200824817 九、發明說明： 【發明所屬之技術領域】 本發明係一種濺鍍靶材的製法，尤其是一種降低粉末 燒結之溫度，以獲得低成本、高品質濺鍍靶材的製法。 【先前技術】 錢鍍製程廣泛地被使用在薄膜製程中，例如電子元 件、儲存媒體、玻璃鍍膜以及刀具鍍膜等產業皆大量使用 濺鍍製程，因此濺鍍製程成為目前各種產業著重的領域。 # 若想要濺鍍後的薄膜品質良好，則濺鍍靶材就需要具 有高純度、高密度、成分分佈均勻、晶粒小以及高機械強 度等特性，而一般製作濺鍍靶材的製法大略可分為熔煉 (1116 11：11^)與叙末冶金（口〇财(|6]：1116七311111^丫）這兩種，其中 在粉末冶金的製程中，又可分為以熱壓（hotpressing，HP) 進行燒結（Sintering)和以熱均壓（h〇t is〇static pressing，HIP)進行燒結。 單獨以熱壓法來燒結粉末原料製成材料體時，若想要 ❿？到高密度及高強度的靶材，則熱壓溫度與壓力就必須提 南’，而’ 一旦溫度增加，就會使模具組成成分擴散至乾 材的虿及深度增加，致使乾材受到污染而降低純度，且言 ，會促使晶粒成長，另外，若壓力提高，則會增加模具: 4的風險，另一方面’當單獨使用熱均壓來燒結粉末原料 製成材料體時則於製程中須經過封罐（canning)的程序， 然而，封罐的程序除費時費工外，尚需耗損大量的乾材材 枓，因此需要較高的成本；所以單獨使用熱壓或熱均壓的 5 200824817 製程均無法獲得兼具有低成本與高密度㈣材，故無法降 低以濺鍍製程鍍膜之產品的價格。 =國專利號帛6165413號的專利案中提到·先利用 “辰動(vlbration)的方法製造出密度為理論密度之 备95%的乾材初胚’再將此初胚進行熱均壓製程，然而， 由於以熱壓或震動方法所製作出來的初胚仍然存有開放孔 洞’因此初胚於熱均壓時尚需進行封罐程序才能提高㈣200824817 IX. DESCRIPTION OF THE INVENTION: TECHNICAL FIELD The present invention is a method for producing a sputtering target, and more particularly, a method for reducing the temperature of powder sintering to obtain a low-cost, high-quality sputtering target. [Prior Art] The money plating process is widely used in the film process. For example, electronic components, storage media, glass coating, and tool coating are widely used in the sputtering process. Therefore, the sputtering process has become an important field in various industries. # If the quality of the film after sputtering is good, the sputtering target needs to have high purity, high density, uniform composition distribution, small crystal grain and high mechanical strength, etc., and the general method for making the sputtering target is generally Can be divided into smelting (1116 11:11^) and the end of the metallurgy (mouth 〇 ( (|6): 1116 seven 311111 ^ 丫) two, which in the powder metallurgy process, can be divided into hot pressing ( Hot pressing, HP) Sintering and sintering by hot pressing (HIP). When the powder material is sintered by hot pressing alone to form a material body, if you want to high to high For dense and high-strength targets, the hot pressing temperature and pressure must be increased, and 'once the temperature increases, the mold components will diffuse to the dryness and depth of the dry material, causing the dry material to be contaminated and reduce the purity. And, in other words, it will promote grain growth. In addition, if the pressure is increased, the risk of the mold: 4 will be increased. On the other hand, when the powder material is sintered by using the heat equalizing pressure alone, it must be sealed in the process. Canning procedure, of course In addition to time-consuming labor, the process of sealing can still consume a large amount of dry materials, so it requires high cost; therefore, the 5 200824817 process using hot pressing or hot equalizing alone cannot obtain both low cost and High-density (four) materials, so it is impossible to reduce the price of products coated with a sputtering process. = Patent No. 帛6165413 mentioned in the patent case. First, use the method of "vlbration" to produce a density with a theoretical density. 95% of the dry primordial embryos will be subjected to a hot homogenization process. However, since the primordial embryos produced by the hot pressing or shaking method still have open pores, the primordial embryos need to be subjected to thermal pressure equalization. Can the can sealing program be improved (4)
