TW201619405A - W-Ti sputtering target - Google Patents
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- 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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- 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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Abstract
Description
本發明關於例如在安裝半導體元件時所用的凸塊與基底電極之間,作為防止互相的元素之擴散的擴散防止層,將W-Ti膜予以成膜用的W-Ti濺鍍靶。 The present invention relates to a W-Ti sputtering target for forming a W-Ti film as a diffusion preventing layer for preventing diffusion of elements between each other, for example, between a bump used for mounting a semiconductor element and a base electrode.
本案係以2014年10月8日在日本申請的特願2014-207343號為基礎,主張優先權,在此援用其內容。 This case is based on the Japanese Patent Application No. 2014-207343 filed on October 8, 2014 in Japan, and claims priority.
以往,於基板上安裝半導體晶片時,例如在Al電極或Cu電極之上形成Au凸塊或焊接凸塊等。 Conventionally, when a semiconductor wafer is mounted on a substrate, for example, Au bumps or solder bumps are formed on the Al electrode or the Cu electrode.
於此,例如當Al電極與Au凸塊直接接觸時,Al與Au互相地擴散,會形成Al與Au的金屬間化合物,有電阻上升或密著性降低之虞。又。例如當Cu電極與焊接凸塊直接接觸時,Cu與焊料中的Sn互相擴散,會形成Cu與Sn的金屬間化合物,有電阻上升或密著性降低之虞。 Here, for example, when the Al electrode is in direct contact with the Au bump, Al and Au diffuse into each other, and an intermetallic compound of Al and Au is formed, which may cause an increase in resistance or a decrease in adhesion. also. For example, when the Cu electrode is in direct contact with the solder bump, Cu and the Sn in the solder mutually diffuse, and an intermetallic compound of Cu and Sn is formed, which may cause an increase in resistance or a decrease in adhesion.
因此,例如使用專利文獻1、2中揭示的W-Ti濺鍍靶,形成W-Ti膜作為在基底電極與凸塊之間防止互相的元素之擴散的擴散防止層。 Therefore, for example, using the W-Ti sputtering target disclosed in Patent Documents 1 and 2, a W-Ti film is formed as a diffusion preventing layer that prevents diffusion of elements between the base electrode and the bump.
再者,專利文獻1、2中記載的W-Ti濺鍍靶係各自藉由粉末燒結法製造。 Further, the W-Ti sputtering target systems described in Patent Documents 1 and 2 are each produced by a powder sintering method.
於此,在基底電極及凸塊之間形成W-Ti膜作為擴散防止層時,在基底電極的全面上形成W-Ti膜後,形成凸塊,以蝕刻去除未形成凸塊的區域之W-Ti膜。然而,此W-Ti膜由於蝕刻速率非常慢,有生產效率差之問題。 Here, when a W-Ti film is formed as a diffusion preventing layer between the base electrode and the bump, after the W-Ti film is formed on the entire surface of the base electrode, a bump is formed to etch away the region where the bump is not formed. -Ti film. However, this W-Ti film has a problem of poor productivity due to the very slow etching rate.
因此,專利文獻3中揭示藉由使用微量添加有Fe的W-Ti濺鍍靶,而使所成膜的W-Ti膜中含有Fe,可改善蝕刻速率。 Therefore, Patent Document 3 discloses that the etching rate can be improved by using a W-Ti sputtering target to which Fe is added in a small amount to form Fe in the formed W-Ti film.
[專利文獻1]日本發明專利第2606946號公報 [Patent Document 1] Japanese Patent No. 2606946
[專利文獻2]特開平05-295531號公報 [Patent Document 2] Japanese Patent Publication No. 05-295531
[專利文獻3]日本發明專利第4747368號公報 [Patent Document 3] Japanese Invention Patent No. 4747368
可是如上述,藉由在W-Ti膜中微量添加Fe,改善其蝕刻速率,但於W-Ti膜中有Fe濃度發生偏差之情況,於W-Ti膜內蝕刻速率會局部地變化,有無法進行均勻的蝕刻之虞。 However, as described above, by slightly adding Fe in the W-Ti film, the etching rate is improved, but in the case where the Fe concentration in the W-Ti film is deviated, the etching rate in the W-Ti film is locally changed, and Uniform etching is not possible.
因此,希望一種W-Ti濺鍍靶,其能形成Fe濃度的偏差小且蝕刻速率均勻的W-Ti膜。 Therefore, a W-Ti sputtering target is desired which is capable of forming a W-Ti film having a small variation in Fe concentration and a uniform etching rate.
本發明係鑒於前述情事而完成者,目的在於提供一種 W-Ti濺鍍靶,其能形成Fe濃度的偏差小且蝕刻速率均勻的W-Ti膜。 The present invention has been accomplished in view of the foregoing, and aims to provide a A W-Ti sputtering target capable of forming a W-Ti film having a small variation in Fe concentration and a uniform etching rate.
