• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A tungsten sputtering target is provided which is capable of forming a tungsten film having a low specific resistance when the tungsten film is formed using the tungsten sputtering target. A tungsten sputtering target wherein a purity of tungsten is 5 N (99.999 wt%) or more, and an impurity of carbon and an impurity of oxygen contained in tungsten are each 50 ppm by weight , or less, and an average tungsten crystal grain size is more than 100 μm.
    公开号:AT522305A2
    申请号:T9286/2018
    申请日:2018-09-07
    公开日:2020-10-15
    发明作者:Sogawa Shinji；Dasai Takafumi；Nakasumi Seiji
    申请人:Jx Nippon Mining & Metals Corp；
    IPC主号:
    专利说明:

    TUNGSTEN SPUTTERING TARGET AND METHOD FOR MANUFACTURING IT
    TECHNICAL FIELD Field of the Invention The present invention relates to a tungsten sputtering target and a method for its manufacture. TECHNICAL BACKGROUND [0002]
    In recent years, with the increase in the higher integration of VLSI, studies have been made to use materials having a lower electrical resistivity as electrode materials and wiring materials. Under these circumstances, tungsten of high purity, which has a low specific resistance and is thermally and chemically stable, is used as an electrode material and a wiring material.
    The electrode material and wiring material for the VLSI are generally manufactured by a sputtering method and a CVD method. The sputtering method is relatively simple in equipment construction and operation, and it is easier to form a film and it is low in cost. Therefore, it is used more widely than the CVD method.
    [0003]
    High purity and high density are for tungsten sputtering targets
    In recent years, however, are required further, in terms of films that are through
    Sputtering electrode materials and wiring materials for VLSI under
    Using a tungsten sputtering target to form materials with a lower electrical resistivity is required. [0004]
    In this regard, Patent Literature 1 discloses a tungsten sintered body sputtering target characterized in that the purity of tungsten is 5 N (99.999 wt%) or more and the carbon as an impurity contained in the tungsten is 5 ppm , by weight, is or less. By forming a film using such a tungsten sintered body sputtering target, there is an excellent effect that, in the tungsten film, a stabilized reduction in electrical resistivity can be achieved.
    [0005]
    As described above, by increasing the purity of a tungsten sputtering target, Patent Literature 1 succeeds in reducing the resistivity of a tungsten film formed by sputtering. [0006]
    However, the lowering of the resistance of the tungsten film using the high purity has reached its limit. Therefore, it is necessary to take other measures to further reduce the resistance.
    LIST OF REFERENCES [Patent Literature] [Patent Literature 1] Japanese Patent No. 5944482 SUMMARY OF THE INVENTION [Problem to be Solved by the Invention]
    [0008]
    Therefore, it is an object of the present invention to provide a tungsten sputtering target capable of forming a tungsten film having a low specific resistance when the tungsten film is formed using the tungsten sputtering target.
    [Means for Solving the Problem] [0009]
    In performing sputtering on a tungsten sputtering target, a method of forming a film can be considered in which a rare gas represented by Ar or K is collided at a high speed and the repelled tungsten element on a substrate surface, such as a silicon (Si) wafer is vapor deposited to have a predetermined thickness. However, a rare gas such as Ar is fixed on the substrate surface together with the tungsten element during film formation, and as a result, a tungsten film including Ar or the like can be formed. Such a tungsten film tends to have a higher specific resistance than a tungsten film in which Ar is not incorporated. [0010]
    Therefore, a method of using Kr gas which has a larger atomic radius is conceivable for reducing the amount of absorbed noble gas atoms. However, since Kr gas is more expensive than Ar gas, it leads to an increase in production cost. Therefore, improvement of the tungsten sputtering target itself is extremely useful.
    [0011]
    On the basis of the above findings, the present invention provides a tungsten sputtering target in which a rare gas such as Ar or Kr is hardly taken into a tungsten film during film formation. This makes it possible
    a tungsten film with a smaller amount of included Ar; and the like
    and form a tungsten film having a lower resistivity. [0012]
    Further, the inventors of the present invention made it possible to form a tungsten film having a lower resistivity by controlling the mean grain size of the tungsten sputtering target to be in the range of more than 100 µm. [0013]
    Accordingly, the present invention is specified as follows: (1) Tungsten sputtering target, wherein a purity of tungsten is 5N (99.999 wt%) or more, and an impurity of carbon and an impurity of oxygen contained in the tungsten are each 50 ppm by weight or less, and an average tungsten crystal grain size is more than 100 µm. (2) The sputtering target according to claim (2), wherein a relative density is 99.3% or more. (3) The sputtering target according to (1) or (2), wherein the carbon and the oxygen are each 10 ppm by weight or less. (4) A method of manufacturing a tungsten sputtering target, in which tungsten powder is formed by a hot press (HP) method and then compacted by a hot isostatic press (HIP) method, wherein
    a temperature in the hot isostatic pressing process is 1,800 ° C. or more; and a sintering time is 5.5 hours or more.
