TW201942400A - TiW alloy target and manufacturing method thereof being used in the diffusion barrier of semiconductors - Google Patents

TiW alloy target and manufacturing method thereof being used in the diffusion barrier of semiconductors Download PDF

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TW201942400A
TW201942400A TW108100969A TW108100969A TW201942400A TW 201942400 A TW201942400 A TW 201942400A TW 108100969 A TW108100969 A TW 108100969A TW 108100969 A TW108100969 A TW 108100969A TW 201942400 A TW201942400 A TW 201942400A
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tiw alloy
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TWI684660B (en
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熊谷卓哉
十亀宏明
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日商日立金屬股份有限公司
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Abstract

The present invention provides a TiW alloy target which can simultaneously suppress the abnormal discharge during sputtering, in addition to suppressing deformation of a target during processing such as pinching or bonding, or abrasion or breakage of a wafer by a cutting tool. This TiW target contains 7 mass% to 13 mass% of Ti, and the remaining contains W and unavoidable impurities. The average value of the Vickers hardness in the sputtering surface is 550 HV to 630 HV, and the content of Ti is preferably 9 mass% to 11 mass%.

Description

TiW合金靶材及其製造方法TiW alloy target and manufacturing method thereof

本發明是有關於一種例如可用於形成半導體元件中所使用的擴散阻擋層等的TiW合金靶材及其製造方法。The present invention relates to, for example, a TiW alloy target that can be used for forming a diffusion barrier layer and the like used in a semiconductor device, and a method for manufacturing the same.

半導體元件隨著其高積體化、高密度化,在Al配線與Si基板的接觸部生成析出物的遷移(migration)成為問題,於接觸部中,有時會將包含TiW合金的薄膜形成為擴散阻擋層。並且,已知該包含TiW合金的薄膜可藉由濺鍍(sputtering)法來形成。With the increase in the density and density of semiconductor devices, migration of precipitates generated at the contact portion between the Al wiring and the Si substrate becomes a problem. In the contact portion, a thin film containing a TiW alloy may be formed as Diffusion barrier. In addition, it is known that the thin film containing a TiW alloy can be formed by a sputtering method.

濺鍍法中所使用的靶材存在當形成薄膜時產生粒子(particle)的問題,正在研究抑制其產生量的技術。關於TiW合金靶材(以下亦簡稱為「靶材」)亦同樣如此,例如,專利文獻1中,藉由具有以微組織的面積率計包含20%以上的TiW合金相、W相及Ti相的組織,且將靶材的表面粗糙度設為Rmax值為3 μm以下,而改善靶材的濺鍍面的凹凸,從而能夠抑制粒子的產生。
[現有技術文獻]
[專利文獻]
The target used in the sputtering method has a problem that particles are generated when a thin film is formed, and a technique for suppressing the amount of the particle is being studied. The same applies to a TiW alloy target (hereinafter also referred to simply as a "target"). For example, in Patent Document 1, a TiW alloy phase, a W phase, and a Ti phase are contained in an area ratio of microstructure of 20% or more. The surface roughness of the target is set to a Rmax value of 3 μm or less, and the unevenness of the sputtering surface of the target is improved, so that generation of particles can be suppressed.
[Prior Art Literature]
[Patent Literature]

[專利文獻1]日本專利特開平5-98435號公報[Patent Document 1] Japanese Patent Laid-Open No. 5-98435

[發明所欲解決之課題][Problems to be Solved by the Invention]

根據本發明者的研究而確認到:若如專利文獻1中所揭示般,將W粉末與氫化的Ti粉末混合、粉碎,於脫氫後以熱均壓(hot isostatic pressing)(以下稱為「HIP」)進行加壓燒結來製作靶材,則有時會在該靶材中存在低硬度的部位,於夾持(chucking)或接合(bonding)等處理中,存在靶材本體變形的情況。According to research by the present inventors, it has been confirmed that if W powder and hydrogenated Ti powder are mixed and pulverized as disclosed in Patent Document 1, after dehydrogenation, hot isostatic pressing (hereinafter referred to as " HIP ") to produce a target by pressure sintering, there may be low hardness parts in the target, and the target body may be deformed during processing such as chucking or bonding.