為了解決上述問題,本發明之一態樣的W-Ti濺鍍靶係具有組成為:以5質量%以上20質量%以下之範圍內含有Ti,以25質量ppm以上100質量ppm以下之範圍內含有Fe,剩餘部分由W及無可避免的雜質所構成,其特徵為:在靶面內的複數個地方測定Fe濃度,當所測定的Fe濃度之最大值為Femax,Fe濃度的最小值為Femin時,滿足(Femax-Femin)/(Femax+Femin)≦0.25之關係式。 In order to solve the above problems, a W-Ti sputtering target system according to an aspect of the present invention has a composition in which Ti is contained in a range of 5 mass% or more and 20 mass% or less, and is in a range of 25 mass ppm or more and 100 mass ppm or less. Containing Fe, the remainder consists of W and inevitable impurities. It is characterized by measuring Fe concentration in a plurality of places in the target surface. When the measured Fe concentration is the maximum value of Fe max and Fe concentration When Fe min is satisfied, the relationship of (Fe max -Fe min )/(Fe max +Fe min )≦0.25 is satisfied.
於如此構成的本發明之W-Ti濺鍍靶中,由於以25質量ppm以上100質量ppm以下之範圍內含有Fe,可改善所成膜的W-Ti膜之蝕刻速率。 In the W-Ti sputtering target of the present invention thus constituted, since Fe is contained in a range of 25 ppm by mass or more and 100 ppm by mass or less, the etching rate of the film-formed W-Ti film can be improved.
而且,在靶面內的複數個地方測定Fe濃度,由於所測定的Fe濃度之最大值(Femax)與Fe濃度之最小值(Femin)滿足上述之關係式,可抑制靶面內的Fe濃度之偏差。因此,可形成Fe濃度的偏差小且蝕刻速率均勻的W-Ti膜。 Further, the Fe concentration is measured in a plurality of places in the target surface, and since the maximum value (Fe max ) of the measured Fe concentration and the minimum value (Fe min ) of the Fe concentration satisfy the above relationship, the Fe in the target surface can be suppressed. The deviation of the concentration. Therefore, a W-Ti film having a small variation in Fe concentration and a uniform etching rate can be formed.
如以上,依照本發明,可提供一種W-Ti濺鍍靶,其能形成Fe濃度的偏差小且蝕刻速率均勻的W-Ti膜。 As described above, according to the present invention, it is possible to provide a W-Ti sputtering target which can form a W-Ti film having a small variation in Fe concentration and a uniform etching rate.
圖1係顯示本發明之一實施形態的W-Ti濺鍍靶之製造方法的流程圖。 Fig. 1 is a flow chart showing a method of manufacturing a W-Ti sputtering target according to an embodiment of the present invention.
圖2係顯示靶面成為圓形的W-Ti濺鍍靶之靶面中的Fe濃度之測定位置的說明圖。 Fig. 2 is an explanatory view showing a measurement position of a Fe concentration in a target surface of a W-Ti sputtering target having a circular target surface.
圖3係顯示靶面成為矩形的W-Ti濺鍍靶之靶面中的Fe濃度之測定位置的說明圖。 Fig. 3 is an explanatory view showing a measurement position of a Fe concentration in a target surface of a W-Ti sputtering target having a rectangular target surface.
圖4係說明實施例中,測定基板上所成膜之W-Ti膜的蝕刻速率之地方的說明圖。 Fig. 4 is an explanatory view showing a place where the etching rate of the W-Ti film formed on the substrate is measured in the embodiment.
以下,參照所附的圖面來說明本發明之實施形態的W-Ti濺鍍靶。 Hereinafter, a W-Ti sputtering target according to an embodiment of the present invention will be described with reference to the accompanying drawings.
本實施形態之W-Ti濺鍍靶,例如係用於為了將液晶驅動IC接合於COF捲帶,在液晶驅動IC上所形成的Au凸塊與Al墊部(基底電極)之間,藉由濺鍍W-Ti膜作為擴散防止層而成膜之際。 The W-Ti sputtering target of the present embodiment is used, for example, for bonding a liquid crystal driver IC to a COF tape, between the Au bump formed on the liquid crystal driver IC and the Al pad portion (base electrode). The W-Ti film is sputtered as a diffusion preventing layer to form a film.
本實施形態之W-Ti濺鍍靶具有組成為:以5質量%以上20質量%以下之範圍內含有Ti,以25質量ppm以上100質量ppm以下之範圍內含有Fe,剩餘部分由W及無 可避免的雜質所構成。 The W-Ti sputtering target of the present embodiment has a composition containing Ti in a range of 5 mass% or more and 20 mass% or less, Fe in a range of 25 mass ppm or more and 100 mass ppm or less, and the remainder being W and none. It can be avoided by impurities that can be avoided.
而且,在靶面內的複數個地方測定Fe濃度,當所測定的Fe濃度之最大值為Femax,Fe濃度的最小值為Femin時,滿足(Femax-Femin)/(Femax+Femin)≦0.25之關係式。 Moreover, the Fe concentration is measured at a plurality of places in the target surface, and when the maximum Fe concentration measured is Fe max and the minimum Fe concentration is Fe min , (Fe max -Fe min )/(Fe max + is satisfied). Fe min ) ≦ 0.25 relationship.
說明如上述規定成分組成之理由。 Explain the reason for the composition of the components specified above.