    (5) A method of manufacturing a tungsten sputtering target, in which tungsten powder is formed by a hot press (HP) method and then by
    a rolling process is compacted, wherein
    a temperature in the rolling process is 1200 ° C. or more and 1700 ° C. or less, and a total rolling reduction is 15% or more and 25% or less. 6. The method for producing a tungsten sputtering target according to claim 5, wherein in the rolling process, a rolling reduction per rolls is 3 to 12%. [Effect of the invention] [0014]
    According to the present invention, it is possible to provide a tungsten sputtering target capable of forming a tungsten film having a low specific resistance when the tungsten film is formed using the tungsten sputtering target.
    BRIEF DESCRIPTION OF THE DRAWINGS [0015]
    FIG. Fig. 1 is a graph showing a correlation between the amount of aromatic atoms included in a tungsten film and the specific resistance of the tungsten film.
    DESCRIPTION OF THE PREFERRED EMBODIMENTS [0016]
    According to the present invention, a tungsten sputtering target has a purity of tungsten of 5 N (99.999 wt%) or more, and an impurity of carbon and an impurity of oxygen contained in tungsten of 50 ppm each, by weight, or less, and an average tungsten crystal grain size greater than 100 µm.
    (Purity) To have a tungsten film with a low specific resistance
    form, it is necessary to suppress impurities contained in the tungsten film
    are included. It is therefore essential to increase the purity of the tungsten sputtering target. Specifically, it is necessary to have a purity of 99.999 wt% (5N) or more.
    [0018]
    (Impurities)
    Further, since impurities such as carbon and oxygen contained in the target are included in the tungsten film at the time of film formation, the resistivity of the tungsten film after film formation by sputtering tends to increase as the amount of carbon increases. Therefore, it is necessary that the impurity of carbon and the impurity of oxygen contained in tungsten are each 50 ppm by weight or less. From the same standpoint, the impurity of carbon and the impurity of oxygen contained in tungsten are each preferably 30 ppm by weight or less, and more preferably each 20 ppm by weight or less. When the carbon content and the oxygen content are each 10 ppm by weight or less, the influence on the specific resistance of the tungsten film almost disappears.
    In order to reduce carbon, when tungsten powder is filled into a graphite mold and hot-pressed, it is preferred that the tungsten powder is isolated so that it does not come into direct contact with the graphite mold.
    (Mean tungsten crystal grain size)
    In the tungsten sputtering target according to the present embodiment, the mean grain size of the tungsten crystal is more than 100 µm. Conventionally, it is known that the average tungsten crystal grain size increases with the density of the
    Tungsten Sputtering Targets is related to the relationship between the mean
    However, the grain size of the tungsten crystal and the amount of Ar atoms trapped in the tungsten film during film formation were not investigated. In the present embodiment, since the average grain size of the tungsten crystal is more than 100 µm, it becomes difficult for Ar atoms to be included in the tungsten film during film formation, and as a result, a tungsten film having a small amount of Ar included can be obtained. In other words, even if the tungsten sputtering targets have the same purity, density, and the like, a tungsten sputtering target with an average grain size of tungsten crystal larger than 100 µm is capable of producing a tungsten film having a lower specific resistance than that of an average grain size of the tungsten crystal of 100 µm or less. Therefore, in the present embodiment, the mean grain size of the tungsten crystal is preferably 120 µm or more, more preferably 150 µm or more, and still more preferably 200 µm or more.
    [0020]
    The average tungsten crystal grain size can be determined by a value according to the average line segment length per crystal grain of an evaluation test line crossing the inside of the crystal grain, evaluated by the cutting method according to JIS G 0551: 2013. Specifically, the structure is observed with an optical microscope. In the structural photograph viewed and obtained, a straight line is drawn on the photograph until the number of particles lying on the straight line N = 200, then using the number of particles (N = 200) and the total length (L ) the straight line calculates the mean grain size of the point under consideration by L / N. [0021]
    (Relativ density)
    The relative density of the tungsten sputtering target is preferably 99.3% or more. When the specific gravity of the target is 99.5% or more, the gas component contained in the target is lower, so that when a film is formed, the resistivity of the film can be further suppressed. Furthermore, generation of dust due to abnormal discharge is also suppressed. From the above standpoint, the specific gravity of the target is more preferably 99.7% or more, and still more preferably 99.9% or more.
