．０％以上の焼結体を作製する。
ここで、Ｍｏ焼結体の酸素含有量を５００ｐｐｍ以下とするのは、Ｍｏターゲット材としては、Ｍｏ焼結体中に数百ｐｐｍ程度の酸素が含有されると酸化物粒子相が多量に形成され、Ｍｏ基地中に分散した焼結組織を有するようになる。そして、この酸化物粒子相を有するＭｏターゲット材を用い、大電力でスパッタリングして高速成膜した場合、パーティクルが発生することは避けられず、特に、焼結体中の酸素含有量が５００ｐｐｍを超えるとパーティクル発生が著しく増加し、成膜特性を大きく阻害するためである。
In the present invention, first, Mo raw material powder is pressure-sintered to produce a sintered body having an oxygen content of 500 ppm or less and a relative density of 99.0% or more required as a Mo target material.
Here, the oxygen content of the Mo sintered body is set to 500 ppm or less because, as the Mo target material, a large amount of oxide particle phase is formed when about several hundred ppm of oxygen is contained in the Mo sintered body. And has a sintered structure dispersed in the Mo base. And, using the Mo target material having this oxide particle phase, when high-speed sputtering and high-speed film formation, it is inevitable that particles are generated, in particular, the oxygen content in the sintered body is 500 ppm. This is because, if it exceeds, the generation of particles is remarkably increased and the film forming characteristics are largely inhibited.
なお、Ｍｏ原料粉末を加圧焼結した焼結体としては、酸素含有量が１００ｐｐｍ程度以上の場合に本発明の製造方法を適用することが特に好ましい。それは、加圧焼結による場合には、Ｍｏ原料粉末の表面や内部に含まれる酸素や酸化物を除去することが困難であるため、実質的に上記程度の酸素を含むためであり、また、後に詳述する理由により、一定程度の酸素を含有した場合にも、本発明の製造方法では十分なＭｏ焼結体の塑性加工が可能となるためである。 In addition, as a sintered compact which pressure-sintered Mo raw material powder, it is especially preferable to apply the manufacturing method of this invention, when oxygen content is about 100 ppm or more. That is because, in the case of pressure sintering, it is difficult to remove oxygen and oxides contained in the surface and inside of the Mo raw material powder, and therefore substantially contains the above-mentioned oxygen, This is because, for the reason described in detail later, even when a certain amount of oxygen is contained, the manufacturing method of the present invention enables sufficient plastic working of the Mo sintered body.
また、焼結体の相対密度が９９．０％に満たないと焼結体中に空隙が多量に分散した焼結組織となり、上述したようにこれらの空隙を起点とし塑性加工中に割れを生じたり、スパッタリング時のパーティクル発生の原因となる。加圧焼結により相対密度９９．０％以上の焼結体とすると、塑性加工後に残存する可能性がある空隙を減少させることができ、パーティクル発生を更に低減することができる。 Further, if the relative density of the sintered body is less than 99.0%, a sintered structure in which a large amount of voids are dispersed in the sintered body is formed, and cracks are generated during plastic working starting from these voids as described above. Or the generation of particles during sputtering. When a sintered body having a relative density of 99.0% or more is obtained by pressure sintering, voids that may remain after plastic working can be reduced, and particle generation can be further reduced.
Ｍｏ原料粉末の加圧焼結方法としては、特に限定されず、相対密度９９．０％以上の焼結体を実現できる方法であればよい。なお、プレス圧力を３次元的に高圧で付加することが可能であり、素材を均一に高密度化できるという理由から熱間静水圧プレスを適用するのが望ましい。
また、均一な相対密度９９．０％以上のＭｏ焼結体を得るためには、焼結温度を１２００℃以上、プレス圧力を１００ＭＰａ以上で１時間以上保持する熱間静水圧プレスを行うことが望ましい。
The pressure sintering method for the Mo raw material powder is not particularly limited as long as it can realize a sintered body having a relative density of 99.0% or more. It is desirable to apply a hot isostatic press because the press pressure can be applied three-dimensionally at a high pressure and the material can be uniformly densified.