W-Ti濺鍍靶中的Ti含量未達5質量%時,所成膜的W-Ti膜與基底電極之密著性有降低之虞。另一方面,W-Ti濺鍍靶中的Ti含量超過20質量%時,所成膜的W-Ti膜之電阻會上升,同時有所成膜的W-Ti膜無法充分防止構成凸塊的元素(本實施形態中為Au)與構成基底電極的元素(本實施形態中的Al)之互相擴散之虞。 When the Ti content in the W-Ti sputtering target is less than 5% by mass, the adhesion between the formed W-Ti film and the base electrode is lowered. On the other hand, when the Ti content in the W-Ti sputtering target exceeds 20% by mass, the electric resistance of the film-formed W-Ti film rises, and the film-formed W-Ti film cannot sufficiently prevent the formation of the bump. The element (in the present embodiment, Au) and the element constituting the base electrode (Al in the present embodiment) are mutually diffused.
因此,於本實施形態中,將W-Ti濺鍍靶中的Ti之含量規定為5質量%以上20質量%以下之範圍內。 Therefore, in the present embodiment, the content of Ti in the W-Ti sputtering target is set to be in the range of 5 mass% or more and 20 mass% or less.
再者,Ti之含量的下限較佳為7質量%以上,更佳為9質量%以上。又,Ti之含量的上限較佳為15質量%以下,更佳為13質量%以下。 Further, the lower limit of the content of Ti is preferably 7% by mass or more, and more preferably 9% by mass or more. Further, the upper limit of the content of Ti is preferably 15% by mass or less, and more preferably 13% by mass or less.
W-Ti濺鍍靶中的Fe之含量未達25質量ppm時,有無法充分改善所成膜的W-Ti膜之蝕刻速率善之虞。另一 方面,W-Ti濺鍍靶中的Fe之含量超過100質量ppm時,有所成膜的W-Ti膜無法充分防止構成凸塊的元素(本實施形態中為Au)與構成基底電極的元素(本實施形態中的Al)之互相擴散之虞。 When the content of Fe in the W-Ti sputtering target is less than 25 ppm by mass, the etching rate of the W-Ti film to be formed may not be sufficiently improved. another When the content of Fe in the W-Ti sputtering target exceeds 100 ppm by mass, the film-formed W-Ti film cannot sufficiently prevent the elements constituting the bump (in the present embodiment, Au) and the elements constituting the base electrode. (Al in the present embodiment) is mutually diffused.
因此,於本實施形態中,將W-Ti濺鍍靶中的Fe之含量規定為25質量ppm以上100質量ppm以下之範圍內。 Therefore, in the present embodiment, the content of Fe in the W-Ti sputtering target is set to be in the range of 25 ppm by mass or more and 100 ppm by mass or less.
再者,Fe之含量的下限較佳為30質量ppm以上,更佳為35質量ppm以上。又,Fe之含量的上限較佳為75質量ppm以下,更佳為50質量ppm以下。 Further, the lower limit of the content of Fe is preferably 30 ppm by mass or more, and more preferably 35 ppm by mass or more. Further, the upper limit of the content of Fe is preferably 75 ppm by mass or less, more preferably 50 ppm by mass or less.
(Femax-Femin)/(Femax+Femin)≦0.25 (Fe max -Fe min )/(Fe max +Fe min )≦0.25
使用本實施形態中的W-Ti濺鍍靶來形成W-Ti膜時,W-Ti濺鍍靶的靶面之全體彈飛各自的原子而成膜。 When the W-Ti film is formed using the W-Ti sputtering target in the present embodiment, the entire surface of the target surface of the W-Ti sputtering target is formed into a film.
於此,在靶面內的複數個地方測定Fe濃度,所測定的Fe濃度之最大值(Femax)與Fe濃度之最小值(Femin)滿足上述之關係式時,靶面內的Fe濃度之偏差變小。因此,於使用此W-Ti濺鍍靶所成膜的W-Ti膜中,Fe濃度之偏差亦變小,蝕刻速率變均勻。 Here, the Fe concentration is measured at a plurality of places in the target surface, and the Fe concentration in the target surface is determined when the maximum value (Fe max ) of the measured Fe concentration and the minimum value (Fe min ) of the Fe concentration satisfy the above relationship. The deviation becomes smaller. Therefore, in the W-Ti film formed by using this W-Ti sputtering target, the variation in Fe concentration also becomes small, and the etching rate becomes uniform.
再者,(Femax-Femin)/(Femax+Femin)較佳為0.2以下,更佳為0.15以下。而且,(Femax-Femin)/(Femax+Femin)愈低愈佳,但使(Femax-Femin)/(Femax+Femin)極度降低者係招致成本的增加,因此(Femax-Femin)/(Femax+Femin)可為0.005以上。 Further, (Fe max -Fe min ) / (Fe max +Fe min ) is preferably 0.2 or less, more preferably 0.15 or less. Moreover, the lower the (Fe max -Fe min ) / (Fe max +Fe min ), the better, but the extreme decrease of (Fe max -Fe min ) / (Fe max +Fe min ) leads to an increase in cost, therefore ( Fe max -Fe min )/(Fe max +Fe min ) may be 0.005 or more.