    [0022] (manufacturing process)
    The manufacturing method of the tungsten sputtering target according to the present embodiment is not particularly limited as long as it has each of the characteristics described above, and if a tungsten sputtering target having such characteristics is to be obtained, a powder metallurgy method can be used in which a hot pressing process (HP) and a hot isostatic pressing process (HIP) can be combined. Further, by controlling the appropriate conditions of the HIP and HP as follows, the characteristics of the tungsten sputtering target according to the present invention as described above can be obtained. Further, in addition to the powder metallurgy method in which the HP method and the HIP method are combined, the above-described characteristics of the tungsten sputtering target according to the present invention can also be obtained by performing rolling treatment under suitable conditions according to the HP method .
    [0023]
    First, in the HP process, a suitable shape is made with tungsten powder as
    Raw material is filled, and heat is applied to it while a load is applied
    becomes. The tungsten powder used here preferably has a grain size of
    5 µm or less. In the HP step, while the temperature is increased at an appropriate rate of temperature rise, an appropriate load is applied to each temperature range until the temperature rises to the HP temperature, and the temperature is maintained at the HP temperature for a predetermined time. At this time, it is preferred that the temperature rise rate be about 2 to
    10 ° C / min. In this HP step, it is preferable to appropriately set and change the applied load in the temperature range of 600 to 1200 ° C. and in the temperature range of 1200 ° C. or more, respectively. In the HP process, degassing occurs in the initial stage of temperature rise. If a high load is applied at this stage, the sintering proceeds without sufficient degassing and the sintered body does not develop a high density. In addition, a large amount of remaining gas components such as oxygen is contained inside. Therefore, in the HP step, the sintered body is densified by applying a small load in a low temperature range and applying a higher load in a high temperature range, and thus a sintered body having a small amount of residual oxygen can be obtained. Specifically, the load pressure in the temperature range of 600 to 1200 ° C. is preferably about 80 to 150 kg / cm , and the load pressure in the temperature range of 1200 ° C. or more is preferably about 200 to 350 kg / cm . In addition, during the temperature rise process, it is effective to introduce a process (s) of holding the workpiece at a certain temperature for a certain period of time a few times to obtain a sintered body having a high density and a random orientation. The HP temperature at this time is preferably about 1600 to 1900 ° C. If the HP temperature is too low, the density does not increase sufficiently, and if it is too high, the formation of a carbide layer occurs
    the tungsten surface, which is not preferred. If the
    The rate of temperature rise is too rapid, the degassing does not progress sufficiently in the HP, which is not preferable. Obviously, too low a rate of temperature rise is not preferable because productivity is lowered. The holding time in this step is about 30 to 240 minutes and can be set appropriately in consideration of conditions such as temperature. The holding time at the HP temperature can be determined and adjusted similarly.
    [0024]
    With respect to the formed body by the HP method, in order to increase the average grain size of tungsten crystal and to increase the density of the formed body, it is effective to subject the body formed by the HP to a HIP process. In the present embodiment, it is important that the temperature during the HIP processing is 1800 ° C. or more, and the processing time is 5.5 hours or more. By setting the conditions of the HIP method to the above conditions, a tungsten sputtering target having an average tungsten crystal grain size larger than 100 µm can be obtained. The pressure of the HIP process can be used as a guide to 1600 to 1900 kg / cm can be set. The upper limit of the temperature during the HIP process is not particularly limited, but is preferably 2200 ° C or less from the standpoint of cost. The upper limit of the time of the HIP process is not particularly limited, but is preferably 8 hours or less from the standpoint of cost.
    [0025]
    In addition, it should be noted that the formed body can be subjected to plastic working by rolling instead of HIP according to the HP process. By setting the conditions of hot rolling, the
    mean tungsten crystal grain size of the tungsten sputtering target according to FIG
    present embodiment can be controlled. Specifically, the rolling temperature must be 1200 ° C. or more and 1700 ° C. or less, and it is important that the total rolling reduction be about 15 to 25%. Here, the total rolling reduction is a value that is multiplied by multiplying the rolling reduction per roll by the number of passes of the rolling process. The rolling reduction per roll is represented by the following equation. The rolling reduction in one rolling process is approximately 3 to 12%. In addition, the number of passes is expediently 4 to 6 times.
