CN113579862A - Method for reducing pre-sputtering time of copper target - Google Patents
Method for reducing pre-sputtering time of copper target Download PDFInfo
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- CN113579862A CN113579862A CN202110907393.4A CN202110907393A CN113579862A CN 113579862 A CN113579862 A CN 113579862A CN 202110907393 A CN202110907393 A CN 202110907393A CN 113579862 A CN113579862 A CN 113579862A
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- polishing
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- sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
Abstract
The invention provides a method for reducing the pre-sputtering time of a copper target, which comprises the following steps: sequentially carrying out mechanical processing, primary polishing and secondary polishing on the sputtering surface of the copper target material, and carrying out pre-sputtering after the secondary polishing; the secondary polishing is grinding and polishing; the grinding fluid used for grinding and polishing comprises aluminum oxide grinding fluid and/or SiO2Grinding fluid; the method effectively reduces the roughness of the sputtering surface of the copper target by combining three processes of mechanical processing, mechanical polishing and grinding and polishing, thereby shortening the pre-sputtering time, improving the production efficiency and being beneficial to industrial application.
Description
Technical Field
The invention belongs to the technical field of sputtering targets, and particularly relates to a method for reducing the pre-sputtering time of a copper target.
Background
With the rapid development of very large scale integrated circuits, the size of chips for semiconductors has been reduced to nanometer level, RC delay and electromigration of metal interconnects have become major factors affecting the performance of chips, and conventional aluminum and aluminum alloy interconnects have not been able to meet the requirements of process of very large scale integrated circuits. Compared with aluminum, copper has higher electromigration resistance and higher conductivity, especially ultra-high-purity copper (the purity is more than or equal to 6N), and has important significance for reducing the resistance of a chip interconnection line and improving the operation speed of the chip interconnection line.
Generally, the target material is unstable in the initial stage of sputtering, which is mainly caused by inconsistency between the physical properties of the surface of the target material and the interior of the target material, namely, a processing strain layer and extremely fine scraps are formed on the surface of the target material during mechanical processing, so that the problems of arc, Particle and the like in the PVD (physical vapor deposition) coating process can be caused, the coating uniformity is seriously affected, meanwhile, the phenomenon of higher RS resistance of the film can be caused, and even the wafer is directly scrapped. To solve the above problems, the conventional wafer manufacturing plant usually performs pre-sputtering on a silicon wafer. The pre-sputtering takes longer time and has lower production efficiency, so the development of the target with shorter pre-sputtering time is a problem which needs to be solved urgently at present.
CN110004420A discloses a method for preparing a target, which comprises the following steps: cleaning raw materials, carrying out heat treatment on the cleaned target material, carrying out cold isostatic pressing operation on the target material with a certain shape, boosting the pressure of the target material at normal temperature, keeping the pressure for 8-15min, and carrying out annealing treatment in a top electrode non-holding mode to remove the surface pressure of the target material; placing the treated target on a sample table of magnetron sputtering, introducing argon at the bottom of the target, performing pre-sputtering on the target, introducing mixed gas of high-purity argon and oxygen, and sputtering the target to finally obtain the target; in the method, the pre-sputtering time is at least 6min, the time consumption is long, and the production efficiency is reduced.
In summary, how to provide a target processing method that can reduce the pre-sputtering time, improve the production efficiency and reduce the cost is a problem to be solved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for reducing the pre-sputtering time of a copper target, which effectively reduces the roughness of the sputtering surface of the copper target by combining three processes of machining, mechanical polishing and grinding and polishing, thereby shortening the pre-sputtering time, improving the production efficiency and being beneficial to industrial application.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for reducing the pre-sputtering time of a copper target, said method comprising the steps of:
sequentially carrying out mechanical processing, primary polishing and secondary polishing on the sputtering surface of the copper target material, and carrying out pre-sputtering after the secondary polishing;
the secondary polishing is grinding and polishing;
the grinding fluid used for grinding and polishing comprises aluminum oxide grinding fluid and/or SiO2And (3) grinding fluid.
