Processing technology of pure molybdenum target material

Abstract

The invention provides a processing technology of a pure molybdenum target material. The processing technology comprises the following steps: carrying out first milling processing on a welding surface of the pure molybdenum target material by using a cutter; carrying out second milling on the welding surface of the pure molybdenum target material by using a cutter; performing third milling on the outline of the pure molybdenum target material by using a cutter; and carrying out fourth milling on the R angle of the pure molybdenum target material by using the cutter. According to the processing technology, the problem that the LCD plane target material is Arcinampp due to stress residue can be effectively solved; the thickness of a stress layer on the surface of the target material after machining is effectively controlled, and normal use of the target material in the sputtering process is guaranteed.

Description

Technical Field

[0001] The invention belongs to the field of LCD target material processing and relates to a processing technology of a pure molybdenum target material. Background Art

[0002] As a rare metal material, molybdenum has many excellent properties such as high melting point, high conductivity, low impedance, corrosion resistance, etc. Based on the above characteristics, molybdenum targets are widely used in the electronics industry. According to market demand, molybdenum targets are mainly used in flat panel displays, thin-film solar cell electrodes, wiring materials, and semiconductor barrier layer materials. Especially in the flat panel display industry, molybdenum is used in LCD components, which can greatly improve the performance of liquid crystal displays in terms of brightness, contrast, color, and life, and has therefore become one of the basic materials for sputtering targets for flat panel displays.

[0003] In recent years, with the continuous expansion of market demand for flat panel displays, the market demand for sputtering molybdenum targets required for the PVD preparation process has become increasingly strong. According to statistics, the global market demand for molybdenum targets is growing at a rate of 20% per year. As a major manufacturing country in the world, China's market demand for molybdenum targets is growing at a rate of more than 30% per year. However, as a capital-intensive, high-tech product, flat panel displays were once China's largest imported commodity after integrated circuit boards, oil, and iron ore. It was not until 2010 that my country's first 8.5-generation line was put into production, and it began to get rid of the dependence of 32-inch and 55-inch LCD TVs on foreign panels. In particular, with the commissioning of G8.5-generation lines and G10.5-generation lines of flat panel display companies represented by BOE, Huaxing Optoelectronics, and China Electronics, the demand for high-generation molybdenum targets has exploded.

[0004] However, pure molybdenum materials are difficult to process, and existing processing techniques make it difficult to effectively control processing efficiency, which often causes abnormalities in pure molybdenum target materials during processing.

[0005] CN108642457A A production method for high-generation molybdenum target materials, the production method comprising: 1. Mixing two molybdenum powders with different particle size ranges under vacuum conditions, and obtaining a mixed powder after sieving; 2. Isostatic pressing the mixed powder; 3. Sintering treatment; 4. Hot rolling treatment; 5; Vacuum annealing; 6. Water cutting, milling, and grinding. The molybdenum target material obtained by this method has a length of more than 3500mm, a thickness of ≤30mm, a width of ≤600mm, a flatness of less than 0.08mm, and a molybdenum content of ≥99.97%. The production method has high production efficiency, and the density of the obtained high-generation molybdenum target material is ≥99.5%. The internal structure of the molybdenum target material has no defects such as pores, cracks, delamination, and inclusions. Its surface roughness is <0.6μm, the average grain size is ≤80μm, and the grain size is uniform. It can be used as a high-purity molybdenum target for the production of G10.5 generation line flat panel displays. However, the thickness of the surface stress layer of the molybdenum target material prepared by this method is still relatively thick, and the Arcing phenomenon will occur in users.

[0006] CN109811318A discloses a method for preparing a high-purity molybdenum sputtering target. The method comprises the following steps: using a molybdenum alloy with a purity of more than 99.9% produced by a sputtering method as a raw material, melting a high-purity molybdenum blank (with a purity of more than 99.98%) by an electron beam cold bed furnace, milling the molybdenum blank, grinding the molybdenum square billet, cutting the head, and then cutting the molybdenum blank into the size required by the forging blank. The forging blank is inspected for flaws, and a qualified forging blank is heated to 980-1020° C. The forging blank is forged by three upsetting and three drawing processes. During the final drawing process, the forging is die-forged into a bar of required specifications, and the surface oxide scale of the bar is removed by turning after the forging is annealed. The forging caps at both ends are removed and the forging blocks are sawn into small columns of required specifications. The two sawn end faces of the small column block are polished, the bottom is milled inside to reserve an edge, the reserved edge is chamfered, and the other end is threaded. After further cleaning, a cylindrical molybdenum sputtering target is obtained. However, the thickness of the stress layer on the surface of the molybdenum target material prepared by this method is also relatively thick, and abnormal discharge may occur during use. Summary of the invention