於此,在本實施形態中,當W-Ti濺鍍靶的靶面為圓形時,如圖2中所示,在圓之中心(1)及通過圓之中心 同時互相正交的2條直線上之外周部分(2)、(3)、(4)、(5)的5點,測定Fe濃度,求得上述的Fe濃度之最大值(Femax)與Fe濃度之最小值(Femin)。外周部分(2)、(3)、(4)、(5)例如可為自靶的周緣起到中心側約10mm之位置。 Here, in the present embodiment, when the target surface of the W-Ti sputtering target is circular, as shown in FIG. 2, two strips are mutually orthogonal at the center of the circle (1) and the center of the circle. The concentration of Fe was measured at five points of the outer peripheral portions (2), (3), (4), and (5) on the straight line, and the maximum value (Fe max ) of the above Fe concentration and the minimum value of Fe concentration (Fe min) were obtained. ). The outer peripheral portions (2), (3), (4), and (5) may be, for example, a position from the periphery of the target to a center side of about 10 mm.
又,當W-Ti濺鍍靶的靶面為矩形時,如圖3中所示,在對角線交叉的交點(1)與各對角線上之角部(2)、(3)、(4)、(5)的5點,測定Fe濃度,求得上述的Fe濃度之最大值(Femax)與Fe濃度之最小值(Femin)。角部(2)、(3)、(4)、(5)例如可為自頂點起到交點側約10mm之位置。 Further, when the target surface of the W-Ti sputtering target is rectangular, as shown in FIG. 3, the intersection (1) at the diagonal crossing and the corner portions (2), (3), (on each diagonal line) At 5 points of 4) and (5), the Fe concentration was measured, and the maximum value (Fe max ) of the above Fe concentration and the minimum value (Fe min ) of the Fe concentration were obtained. The corner portions (2), (3), (4), and (5) may be, for example, positions from the vertex to the intersection side of about 10 mm.
Fe濃度的測定地方之數目亦可為5點以上20點以下。當時,測定地方係可為靶中心點與自通過其中心的直線與靶外周緣之交點起往中心側約10mm之點。 The number of places where the Fe concentration is measured may be 5 or more and 20 or less. At that time, the measurement local system may be a point where the target center point is about 10 mm from the intersection of the straight line passing through the center and the outer periphery of the target toward the center side.
其次,參照圖1之流程圖說明製造本實施形態之W-Ti濺鍍靶的一實施形態。 Next, an embodiment in which the W-Ti sputtering target of the present embodiment is manufactured will be described with reference to a flowchart of Fig. 1.
本實施形態之W-Ti濺鍍靶的製造方法係如圖1中所示,具備:將經指定的配合量所配合的原料粉予以混合粉碎之混合粉碎步驟S01,與經混合粉碎的原料粉予以加熱而使燒結之燒結步驟S02,與加工所得的燒結體之加工步驟S03。 As shown in Fig. 1, the method for producing a W-Ti sputtering target according to the present embodiment includes a mixing and pulverizing step S01 in which a raw material powder blended with a predetermined blending amount is mixed and pulverized, and a mixed pulverized raw material powder. The sintering step S02 is performed by heating, and the processing step S03 of the sintered body obtained by the processing.
首先,準備Ti粉末、W粉末及Fe粉末作為原料粉。於此,作為Ti粉末,較佳使用純度為99.999質量%以上、平均粒徑為1μm以上40μm以下者。又,作為W粉 末,較佳使用純度為99.999質量%以上、平均粒徑為0.5μm以上20μm以下者。再者,作為Fe粉末,較佳使用純度為99.999質量%以上、平均粒徑為75μm以上150μm以下者。 First, Ti powder, W powder, and Fe powder were prepared as raw material powders. Here, as the Ti powder, a purity of 99.999 mass% or more and an average particle diameter of 1 μm or more and 40 μm or less are preferably used. Also, as W powder At the end, it is preferred to use a purity of 99.999 mass% or more and an average particle diameter of 0.5 μm or more and 20 μm or less. Further, as the Fe powder, those having a purity of 99.999 mass% or more and an average particle diameter of 75 μm or more and 150 μm or less are preferably used.
秤量此等原料粉,使成為以5質量%以上20質量%以下之範圍內含有Ti,以25質量ppm以上100質量ppm以下之範圍內含有Fe,剩餘部分由W及無可避免的雜質所構成之組成,同時將此原料粉予以混合粉碎。於本實施形態中,藉由球磨機來混合所秤量的原料粉,更且使用超硬合金製的球,藉由磨碎裝置進行混合粉碎。 When the raw material powder is weighed, Ti is contained in a range of 5 mass% or more and 20 mass% or less, Fe is contained in a range of 25 mass ppm or more and 100 mass ppm or less, and the remainder is composed of W and inevitable impurities. The composition is simultaneously mixed and pulverized. In the present embodiment, the weighed raw material powder is mixed by a ball mill, and a ball made of a cemented carbide is used, and the mixture is pulverized by a grinding device.
藉由此混合粉碎步驟S01,Fe粉末係被粉碎至平均粒徑成為10μm以下。 By this mixing pulverization step S01, the Fe powder is pulverized until the average particle diameter becomes 10 μm or less.
其次,將如上述經混合粉碎的原料粉(混合粉),在真空或惰性氣體環境中或還原環境中進行燒結。於此燒結步驟S02中,經粉碎到平均粒徑為10μm以下的Fe粉末係在W中均勻擴散。 Next, the raw material powder (mixed powder) which has been mixed and pulverized as described above is sintered in a vacuum or an inert gas atmosphere or a reducing atmosphere. In the sintering step S02, the Fe powder which has been pulverized to have an average particle diameter of 10 μm or less is uniformly diffused in W.