In the invention, the method adopts alumina grinding fluid and/or SiO on the basis of mechanical processing and primary polishing2The grinding liquid is used for grinding and polishing, so that scratches of mechanical processing and primary polishing can be further removed, the surface roughness is reduced, and the roughness of the target ejection surface can be effectively improved, so that the pre-sputtering time is shortened, the cost of a silicon test piece is saved, and the stability of the performance of the copper target sputtering process is ensured; the method has simple process, effectively improves the production efficiency and has better industrial application prospect.
In the invention, the primary polishing belongs to a mechanical polishing means.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferred technical solution of the present invention, the copper target includes an ultra-high pure copper target or a copper alloy target.
The purity of the ultra-high purity copper is not less than 6N, such as 99.99991%, 99.99992%, 99.99994%, 99.99996% or 99.99998%, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, the vertical feed amount of the machining is 0.05 to 0.15mm, for example, 0.05mm, 0.06mm, 0.07mm, 0.08mm, 0.09mm, 0.1mm, 0.11mm, 0.12mm, 0.13mm, 0.14mm, or 0.15mm, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range of values are also applicable, and preferably 0.09 to 0.11 mm.
As a preferred technical scheme of the invention, the rotation speed of the tool for machining is 300-.
Preferably, the machining has a horizontal feed of 0.05 to 0.12mm, for example 0.05mm, 0.06mm, 0.07mm, 0.08mm, 0.09mm, 0.1mm, 0.11mm, 0.12mm, etc., but is not limited to the recited values, and other values not recited within the range of values are equally applicable, preferably 0.07 to 0.09 mm.
As a preferable technical scheme of the invention, the primary polishing is carried out by using scouring pad.
Preferably, the mesh size of the scouring pad is 600-1000 meshes, such as 600 meshes, 650 meshes, 700 meshes, 750 meshes, 800 meshes, 850 meshes, 900 meshes, 850 meshes or 1000 meshes, but not limited to the enumerated values, and other non-enumerated values within the numerical range are also applicable, preferably 750-850 meshes.
Preferably, after the primary polishing, the roughness of the copper target sputtering surface is 1.3 to 1.6 μm, for example, 1.3 μm, 1.4 μm, 1.5 μm, or 1.6 μm, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred technical solution of the present invention, the SiO2SiO in grinding fluid2The particle diameter of (B) is 0.4 to 0.6. mu.m, for example, 0.4. mu.m, 0.42. mu.m, 0.46. mu.m, 0.48. mu.m, 0.5. mu.m, 0.52. mu.m, 0.54. mu.m, 0.56. mu.m, 0.58. mu.m or 0.6. mu.m, but the particle diameter is not limited to the above-mentioned numerical values, and other numerical values not listed in the numerical value range are also applicable.
Preferably, the particle size of the alumina in the alumina polishing slurry is 0.4 to 0.6. mu.m, for example, 0.4. mu.m, 0.42. mu.m, 0.46. mu.m, 0.48. mu.m, 0.5. mu.m, 0.52. mu.m, 0.54. mu.m, 0.56. mu.m, 0.58. mu.m, or 0.6. mu.m, but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
In the present invention, the particle size of the abrasive used in the polishing liquid needs to be controlled, and if the particle size is too large, the surface roughness after mechanical polishing cannot be further reduced; if the particle size is too small, the production efficiency is extremely low, which is not favorable for industrial production.
As a preferable technical scheme of the invention, the grinding pad used for grinding and polishing comprises a wool pad.
According to the invention, the wool pad and the grinding fluid are matched for use, so that the surface roughness of the target can be effectively reduced and can reach 0.3-0.6 mu m.