[0007] In order to solve the above technical problems, the present invention provides a processing technology for pure molybdenum target material, which can effectively solve the abnormal discharge phenomena such as Arcing & splash of LCD flat target material caused by residual stress, effectively control the thickness of the stress layer on the surface of the target material after machining, and ensure the normal use of the target material during the sputtering process.

[0008] In order to achieve the above technical effects, the present invention adopts the following technical solutions:

[0009] The present invention provides a processing technology for a pure molybdenum target material, and the processing technology comprises:

[0010] Using a tool to perform a first milling process on the welding surface of the pure molybdenum target material;

[0011] Using a tool to perform a second milling process on the welding surface of the pure molybdenum target material;

[0012] Using a tool to perform a third milling process on the outer contour of the pure molybdenum target material;

[0013] The R corner of the pure molybdenum target material is subjected to a fourth milling process using a tool.

[0014] As a preferred technical solution of the present invention, the tool used in the first milling process is an R245 tool.

[0015] Preferably, the model of the R245 tool is 12T3K-MM2030.

[0016] Preferably, the number of blades used in the first milling process is 5 to 15, such as 6, 7, 8, 9, 10, 11, 12, 13 or 14, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0017] As a preferred technical solution of the present invention, the rotation speed of the first milling process is 200-300 rpm, such as 210 rpm, 220 rpm, 230 rpm, 240 rpm, 250 rpm, 260 rpm, 270 rpm, 280 rpm or 290 rpm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0018] Preferably, the feed rate of the first milling process is 500-700, such as 520, 550, 580, 600, 620, 650 or 680, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0019] As a preferred technical solution of the present invention, the tool used in the second milling process is an R245 tool.

[0020] Preferably, the model of the R245 tool is 12T3K-MM2030.

[0021] Preferably, the number of blades used in the second milling process is 2 to 5, such as 2, 3, 4 or 5, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0022] As a preferred technical solution of the present invention, the rotation speed of the second milling process is 200-300 rpm, such as 210 rpm, 220 rpm, 230 rpm, 240 rpm, 250 rpm, 260 rpm, 270 rpm, 280 rpm or 290 rpm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0023] Preferably, the feed rate of the second milling process is 100-300, such as 120, 150, 180, 200, 220, 250 or 280, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0024] As a preferred technical solution of the present invention, the tool used in the third milling process is a D20 tool.

[0025] Preferably, the D20 tool is made of tungsten steel.

[0026] As a preferred technical solution of the present invention, the rotation speed of the third milling process is 1600-2000rpm, such as 1650rpm, 1700rpm, 1750rpm, 1800rpm, 1850rpm, 1900rpm or 1950rpm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0027] Preferably, the feed rate of the third milling process is 800-1200, such as 850, 900, 950, 1000, 1050, 1100 or 1150, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0028] As a preferred technical solution of the present invention, the tool used in the fourth milling process is an R3.5 tool.

[0029] Preferably, the model of the R3.5 tool is R3.5*75*D10MM.

[0030] As a preferred technical solution of the present invention, the rotation speed of the fourth milling process is 2500-3500rpm, such as 2600rpm, 2700rpm, 2800rpm, 2900rpm, 3000rpm, 3100rpm, 3200rpm, 3300rpm or 3400rpm, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0031] Preferably, the feed rate of the fourth milling process is 800-1200, such as 850, 900, 950, 1000, 1050, 1100 or 1150, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0032] As a preferred technical solution of the present invention, the processing technology of the above-mentioned pure molybdenum target material includes:

[0033] The welding surface of the pure molybdenum target is first milled using an R245 tool of model 12T3K-MM2030, with 5 to 15 blades, a rotation speed of 200 to 300 rpm, and a feed rate of 500 to 700;

[0034] The welding surface of the pure molybdenum target is subjected to a second milling process using an R245 tool of model 12T3K-MM2030, with 2 to 5 blades, a rotation speed of 200 to 300 rpm, and a feed rate of 100 to 300;

[0035] The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 1600-2000 rpm and a feed rate of 800-1200;

[0036] The R3.5 cutter with the model of R3.5*75*D10MM is used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 2500-3500rpm and a feed rate of 800-1200.