於此,燒結步驟中的燒結溫度較佳為按照所製造的W-Ti合金之熔點Tm來設定。 Here, the sintering temperature in the sintering step is preferably set in accordance with the melting point Tm of the W-Ti alloy to be produced.
於此燒結步驟S02中,作為燒結方法,可採用常壓燒結、熱壓、熱靜水壓加壓。 In the sintering step S02, as the sintering method, normal pressure sintering, hot pressing, or hot hydrostatic pressure pressing may be employed.
於本實施形態中,將原料粉(混合粉)填充於石墨製模具中,藉由壓力為10MPa以上60MPa以下、溫度為1000C以上1500℃的真空熱壓,進行燒結。 In the present embodiment, the raw material powder (mixed powder) is filled in a graphite mold, and is sintered by a vacuum hot pressing at a pressure of 10 MPa or more and 60 MPa or less and a temperature of 1000 C or more and 1500 ° C.
藉由對於燒結步驟S02所得之燒結體,施予切削加工或研削加工,而加工成指定形狀的濺鍍靶。 The sintered body obtained in the sintering step S02 is subjected to a cutting process or a grinding process to be processed into a sputtering target of a predetermined shape.
藉由如以上之步驟,製造本實施形態之W-Ti濺鍍靶。此W-Ti濺鍍靶係以In作為焊料,接合於由Cu或SUS(不銹鋼)或其他金屬(例如Mo)所成之背板。 The W-Ti sputtering target of this embodiment was produced by the above steps. This W-Ti sputtering target is bonded to a back sheet made of Cu or SUS (stainless steel) or other metal (for example, Mo) using In as a solder.
藉由如以上構成之本實施形態的W-Ti濺鍍靶,由於以25質量ppm以上100質量ppm以下之範圍內含有Fe,可改善所成膜的W-Ti膜之蝕刻速率。 According to the W-Ti sputtering target of the present embodiment configured as described above, since Fe is contained in a range of 25 ppm by mass or more and 100 ppm by mass or less, the etching rate of the W-Ti film formed can be improved.
然後,在靶面內的複數個地方測定Fe濃度,由於所測定的Fe濃度之最大值(Femax)與Fe濃度之最小值(Femin)滿足(Femax-Femin)/(Femax+Femin)≦0.25之關係式,而抑制靶面內的Fe濃度之偏差。因此,可形成Fe濃度之偏差小且蝕刻速率均勻的W-Ti膜。 Then, the Fe concentration is measured at a plurality of places in the target surface, and the maximum value (Fe max ) of the measured Fe concentration and the minimum Fe concentration (Fe min ) satisfy (Fe max -Fe min ) / (Fe max + Fe min ) ≦ 0.25 relationship, and suppress the deviation of Fe concentration in the target surface. Therefore, a W-Ti film having a small variation in Fe concentration and a uniform etching rate can be formed.
又,於本實施形態中,藉由混合粉碎Ti粉末、W粉末及Fe粉末,由於燒結前的Fe粉末之粒徑成為10μm以下,在燒結時,可使Fe粒子均勻地擴散於成為母相的W中,可使Fe均勻地分布於燒結體全體中。燒結前的Fe粉末之粒徑較佳為5μm以下,更佳為2μm以下,惟不受此 所限定。另外,燒結前的Fe粉末之粒徑係愈小愈佳,但若使燒結前的Fe粉末之粒徑極度地降低,則招致成本的增加。因此,燒結前的Fe粉末之粒徑可為0.1μm以上。 In addition, in the present embodiment, the Ti powder, the W powder, and the Fe powder are mixed and pulverized, and the Fe powder before sintering has a particle diameter of 10 μm or less, so that Fe particles can be uniformly diffused in the mother phase during sintering. In W, Fe can be uniformly distributed throughout the sintered body. The particle diameter of the Fe powder before sintering is preferably 5 μm or less, more preferably 2 μm or less, but is not affected by this. Limited. Further, the smaller the particle diameter of the Fe powder before sintering, the better, but if the particle diameter of the Fe powder before sintering is extremely lowered, the cost is increased. Therefore, the particle diameter of the Fe powder before sintering can be 0.1 μm or more.
再者,直接使用含有全體之50%以上的50μm以下之粒子的微細Fe粉末時,必須作為危險物操作,但於本實施形態中,藉由將平均粒徑為75μm以上150μm以下的Fe粉末與其他的原料粉(Ti粉末、W粉末)一起混合粉碎而使粒徑成為10μm以下,更且由於Fe粉末之比率為充分低,操作變容易。 In addition, when a fine Fe powder containing 50% or more of the entire particles of 50 μm or less is used as it is, it is necessary to operate as a dangerous substance. However, in the present embodiment, Fe powder having an average particle diameter of 75 μm or more and 150 μm or less is used. The other raw material powders (Ti powder and W powder) are mixed and pulverized to have a particle diameter of 10 μm or less, and the ratio of the Fe powder is sufficiently low, and the handling becomes easy.
以上,說明本發明之實施形態,惟本發明不受此所限定,在不脫離本發明之技術思想的範圍內可適宜變更。 The embodiment of the present invention has been described above, but the present invention is not limited thereto, and can be appropriately modified without departing from the scope of the present invention.