TiW合金為機械加工時產生破裂或缺損的可能性高的所謂的難磨削材料,而且,若靶材中存在高硬度或低硬度的部位,則會導致切削工具對晶片的磨耗或破損,有時所獲得的靶材的表面粗糙度變大、或視情況而使靶材本體破損。
另外,若於靶材的濺鍍面中的中央部的侵蝕區域存在例如包括純Ti相或純W相等的低硬度的部位,則僅低硬度的部位殘存或脫落,由此,侵蝕區域的表面粗糙度變粗,容易引發濺鍍時的異常放電。
TiW alloy is a so-called hard-to-grind material that is highly likely to be cracked or chipped during machining. In addition, if there are high or low hardness parts in the target, it will cause wear or damage to the wafer by the cutting tool. The surface roughness of the target obtained at this time becomes large, or the target body is damaged, as the case may be.
In addition, if there is a low-hardness portion including, for example, pure Ti phase or pure W, in the eroded area in the center portion of the sputtering surface of the target, only the low-hardness portion remains or falls off, and thus the surface of the eroded area The roughness becomes rough, which may cause abnormal discharge during sputtering.

本發明的目的在於提供一種除抑制夾持或接合等處理中靶材的變形、或者切削工具對晶片的磨耗或破損以外,亦可同時達成濺鍍時異常放電的抑制的TiW合金靶材。
[解決課題之手段]
An object of the present invention is to provide a TiW alloy target that can suppress the deformation of a target during processing such as clamping or bonding, or the abrasion or damage of a wafer by a cutting tool, and can also suppress abnormal discharge during sputtering.
[Means for solving problems]

本發明的TiW合金靶材含有7質量%~13質量%的Ti,且剩餘部分包含W及不可避免的雜質,濺鍍面中維氏硬度(Vickers hardness)的平均值為550 HV~630 HV。
本發明的靶材更佳為Ti的含量為9質量%~11質量%。
並且,本發明的靶材更佳為所述維氏硬度的平均值為602 HV~620 HV。
The TiW alloy target material of the present invention contains 7 mass% to 13 mass% of Ti, and the remaining portion contains W and unavoidable impurities. The average value of Vickers hardness in the sputtered surface is 550 HV to 630 HV.
In the target of the present invention, the Ti content is more preferably 9% by mass to 11% by mass.
In addition, the target of the present invention is more preferably such that the average value of the Vickers hardness is 602 HV to 620 HV.

本發明的TiW合金靶材可藉由如下製造方法而獲得,所述製造方法包括:
以含有7質量%~13質量%的Ti、且剩餘部分為W及不可避免的雜質的方式,將Ti粉末與W粉末混合而獲得混合粉末的步驟;
對所述混合粉末進行加壓而獲得成形體的步驟;
於將所述成形體粉碎後過篩而獲得不足1.5 mm的粉碎粉末的步驟;以及
於燒結溫度為1500℃~1600℃、加壓力為20 MPa~40 MPa、保持時間為1小時~10小時的條件下對所述粉碎粉末進行加壓燒結而獲得TiW合金燒結體的步驟。
[發明的效果]
The TiW alloy target of the present invention can be obtained by the following manufacturing method, which includes:
A step of mixing a Ti powder with a W powder to obtain a mixed powder in a manner that contains 7 to 13% by mass of Ti and the remaining portion is W and unavoidable impurities;
A step of pressing the mixed powder to obtain a shaped body;
A step of pulverizing the formed body and sieving to obtain a pulverized powder of less than 1.5 mm; and a sintering temperature of 1500 ° C to 1600 ° C, a pressure of 20 MPa to 40 MPa, and a holding time of 1 to 10 hours A step of sintering the pulverized powder under pressure to obtain a TiW alloy sintered body.
[Effect of the invention]

本發明可提供一種除抑制夾持或接合等處理中靶材的變形、或者切削工具對晶片的磨耗或破損以外,亦可同時達成濺鍍時異常放電的抑制的靶材。因此,對於以上所述的例如半導體元件的Al配線與Si基板的擴散阻擋層的形成而言,為有用的技術。The present invention can provide a target which can suppress the abnormal discharge during sputtering, in addition to suppressing deformation of the target during processing such as clamping or bonding, or abrasion or damage of a wafer by a cutting tool. Therefore, it is a useful technique for forming, for example, the Al wiring of the semiconductor element and the formation of the diffusion barrier layer of the Si substrate as described above.