Further, in order to obtain a Mo sintered body having a uniform relative density of 99.0% or more, hot isostatic pressing is performed in which the sintering temperature is maintained at 1200 ° C. or higher and the pressing pressure is maintained at 100 MPa or higher for 1 hour or longer. desirable.
次に、Ｍｏ焼結体を２００〜８００℃で塑性加工する理由について説明する。
Ｍｏは体心立方格子（ＢＣＣ）の結晶構造をもつ高融点金属であり、通常、マイナス数十〜百数十℃付近にある延性脆性遷移温度（ＤＢＴＴ）を超えると、急激に延性が向上し、塑性加工が可能となると考えられている。
本発明者がＭｏの加圧焼結体の引張試験を実施したところ、Ｍｏ加圧焼結体は、図１に示すように、２００℃未満では非常に延性が低いが、２００℃以上から延性が高まり、４００〜７００℃をピークにして、約８００℃の高温域まで高い延性を示すという特徴があることを発見した。
Next, the reason for plastic working the Mo sintered body at 200 to 800 ° C. will be described.
Mo is a refractory metal having a body-centered cubic lattice (BCC) crystal structure, and when the ductile brittle transition temperature (DBTT), which is usually in the vicinity of minus tens to hundreds of degrees Celsius, is exceeded, the ductility rapidly increases. It is believed that plastic working becomes possible.
When the inventor conducted a tensile test of the Mo pressure-sintered body, the Mo pressure-sintered body had a very low ductility below 200 ° C., as shown in FIG. It has been discovered that there is a characteristic that it exhibits a high ductility up to a high temperature range of about 800 ° C. with a peak at 400 to 700 ° C.
なお、図１に示す延性の挙動を示す理由は明確ではないが本発明者等は以下のように考える。加圧焼結したＭｏ焼結体は、Ｍｏ原料粉末を加圧容器や加圧モールド内に減圧封止して焼結を進行させるため、Ｍｏ原料粉末中に存在する酸素の低減には限界があり、酸素含有量が比較的高く数百ｐｐｍレベルとなる。ここで含有される酸素は、Ｍｏ焼結体の組織中で酸化物の粒子や酸化物相として分散し、特にＭｏ焼結体の結晶粒界に酸化物粒子として集中して存在している。そして、このＭｏ焼結体の結晶粒界に集中して存在するＭｏＯｘ等の酸化物粒子は約８００℃と融点が低いため、１０００℃を超える温度域では結晶粒界を著しく脆弱化させ、これより高温域での塑性加工性を著しく低下させるものと考えられる。一方、２００℃未満で延性が低い理由としては、前記酸素等の不純物の影響により粒界強度が十分でないことが考えられる。
以上により、Ｍｏ焼結体を塑性加工するための延性が十分にある温度域２００〜８００℃で塑性加工をするのがよい。
The reason for the ductile behavior shown in FIG. 1 is not clear, but the present inventors consider as follows. Since the sintered Mo sintered body is sealed under reduced pressure by sealing the Mo raw material powder in a pressure vessel or pressure mold, there is a limit to reducing the oxygen present in the Mo raw material powder. Yes, the oxygen content is relatively high, at a level of several hundred ppm. The oxygen contained here is dispersed as oxide particles and oxide phases in the structure of the Mo sintered body, and is particularly concentrated as oxide particles at the crystal grain boundaries of the Mo sintered body. And since the oxide particles such as MoO x that are concentrated in the crystal grain boundaries of this Mo sintered body have a melting point as low as about 800 ° C., the crystal grain boundaries are significantly weakened in the temperature range exceeding 1000 ° C. It is considered that the plastic workability at a high temperature range is remarkably lowered. On the other hand, the reason why the ductility is low at less than 200 ° C. is considered that the grain boundary strength is not sufficient due to the influence of the impurities such as oxygen.
As described above, it is preferable to perform plastic working in a temperature range of 200 to 800 ° C. where the ductility for plastic working the Mo sintered body is sufficient.