In a preferred embodiment of the present invention, the rotation speed of the polishing head during the polishing process is 50 to 80r/min, for example, 50r/min, 55r/min, 60r/min, 65r/min, 70r/min, 75r/min, or 80r/min, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned value range are also applicable.
In the invention, the rotation speed of the grinding head has certain influence on the final polishing effect. If the rotating speed is too slow, the production efficiency is reduced; if the rotation speed is too high, the surface of the material is heated and oxidized.
In a preferred embodiment of the present invention, the time for polishing is 2 to 3 hours, such as 2 hours, 2.2 hours, 2.4 hours, 2.6 hours, 2.8 hours, or 3 hours, but is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
As a preferred embodiment of the present invention, after the polishing, the roughness of the sputtering surface of the copper target is 0.3 to 0.6. mu.m, for example, 0.3. mu.m, 0.35. mu.m, 0.4. mu.m, 0.45. mu.m, 0.5. mu.m, 0.55. mu.m, or 0.6. mu.m, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned numerical value range are also applicable.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method combines three processes of mechanical processing, mechanical polishing and grinding and polishing, and effectively reduces the roughness of the sputtering surface of the target by further controlling the process conditions in the grinding and polishing, so that the roughness reaches 0.3-0.6 mu m, the pre-sputtering time is shortened, the cost of a silicon test piece is saved, the pre-sputtering time is within 5min, and the silicon test piece can be saved by more than 10 pieces, and can reach 13 pieces at most;
(2) the method has the advantages of simple process flow and low cost, and is suitable for industrial production.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a method for reducing the pre-sputtering time of a copper target, which comprises the following steps:
providing an ultra-high pure copper target material with the diameter of 460mm and the purity of 6N;
(1) and machining the sputtering surface of the ultra-high pure copper target, wherein the parameter conditions in the machining process are as follows: the rotating speed of the cutter is 500r/min, the vertical feed amount is 0.1mm, and the horizontal feed amount is 0.08 mm;
(2) after the mechanical processing, the scouring pad with 800 meshes is adopted for polishing once, so that the roughness of the sputtering surface reaches 1.2 mu m;
(3) after the primary polishing, the ultra-high pure copper target material is placed on a wool pad, and SiO with the grain diameter of 0.5 mu m is adopted2The polishing liquid was applied to the sputtering surface at a rate of 50r/min for 2 hours to obtain a surface roughness of 0.5. mu.m.
Example 2:
the embodiment provides a method for reducing the pre-sputtering time of a copper target, which comprises the following steps:
providing a copper alloy target (Cu-0.25 at% Al) with a diameter of 460 mm;
(1) and machining the sputtering surface of the copper alloy target, wherein the parameter conditions in the machining process are as follows: the rotating speed of the cutter is 300r/min, the vertical feed amount is 0.05mm, and the horizontal feed amount is 0.05 mm;
(2) after the mechanical processing, the scouring pad with 600 meshes is adopted for polishing once, so that the roughness of the sputtering surface reaches 1.6 mu m;
(3) after the primary polishing, the copper alloy target material is placed on a wool pad, and SiO with the grain diameter of 0.4 mu m is adopted2The polishing liquid was applied to the sputtering surface at a rate of 80r/min for 3 hours to obtain a sputtering surface having a roughness of 0.3. mu.m.
Example 3:
the embodiment provides a method for reducing the pre-sputtering time of a copper target, which comprises the following steps:
providing an ultra-high pure copper target material with the diameter of 460mm and the purity of 99.99995 percent;
(1) and machining the sputtering surface of the ultra-high pure copper target, wherein the parameter conditions in the machining process are as follows: the rotating speed of the cutter is 600r/min, the vertical feed amount is 0.15mm, and the horizontal feed amount is 0.12 mm;
(2) after the mechanical processing, the scouring pad with 800 meshes is adopted for polishing once, so that the roughness of the sputtering surface reaches 1.3 mu m;
(3) after the primary polishing, the ultra-high pure copper target material is placed on a wool pad, and the sputtering surface is ground for 2.4 hours at the rotating speed of 60r/min by using alumina grinding fluid, so that the roughness of the sputtering surface reaches 0.4 mu m.