讀、，但如上所述，封罐的程序會增加成本，故此方法還 疋無法解決成本過高的問題。 而在美國專利號第6582535號的專利案中提到利用熱 壓與熱均壓的製程來製造高密度的鶴⑺靶材，然而，該 製程所需的靶材材料粉末的粒徑必須很小，才能以較低的 溫度進行熱壓製程’以減低晶粒的成長，但小粒徑的粉末 必須耗費較高的成本，因此亦無法解決成本過高的問題。 另外，有人提到使用熱壓與熱均壓製程來製造高密度 的矽（Si )燒結體，然而該製程之矽粉須先於高溫減壓下進 行脫氧處理，方能獲得高密度燒結體，然而高溫之脫氧處 理除了會造成粉末彼此間有黏合現象外，亦大幅提高製作 成本。 【發明内容】 本發明人有鑒於目w製作濺鍍靶材的成本在兼顧靶材 特性的情況下無法降低，因此針對此問題不斷反覆的實 驗，終於發明出此濺鍍靶材的製造方法。 本發明之目的係在於提供一種在低成本下製作出高品 6 200824817 質濺鍍靶材的方法。 為達上述目的，本發明之濺鍍靶材的製造方 包括以下步驟·· ” 將靶材原料粉末置入模具中，在溫度範圍⑨85『c至 1400°C之間，而壓力範圍於35〇〇〜8〇〇〇磅,平方英寸（Mi)Read, but as mentioned above, the process of sealing can increase the cost, so this method can not solve the problem of excessive cost. In the patent of U.S. Patent No. 6,582,535, it is mentioned that a high-density crane (7) target is produced by a process of hot pressing and hot equalizing. However, the particle size of the target material powder required for the process must be small. In order to reduce the growth of crystal grains at a lower temperature, the growth of the crystal grains is reduced, but the powder of a small particle size must be costly, and thus the problem of excessive cost cannot be solved. In addition, it has been mentioned that a high-density yttrium (Si) sintered body is produced by using a hot press and a hot press process. However, the tantalum powder of the process must be subjected to deoxidation treatment under high temperature and reduced pressure to obtain a high-density sintered body. However, in addition to the high temperature deoxidation treatment, the powders adhere to each other, and the production cost is also greatly increased. SUMMARY OF THE INVENTION The inventors of the present invention have invented a method for producing a sputtering target in view of the fact that the cost of producing a sputtering target cannot be lowered in consideration of the characteristics of the target. It is an object of the present invention to provide a method for producing a high-quality 6 200824817 quality sputter target at low cost. In order to achieve the above object, the manufacturer of the sputtering target of the present invention includes the following steps: "" The target material powder is placed in a mold at a temperature ranging from 985 s to 1400 ° C, and the pressure is in the range of 35 〇. 〇~8 lbs, square inch (Mi)
之間的情形下，進行12〇〜18〇分鐘的埶、PS …、&万式進行燒結以 形成初胚，且其初胚不具有開放性孔洞；In the case of between, 12埶~18〇 minutes of 埶, PS ..., & 10,000 are sintered to form the blast, and the primordial embryo has no open pores;