例如,於本實施形態中,說明使用磨碎裝置將用原料粉予以混合粉碎者,惟不受此所限定,亦可藉由其他的方法將原料粉予以混合粉碎。 For example, in the present embodiment, the raw material powder may be mixed and pulverized by using a grinding device, but the raw material powder may be mixed and pulverized by another method.
再者,將原料粉予以混合粉碎之方法,可舉出行星球磨機、振動球磨機等。 Further, a method of mixing and pulverizing the raw material powder includes a planetary ball mill, a vibration ball mill, and the like.
作為W-Ti濺鍍靶中之無可避免的雜質,可舉出Na、K、Ca、Ni、Cr、Mn等。此等之無可避免的雜質係合計較佳為0.01質量%以下,惟不受此所限定。 Examples of the inevitable impurities in the W-Ti sputtering target include Na, K, Ca, Ni, Cr, Mn, and the like. The total of these unavoidable impurities is preferably 0.01% by mass or less, but is not limited thereto.
以下,說明對於本發明之W-Ti濺鍍靶的作用效果所評價之評價試驗的結果。 Hereinafter, the results of an evaluation test evaluated for the effects of the W-Ti sputtering target of the present invention will be described.
作為原料粉末,準備純度為99.999質量%且平均粒徑為15μm的Ti粉末、純度為99.999質量%且平均粒徑為1μm的W粉末、純度為99.999質量%且平均粒徑為100μm的Fe粉末,以成為表1所示的組成之方式,秤量Ti粉末、Fe粉末及W粉末。 As the raw material powder, a Ti powder having a purity of 99.999 mass% and an average particle diameter of 15 μm, a W powder having a purity of 99.999 mass% and an average particle diameter of 1 μm, and an Fe powder having a purity of 99.999 mass% and an average particle diameter of 100 μm were prepared. The Ti powder, the Fe powder, and the W powder were weighed in such a manner as to have the composition shown in Table 1.
於所秤量的Ti粉末、Fe粉末及W粉末之中,將W粉末與Fe粉末與直徑約5mm的超硬合金製球一起投入磨碎裝置(NIPPON COKE工業股份有限公司MA1D)中,於旋轉數300ppm之條件下在Ar環境下實施1小時的混合粉碎。再者,於此磨碎機的混合容器之內側,為了防止來自粉碎混合時的容器之雜質的混入,施予W箔的內貼。於此,超硬合金製球的投入重量為W粉末與Fe粉末之投入重量的約10倍。 Among the Ti powder, Fe powder and W powder weighed, W powder and Fe powder were placed in a grinding device (NIPPON COKE Industrial Co., Ltd. MA1D) together with a super hard alloy ball having a diameter of about 5 mm. The mixture was pulverized in an Ar environment under conditions of 300 ppm for 1 hour. Further, inside the mixing container of the attritor, in order to prevent the incorporation of impurities from the container during the pulverization and mixing, the inner layer of the W foil is applied. Here, the input weight of the superhard alloy ball is about 10 times the input weight of the W powder and the Fe powder.
藉由轉動球磨機裝置,混合經混合粉碎的W粉末及Fe粉末以及Ti粉末,而得到混合粉末。於此,用EPMA裝置觀察燒結前的混合粉末,藉由特性X射線之面分析影像來鑑定Fe粒子,確認其粒徑。表1中顯示其粒徑。所檢測的Fe粒子係皆具有未達10μm的粒徑。 The mixed powder of the W powder, the Fe powder, and the Ti powder were mixed by a rotary ball mill apparatus to obtain a mixed powder. Here, the mixed powder before sintering was observed by an EPMA apparatus, and the Fe particles were identified by analyzing the image by the characteristic X-ray surface, and the particle diameter was confirmed. The particle size is shown in Table 1. The Fe particle systems tested all had particle sizes of less than 10 μm.
將所得之混合粉末填充於石墨製模具中,於壓力:15MPa、溫度:1200℃、3小時保持之條件下,藉由真空熱壓而製作熱壓燒結體,機械加工所得之熱壓燒結體,製作具有直徑:152.4mm、厚度:6mm的本發明例之W-Ti濺鍍靶。 The obtained mixed powder was filled in a graphite mold, and a hot-pressed sintered body was produced by vacuum hot pressing under the conditions of pressure: 15 MPa, temperature: 1200 ° C, and holding for 3 hours, and the obtained hot-pressed sintered body was machined. A W-Ti sputtering target of the present invention having a diameter of 152.4 mm and a thickness of 6 mm was produced.
作為原料粉末,準備純度為99.999質量%且平均粒徑為15μm的Ti粉末、純度為99.999質量%且平均粒徑為1μm的W粉末、純度為99.999質量%且平均粒徑為100μm的Fe粉末,以成為表1所示的組成之方式,秤量Ti粉末、Fe粉末及W粉末。 As the raw material powder, a Ti powder having a purity of 99.999 mass% and an average particle diameter of 15 μm, a W powder having a purity of 99.999 mass% and an average particle diameter of 1 μm, and an Fe powder having a purity of 99.999 mass% and an average particle diameter of 100 μm were prepared. The Ti powder, the Fe powder, and the W powder were weighed in such a manner as to have the composition shown in Table 1.