Example 4:
this example provides a method for reducing the pre-sputtering time of a copper target, which is described with reference to the method of example 2, except that: and (4) grinding the sputtering surface at the rotating speed of 100r/min in the step (3) to ensure that the roughness of the sputtering surface is 0.6 mu m.
The surface of the sputtering surface is oxidized due to the over-high rotating speed, so that the use requirement is not met.
Example 5:
this example provides a method for reducing the pre-sputtering time of a copper target, which is described with reference to the method of example 1, except that: the polishing pad used in step (3) was a velvet polishing pad, so that the roughness of the sputtering surface was 0.8 μm.
Example 6:
this example provides a method for reducing the pre-sputtering time of a copper target, which is described with reference to the method of example 1, except that: step (3) SiO2SiO in grinding fluid2The grain size of (2) was 0.7 μm so that the roughness of the sputtered surface was 0.8. mu.m.
Comparative example 1:
this example provides a method for reducing the pre-sputtering time of a copper target, which is described with reference to the method of example 1, except that: the grinding liquid adopted in the step (3) is conventional SiO2Polishing slurry of SiO2Has a grain size of 50 μm so that the roughness of the sputtered surface becomes 55 μm.
Comparative example 2:
this example provides a method for reducing the pre-sputtering time of a copper target, which is described with reference to the method of example 1, except that: grinding and polishing in the step (3) are not carried out.
The targets obtained in examples 1 to 6 and comparative examples 1 to 2 were subjected to pre-sputtering using silicon test pieces, the time taken for the pre-sputtering was measured, and the number of the silicon test pieces used for the pre-sputtering was calculated, and the results are shown in table 1.
TABLE 1
| Pre-sputtering time/min | Number of silicon test pieces/piece | |
| Example 1 | 4 | 1 |
| Example 2 | 5 | 1 |
| Example 3 | 4.5 | 1 |
| Example 4 | 7.8 | 11 |
| Example 5 | 8.5 | 11 |
| Example 6 | 10.5 | 12 |
| Comparative example 1 | 10.6 | 13 |
| Comparative example 2 | 11 | 14 |
In the embodiment 1-3, the roughness of the sputtering surface of the copper target is reduced by combining three processes of mechanical processing, primary polishing and grinding and polishing, so that the pre-sputtering time is shortened to be within 5min, and the use amount of a silicon test piece is controlled to be 1; in example 4, the rotation speed of the grinding and polishing was increased, which affected the roughness of the sputtering surface, resulting in a longer pre-sputtering time, a larger amount of silicon test pieces used, and the surface of the sputtering surface appeared due to the excessively high rotation speedThermal oxidation is not in line with the use requirement; in example 5, the velvet grinding pad is used for grinding and polishing, so that the surface roughness of the sputtering surface is large, the pre-sputtering time is prolonged, and the number of used silicon test pieces is obviously increased; example 6 increases SiO in the millable liquid2The grain size of (2) causes a deterioration in the polishing effect, and thus the pre-sputtering time is long, and the number of silicon test pieces used is significantly increased.
While in comparative example 1 conventional SiO was used2The grinding liquid is ground and polished to cause the roughness of a sputtering surface to be obviously increased, thereby influencing the time of pre-sputtering; in comparative example 2, no lapping and polishing was performed, and the pre-sputtering time and the number of silicon test pieces used were significantly increased.