將上述之初胚在溫度與壓力分別為8〇〇〜u⑽。C、 22000〜2_G碎/平方英寸的情況下進行15(M8q分鐘的熱 均壓，以得到濺鍍靶材，且該乾材密 刊山沒杈升至不小於理論 密度之96%。 其中該㈣係C。基合金、釘、釕基合金及Cr基合金 靶材。 口 藉由低溫低壓的熱壓方式就可以讓初胚密度不具有開 放性孔洞，再經由熱均壓的方式即可將靶材密度提2至以 上，而且所使用的粉末粒徑並無限制，因此革巴材原料粉末 _僅需要使用-般可方便獲得的材料即可，另外，本發明還 具有以下優點： (1)藉由降低熱壓的溫度，可降低模具成分向初胚 擴散的罝與洙度，以增加靶材得料率，也因此提 高靶材的純度。 ⑺藉由降低熱Μ的壓力，可減少模具破裂的風 險，以降低生產成本。 (3)由於上述成本的減少，因此工廠可接受小批 7 200824817 里、多樣的訂單，不必擔心成本無法負荷，故可 快速反應目前靶材市場多變的需求，而且小批量 的乾材原料粉末的混料量較少，所以能獲得成分 較均勻的靶材，以減少巨觀偏析 (macrosegregation)的問題。 U)由於製作出來的靶材密度提高，故靶材的強 度也因此提升，以避免該靶材在之後的濺鍍過程 中因熱應力（thermal stress)及冷卻液液壓而破 # 裂。 (5)本發明之方法用熱壓取代了熱均壓的封罐製 私，熱壓時可直接製做近淨成形（near net shape) 的初胚，不只可省去因封罐而耗費之材料，近淨 成形亦可節約材料之損耗，藉此可大幅提昇靶材 于步斗率〇 【實施方式】 本發明之濺鍍靶材的製造方法，其係包括以下步驟： 9 絲材原料粉末置入模具中，此原料粉末並不需要求 粒徑，以低溫低壓的熱壓方式進行燒結以形成初胚，如釕 (RU)釕基合金〇?114336(1311(^)、（：〇-(：了-？卜1^02、（：〇-The above embryos were subjected to temperature and pressure of 8 〇〇 to u (10), respectively. C, 22000~2_G broken/square inch, 15 (M8q minutes heat equalization is performed to obtain a sputtering target, and the dry material is not soared to not less than 96% of the theoretical density. (4) C. Base alloys, nails, bismuth-based alloys and Cr-based alloy targets. The low-pressure and low-pressure hot-pressing method allows the initial embryo density to have no open pores, and then through hot pressure equalization. The target material has a density of 2 or more, and the particle size of the powder to be used is not limited. Therefore, the raw material powder of the leather material is only required to be used as a material which can be easily obtained. In addition, the present invention has the following advantages: (1) By reducing the temperature of the hot pressing, the enthalpy and twist of the mold component to the initial embryo can be reduced to increase the target yield and thus the purity of the target. (7) The mold can be reduced by reducing the pressure of the enthalpy The risk of rupture to reduce production costs. (3) Due to the above-mentioned cost reduction, the factory can accept a small batch of 7 200824817, a variety of orders, do not have to worry about the cost can not be loaded, so it can quickly reflect the current needs of the target market ,and The batch of dry material raw material powder has a small amount of mixed material, so that a target having a relatively uniform composition can be obtained to reduce the problem of macrosegregation. U) The strength of the target is increased due to the density of the produced target. It is also upgraded to avoid the target being broken by thermal stress and coolant hydraulic pressure during subsequent sputtering. (5) The method of the present invention replaces the heat-pressure equalization of the cans with hot pressing, and can directly produce the near net shape of the initial embryo during hot pressing, which not only saves the cost of sealing the cans. The material and the near net shape can also save the loss of the material, thereby greatly improving the target in the stepping rate. [Embodiment] The method for manufacturing the sputtering target of the present invention comprises the following steps: 9 wire raw material powder The raw material powder is placed in a mold, and the raw material powder is not required to have a particle diameter, and is sintered by a low-temperature low-pressure hot pressing method to form an initial embryo, such as a ruthenium (RU) ruthenium-based alloy 〇 114336 (1311 (^), (: 〇- (: - - Bu 1 ^ 02, (: 〇 -