また、Ｍｏ焼結体は大気中で加熱すると、５００℃付近で表面が酸化し始め、８００℃を超えると表面酸化物昇華に伴う白煙であるヒュームが発生し、作業環境を汚染するという問題もある。よって、Ｍｏ焼結体を軟鉄製の缶等でパックせずに塑性加工を施す場合には、作業環境を考慮して、７００℃以下の温度で塑性加工をするのが望ましい。 In addition, when the Mo sintered body is heated in the atmosphere, the surface starts to oxidize at around 500 ° C., and when it exceeds 800 ° C., fumes that are white smoke accompanying sublimation of the surface oxide are generated, which contaminates the work environment. There is also. Therefore, when plastic working is performed without packing the Mo sintered body with a soft iron can or the like, it is desirable to perform plastic working at a temperature of 700 ° C. or less in consideration of the working environment.
また、本発明におけるＭｏ焼結体の塑性加工としては、鍛造、圧延、押出し、引抜き等が利用できる。なお、好適な塑性加工としては、大型のターゲット材でも対応が容易な鍛造、もしくは圧延が望ましく、その際の加工条件は、１回の加工率を１０％以下で毎回の終了温度が２００℃以下にならないように制御し、数回加工を行うとよい。 Moreover, forging, rolling, extrusion, drawing, etc. can be utilized as plastic working of the Mo sintered body in the present invention. In addition, as a suitable plastic working, forging or rolling that can be easily handled even with a large target material is desirable, and the working conditions at that time are 10% or less for a single processing rate and 200 ° C. or less for each finish temperature. It is good to control so that it does not become and to process several times.
また、上記本発明の製造方法により、抗折力が１２００Ｎ／ｍｍ２以上で、かつ吸収エネルギーが１０００Ｎ・ｍｍ以上である靭性の高いＭｏターゲット材を実現できる。上述の数値の機械的特性を実現することで、スパッタリングターゲット材を作製する際の機械加工等の取扱い時に割れが発生するのを抑制することが可能となる。また、加工時等で発生した曲がり等の形状不具合を容易に修正することが出来る。 Moreover, by the manufacturing method of the present invention, a Mo target material having high toughness with a bending strength of 1200 N / mm 2 or more and an absorbed energy of 1000 N · mm or more can be realized. By realizing the above-described numerical mechanical properties, it is possible to suppress the occurrence of cracks during handling such as machining when producing a sputtering target material. Further, it is possible to easily correct a shape defect such as a bend that occurs during processing.
また、上記本発明の製造方法により、ＢＣＣ結晶構造を有するＭｏの最稠密面である（１１０）面の相対強度比を高めることによって、スパッタリング成膜時に、スパッタレートが高くなり、生産性を向上させる効果が実現できる。具体的には、Ｘ線回折における主ピーク４点で規格化した（１１０）面の相対強度比Ｒ（１１０）が４０％以上であることが望ましい。更に生産性を向上させるためには、相対強度比Ｒ（１１０）を５０％以上にすることがより望ましい。なお、相対強度比Ｒ（ｈｋｌ）は、以下の式で定義される値である。Ｒ（ｈｋｌ）＝（Ｉ（ｈｋｌ）／Ｉ０（ｈｋｌ））／Σ（Ｉ（ｈｋｌ）／Ｉ０（ｈｋｌ））
但し、
Ｉ（ｈｋｌ）は、（ｈｋｌ）面の回折強度
Ｉ０（ｈｋｌ）は、（ｈｋｌ）面のリファレンス強度
主ピークの４点の面指数（ｈｋｌ）とは、（１１０）面、（２００）面、（２１１）面、（３１０）面である。この式は、リファレンスを利用して規格化しているため、絶対強度の異なる回折ピークの配向性を比較することが出来る。なお、全く無配向の場合には、回折強度とリファレンス強度が等しくなるために、Ｉ（ｈｋｌ）／Ｉ０（ｈｋｌ）は１となり、Ｒ（ｈｋｌ）は全て２５％となる。
In addition, by increasing the relative intensity ratio of the (110) plane, which is the Mo densest surface of Mo having the BCC crystal structure, the production rate of the present invention increases the sputtering rate and improves productivity. Effect can be realized. Specifically, it is desirable that the relative intensity ratio R (110) of the (110) plane normalized by four main peaks in X-ray diffraction is 40% or more. In order to further improve productivity, the relative intensity ratio R (110) is more preferably set to 50% or more. The relative intensity ratio R (hkl) is a value defined by the following equation. R (hkl) = (I (hkl) / I0 (hkl) ) / Σ (I (hkl) / I0 (hkl) )
However,
I (hkl) is the diffraction intensity I 0 (hkl) of the (hkl) plane, and the four plane indices (hkl) of the reference intensity main peak of the (hkl) plane are the (110) plane and the (200) plane , (211) plane, (310) plane. Since this equation is normalized using a reference, the orientations of diffraction peaks having different absolute intensities can be compared. In the case of no orientation at all, since the diffraction intensity and the reference intensity are equal, I (hkl) / I 0 (hkl) is 1, and R (hkl) is all 25%.
