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Preparation method of chromium-silicon alloy sputtering target material

A chromium-silicon alloy and sputtering target technology, which is applied in the field of preparation of chromium-silicon alloy sputtering targets, and achieves the effects of meeting the requirements of purity and density and having a simple preparation method.

Active Publication Date: 2021-07-06
KONFOONG MATERIALS INTERNATIONAL CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The preparation method can only realize the preparation of chromium-silicon alloy sputtering targets with a silicon content of 40-70wt%, and for the preparation of sputtering targets with a silicon content of <40wt% and a low silicon content, new conditions need to be explored. To ensure that the density and purity of the low-silicon content sputtering target can meet the process requirements

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  • Preparation method of chromium-silicon alloy sputtering target material
  • Preparation method of chromium-silicon alloy sputtering target material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] 本实施例提供了一种铬硅合金溅射靶材的制备方法,所述制备方法包括如下步骤:

[0064] (1)V型混粉机中,氮气气氛下球磨混合铬粉与硅粉,得到混合料,混合料中硅粉的质量分数为15wt%;所述铬粉的粒径范围为30-60μm,铬粉的纯度为5N,所述硅粉的粒径<2μm,硅粉的纯度为5N;所述球磨混合所用研磨球为硅球,料球比为10:1,球磨混合的时间为40h;

[0065] (2)步骤(1)所得混合料装入石墨模具,压实使平面度≤0.3mm,然后抽真空至真空度降至70Pa;

[0066] (3)完成步骤(2)所述抽真空处理后,进行第一热处理,第一热处理过程中压力不超过6MPa;所述第一热处理的温度为1150℃;第一热处理的升温速率为8℃ / min;第一热处理的保温时间为90min;

[0067] (4)依次进行第二热处理、第一加压、第二加压与保温保压;所述第二热处理的温度为1320℃,升温速率为5℃ / min,保温时间80min;所述第一加压为45min均匀加压至20MPa;所述第二加压为45min均匀加压至30MPa;所述保温保压的时间为120min;

[0068] (5)保温保压结束后进行氮气置换,至压力为-0.07MPag,然后随炉冷却至150℃;

[0069] (6)机加工至所需尺寸,完成铬硅合金溅射靶材的制备。

Embodiment 2

[0071] 本实施例提供了一种铬硅合金溅射靶材的制备方法,所述制备方法包括如下步骤:

[0072] (1)V型混粉机中,氩气气氛下球磨混合铬粉与硅粉,得到混合料,混合料中硅粉的质量分数为15wt%;所述铬粉的粒径范围为30-60μm,铬粉的纯度为5N,所述硅粉的粒径<3μm,硅粉的纯度为5N;所述球磨混合所用研磨球为铬球,料球比为9:1,球磨混合的时间为38h;

[0073] (2)步骤(1)所得混合料装入石墨模具,压实使平面度≤0.2mm,然后抽真空至真空度降至80Pa;

[0074] (3)完成步骤(2)所述抽真空处理后,进行第一热处理,第一热处理过程中压力不超过6MPa;所述第一热处理的温度为1120℃;第一热处理的升温速率为6℃ / min;第一热处理的保温时间为95min;

[0075] (4)依次进行第二热处理、第一加压、第二加压与保温保压;所述第二热处理的温度为1300℃,升温速率为4.5℃ / min,保温时间90min;所述第一加压为40min均匀加压至20MPa;所述第二加压为40min均匀加压至30MPa;所述保温保压的时间为110min;

[0076] (5)保温保压结束后进行氩气置换,至压力为-0.07MPag,然后随炉冷却至180℃;

[0077] (6)机加工至所需尺寸,完成铬硅合金溅射靶材的制备。

Embodiment 3

[0079] 本实施例提供了一种铬硅合金溅射靶材的制备方法,所述制备方法包括如下步骤:

[0080] (1)V型混粉机中,氦气气氛下球磨混合铬粉与硅粉,得到混合料,混合料中硅粉的质量分数为15wt%;所述铬粉的粒径范围为30-60μm,铬粉的纯度为5N,所述硅粉的粒径<3μm,硅粉的纯度为5N;所述球磨混合所用研磨球为铬球,料球比为11:1,球磨混合的时间为42h;

[0081] (2)步骤(1)所得混合料装入石墨模具,压实使平面度≤0.4mm,然后抽真空至真空度降至60Pa;

[0082] (3)完成步骤(2)所述抽真空处理后,进行第一热处理,第一热处理过程中压力不超过6MPa;所述第一热处理的温度为1180℃;第一热处理的升温速率为9℃ / min;第一热处理的保温时间为85min;

[0083](4) Carry out the second heat treatment, the first pressurization, the second pressurization and heat preservation and pressure keeping in sequence; the temperature of the second heat treatment is 1330°C, the heating rate is 5.5°C / min, and the holding time is 70min; the first The pressurization is uniformly pressurized to 20MPa for 50min; the second pressurization is uniformly pressurized to 30MPa for 50min; the time for the heat preservation and pressure holding is 140min;

[0084] (5) After heat preservation and pressure holding, helium replacement is carried out until the pressure is -0.07MPag, and then cooled to 180°...

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Abstract

The invention provides a preparation method of a chromium-silicon alloy sputtering target material. The preparation method comprises the following steps that chromium powder and silicon powder are subjected to ball-milling and mixing in a protective atmosphere to obtain a mixture, and the mass fraction of the silicon powder in the mixture is not more than 16wt%; the obtained mixture is loaded into a mold and compacted, and then vacuum-pumping treatment is carried out; after the vacuumizing treatment is completed, first heat treatment is carried out, and the pressure in the first heat treatment process does not exceed 6 MPa; second heat treatment, first pressurization, second pressurization and heat preservation and pressure maintaining are carried out in sequence; after heat preservation and pressure maintaining are finished, protective gas replacement is carried out till the pressure ranges from-0.06 MPag to-0.08 MPag, and then cooling in furnace is carried out; and machining is carried out to a required size to complete the preparation of the chromium-silicon alloy sputtering target material. According to the preparation method, the chromium-silicon alloy target material with the silicon content not exceeding 16wt% can be prepared, and the density of the prepared target material is greater than 99%, the purity is greater than or equal to 99.95%, and the requirements of magnetron sputtering on the purity and density of the target material are met.

Description

technical field [0001] The invention belongs to the technical field of semiconductors and relates to a method for preparing a target, in particular to a method for preparing a chromium-silicon alloy sputtering target. Background technique [0002] Physical vapor deposition refers to the use of low-voltage, high-current arc discharge technology under vacuum conditions, using gas discharge to evaporate the material source and ionize both the evaporated substance and the gas, and then through the acceleration of the electric field, the vaporized Substances and their reaction products are deposited on the workpiece to form a thin film with a special function. PVD technology is the core technology of various industries such as semiconductor chip manufacturing, solar energy industry, and LCD manufacturing industry. The main methods include vacuum coating, arc plasma plating, ion coating, molecular beam epitaxy and sputtering coating, etc. [0003] Sputtering is one of the main me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35C23C14/14C22C27/06B22F9/04B22F3/02B22F3/24
CPCC23C14/3414C23C14/35C23C14/14B22F9/04B22F3/02B22F3/24C22C27/06B22F2009/043B22F2003/248
Inventor 姚力军边逸军潘杰王学泽杨慧珍
Owner KONFOONG MATERIALS INTERNATIONAL CO LTD
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