Cr Pt Si02 Co-Cr-Pt-B-Si02 以及 Cr-Μο-Μη 等，該溫度範 2係在850 C至14〇〇°C之間，該塵力範圍係在35〇〇〜85〇〇 方/平方英寸（psi)之間，而熱壓的時間需要1別〜〗㈣分鐘,· 將上述之初胚在溫度與壓力分別為〜Η⑽。C、 22000 26000石旁/平方英寸的情況下進行〜剛分鐘的熱 8 200824817 .均壓，以得到濺鍍靶材。 上述之溫度及壓力值會因組成原料及成分比例之不同 而有所調整，甚έ日士、js w 左^ 、、且成原料之熔點較高，則所需熱壓溫度要 P您之凋回，另外，熱均壓之溫度需低於熱壓溫度，以確保 2熱均壓時材料不會熔融，此時熱均壓處理之壓力就需提 面，以獲得非常緻密之材料。 實施例一 響 I、、屯舒（如）或舒基合金（Ru-based al loy )之金屬粉末 放入模具中，經過120〜18〇分鐘的熱壓後形成初胚，其溫 度約在U50〜140 0°C，而壓力約在4000〜80 00磅/平方英寸 (psi)，該初胚的抗折強度為95〇±5〇百萬帕，且其 已不具開放性孔洞，再將此初胚經過11〇(rc、22〇〇〇磅〆 平方英寸（psi)的熱均壓過程18〇分鐘後，即可得到濺鍍 靶材成品，而此時該靶材的密度增加至96〜1〇〇%，且抗折 強度增加為11〇〇±50百萬帕（MPa)。 實施例二 將Co、Cr、Pt、Ti〇2各成份之粉末經過混料後放入模 具中，經過180分鐘的熱壓後形成初胚，其溫度約在 1100〜1275°C，而壓力在4000〜8000磅/平方英寸（psi)之 間，該初胚的抗折強度為12〇〇±5〇百萬帕（MPa)，且其已 不具開放性孔洞，再將此初胚經過105(rc、24〇〇〇碎〆平 方英寸（psi)的熱均壓過程15〇分鐘後，即可得到c〇 —以― 9 200824817Cr Pt Si02 Co-Cr-Pt-B-Si02 and Cr-Μο-Μη, etc., the temperature range 2 is between 850 C and 14 ° C, and the dust range is between 35 〇〇 and 85 〇〇. Between square/square inch (psi), and the time of hot pressing requires 1 to ~ (four) minutes, · The above embryos are at temperatures and pressures of ~ Η (10). C, 22000 26000 stone side / square inch case carried out ~ just minutes of heat 8 200824817 . Pressure equalization to get a sputter target. The above temperature and pressure values will be adjusted due to the difference in the proportion of raw materials and components. Even if the melting point of the raw materials is higher, the required hot pressing temperature should be P In addition, the temperature of the hot equal pressure should be lower than the hot pressing temperature to ensure that the material does not melt when the two heat equalizing pressure is applied. At this time, the pressure of the heat equalizing treatment needs to be lifted to obtain a very dense material. In the first embodiment, the metal powder of the ring I, ruthenium (such as) or Ru-based al loy is placed in a mold, and after 120~18 minutes of hot pressing, an initial embryo is formed, and the temperature is about U50. ~140 0 ° C, and the pressure is about 4000 ~ 80 00 psi, the initial embryo has a flexural strength of 95 〇 ± 5 〇 MPa, and it has no open pores, and then After the initial embryo is subjected to a thermal grading process of 11 〇 (rc, 22 〆 〆 square inch (psi) for 18 〇, the finished target of the sputtering target can be obtained, and at this time the density of the target is increased to 96~ 1〇〇%, and the flexural strength is increased to 11〇〇±50 MPa (MPa). In the second embodiment, the powders of Co, Cr, Pt and Ti〇2 are mixed and put into a mold. After 180 minutes of hot pressing, the blast is formed at a temperature of about 1100 to 1275 ° C, and the pressure is between 4000 and 8000 psi. The initial embryo has a flexural strength of 12 〇〇 ± 5 〇. Million Pascals (MPa), and it has no open pores, and then the initial embryos are passed through 105 (rc, 24 〆 〆 square inch (psi) heat equalization process for 15 〇, then you can get c〇 - to --9,200,824,817