以下の実施例で本発明を更に詳しく説明する。
平均粒経が４５μｍ以下の純Ｍｏ粉末を軟鉄缶に充填した後に、４００℃で加熱しながら１×１０−３Ｐａまで減圧脱気して封止した。この密閉した軟鉄缶を熱間静水圧プレス装置の炉体内部に設置して、１２５０℃、１４８ＭＰａ、５時間の加圧焼結を施した。加圧焼結後に軟鉄缶を機械加工によって除去してＭｏ焼結体を得た。上記で作製したＭｏ焼結体の密度をアルキメデス法により測定したところ、相対密度は９９．８％に達していた。Ｍｏ焼結体の酸素含有量を赤外線吸収法により測定したところ、４１７ｐｐｍであった。
The following examples further illustrate the present invention.
After filling pure iron powder with an average particle size of 45 μm or less into a soft iron can, it was deaerated under reduced pressure to 1 × 10 −3 Pa while being heated at 400 ° C. and sealed. This sealed soft iron can was placed inside a furnace body of a hot isostatic pressing apparatus and subjected to pressure sintering at 1250 ° C., 148 MPa for 5 hours. After pressure sintering, the soft iron can was removed by machining to obtain a Mo sintered body. When the density of the Mo sintered body produced above was measured by the Archimedes method, the relative density reached 99.8%. When the oxygen content of the Mo sintered body was measured by an infrared absorption method, it was 417 ppm.
その後、熱間静水圧プレスにより作製したＭｏ焼結体を、長さ３８０ｍｍ、幅１１０ｍｍ、厚さ８．１ｍｍの板状に切出した。このＭｏ焼結体を大気雰囲気の加熱炉で７００℃に加熱後、圧延終了時のＭｏ焼結体の温度が２００℃以下にならない温度範囲で厚さ４．６ｍｍになるまで圧延による塑性加工を行った。なお、その際の１回の圧下率は４％とした。そして、圧延終了後の、長さ６６８ｍｍ、幅１１２ｍｍ、厚さ４．６ｍｍのＭｏ焼結体を機械加工してＭｏターゲット材を得た。上記の温度制御によりＭｏ焼結体は割れを生じることなく塑性加工を行うことができた。 Thereafter, the Mo sintered body produced by hot isostatic pressing was cut into a plate shape having a length of 380 mm, a width of 110 mm, and a thickness of 8.1 mm. After this Mo sintered body is heated to 700 ° C. in a heating furnace in the air atmosphere, plastic working by rolling is performed until the thickness of the Mo sintered body at the end of rolling is 4.6 mm within a temperature range that does not become 200 ° C. or less. went. In addition, the rolling reduction rate at that time was 4%. And the Mo target material was obtained by machining the Mo sintered body of length 668mm, width 112mm, and thickness 4.6mm after completion | finish of rolling. With the above temperature control, the Mo sintered body could be plastically processed without causing cracks.
