1304757 九、發明說明： 【發明所屬之技術領域】 本發明係一種濺鍍粗材的製法 .燒社n “士是一種降低粉末 n 皿度’以獲付低成本、高品質濺鍍靶材。 【先前技術】1304757 IX. Description of the Invention: [Technical Field of the Invention] The present invention is a method for producing a sputtered coarse material. The roasting society n is a kind of reducing the powder n-degree to obtain a low-cost, high-quality sputtering target. [Prior Art]
濺鍍製程廣泛地被使用在薄膜製程中，例如電子一 件、儲存媒體、玻璃鑛膜以及刀具鑛膜等產業皆大量使= 舰製程，因此㈣製程成為目前各種產業著重的領域。 若想要濺鑛後的薄膜品質良好，則賤鐘乾材就需要呈 有高純度、高密度、成分分佈均句、晶粒小以及高機械強 度等特性’而-般製作濺㈣材的製法大略可分為溶煉 (meltind與粉末冶金（powder metaUurgy)這兩種，其中 在粉末冶金的製程中，又可分為以熱壓( — res —，Η。 進行燒結（sintering)和以熱均壓（㈣―他… 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 得到高密度及高強度的靶材，則熱壓溫度與壓力就必；提 高，然而，一旦溫度增加，就會使模具組成成分擴散至靶 材的量及深度增加，致使靶材受到污染而降低純度，且高 溫會促使晶粒成長，另夕卜^壓力提高，則會增加模具破 裂的風險；另-方面，t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程序， 然而，封罐的程序除費時費工外，尚需耗損大量的靶材材 料，因此需要較高的成本；所以單獨使用熱壓或熱均壓的 1304757 製程均無法獲得兼具有低成本與 '、阿在度的靶材，故無法降 低以濺艘製程鑛膜之產品的價格。 在美國專利號第6脳13號的專利案中提到：先利用 …、恩或震動（vlbratlGn)的方法製造出密度為理論密度之 50-95%妹材初胚’再將此初胚進行熱均壓製程，芦而， 由於以熱麼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乾材 密度’但如上所述’封罐的程序會增加成本，故此方法還 是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 Μ與熱均壓的製程來製造高密度的鶴⑺無材，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】 本發明人有鑒於目前製作濺鍍靶材的成本在兼顧靶材 特14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 1304757 質濺鍍靶材的方法。 、.兰- - ‘、、、運上述目的，本發明之濺鍍靶材的製造方法，其係 包括以下步驟： 八” 將勒*材原料粉末置入模具中，在溫度範圍於8501至 14〇〇C之間，而壓力範圍於3500〜8000磅/平方英寸（psi) 之間的情形下，進# 120〜180分鐘的熱壓方式進行燒結以 形成初胚，且其初胚不具有開放性孔洞；Sputtering processes are widely used in thin film processes. For example, electronics, storage media, glass mineral film, and tool mineral film industries have made a large number of industries, so (4) processes have become the focus of various industries. If the quality of the film after the splashing is good, the dry material of the Cuckoo clock needs to have the characteristics of high purity, high density, uniform composition, small grain size and high mechanical strength, and the method of making the splash (four) material can be roughly Divided into two kinds of melting (meltind and powder metallurgy (powder metaUurgy), which in the powder metallurgy process, can be divided into hot pressing (-res-, Η. sintering (sintering) and with heat equalization ( (4) “He...press, HIP) for sintering. When the powder material is sintered by hot pressing alone to form a material body, if a high-density and high-strength target is to be obtained, the hot pressing temperature and pressure will be increased; However, as the temperature increases, the amount and depth of the mold components diffuse to the target increase, causing the target to be contaminated to reduce the purity, and the high temperature will promote the grain growth, and the pressure will increase, and the mold will be increased. The risk of rupture; on the other hand, when the thermal pressure equalization is used alone to sinter the powder raw material into the material body, the sealing process must be carried out in the process. However, the process of sealing the tank requires a lot of time and labor. The target material, therefore, requires a higher cost; therefore, the 1304757 process using hot pressing or hot equalizing alone cannot obtain a target with low cost and ', and can't reduce the process of splashing the ship. The price of the product of the film. In the patent case No. 6脳13 of the United States Patent No.: First, the method of using,, or vibrating (vlbratlGn) is used to produce a density of 50-95% of the theoretical density of the embryo. Then, the primordial embryo is subjected to a heat-smoothing process, and the primordial embryos produced by the method of heat or vibration still have open pores. Therefore, the initial embryos need