[0037] Compared with the prior art, the present invention has at least the following beneficial effects:

[0038] The present invention provides a processing technology for a pure molybdenum target material, which can effectively solve abnormal discharge phenomena such as arcing and splashing of LCD flat target materials caused by residual stress, effectively control the thickness of the stress layer on the surface of the target material after machining, and ensure the normal use of the target material during the sputtering process. DETAILED DESCRIPTION

[0039] For the convenience of understanding the present invention, the present invention lists the following embodiments. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0040] Example 1

[0041] This embodiment provides a processing technology for a pure molybdenum target material, and the process includes:

[0042] The welding surface of the pure molybdenum target material is first milled using an R245 tool with a model of 12T3K-MM2030, with 5 blades, a rotation speed of 300 rpm, and a feed rate of 700;

[0043] The welding surface of the pure molybdenum target material is subjected to a second milling process using an R245 tool with a model number of 12T3K-MM2030, with two blades, a rotation speed of 300 rpm, and a feed rate of 300;

[0044] The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 1600 rpm and a feed rate of 800;

[0045] The R3.5 cutter with the model of R3.5*75*D10MM was used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 2500 rpm and a feed rate of 800.

[0046] Example 2

[0047] This embodiment provides a processing technology for a pure molybdenum target material, and the process includes:

[0048] The welding surface of the pure molybdenum target material is first milled using an R245 tool with a model of 12T3K-MM2030, with 15 blades, a rotation speed of 200 rpm, and a feed rate of 500;

[0049] The welding surface of the pure molybdenum target material is subjected to a second milling process using an R245 tool with a model number of 12T3K-MM2030, with 5 blades, a rotation speed of 200 rpm, and a feed rate of 100;

[0050] The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 2000 rpm and a feed rate of 1200;

[0051] The R3.5 cutter with the model of R3.5*75*D10MM was used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 3500 rpm and a feed rate of 1200.

[0052] Example 3

[0053] This embodiment provides a processing technology for a pure molybdenum target material, and the process includes:

[0054] The welding surface of the pure molybdenum target material is first milled using an R245 tool with a model of 12T3K-MM2030, with 10 blades, a rotation speed of 240 rpm, and a feed rate of 600;

[0055] The welding surface of the pure molybdenum target material is subjected to a second milling process using an R245 tool with a model number of 12T3K-MM2030, with 3 blades, a rotation speed of 240 rpm, and a feed rate of 200;

[0056] The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 1800 rpm and a feed rate of 1000;

[0057] The R3.5 cutter with the model of R3.5*75*D10MM was used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 3000 rpm and a feed rate of 1000.

[0058] Example 4

[0059] This embodiment provides a processing technology for a pure molybdenum target material, and the process includes:

[0060] The welding surface of the pure molybdenum target material is first milled using an R245 tool with a model of 12T3K-MM2030, with 8 blades, a rotation speed of 280 rpm, and a feed rate of 650;

[0061] The welding surface of the pure molybdenum target material is subjected to a second milling process using an R245 tool with a model number of 12T3K-MM2030, with 3 blades, a rotation speed of 280 rpm, and a feed rate of 250;

[0062] The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 1900 rpm and a feed rate of 1100;

[0063] The R3.5 cutter with the model of R3.5*75*D10MM was used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 3200 rpm and a feed rate of 1100.

[0064] Example 5

[0065] This embodiment provides a processing technology for a pure molybdenum target material, and the process includes:

[0066] The welding surface of the pure molybdenum target material is first milled using an R245 tool with a model number of 12T3K-MM2030, with 12 blades, a rotation speed of 220 rpm, and a feed rate of 550;

[0067] The welding surface of the pure molybdenum target material is subjected to a second milling process using an R245 tool with a model number of 12T3K-MM2030, with 4 blades, a rotation speed of 220 rpm, and a feed rate of 150;

[0068] The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 1700 rpm and a feed rate of 900;

[0069] The R3.5 cutter with the model of R3.5*75*D10MM was used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 2800 rpm and a feed rate of 900.