本發明的靶材具有以下特徵,即,濺鍍面中,由日本工業標準(Japanese Industrial Standards,JIS)Z 2244所規定的維氏硬度的平均值處於550 HV~630 HV的範圍。以下,亦將「濺鍍面的維氏硬度」簡稱為「維氏硬度」。
本發明的靶材藉由將維氏硬度的平均值設為550 HV以上,而可在機械加工中的夾持或接合等處理中抑制靶材本體的變形。
The target of the present invention has a feature that the average value of the Vickers hardness specified by Japanese Industrial Standards (JIS) Z 2244 is in a range of 550 HV to 630 HV in the sputtered surface. Hereinafter, the "Vickers hardness of the sputtered surface" is also simply referred to as "Vickers hardness".
By setting the average value of the Vickers hardness of the target of the present invention to 550 HV or more, it is possible to suppress deformation of the target body during processing such as clamping or joining during machining.

另外,本發明的靶材藉由將維氏硬度的平均值設為550 HV以上,例如可抑制於銑床或車床等的晶片中生成刃口積屑緣(built-up edge)。即,本發明的靶材可抑制隨著切削加工的進行而晶片的切入量逐漸變大,可減小切削開始時與切削結束時靶材的尺寸差,此外亦可抑制伴隨刃口積屑緣的剝離而使晶片破損。In addition, by setting the average value of the Vickers hardness of the target of the present invention to 550 HV or more, it is possible to suppress generation of a built-up edge in a wafer such as a milling machine or a lathe. In other words, the target material of the present invention can prevent the chipping amount of the wafer from gradually increasing with the progress of the cutting process, can reduce the difference in the size of the target material at the start of cutting and the end of cutting, and can also suppress the chip edge accompanying the cutting edge. The wafer is broken and the wafer is damaged.

另一方面,若於靶材的濺鍍面中的中央部的侵蝕區域存在例如包括純Ti相或純W相等的柔軟部位,則有時僅低硬度的部位殘存或脫落,靶材中,其侵蝕區域的表面粗糙度變粗,容易引發濺鍍時的異常放電。因此,本發明的靶材將維氏硬度的平均值設為550 HV以上。另外,就與以上相同的理由而言,本發明的實施形態的靶材較佳為將維氏硬度的平均值設為602 HV以上。On the other hand, if there is a soft part including, for example, pure Ti phase or pure W, in the erosion area in the center of the sputtering surface of the target, only a low-hardness part may remain or fall off. The surface roughness of the eroded area becomes coarse, which easily causes abnormal discharge during sputtering. Therefore, the target of the present invention has an average value of Vickers hardness of 550 HV or more. In addition, for the same reason as above, it is preferable that the target of the embodiment of the present invention has an average value of Vickers hardness of 602 HV or more.

本發明的靶材藉由將維氏硬度的平均值設為630 HV以下,例如可抑制銑床或車床等對晶片的磨耗量。即,本發明的靶材中,隨著切削加工的進行而晶片的切入量逐漸變小,可抑制切削開始時與切削結束時靶材的尺寸差變大,此外亦可抑制晶片的破損。
另外,本發明的靶材藉由將維氏硬度的平均值設為630 HV以下,可在夾持於切削機械、以及接合於背板(backing plate)或背管(backing tube)時的處理等中抑制靶材本體的破損。並且,就與所述相同的理由而言,本發明的實施形態的靶材較佳為將維氏硬度的平均值設為620 HV以下。
By setting the average value of the Vickers hardness of the target of the present invention to 630 HV or less, for example, the amount of wear on the wafer by a milling machine or a lathe can be suppressed. That is, in the target material of the present invention, the cutting amount of the wafer gradually decreases with the progress of the cutting process, it is possible to suppress a large difference in the size of the target material at the start of cutting and the end of cutting, and it is also possible to suppress damage to the wafer.
In addition, the target of the present invention has an average value of Vickers hardness of 630 HV or less, and can be handled while being clamped in a cutting machine and bonded to a backing plate or a backing tube. It suppresses damage to the target body. In addition, for the same reason as described above, it is preferable that the target of the embodiment of the present invention has an average value of Vickers hardness of 620 HV or less.