to be sealed in order to improve the dry materials. Density 'but as described above' the process of sealing can increase the cost, so this method still can not solve the problem of excessive cost. In the patent of US Pat. No. 6,582,535, the process of using heat and heat equalization is mentioned. The high-density crane (7) is made of no material. However, the particle size of the target material powder required for the process must be small, so that the hot pressing process can be performed at a lower temperature to reduce the growth of the crystal grains, but the particle size is small. Powder must be consumed The higher cost's therefore cannot solve the problem of excessive cost. In addition, it has been mentioned that the high-density/cerium (Si) sintered body is produced by hot pressing and hot pressing, but the process must be prior to the powder. High-density sintered body can be obtained by deoxidation treatment under high-temperature decompression. However, in addition to the high-temperature deoxidation treatment, the powders are bonded to each other, and the production cost is also greatly increased. [Inventors] The present inventors have made Since the cost of the plating target cannot be lowered in consideration of the target material 14, the method of manufacturing the sputtering target has finally been invented in an experiment which has been repeatedly repeated in response to this problem. The object of the present invention is to provide a low cost. A method for producing high-quality 6 1304757 sputter targets. The present invention relates to a method for producing a sputtering target according to the present invention, which comprises the steps of: 八" placing a raw material powder into a mold at a temperature ranging from 8501 to 14 Between C and C, and the pressure range is between 3500 and 8000 psi, the hot pressing method of #120 to 180 minutes is performed to form the blast, and the blast is not open. Sexual hole
將上述之初胚在溫度與壓力分別為8〇〇〜ii〇〇t、 22000-26000 -+ΑΛ Κ*- 'W IT ^ irn 嘮/十方央寸的情況下進行15(Μ80分鐘的熱 均壓’以得到錢鍍㈣，且該㈣密度提升至*小於理論 密度之96%。 4 其中該靶材係 乾材》The above-mentioned primordial embryos were subjected to 15 (Μ80 minutes of heat) at a temperature and pressure of 8 〇〇 〇〇 〇〇 、, 22000-26000 - + ΑΛ Κ * - 'W IT ^ irn 唠 / ten square inches, respectively. The pressure is equalized to obtain the money plating (4), and the density of the (4) is increased to * less than 96% of the theoretical density. 4 wherein the target is dry material
Co基合金、釕、釕基合金及基合金Co-based alloy, niobium, niobium based alloy and base alloy
藉由低溫低壓的熱壓方式 放性孔洞’再經由熱均壓的方 上’而且所使用的粉末粒徑並 僅需要使用一般可方便獲得的 具有以下優點： 就可以讓初胚密度不具有開 式即可將靶材密度提升至以 無限制，因此靶材原料粉末 材料即可，另外，本發明還 (1)藉由降低熱壓的溫度，可膝 又 了降低楔具成分向初胚 擴散的量與深度，以増加知分 ^ ㈢加靶材侍料率，也因此提 尚粗材的純度。 可減少模具破裂的風 因此工廠可接受小批 (2) 藉由降低熱壓的壓力， 險，以降低生產成本。 (3) 由於上述成本的減少， 7 1304757 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 的靶材原料粉末的混料量較少，所以能獲得成分 較均勻的乾材，以減少巨觀偏析 (macrosegregation)的問題。 (4)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 寿王熱壓時可直接製做近淨成形（near net shape) 的初胚不，、可省去因封罐而耗費之材料，近淨 成形亦可節約材料之損&，藉此可大幅提昇靶材 得料率。 【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： -將靶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 ⑽、釘基合金（Ru-based all〇y)、c〇 Cr_pt Ti()2、c〇_ cr-Pt-si〇2 Co-c卜Pt—B_Si〇2 以及 Cr_M〇—Mn 等，該溫度範 圍係在85代至⑷代之間，該壓力範圍係在3500 8500 碎/平方英寸（pSi)之間，而熱壓的時間需要12G18D分鐘； 將上述之初胚在溫度與壓力分别為8〇〇〜u〇(rc、 22000〜26_碎/平方英寸的情況下進行抓刚分鐘的熱 1304757 均藶’以得到錢鐘粗材。 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，若組成原料之熔點較高，則所需熱壓溫度要 隨之調高；另外，熱均壓之溫度需低於熱壓溫度，以確保 於熱均壓時材料不會熔融，此時熱均壓處理之壓力就需提 高’以獲得非常緻密之材料。 實施例一 _ 將純釕（Ru)或釕基合金（Ru-based alloy)之金屬粉末 放入模具中，經過120~ 180分鐘的熱壓後形成初胚，其溫 度約在1150〜1400 °C，而壓力約在4〇 00〜8000磅/平方英寸 (psi)，該初胚的抗折強度為95〇±5〇百萬帕（Mpa)，且其 已不具開放性孔洞，再將此初胚經過ll〇〇〇c、22〇〇〇磅/ 平方英寸（psi)的熱均壓過程18〇分鐘後，即可得到賤鍛 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1100±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 1100〜1275C ’而壓力在4000~8000碎/平方英寸（psi)之 間’該初胚的抗折強度為1200±50百萬帕（jjpa)，且其已 不具開放性孔洞，再將此初胚經過1〇5〇。