[0070] Comparative Example 1

[0071] In this comparative example, except that the tools for the first milling process and the second milling process are replaced by R245 tools of 12T3M-PM4230, the other conditions are the same as those of Example 3.

[0072] Comparative Example 2

[0073] In this comparative example, except that the tool for the first milling process is replaced by R24 of 12T3M-PM4230, the other conditions are the same as those of Example 3.

[0074] Comparative Example 3

[0075] In this comparative example, except that the tool for the second milling process is replaced by R24 of 12T3M-PM4230, the other conditions are the same as those of Example 3.

[0076] The pure molybdenum target materials obtained after processing in Examples 1-5 and Comparative Examples 1-3 were sputtered 50 times respectively, and the number of times the arcing & splashing problems occurred was recorded, 0 times was level I, 1-2 times was level II, and the rest were level III. The results are shown in Table 1.

[0077] Table 1

[0078] Pure Molybdenum Target Grade Example 1 Level I Example 2 Level I Example 3 Level I Example 4 Level I Example 5 Level II Comparative Example 1 Level III Comparative Example 2 Level II Comparative Example 3 Level II

[0079] The applicant declares that the present invention illustrates the detailed process equipment and process flow of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, that is, it does not mean that the present invention must rely on the above-mentioned detailed process equipment and process flow to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A processing technology for pure molybdenum target material, characterized in that: The processing technology includes: Using a tool to perform a first milling process on the welding surface of the pure molybdenum target material; Using a tool to perform a second milling process on the welding surface of the pure molybdenum target material; Using a tool to perform a third milling process on the outer contour of the pure molybdenum target material; The R corner of the pure molybdenum target material is subjected to a fourth milling process using a tool.

2. The processing technology according to claim 1, characterized in that: The tool used in the first milling process is an R245 tool; Preferably, the model of the R245 tool is 12T3K-MM2030+Santak; Preferably, the number of blades used in the first milling process is 5 to 15.

3. The processing technology according to claim 1 or 2, characterized in that: The first milling process has a rotation speed of 200 to 300 rpm; Preferably, the feed rate of the first milling process is 500-700.

4. The processing technology according to any one of claims 1 to 3, characterized in that: The tool used in the second milling process is an R245 tool; Preferably, the model of the R245 tool is 12T3K-MM2030; Preferably, the number of blades used in the second milling process is 2 to 5.

5. The processing technology according to any one of claims 1 to 4, characterized in that: The second milling process has a rotation speed of 200 to 300 rpm; Preferably, the feed rate of the second milling process is 100-300.

6. The processing technology according to any one of claims 1 to 5, characterized in that: The tool used in the third milling process is a D20 tool; Preferably, the D20 tool is made of tungsten steel.

7. The processing technology according to any one of claims 1 to 6, characterized in that: The rotation speed of the third milling process is 1600-2000 rpm; Preferably, the feed rate of the third milling process is 800-1200.

8. The processing technology according to any one of claims 1 to 7, characterized in that: The tool used in the fourth milling process is an R3.5 tool; Preferably, the model of the R3.5 tool is R3.5*75*D10MM.

9. The processing technology according to any one of claims 1 to 8, characterized in that: The fourth milling process has a rotation speed of 2500-3500 rpm; Preferably, the feed rate of the fourth milling process is 800-1200.

10. The processing technology according to any one of claims 1 to 9, characterized in that: The processing technology includes: The welding surface of the pure molybdenum target is first milled using an R245 tool of model 12T3K-MM2030, with 5 to 15 blades, a rotation speed of 200 to 300 rpm, and a feed rate of 500 to 700; The welding surface of the pure molybdenum target is subjected to a second milling process using an R245 tool of model 12T3K-MM2030, with 2 to 5 blades, a rotation speed of 200 to 300 rpm, and a feed rate of 100 to 300; The outer contour of the pure molybdenum target material is subjected to a third milling process using a tungsten steel D20 tool, with a rotation speed of 1600-2000 rpm and a feed rate of 800-1200; The R3.5 cutter with the model of R3.5*75*D10MM is used to perform the fourth milling process on the R angle of the pure molybdenum target material, with a rotation speed of 2500-3500rpm and a feed rate of 800-1200.