藉由轉動球磨機裝置,混合所秤量的Ti粉末、Fe粉末及W粉末,而得到混合粉末。即,於比較例中,未實施原料粉的粉碎。於此,用EPMA裝置觀察燒結前的混合粉末,藉由特性X射線之面分析影像來鑑定Fe粒子,確認其粒徑。表1中顯示其粒徑。所檢測的Fe粒子係大致具有表1中所示的值作為最大值之粒徑。 The Ti powder, the Fe powder, and the W powder were weighed by rotating a ball mill apparatus to obtain a mixed powder. That is, in the comparative example, the pulverization of the raw material powder was not performed. Here, the mixed powder before sintering was observed by an EPMA apparatus, and the Fe particles were identified by analyzing the image by the characteristic X-ray surface, and the particle diameter was confirmed. The particle size is shown in Table 1. The Fe particles detected had a particle diameter substantially as shown in Table 1 as the maximum value.
將所得之混合粉末填充於石墨製模具中,於壓力:15MPa、溫度:1200℃、3小時保持之條件下,藉由真空熱壓而製作熱壓燒結體,機械加工所得之熱壓燒結體,製作具有直徑:152.4mm、厚度:6mm的比較例之W-Ti濺鍍靶。 The obtained mixed powder was filled in a graphite mold, and a hot-pressed sintered body was produced by vacuum hot pressing under the conditions of pressure: 15 MPa, temperature: 1200 ° C, and holding for 3 hours, and the obtained hot-pressed sintered body was machined. A W-Ti sputtering target of a comparative example having a diameter of 152.4 mm and a thickness of 6 mm was produced.
當所得之W-Ti濺鍍靶的靶面為圓形(圓型靶)時,如圖2所示,自圓之中心(1)與通過中心且互相正交的2條直線上之外周起約10mm的位置(2)、(3)、(4)、(5)之5點,使用超硬合金製的鑽頭來採集組成 分析用的試料。 When the target surface of the obtained W-Ti sputtering target is a circular (circular target), as shown in FIG. 2, the center of the circle (1) and the two straight lines passing through the center and orthogonal to each other At a position of about 10 mm (2), (3), (4), (5), using a bit made of a superhard alloy to collect the composition Samples for analysis.
又,當所得之W-Ti濺鍍靶的靶面為矩形(方型靶)時,如圖3所示,自對角線交叉之交點(1)與自各對角線上的角部起約10mm的位置(2)、(3)、(4)、(5)之5點,使用超硬合金製的鑽頭來採集組成分析用的試料。 Further, when the target surface of the obtained W-Ti sputtering target is a rectangular shape (square type target), as shown in FIG. 3, the intersection point (1) from the diagonal intersection and the corner portion from each diagonal line are about 10 mm. At the five points of positions (2), (3), (4), and (5), a sample for composition analysis was collected using a drill made of a cemented carbide.
藉由ICP發光分光分析法分析此等試料的Fe濃度。表2中顯示測定結果。 The Fe concentration of these samples was analyzed by ICP emission spectrometry. The measurement results are shown in Table 2.
其次,將上述的本發明例及比較例之W-Ti濺鍍靶焊接於無氧銅製的背板,將此安裝於濺鍍裝置(股份有限公司ULVAC製SIH-450H),於以下之條件下實施濺鍍成膜。 Next, the above-described examples of the invention and the W-Ti sputtering target of the comparative example were welded to a back sheet made of oxygen-free copper, and this was mounted on a sputtering apparatus (SIH-450H manufactured by ULVAC Co., Ltd.) under the following conditions. Sputtering is performed to form a film.
基板:直徑100mm的Si基板 Substrate: Si substrate with a diameter of 100 mm
到達真空度:<5×10-5Pa Reaching vacuum: <5×10 -5 Pa
基板與靶之距離:70mm Distance between substrate and target: 70mm
電力:直流600W Electricity: DC 600W
氣體壓力:Ar 1.0Pa Gas pressure: Ar 1.0Pa
基板加熱無 Substrate heating
膜厚:300nm Film thickness: 300nm
於如此所得之直徑100mm的Si基板之中,自圖4所 示的3個地方之位置切出20mm見方的試料。再者,將此試料切斷成10mm×20mm的二個部分,將經切斷的一個試料浸漬在藉由水浴設定在液溫30℃的31vol%過氧化水氫水中5分鐘。自過氧化氫中取出後,以純水充分地洗濯,更且噴吹乾燥空氣而吹掉所附著的純水之液滴,使試料乾燥。 Among the 100 mm diameter Si substrates thus obtained, from Fig. 4 A sample of 20 mm square was cut out at the position of the three places shown. Further, the sample was cut into two portions of 10 mm × 20 mm, and one of the cut samples was immersed in 31 vol% hydrogen peroxide water at a liquid temperature of 30 ° C for 5 minutes by a water bath. After taking out from hydrogen peroxide, the sample was sufficiently washed with pure water, and the dry air was blown off to blow off the droplets of the adhered pure water, and the sample was dried.