就以上所述的除抑制靶材的變形、或者切削工具對晶片的磨耗或破損以外,亦抑制濺鍍時的異常放電的觀點而言,本發明中所謂的維氏硬度是指靶材的濺鍍面中在任意三個部位所測定的維氏硬度的平均值處於550 HV~630 HV的範圍。
另外,本發明的靶材較佳為具有包含維氏硬度的平均值處於550 HV~630 HV的範圍的TiW合金的組織。並且,就將維氏硬度的平均值設為602 HV~620 HV的觀點而言,本發明的實施形態的靶材較佳為濺鍍面中無Ti相及W相,即,Ti相及W相的面積率為0面積%。此外,本發明的面積%是指測定由使用場發射型電子探針顯微分析儀(field emission-electron probe microanalyzer,FE-EPMA)的色彩映射(color mapping)所獲得的各元素所佔的濃度分佈而得出的值。
From the viewpoint of suppressing the deformation of the target or the abrasion or damage of the wafer by the cutting tool, as well as suppressing the abnormal discharge during sputtering, the Vickers hardness in the present invention refers to the sputtering of the target. The average value of the Vickers hardness measured at any three locations on the plated surface is in the range of 550 HV to 630 HV.
In addition, the target of the present invention preferably has a structure including a TiW alloy having an average Vickers hardness in a range of 550 HV to 630 HV. In addition, from the viewpoint that the average value of the Vickers hardness is 602 HV to 620 HV, it is preferable that the target of the embodiment of the present invention has no Ti phase and W phase in the sputtering surface, that is, Ti phase and W The area ratio of the phase is 0 area%. In addition, the area% of the present invention refers to the concentration occupied by each element obtained by color mapping using a field emission-electron probe microanalyzer (FE-EPMA). Distribution.

本發明的靶材具有含有7質量%~13質量%的Ti,且剩餘部分包含W及不可避免的雜質的組成。將Ti的含量以不會使Al配線與Si基板的擴散阻擋性大大受損的範圍規定為7質量%~13質量%。並且,就與所述相同的理由而言,Ti的含量較佳為9質量%~11質量%的範圍,更佳為10±0.5質量%的範圍。The target of the present invention has a composition containing 7 to 13% by mass of Ti, and the remainder contains W and unavoidable impurities. The content of Ti is set to 7 to 13% by mass in a range that does not significantly impair the diffusion barrier properties of the Al wiring and the Si substrate. For the same reason as described above, the content of Ti is preferably in the range of 9% by mass to 11% by mass, and more preferably in the range of 10 ± 0.5% by mass.

本發明的靶材可藉由以下製造方法而獲得,並對其一般的形態進行說明。此外,本發明並不受限於以下所說明的形態。
首先,以含有7質量%~13質量%的Ti,且剩餘部分為W及不可避免的雜質的方式,將Ti粉末與W粉末混合而獲得混合粉末。並且,於常溫(JIS Z 8703中所規定的20±15℃)下,例如使用冷均壓(cold isostatic pressing)(以下稱為「CIP」)而將該混合粉末製成成形體。
其次,於利用例如盤式磨機(disk mill)等將該成形體粉碎後,過篩而製作不足1.5 mm的粉碎粉末。並且,對該粉碎粉末進行加壓燒結,獲得TiW合金燒結體,藉由對該TiW合金燒結體實施機械加工而可獲得本發明的靶材。
The target of the present invention can be obtained by the following production method, and its general form will be described. The present invention is not limited to the embodiments described below.
First, a Ti powder and a W powder are mixed to obtain a mixed powder so that Ti contains 7 to 13% by mass and the remainder is W and unavoidable impurities. Then, the mixed powder is formed into a molded body at room temperature (20 ± 15 ° C. specified in JIS Z 8703), for example, using cold isostatic pressing (hereinafter referred to as “CIP”).
Next, the compact is pulverized by, for example, a disk mill or the like, and then sieved to produce a pulverized powder of less than 1.5 mm. Then, the pulverized powder is subjected to pressure sintering to obtain a TiW alloy sintered body, and the target of the present invention can be obtained by machining the TiW alloy sintered body.

加壓燒結例如能夠適用HIP或熱壓(hot press)(以下稱為「HP」)。並且,加壓燒結是於燒結溫度為1500℃~1600℃、加壓力為20 MPa~40 MPa、保持時間為1小時~10小時的條件下進行。該些條件的設定可根據加壓燒結設備的規格而決定,對於HIP而言容易適用低溫高壓的條件,對於HP而言容易適用高溫低壓的條件。本發明中,較佳為在加壓燒結中適用HP,藉此,除可抑制純Ti相或純W相的形成以外,亦可獲得高密度的燒結體。For the pressure sintering, for example, HIP or hot press (hereinafter referred to as "HP") can be applied. The pressure sintering is performed under conditions of a sintering temperature of 1500 ° C to 1600 ° C, a pressure of 20 MPa to 40 MPa, and a holding time of 1 hour to 10 hours. The setting of these conditions can be determined according to the specifications of the pressure sintering equipment. For HIP, it is easy to apply low temperature and high pressure conditions, and for HP, it is easy to apply high temperature and low pressure conditions. In the present invention, it is preferable to apply HP to the pressure sintering, so that in addition to suppressing the formation of a pure Ti phase or a pure W phase, a high-density sintered body can also be obtained.