    Roll reduction per roll = (hn-ı - hr) / ho
    In the equation, ho is the initial thickness of the formed body, hn-1 is the thickness of the formed body immediately before rolling in the current pass, and h, is the thickness of the formed body after rolling in that pass.
    EXAMPLES [0026]
    Hereafter, some embodiments of the present invention will be specifically described based on examples and comparative examples. The description of the following examples and comparative examples refers only to specific examples for better understanding the technical content of the present invention, and the technical scope of the present invention is not limited by these specific examples. [0027]
    (Examples 1 to 3)
    A carbon mold was filled with tungsten powder with a purity of 5N (99.999 wt%) and an average grain size of 1 µm, and became an HP at a maximum temperature of 1600 ° C in a vacuum chamber
    subject. The applied HP load in this process was 240 kgf / cm . The so
    obtained HP-formed bodies were further subjected to a HIP process under the conditions shown in Table 1. The shape of the sintered body subjected to the HIP process was processed to obtain a sputtering target having a diameter of 400 mm and a thickness of 6 mm. [0028]
    (Example 4)
    A carbon mold was filled with tungsten powder with a purity of 5N (99.999 wt%) and an average grain size of 1 µm, and was subjected to HP at a maximum temperature of 1600 ° C in a vacuum chamber. The applied HP load in this process was 240 kgf / cm . The HP formed body obtained as described above was further subjected to a rolling process at 1,400 ° C, the number of times of rolling was 6 times, the rolling reduction per roll was 4.2%, and the total rolling reduction was 25 % amounted to.
    (Example 5)
    A carbon mold was filled with tungsten powder with a purity of 5N (99.999 wt%) and an average grain size of 1 µm, and was subjected to HP at a maximum temperature of 1600 ° C in a vacuum chamber. The applied HP load in this process was 240 kgf / cm . The HP formed body obtained as described above was further subjected to a rolling process at 1,400 ° C, the number of times of rolling being 5 times, the rolling reduction per roll being 5.0%, and the total rolling reduction being 25 times % amounted to.
    [0029]
    (Example 6)
    A carbon mold was filled with tungsten powder with a purity of 5N (99.999 wt%) and an average grain size of 1 µm, and was subjected to HP at a maximum temperature of 1600 ° C in a vacuum chamber. The applied HP load in this process was 240 kgf / cm . The HP formed body obtained as described above was further subjected to a rolling process at 1700 ° C, the number of times of rolling was 4 times, the rolling reduction per roll was 3.8%, and the total rolling reduction was 15 % amounted to.
    (Comparative Examples 1 to 3)
    A carbon mold was filled with tungsten powder having a purity of 5 N (99.999 wt%) and an average grain size of 1 µm, and was subjected to HP at a maximum temperature shown in Table 1 in a vacuum chamber. The applied HP load in this process was 240 kgf / cm . The HP-formed body thus obtained was further subjected to an HIP process under the conditions shown in Table 1. The shape of the sintered body subjected to the HIP process was processed to obtain a sputtering target having a diameter of 400 mm and a thickness of 6 mm. [0032]
    (Comparative example 4)
    A carbon mold was filled with tungsten powder having a purity of 5N (99.999 wt%) and an average grain size of 1 µm, and was subjected to HP at a maximum temperature of 1200 ° C in a vacuum chamber. The applied HP load in this process was 240 kgf / cm . The formed body according to HP, which was obtained as described above,
    was further subjected to a rolling process at 1400 ° C, the number of
    The times of rolling was 8 times, the rolling reduction per roll was 11.3%, and the total rolling reduction was 90%. [0033]
    The obtained tungsten sputtering target was measured as follows: (impurity concentration)
    The carbon concentration was measured by sputtering each tungsten sputtering target and then using an inert gas melting method for the sample with a carbon analyzer (CSLS600, manufactured by LECO).
    The oxygen concentration was measured by an inert gas melting method for the above-described sample using a simultaneous oxygen / nitrogen analyzer (TC-600, manufactured by LECO Corporation).
    (Mean tungsten crystal grain size)
    The structure was observed with an optical microscope. In the structural photograph observed and obtained, a straight line was drawn on the photograph until the number of particles lying on the straight line N = 200, then using the number of particles (N = 200) and the total length (L ) the straight line calculates the mean grain size of the point under consideration by L / N.
    (Relativ density)
    The relative density, as stated here, refers to the ratio of the measured density to the theoretical density. The measured density refers to the value measured by the Archimedes ‘method using pure water as the solvent. The theoretical density is used as the theoretical density when the tungsten content is 100%.