對於此試料之未浸漬於過氧化氫水中之側與已浸漬之側的兩者,用場發射式的掃描電子顯微鏡(FE-SEM:股份有限公司日立高科技製SU-70)觀察剖面,測定W-Ti膜之膜厚。求得已浸漬於過氧化氫中之側與未浸漬之側的膜厚差,將此膜厚差除以浸潰時間(5分鐘),算出在直徑100mm的基板之各位置的蝕刻速率。表3中顯示其結果。 For both the side of the sample which was not immersed in the hydrogen peroxide water and the side which was immersed, the cross section was observed by a field emission type scanning electron microscope (FE-SEM: Hitachi High-Tech Co., Ltd. SU-70). The film thickness of the W-Ti film. The film thickness difference between the side immersed in hydrogen peroxide and the side not immersed was determined, and the film thickness difference was divided by the immersion time (5 minutes), and the etching rate at each position of the substrate having a diameter of 100 mm was calculated. The results are shown in Table 3.
於比較例1-6中,如表2所示,確認靶面內之Fe濃度的偏差變大。靶面內之Fe濃度的偏差變大者,推測係因為不進行原料粉的粉碎,使用粒徑大的Fe粒子進行燒結。 In Comparative Example 1-6, as shown in Table 2, it was confirmed that the variation in the Fe concentration in the target surface became large. When the variation in the Fe concentration in the target surface is large, it is presumed that the raw material powder is not pulverized, and Fe particles having a large particle diameter are used for sintering.
特別地,於Fe濃度低的比較例2、5中,Fe濃度係局部地變少,Fe濃度之最大差亦變大。 In particular, in Comparative Examples 2 and 5 in which the Fe concentration was low, the Fe concentration was locally small, and the maximum difference in Fe concentration was also increased.
於使用該比較例1-6的W-Ti濺鍍靶所成膜的比較例11-16之W-Ti膜中,確認蝕刻速率不均勻。 In the W-Ti film of Comparative Example 11-16 formed by using the W-Ti sputtering target of Comparative Example 1-6, it was confirmed that the etching rate was not uniform.
又,於使用Fe濃度低的比較例2、5之W-Ti濺鍍靶所成膜的比較例12、15之W-Ti膜中,確認局部地蝕刻速率變非常慢。 Further, in the W-Ti films of Comparative Examples 12 and 15 formed by using the W-Ti sputtering targets of Comparative Examples 2 and 5 having a low Fe concentration, it was confirmed that the local etching rate was extremely slow.
相對於其,於本發明例1-6中,確認靶面內之Fe濃度的偏差變小。推測係因為靶面內之Fe濃度的偏差變小,進行原料粉的混合粉碎,使用粒徑小的Fe粒子進行燒結。 With respect to this, in the inventive examples 1-6, it was confirmed that the variation in the Fe concentration in the target surface became small. It is estimated that the variation in the Fe concentration in the target surface is small, and the raw material powder is mixed and pulverized, and the Fe particles having a small particle diameter are used for sintering.
又,於Fe濃度低的本發明例2、5或Fe濃度高的本發明例3、6中,Fe濃度的偏差亦小而安定。 Further, in Examples 3 and 6 of the present invention in which the concentrations of Examples 2, 5 or Fe of the present invention having a low Fe concentration were low, the variation in Fe concentration was small and stable.
於使用此本發明例1-6之W-Ti濺鍍靶所成膜的本發明例11-16之W-Ti膜中,確認蝕刻速率均勻。 In the W-Ti film of Inventive Example 11-16 formed by using the W-Ti sputtering target of Inventive Example 1-6, it was confirmed that the etching rate was uniform.
特別地,於使用Fe濃度低的本發明例2、5之W-Ti濺鍍靶所成膜的本發明例12、15之W-Ti膜中,亦在W-Ti膜中確實地添加Fe,蝕刻速率安定。 In particular, in the W-Ti film of the inventive examples 12 and 15 formed by using the W-Ti sputtering target of the inventive examples 2 and 5 having a low Fe concentration, Fe is also surely added to the W-Ti film. The etch rate is stable.
又,於使用Fe濃度高的本發明例3、6之W-Ti濺鍍靶所成膜的本發明例13、16之W-Ti膜中,亦充分地抑制蝕刻速率的偏差。 Further, in the W-Ti films of the inventive examples 13 and 16 formed by using the W-Ti sputtering targets of the inventive examples 3 and 6 having a high Fe concentration, variations in the etching rate were sufficiently suppressed.
根據以上的確認實驗之結果,依照本發明例,確認可形成Fe濃度的偏差小且蝕刻速率均勻之W-Ti膜。 According to the results of the above confirmation experiment, it was confirmed that a W-Ti film having a small variation in Fe concentration and a uniform etching rate can be formed according to the example of the present invention.
藉由本發明之W-Ti濺鍍靶,可形成Fe濃度的偏差小且蝕刻速率均勻之W-Ti膜。本發明之W-Ti濺鍍靶例如適合於形成作為擴散防止層的W-Ti膜,該膜係在安裝半導體元件時所用的凸塊與基底電極之間,防止互相的元素之擴散。 According to the W-Ti sputtering target of the present invention, a W-Ti film having a small variation in Fe concentration and a uniform etching rate can be formed. The W-Ti sputtering target of the present invention is suitable, for example, for forming a W-Ti film as a diffusion preventing layer which prevents diffusion of elements between each other between the bumps used for mounting the semiconductor element and the substrate electrode.
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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 |
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JPH05295531A (en) * | 1992-04-21 | 1993-11-09 | Toshiba Corp | Ti-w based sputtering target and its production |
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