藉由將燒結溫度設為1500℃以上,而促進燒結,可獲得高密度的燒結體。另外,就與所述相同的理由而言,燒結溫度較佳為設為1510℃以上。另外,藉由將結燒溫度設為1600℃以下,除可適用通用的加壓燒結設備以外,亦抑制燒結體內的晶粒的成長,可獲得均勻的微細組織。另外,就與所述相同的理由而言,燒結溫度較佳為設為1580℃以下。
藉由將加壓力設為20 MPa以上,而促進燒結,可獲得高密度的燒結體。另外,藉由將加壓力設為40 MPa以下,而可適用通用的加壓燒結設備。
藉由將燒結時間設為1小時以上,而促進燒結,可獲得高密度的燒結體。另外,藉由將燒結時間設為10小時以下,可不妨礙製造效率地進行製造。
By setting the sintering temperature to 1500 ° C. or higher, sintering is promoted, and a high-density sintered body can be obtained. In addition, for the same reason as described above, the sintering temperature is preferably 1510 ° C or higher. In addition, by setting the sintering temperature to 1600 ° C. or lower, in addition to the application of general-purpose pressure sintering equipment, the growth of crystal grains in the sintered body can be suppressed, and a uniform fine structure can be obtained. In addition, for the same reason as described above, the sintering temperature is preferably 1580 ° C or lower.
By setting the applied pressure to 20 MPa or more, sintering is promoted, and a high-density sintered body can be obtained. In addition, by setting the applied pressure to 40 MPa or less, general-purpose pressure sintering equipment can be applied.
By setting the sintering time to 1 hour or more to promote sintering, a high-density sintered body can be obtained. In addition, by setting the sintering time to 10 hours or less, production can be performed without hindering production efficiency.

藉由提高靶材的相對密度,可減少靶材中所存在的空隙,硬度的不均減少,有助於提升機械加工性。另外,藉由提高靶材的相對密度,可增大靶材的抗折力,有助於在夾持於切削機械、或接合於背板或背管時的處理等中抑制靶材的破損。因此,本發明的實施形態的靶材較佳為相對密度超過101.0%。
此處,本發明中所謂的相對密度,是指將藉由阿基米德(Archimedes)法所測定出的體積密度,除以對基於由本發明的靶材的組成比所獲得的質量比而算出的元素單體進行加權平均而得的理論密度,並對該所得值乘以100而得出的值。
[實施例]
By increasing the relative density of the target material, the voids existing in the target material can be reduced, and unevenness in hardness can be reduced, which contributes to improving the machinability. In addition, by increasing the relative density of the target material, the bending resistance of the target material can be increased, which helps to suppress the damage of the target material during clamping when it is clamped to a cutting machine or when it is bonded to a back plate or a back pipe. Therefore, the target of the embodiment of the present invention preferably has a relative density exceeding 101.0%.
Here, the relative density in the present invention refers to a volume density measured by the Archimedes method divided by a mass ratio obtained based on a composition ratio based on a target ratio of the present invention. The theoretical density obtained by weighted averaging of the elemental elements of, and a value obtained by multiplying the obtained value by 100.
[Example]