(：、24000碎/平 方英寸（psi)的熱均壓過程150分鐘後，即可得到c〇 — Cr_ 9 1304757The low-pressure and low-pressure hot-pressing method is used to release the pores 'on the side of the hot-pressure equalization' and the particle size of the powder used is only conveniently used, which has the following advantages: In this way, the target density can be raised to an unlimited extent, so that the target raw material powder material can be used. In addition, the present invention (1) can reduce the diffusion of the wedge component to the embryo by lowering the temperature of the hot pressing. The amount and depth of the amount, to know the points ^ (three) plus the target material rate, and therefore the purity of the crude material. It can reduce the wind of mold rupture. Therefore, the factory can accept small batches. (2) Reduce the production cost by reducing the pressure and risk of hot pressing. (3) Due to the above-mentioned cost reduction, 7 1304757, various orders, do not have to worry about the cost can not be loaded, so it can quickly reflect the changing needs of the current target market, and the small batch of target material powder is less mixed. Therefore, it is possible to obtain a dry material with a relatively uniform composition to reduce the problem of macrosegregation. (4) Since the density of the produced target is increased, the strength of the target is also increased to prevent the target from being broken by thermal stress and coolant hydraulic pressure in the subsequent sputtering process. (5) The method of the present invention replaces the hot-pressurization of the sealed cup by the hot pressing, and can directly make the near net shape of the initial embryo without heating, and can save the cost of sealing the can. The material, near net shape can also save material damage &, which can greatly increase the target yield. [Embodiment] The method for producing a sputtering target according to the present invention comprises the steps of: - placing a target material powder into a mold, the raw material powder is not required to be subjected to a low temperature and low pressure hot pressing method. Sintering to form primaries, such as ruthenium (10), Ru-based all〇y, c〇Cr_pt Ti() 2, c〇_ cr-Pt-si〇2 Co-c, Pt-B_Si〇2, and Cr_M〇-Mn, etc., the temperature range is between the 85th and (4) generations, the pressure range is between 3500 8500 cc/p (pSi), and the hot pressing time requires 12G18D minutes; In the case of temperature and pressure of 8 〇〇 ~ u 〇 (rc, 22000 ~ 26 _ broken / square inch, the heat of the first minute of 1304757 is uniformly 苈 ' to get the thick material of Qian Zhong. The above temperature and pressure values will Due to the difference in composition ratio and composition ratio, if the melting point of the constituent raw materials is higher, the required hot pressing temperature should be increased; in addition, the temperature of the hot equalizing pressure should be lower than the hot pressing temperature to ensure The material does not melt when hot equalizing, and the pressure of the heat equalizing treatment needs to be increased to obtain a non- Dense material. Example 1 _ Putting pure Ru (Ru) or Ru-based alloy metal powder into the mold, after 120~180 minutes of hot pressing, the initial embryo is formed, and the temperature is about 1150. ~1400 ° C, and the pressure is about 4 〇 00 ~ 8000 psi (psi), the initial embryo has a flexural strength of 95 〇 ± 5 〇 MPa (Mpa), and it has no open pores, After the initial embryo is passed through a thermal pressure