Pt-Ti〇2之合金錢鍍乾材成品，而此時該靶材的密度增加 至97〜100%，且抗折強度增加為125〇±5〇百萬帕（Mpa)。 實施例三 將Co、Cr、Pt、Si〇2各成份之粉末經過混料後放入模 具中，經過180分鐘的熱壓後形成初胚，其溫度約在 1 000〜1 200X：，而壓力在35〇〇〜8〇〇〇磅/平方英寸（psi)之 間，該初胚的抗折強度為12〇〇±5〇百萬帕（Mpa)，且其已 不具開放性孔洞，再將此初胚經過95(rc、26〇⑽磅/平方 英寸（psi)的熱均壓過程180分鐘後，即可得到c〇_Cr —Μ — Si〇2之合金濺鍍靶材成品，而此時該靶材的密度增加至 97〜100%，且抗折強度增加為125〇±5〇百萬帕（Mpa)。 實施例四 將Co、Cr、Pt、B & Si〇2各成份之粉末經過混料後放 入模具中，經過180分鐘的熱壓後形成初胚，其溫度約在 850〜1100°C，而壓力在350〇〜8〇〇〇磅/平方英寸（psi)之間， 該初胚的抗折強度為USOiSO百萬帕（MPa)，且其已不具 開放性孔洞，再將此初胚經過8〇(rc、26〇〇〇磅/平方英寸 (psi)的熱均壓過程180分鐘後，即可得到。气卜以―b — 之合金濺鍍靶材成品，而此時該靶材的密度增加至 96〜10 0%，且抗折強度增加為13〇〇±5〇百萬帕（Mpa)。 藉由低溫低壓的熱壓方式就可以讓初胚且其已不具開 放性孔洞，而再經由熱均壓的方式即可將靶材密度提升至 200824817 y D 7ο Μ 户W >r王，叩几ΊΒ* α丹1氐通的熱壓方* 讓模具成分不會大瞀抽^ 、 擴政至初胚内，並降低模且破到沾她 會，因此能夠節省成本，另 -保/、硬4的機 料粉末粒徑並無限制，因此卜本發明之方法所使用的原 市場上方便購得的材料即可。材原料粉末僅需要使用一般 【圖式簡單說明】The alloy of Pt-Ti〇2 is coated with dry material, and the density of the target is increased to 97~100%, and the flexural strength is increased to 125〇±5〇 MPa (Mpa). In the third embodiment, the powders of the components of Co, Cr, Pt and Si〇2 are mixed and put into a mold, and after 180 minutes of hot pressing, an initial embryo is formed, and the temperature is about 1 000~1 200X:, and the pressure is Between 35 〇〇 and 8 〇〇〇 pounds per square inch (psi), the initial embryo has a flexural strength of 12 〇〇 ± 5 〇 MPa (Mpa), and it has no open pores. After the initial embryo is subjected to a heat equalization process of 95 (rc, 26 〇 (10) psi) for 180 minutes, the finished product of the c溅_Cr —Μ —Si〇2 alloy sputtering target can be obtained. When the density of the target is increased to 97~100%, and the flexural strength is increased to 125〇±5〇 MPa (Mpa). The fourth embodiment will be Co, Cr, Pt, B & The powder is mixed and placed in a mold. After 180 minutes of hot pressing, the initial embryo is formed at a temperature of about 850 to 1100 ° C, and the pressure is between 350 〇 and 8 〇〇〇 pounds per square inch (psi). The initial embryo has a flexural strength of USOiSO MPa, and it has no open pores, and the blast is passed through 8 〇 (rc, 26 〇〇〇 psi) Pressure process 180 After the clock, you can get it. The gas is sprayed with the alloy of “b—the target, and the density of the target increases to 96~10 0%, and the flexural strength increases to 13〇〇±5〇100. 10,000 Pa (Mpa). The low temperature and low pressure hot pressing method can make the initial embryo and it has no open pores, and then the target density can be raised to 200824817 by the thermal pressure equalization. >r king, 叩 ΊΒ α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α α The particle size of the powder of the other-protected/hard 4 is not limited, so the material which is conveniently available on the market by the method of the present invention can be used. The raw material powder only needs to be used generally. 】
Γ要元件符號說明Main component symbol description
IIII