將體積基準的累積粒度分佈的50%粒徑(以下稱為「D50」)為30 μm的Ti粉末、及D50為4.5 μm的W粉末,以含有10質量%的Ti且剩餘部分為W及不可避免的雜質的方式混合而獲得混合粉末。並且,將該混合粉末填充至橡膠製的模具內,於成形壓力為2.0 ton/cm2 (≒196.133 MPa)的條件下進行CIP處理而獲得成形體。
其次,利用盤式磨機將以上所獲得的成形體粉碎並過篩,獲得不足1.5 mm的粉碎粉末。
並且,將該粉碎粉末填充至C(碳)製的加壓容器中,並將該加壓容器設置於HP裝置的爐體內部,於1520℃、30 MPa、2小時的條件下進行加壓燒結,獲得作為本發明例1的靶材的TiW合金燒結體。
另外,藉由與所述相同的條件,亦獲得作為本發明例2~本發明例10的靶材的TiW合金燒結體。
Ti powder with a 50% particle size (hereinafter referred to as "D50") of a volume-based cumulative particle size distribution of 30 μm, and W powder with a D50 of 4.5 μm were used to contain 10% by mass of Ti and the remaining portion was W and Avoid the impurities by mixing to obtain a mixed powder. Then, the mixed powder was filled into a rubber mold, and CIP treatment was performed under a condition of a molding pressure of 2.0 ton / cm 2 (≒ 196.133 MPa) to obtain a molded body.
Next, the formed body obtained above was pulverized by a disc mill and sieved to obtain a pulverized powder of less than 1.5 mm.
Then, the crushed powder was filled into a C (carbon) pressurized container, and the pressurized container was installed inside a furnace of an HP device, and was subjected to pressure sintering under conditions of 1520 ° C, 30 MPa, and 2 hours. A TiW alloy sintered body was obtained as a target of Example 1 of the present invention.
In addition, under the same conditions as those described above, TiW alloy sintered bodies that are targets of Inventive Example 2 to Inventive Example 10 were also obtained.

將D50為30 μm的Ti粉末及D50為4.5 μm的W粉末,以含有10質量%的Ti且剩餘部分為W及不可避免的雜質的方式混合而獲得混合粉末。並且,將該混合粉末填充至橡膠製的模具內,於成形壓力為2.0 ton/cm2 (≒196.133 MPa)的條件下進行CIP處理而獲得成形體。
其次,利用盤式磨機將以上所獲得的成形體粉碎並過篩,獲得不足1.5 mm的粉碎粉末。
將該粉碎粉末填充至軟鋼性的加壓容器中,於450℃的溫度下進行真空脫氣,並於1180℃、100 MPa、2小時的條件下藉由HIP而進行加壓燒結,獲得作為比較例的靶材的TiW合金燒結體。
A Ti powder having a D50 of 30 μm and a W powder having a D50 of 4.5 μm were mixed so as to contain 10% by mass of Ti and the remaining portion was W and unavoidable impurities to obtain a mixed powder. Then, the mixed powder was filled into a rubber mold, and CIP treatment was performed under a condition of a molding pressure of 2.0 ton / cm 2 (≒ 196.133 MPa) to obtain a molded body.
Next, the formed body obtained above was pulverized by a disc mill and sieved to obtain a pulverized powder of less than 1.5 mm.
This crushed powder was filled into a soft steel pressure vessel, vacuum degassed at a temperature of 450 ° C, and pressure sintered by HIP under conditions of 1180 ° C, 100 MPa, and 2 hours to obtain a comparison. TiW alloy sintered body of the target of the example.

自以上所獲得的各燒結體的作為濺鍍面的位置,藉由機械加工而採取試驗片,測定維氏硬度及相對密度。此外,作為本發明例的試樣No.1~No.10的TiW合金燒結體中確認到,於用以製成靶材形狀的機械加工時,無晶片的磨耗或破損。另外,在其機械加工中,亦無TiW燒結體的脫落,因此亦可期待濺鍍時的異常放電的抑制。另外,於夾持於切削機械等處理中,亦不存在TiW燒結體變形或破損的情況。From the position of each sintered body obtained as the sputtered surface, a test piece was taken by machining, and the Vickers hardness and relative density were measured. In addition, as TiW alloy sintered bodies of samples No. 1 to No. 10 as examples of the present invention, it was confirmed that there was no abrasion or breakage of the wafer during machining for forming a target shape. In addition, since the TiW sintered body does not fall off even during the machining, it is also possible to suppress the abnormal discharge during sputtering. In addition, there is no case where the TiW sintered body is deformed or broken during a process such as being clamped in a cutting machine.

維氏硬度是依據JIS Z 2244,使用明石製作所公司股份有限公司製造的MVK-E,測定負荷為9.8 N時的值。
另外,相對密度設為將藉由阿基米德法所測定出的體積密度,除以對基於由各靶材的組成比所獲得的質量比而算出的元素單體進行加權平均而得的理論密度,並對該所得值乘以100而得出的值。此外,測定是使用研精工業股份有限公司製造的電子比重計SD-120L來進行。
The Vickers hardness is a value at a measurement load of 9.8 N using MVK-E manufactured by Akashi Seisakusho Co., Ltd. in accordance with JIS Z 2244.
The relative density is a theory obtained by dividing the bulk density measured by the Archimedes method by the weighted average of the elemental monomers calculated based on the mass ratio obtained from the composition ratio of each target. Density, and multiplying the resulting value by 100. The measurement was performed using an electronic hydrometer SD-120L manufactured by Kensei Industry Co., Ltd.