equalization process of ll 〇〇〇 c, 22 〇〇〇 pounds per square inch (psi) for 18 minutes, the finished product of the upset target can be obtained, and the density of the target at this time Increase to 96~1〇〇%, and increase the flexural strength to 1100±50 MPa. In the second embodiment, the powders of Co, Cr, Pt and Ti〇2 are mixed and put into the mold. After 180 minutes of hot pressing, the initial embryo is formed, and the temperature is about 1100~1275C' and the pressure is between 4000~8000 pieces/square inch (psi). The initial embryo has a flexural strength of 1200±50 MPa. (jjpa), and it has no open pores, and then the initial embryo is passed 1〇5〇. (:, 24,000 pieces per square inch (psi) of the heat equalization process 150 minutes later, Get c〇 - Cr_ 9 1304757
Pt-Ti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1250±50百萬帕（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1 8 0分鐘的熱壓後形成初胚，其溫度約在 1 000~ 1 200°C ’而壓力在3500~8000磅/平方英寸（psi)之 間’該初胚的抗折強度為_ 1200±50百萬帕（Mpa)，且其已 ® 不具開放性孔洞，再將此初胚經過950°C、26000碎/平方 英寸（psi)的熱均壓過程180分鐘後，即可得到C0_Cr_p卜 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1250±50百萬帕（MPa)。 實施例四 將Co、Cr、Pt、B及Si〇2各成份之粉末經過混料後放 入模具中，經過18 0分鐘的熱壓後形成初胚，其溫度約在 850〜1100°C，而壓力在3500^8000磅/平方英寸（psi)之間， 該初胚的抗折強度為1 250±50百萬帕（MPa)，且其已不具 開放性孔洞，再將此初胚經過80(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c〇_c卜pt_B_Si〇; 之合金濺鍍靶材成品，而此時該靶材的密度增加至 96~100%，且抗折強度增加為13〇〇±5〇百萬帕（Μρ&)。 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 .1304757 96%以上’故不需封 讓模具成分不會大量擴散至，氏壓與低溫的熱壓方式 會，因此能夠節省成本，另=胚内，並降低模具破裂的機 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。椅原料粉末僅f要使用—般 【圖式簡單說明】 無The alloy of Pt-Ti〇2 is sputtered to the finished product, while the density of the target is increased to 97 to 100%, and the flexural strength is increased to 1250 ± 50 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 1000 minutes of hot pressing, an initial embryo is formed, and the temperature is about 1 000 to 1 200 ° C. 'And the pressure is between 3500 and 8000 psi (psi)' The initial embryo has a flexural strength of _ 1200 ± 50 MPa (Mpa), and it has no open pores, and then this embryo After 180 minutes of heat equalization in 950 ° C, 26,000 rpm, the finished product of C0_Cr_p 〇Si〇2 alloy sputtering target is obtained, and the density of the target is increased to 97~ 100% 'and the flexural strength is increased to 1250 ± 50 MPa. In the fourth embodiment, the powders of the components of Co, Cr, Pt, B and Si〇2 are mixed and put into a mold, and after 18 hours of hot pressing, an initial embryo is formed, and the temperature is about 850 to 1100 ° C. The pressure is between 3,500 and 8,000 psi. The initial embryo has a flexural strength of 1,250 ± 50 MPa, and it has no open pores. (rc, 26 〇〇〇 pounds per square inch (psi) of the heat equalization process after 180 minutes, you can get c〇_c pt_B_Si〇; the alloy splash target finished product, and the density of the target at this time Increase to 96~100%, and increase the flexural strength to 13〇〇±5〇 MPa(Μρ&). The low temperature and low pressure hot pressing method can make the blast and it has no open pores, and then The density of the target can be increased to more than .1304757 by more than 96% by heat equalization. Therefore, it is not necessary to seal the mold components without a large amount of diffusion, and the hot pressing method of the low pressure and low temperature will save the cost. There is no limit to the particle size of the material in the embryo and reducing the rupture of the mold, so the original market used in the method of the invention is conveniently purchased. The material can seat material powder to be used only f - briefly described general formula [FIG None
【主要元件符號說明】 無[Main component symbol description] None
1111