It can be seen from the above examples and comparative examples that the method of the present invention combines three processes of machining, mechanical polishing and grinding and polishing, and further controls the process conditions in grinding and polishing to effectively reduce the roughness of the sputtering surface of the target material to 0.3-0.6 μm, thereby shortening the pre-sputtering time and saving the cost of the silicon test piece, so that the pre-sputtering time is within 5min, and the silicon test piece can be saved by more than 10 pieces, up to 13 pieces; the method has simple process flow and low cost, and is suitable for industrial production.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents thereof, additions of additional operations, selection of specific ways, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A method for reducing the pre-sputtering time of a copper target, comprising the steps of:
sequentially carrying out mechanical processing, primary polishing and secondary polishing on the sputtering surface of the copper target material, and carrying out pre-sputtering after the secondary polishing;
the secondary polishing is grinding and polishing;
the grinding fluid used for grinding and polishing comprises aluminum oxide grinding fluid and/or SiO2And (3) grinding fluid.
2. The method of claim 1, wherein the copper target comprises an ultra-high purity copper target or a copper alloy target; the purity of the ultra-high purity copper is not less than 6N.
3. A method according to claim 1 or 2, characterized in that the machining has a vertical feed of 0.05-0.15mm, preferably 0.09-0.11 mm.
4. The method as claimed in any one of claims 1 to 3, wherein the tool rotation speed for the mechanical processing is 300-600r/min, preferably 450-550 r/min;
preferably, the machining has a horizontal feed of 0.05 to 0.12mm, preferably 0.07 to 0.09 mm.
5. The method according to any one of claims 1 to 4, wherein the primary polishing is performed with a scouring pad;
preferably, the mesh number of the scouring pad is 600-1000 meshes, preferably 750-850 meshes;
preferably, after the primary polishing, the roughness of the sputtering surface of the copper target is 1.3-1.6 μm.
6. The method of any of claims 1-5, wherein the SiO is2SiO in grinding fluid2The particle diameter of (A) is 0.4-0.6 μm;
preferably, the particle size of the alumina in the alumina grinding fluid is 0.4-0.6 μm.
7. The method as claimed in any one of claims 1 to 6, wherein the abrasive pad used for the abrasive polishing comprises a wool pad.
8. The method of any one of claims 1-7, wherein the rotational speed of the grinding head during the grinding and polishing is 50-80 r/min.
9. The method according to any one of claims 1 to 8, wherein the time for the grinding and polishing is 2 to 3 hours.
10. The method according to any one of claims 1 to 9, wherein the roughness of the copper target sputtering surface after the grinding and polishing is 0.3 to 0.6 μm.
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| JP4897113B2 (en) * | 2009-12-25 | 2012-03-14 | Ｊｘ日鉱日石金属株式会社 | Sputtering target with less generation of particles and method of manufacturing the target |
| TW201343329A (en) * | 2012-04-27 | 2013-11-01 | China Steel Corp | Method for increasing sputtering rate of metal target |
| CN106346344A (en) * | 2015-07-15 | 2017-01-25 | 宁波江丰电子材料股份有限公司 | Copper target material surface processing method |
| CN107866721A (en) * | 2016-09-26 | 2018-04-03 | 合肥江丰电子材料有限公司 | The processing method of target material assembly |
| CN113182941A (en) * | 2021-04-29 | 2021-07-30 | 合肥江丰电子材料有限公司 | Automatic polishing process method of copper-containing target material |
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2021
- 2021-08-09 CN CN202110907393.4A patent/CN113579862A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4897113B2 (en) * | 2009-12-25 | 2012-03-14 | Ｊｘ日鉱日石金属株式会社 | Sputtering target with less generation of particles and method of manufacturing the target |
| TW201343329A (en) * | 2012-04-27 | 2013-11-01 | China Steel Corp | Method for increasing sputtering rate of metal target |
| CN106346344A (en) * | 2015-07-15 | 2017-01-25 | 宁波江丰电子材料股份有限公司 | Copper target material surface processing method |
| CN107866721A (en) * | 2016-09-26 | 2018-04-03 | 合肥江丰电子材料有限公司 | The processing method of target material assembly |
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Application publication date: 20211102 |