    [0034]
    Further, a tungsten film was formed on a silicon substrate by sputtering using Ar gas using each of the tungsten sintered body targets prepared in Examples 1 to 6 and Comparative Examples 1 to 4 and the carbon concentration, oxygen concentration, Ar concentration and resistivity the films formed were measured as follows.
    (Carbon concentration, oxygen concentration, Ar concentration)
    The measurement was made by secondary ion mass spectrometry (SIMS). As a measuring device, PHI ADEP1010 manufactured by ULVACPHI Incorporated was used. In addition, “undetectable” in Table 1 means that the value is lower than the detection limit value of the SIMS method. (Method of Measuring Resistivity)
    The sheet resistance at seven points of the wafer was measured using OMNIMAP RS75 manufactured by KLA-Tencor Corporation, each multiplied by the film thickness measured by XRR (X-ray reflectance measurement), and the average value was defined as the resistivity of the film.
    [0035]
    [Table 1]
    MS>
    Si 88 A Ca Dr iS
    PS
    3
    sioalie N RN N + + + + as) ass EM 1 u Ni m 6 8 Ri EG a eier ls x = S = + © a: ® | ug Cr X x> Le Do S LO SS SS + & Si + wa il Ei w Sa PN = & DD Sg £ ei ES N 5 MD & = ER DDR SS iS 8 X SR 5:35:08 8
    (x
    ON EN RS m ESF BONEDEM iS io Qi BA fr al ts A EI iss DL a in Es AZ XE zZ & 503 3 BB £ 5 3 KEG * x € S% 3a holwierf: »1 @ SX 5 Has> hd © .xs <* € we S = & A a By S lilate ‚id 18 5 3 $ N ACT € ©. X £ Dis ml; Ss 5 an 5 & Si 8 X Do = & ia iD
    WO2019 / 092969
    [0036]
    In Examples 1 to 6, since the average tungsten crystal grain size was more than 100 µm, the amount of Ar atoms included in the film during film formation was small and the specific resistance of the film was low.
    On the other hand, since the average tungsten crystal grain size of Comparative Examples 1 to 4 was 100 µm or less, a large amount of Ar atoms was included in the film at the time of film formation, and the
    the specific resistance of the film was high.
    权利要求:
    Claims (6)
    [1]
    Claims: 1. Tungsten sputtering target, wherein a purity of tungsten is 5 N (99.999 wt%) or more, and an impurity of carbon and an impurity of oxygen contained in tungsten are each 50 ppm, based on by weight, or less, and an average tungsten crystal grain size is more than 100 µm.
    [2]
    2. The sputtering target according to claim 1, wherein a relative density is 99.3% or more.
    [3]
    3. The sputtering target according to claim 1 or 2, wherein the carbon and the oxygen are each 10 ppm by weight or less.
    [4]
    4. A method of manufacturing a tungsten sputtering target, in which tungsten powder is formed by a hot press (HP) process and then compacted by a hot isostatic press (HIP) process, wherein
    a temperature in the hot isostatic pressing process is 1,800 ° C. or more; and a sintering time is 5.5 hours or more.
    [5]
    5. A method for producing a tungsten sputtering target, in which tungsten powder is formed by a hot press (HP) method and then compacted by a rolling method, wherein
    a temperature in the rolling process of 1200 ° C or more and 1700 ° C
    or less, and a total rolling reduction is 15% or more and 25% or less.
    [6]
    6. A method for producing a tungsten sputtering target according to claim
    5, wherein in the rolling process, a rolling reduction per roll is 3 to 12%.
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    同族专利:
    公开号 | 公开日
    AT522305A5|2021-10-15|
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    US20200370167A1|2020-11-26|
    引用文献:
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    KR20140129249A|2012-03-02|2014-11-06|제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤|Tungsten sintered compact sputtering target and tungsten film formed using same target|
    CN105102670B|2013-03-22|2017-06-23|吉坤日矿日石金属株式会社|Tungsten sinter sputtering target and its manufacture method|CN113088899A|2021-03-19|2021-07-09|有研亿金新材料有限公司|Preparation method of high-purity low-oxygen tungsten-silicon alloy target material|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP2017217737A|JP2019090071A|2017-11-10|2017-11-10|Tungsten sputtering target, and manufacturing method thereof|
    PCT/JP2018/033273|WO2019092969A1|2017-11-10|2018-09-07|Tungsten sputtering target and method for producing same|
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