次に、上記のＭｏターゲット材および塑性加工前のＭｏ焼結体からそれぞれ試験片を採取し、抗折力と吸収エネルギーを測定した。具体的には、試験片は塑性加工後のＭｏターゲット材より、圧延方向と試験片の長手方向が平行になるように３．５ｍｍ×３．５ｍｍ×６０ｍｍのサイズで５本採取した。また塑性加工前のＭｏ焼結体からも、任意に５本の同一寸法の試験片を採取した。
なお、抗折力と吸収エネルギーの測定方法は、以下の通りとした。抗折力は、試験片を２つのささえにのせ、中央部に押し金具を当てて移動速度２０ｍｍ／ｍｉｎで徐々に荷重を加えて静的に破断したときの荷重とした。また、吸収エネルギーは、押し金具が移動し、試験片に接触した時点から、試験片が破断するまでの仕事量（押し金具の荷重と移動距離の積）で算出した。以上の抗折力の測定と吸収エネルギーの算出結果を表１に示す。
Next, test pieces were sampled from the Mo target material and the Mo sintered body before plastic working, and the bending strength and absorbed energy were measured. Specifically, five test pieces with a size of 3.5 mm × 3.5 mm × 60 mm were collected from the Mo target material after plastic working so that the rolling direction and the longitudinal direction of the test piece were parallel. In addition, five test pieces having the same dimensions were arbitrarily collected from the Mo sintered body before plastic working.
In addition, the measuring method of bending strength and absorbed energy was as follows. The bending strength was defined as the load when the test piece was placed on two supports, a pressing metal fitting was applied to the center portion, and a load was gradually applied at a moving speed of 20 mm / min to break statically. Absorbed energy was calculated by the amount of work (product of the load of the metal fitting and the moving distance) from the time when the metal piece moved and contacted the test piece until the test piece broke. Table 1 shows the results of measurement of the bending strength and calculation of absorbed energy.
表１より、塑性加工前のＭｏ焼結体の抗折力は１０００Ｎ／ｍｍ２以下であるのに対して、本発明によるＭｏターゲット材は１５００Ｎ／ｍｍ２以上となり、また、吸収エネルギーにおいても、本発明のＭｏターゲット材は２０００Ｎ・ｍｍ以上となり、高い靭性を有していることが分かる。 From Table 1, the bending strength of the Mo sintered body before plastic working is 1000 N / mm 2 or less, whereas the Mo target material according to the present invention is 1500 N / mm 2 or more, and also in the absorbed energy, It can be seen that the Mo target material of the present invention has a high toughness of 2000 N · mm or more.
また、図２に本発明のＭｏターゲット材、図３に塑性加工前のＭｏ焼結体のＸ線回折による主ピーク（１１０）面、（２００）面、（２１１）面、（３１０）面の相対強度比を示す。その結果、塑性加工前のＭｏ焼結体は相対強度比がいずれもほぼ等しく無配向であるのに対して、本発明のＭｏターゲット材は、Ｍｏの最稠密面である（１１０）面の相対強度比Ｒ（１１０）は４０％以上を示し、最稠密面に強配向していることが分かる。 2 shows the Mo target material of the present invention, and FIG. 3 shows the main peaks (110) plane, (200) plane, (211) plane, and (310) plane of the Mo sintered body before plastic working by X-ray diffraction. Relative intensity ratio is shown. As a result, the Mo sintered body before plastic working has a relative strength ratio that is almost equal and non-oriented, whereas the Mo target material of the present invention has a relative to the (110) plane that is the most dense surface of Mo. The intensity ratio R (110) is 40% or more, and it can be seen that it is strongly oriented on the densest surface.