[表1]
[Table 1]

如表1所示,作為比較例的試樣No.11為圖2所示的以白色部份所示的Ti相散佈在於呈矩陣的W相中的金屬組織,確認到存在維氏硬度低於550 HV的柔軟部位。
另一方面,作為本發明例1~本發明例10的試樣No.1~No.10僅包含圖1中由灰色部份所表示的TiW合金相,並無比較例中觀察到的柔軟部位,可確認到,除將維氏硬度調整為550 HV~630 HV的範圍以外,相對密度亦具有高的值。
藉此,本發明的靶材可期待除抑制機械加工中晶片的磨耗或破損以外,亦能夠抑制靶材本體的變形或破損。
As shown in Table 1, Sample No. 11 as a comparative example is a metal structure in which the Ti phase shown in the white portion is dispersed in the W phase in a matrix shown in FIG. 2, and it is confirmed that the Vickers hardness is lower than 550 HV soft parts.
On the other hand, Samples No. 1 to No. 10 which are Examples 1 to 10 of the present invention include only the TiW alloy phase indicated by the gray portion in FIG. 1, and have no soft parts observed in the comparative example. It was confirmed that in addition to adjusting the Vickers hardness to the range of 550 HV to 630 HV, the relative density also has a high value.
Thereby, the target of the present invention can be expected to suppress deformation or breakage of the target body in addition to suppressing abrasion or breakage of the wafer during machining.

A、B、C‧‧‧測定點A, B, C‧‧‧Measurement points

圖1是本發明例1的靶材的濺鍍面的光學顯微鏡觀察照片。FIG. 1 is an optical microscope observation photograph of a sputtering surface of a target in Example 1 of the present invention.

圖2是比較例的靶材的濺鍍面的光學顯微鏡觀察照片。 FIG. 2 is an optical microscope observation photograph of a sputtering surface of a target of a comparative example.

Claims (4)

一種TiW合金靶材,其含有7質量%~13質量%的Ti,且剩餘部分包含W及不可避免的雜質,濺鍍面中維氏硬度的平均值為550 HV~630 HV。A TiW alloy target contains 7 mass% to 13 mass% of Ti, and the remaining part contains W and unavoidable impurities. The average Vickers hardness in the sputtered surface is 550 HV to 630 HV. 如申請專利範圍第1項所述的TiW合金靶材,其中Ti的含量為9質量%~11質量%。The TiW alloy target according to item 1 of the scope of the patent application, wherein the Ti content is 9% to 11% by mass. 如申請專利範圍第1項或第2項所述的TiW合金靶材,其中所述維氏硬度的平均值為602 HV~620 HV。The TiW alloy target material according to item 1 or item 2 of the patent application scope, wherein the average value of the Vickers hardness is 602 HV to 620 HV. 一種TiW合金靶材的製造方法,其包括: 以含有7質量%~13質量%的Ti、且剩餘部分為W及不可避免的雜質的方式,將Ti粉末與W粉末混合而獲得混合粉末的步驟; 對所述混合粉末進行加壓而獲得成形體的步驟; 於將所述成形體粉碎後過篩而獲得不足1.5 mm的粉碎粉末的步驟;以及 於燒結溫度為1500℃~1600℃、加壓力為20 MPa~40 MPa、保持時間為1小時~10小時的條件下對所述粉碎粉末進行加壓燒結而獲得TiW合金燒結體的步驟。A method for manufacturing a TiW alloy target includes: A step of mixing a Ti powder with a W powder to obtain a mixed powder in a manner that contains 7 to 13% by mass of Ti and the remaining portion is W and unavoidable impurities; A step of pressing the mixed powder to obtain a shaped body; A step of pulverizing the formed body and sieving to obtain a pulverized powder of less than 1.5 mm; and A step of sintering the pulverized powder under pressure to obtain a TiW alloy sintered body under conditions of a sintering temperature of 1500 ° C to 1600 ° C, a pressure of 20 MPa to 40 MPa, and a holding time of 1 hour to 10 hours.
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