Claims (3)
Ｒ（ｈｋｌ）は、以下の式で定義される値である。
Ｒ（ｈｋｌ）＝（Ｉ（ｈｋｌ）／Ｉ０（ｈｋｌ））／Σ（Ｉ（ｈｋｌ）／Ｉ０（ｈｋｌ））
但し、
Ｉ（ｈｋｌ）は、（ｈｋｌ）面の回折強度
Ｉ０（ｈｋｌ）は、（ｈｋｌ）面のリファレンス強度
主ピーク４点の面指数（ｈｋｌ）とは、（１１０）、（２００）、（２１１）、（３１０）である。 The Mo target material according to claim 2, wherein the relative intensity ratio R (110) of the (110) plane normalized by four main peaks in the X-ray diffraction of the sputter surface is 40% or more.
R (hkl) is a value defined by the following equation.
R (hkl) = (I (hkl) / I0 (hkl) ) / Σ (I (hkl) / I0 (hkl) )
However,
I (hkl) is the diffraction intensity I 0 (hkl) of the (hkl) plane, and the plane index (hkl) of the four reference intensity main peaks of the (hkl) plane is (110), (200), (211) ), (310).
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| US20100108501A1 (en) * | 2007-01-12 | 2010-05-06 | Nippon Steel Materials Co., Ltd | Mo-based sputtering target plate and method for manufacturing the same |
| CN101792897A (en) * | 2010-04-06 | 2010-08-04 | 韩伟东 | High-purity molybdenum target for thin-film solar cell and preparation method thereof |
| JP2011132563A (en) * | 2009-12-22 | 2011-07-07 | Toshiba Corp | Mo SPUTTERING TARGET AND MANUFACTURING METHOD THEREFOR |
| US8415194B2 (en) * | 2007-06-12 | 2013-04-09 | Guardian Industries Corp. | Rear electrode structure for use in photovoltaic device such as CIGS/CIS photovoltaic device and method of making same |
| WO2013088785A1 (en) * | 2011-12-12 | 2013-06-20 | Jx日鉱日石金属株式会社 | Indium sputtering target member and method for producing same |
| JP2013122082A (en) * | 2012-07-27 | 2013-06-20 | Jx Nippon Mining & Metals Corp | Indium sputtering target member and manufacturing method thereof |
| CN103459631A (en) * | 2011-03-25 | 2013-12-18 | 联合材料公司 | Molybdenum material |
| CN104520466A (en) * | 2012-05-09 | 2015-04-15 | H·C·施塔克公司 | Multi-block sputtering target with interface portions and associated methods and articles |
| KR20150124391A (en) | 2014-04-28 | 2015-11-05 | 가부시끼가이샤 아라이도 마테리아루 | Material for sputtering target |
| CN105525260A (en) * | 2014-10-22 | 2016-04-27 | 宁波江丰电子材料股份有限公司 | Production methods of Mo target blank and Mo target material |
| JP7394249B1 (en) * | 2023-05-15 | 2023-12-07 | 株式会社アルバック | Molybdenum target and its manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100108501A1 (en) * | 2007-01-12 | 2010-05-06 | Nippon Steel Materials Co., Ltd | Mo-based sputtering target plate and method for manufacturing the same |
| US8415194B2 (en) * | 2007-06-12 | 2013-04-09 | Guardian Industries Corp. | Rear electrode structure for use in photovoltaic device such as CIGS/CIS photovoltaic device and method of making same |
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| CN101792897A (en) * | 2010-04-06 | 2010-08-04 | 韩伟东 | High-purity molybdenum target for thin-film solar cell and preparation method thereof |
| CN103459631A (en) * | 2011-03-25 | 2013-12-18 | 联合材料公司 | Molybdenum material |
| WO2013088785A1 (en) * | 2011-12-12 | 2013-06-20 | Jx日鉱日石金属株式会社 | Indium sputtering target member and method for producing same |
| CN104520466A (en) * | 2012-05-09 | 2015-04-15 | H·C·施塔克公司 | Multi-block sputtering target with interface portions and associated methods and articles |
| JP2013122082A (en) * | 2012-07-27 | 2013-06-20 | Jx Nippon Mining & Metals Corp | Indium sputtering target member and manufacturing method thereof |
| KR20150124391A (en) | 2014-04-28 | 2015-11-05 | 가부시끼가이샤 아라이도 마테리아루 | Material for sputtering target |
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