A method for press forming a titanium pot-shaped target material, an integrally formed pot-shaped target material

Abstract

The application relates to a stamping forming method of a titanium pot-shaped target material and an integrally-formed pot-shaped target material, and particularly relates to the field of target material preparation. The stamping forming method comprises the following steps: sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on a titanium blank plate to obtain a titanium pot-shaped target material; the heat preservation temperature of the heat preservation treatment is 550-600 DEG C. The stamping forming method provided by the application integrally forms a flange and a pot body through a two-time stamping mode, guarantees the reliability and stability of the connection between the flange and the pot body, introduces heat preservation treatment between the two-time stamping, can obviously refine grains and optimize grain distribution, is beneficial to improving the use performance of the pot-shaped target material, and omits a welding process, and improves production efficiency.

Description

Technical Field

[0001] This invention relates to the field of target material preparation, specifically to a stamping method for titanium pot-shaped target material and an integrally formed pot-shaped target material. Background Technology

[0002] The HCM series sputtering targets are pot-shaped irregular targets, with the inner wall of the pot serving as the sputtering surface and the outer wall as the water-cooled surface. Raw materials for the HCM series targets include Cu, Ta, and Ti, and the core forming process is stamping. During use, the HCM series targets are assembled and fixed to the sputtering machine via flanges. Currently, the pot body and flange of the HCM series targets are generally connected using electron beam welding.

[0003] For example, CN113319417A discloses a method for electron beam welding of a target material for an HCM machine. The method includes: machining a raw material into a pot-shaped target body, machining the end face of the opening of the target body into a bevel, and machining one end face of the flange into a bevel as well; assembling the target body and the bevel of the flange into contact and fixing them into a tooling fixture; starting the electron beam welding equipment, evacuating the vacuum, and performing electron beam welding, with the direction of the electron beam parallel to the assembly surface, and obtaining the target material after welding.

[0004] CN115401304A discloses a method for connecting a pot-shaped target and a flange. The method includes the following steps: (1) machining a circular assembly groove around the outer wall of the pot-shaped target; (2) machining the flange and then dividing it radially to obtain a first flange and a second flange with identical shapes; the first flange and the second flange are both semi-circular in shape; (3) dividing the first flange and the second flange obtained in step (2) into left and right parts and inserting them into the assembly groove obtained in step (1), and then performing first electron beam welding, second electron beam welding and third electron beam welding in sequence to obtain a pot-shaped target for connecting the flange.

[0005] However, when using electron beam welding, the welding structure is usually welded in multiple passes. Multiple passes may cause the molten pool to interfere with each other, affecting the welding strength. The complex welding structure itself may also lead to a low welding qualification rate, which is not conducive to the efficient use of the pot-shaped target material. Summary of the Invention

[0006] In view of the problems existing in the prior art, the purpose of the present invention is to provide a stamping forming method for titanium pot-shaped target material and an integrally formed pot-shaped target material, so as to solve the defects of poor reliability and stability of flange and pot body connection in the existing titanium pot-shaped target material preparation method, as well as large grains and uneven grain distribution of target material after forming.

[0007] To achieve this objective, the present invention adopts the following technical solution:

[0008] In a first aspect, the present invention provides a method for stamping a titanium pot-shaped target, the stamping method comprising:

[0009] Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium billet;

[0010] The insulation temperature for the insulation treatment is 550-600℃.

[0011] The stamping forming method provided by the present invention integrally forms the flange and the pot body through two stamping processes, ensuring the reliability and stability of the connection between the flange and the pot body. At the same time, the heat preservation treatment introduced between the two stamping processes can significantly refine the grains and optimize the grain distribution, which is beneficial to improving the performance of the pot-shaped target material. Furthermore, the welding process is eliminated, thereby improving production efficiency.

[0012] As a preferred technical solution of the present invention, the stamping method of the pot shape includes: cold stamping.

[0013] Preferably, the heat preservation time is 60-120 minutes.

[0014] Preferably, the flange stamping method includes hot stamping.

[0015] As a preferred technical solution of the present invention, the heat preservation treatment is supplemented by ultrasound.

[0016] Preferably, the frequency of the ultrasound is 20-40 kHz.

[0017] Preferably, the power density of the ultrasound is 10-40 W / cm². 2 .

[0018] As a preferred embodiment of the present invention, the process of obtaining the titanium billet includes:

[0019] The titanium material is subjected to forging, first annealing, air cooling, cold rolling, second annealing and air cooling in sequence to obtain a titanium billet.

[0020] As a preferred technical solution of the present invention, the titanium material is preheated at 600-800℃ for 30-60 minutes before the forging begins.

[0021] As a preferred technical solution of the present invention, the deformation amount is controlled to be 60-80% during the forging process.

[0022] As a preferred technical solution of the present invention, the holding temperature of the first annealing is 500-700℃.

[0023] Preferably, the holding time for the first annealing is 60-120 minutes.

[0024] As a preferred technical solution of the present invention, the total deformation in the cold rolling process is controlled to be 50-70%.

[0025] As a preferred embodiment of the present invention, the holding temperature of the second annealing is 500-700℃.

[0026] Preferably, the holding time for the second annealing is 90-120 minutes.

[0027] Secondly, the present invention provides an integrally molded pot-shaped target material, which is prepared by the stamping forming method described in the first aspect.

[0028] Compared with existing technical solutions, the present invention has the following beneficial effects:

[0029] The stamping method provided by this invention introduces ultrasonic treatment during the heat preservation process. During the heat preservation process, the ultrasonic waves propagate within the grains and at the grain boundaries, generating periodic alternating shear stress and local micro-strain. This reduces the critical shear stress for dislocation slip and climb, thereby alleviating grain boundary segregation and second-phase agglomeration, avoiding grain size inhomogeneity caused by local compositional differences, and weakening the anisotropy of grain growth. This restricts the abnormal growth of dominant grains and achieves a narrow range of grain size distribution, thus enabling the preparation of high-performance pot-shaped targets. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the stamping process of the pot shape in the stamping forming method provided in the embodiment of the present invention;

[0031] Figure 2 This is a schematic diagram of the flange stamping process in the stamping forming method provided in the embodiment of the present invention.

[0032] The present invention will now be described in further detail. However, the examples described below are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention is determined by the claims. Detailed Implementation

[0033] To better illustrate the present invention and facilitate understanding of its technical solutions, typical but non-limiting embodiments of the present invention are as follows:

[0034] Currently, the forming of HCM series targets is based on stamping technology. During use, HCM series targets are assembled and fixed to the sputtering machine via flanges. Currently, the HCM series target body and flange are generally connected using electron beam welding. However, existing methods for preparing titanium pot-shaped targets suffer from poor reliability and stability in the flange-pot connection, as well as defects such as large and uneven grain size in the target material after forming. Therefore, this invention optimizes the stamping process, enabling the flange and pot body to be integrally formed, while significantly refining the grain size and optimizing the grain distribution. This results in a more uniform film layer obtained when the pot-shaped target is sputtered, as detailed below:

[0035] I. This embodiment provides a stamping forming method for a titanium pot-shaped target material, the stamping forming method comprising:

[0036] Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium blank.

[0037] In this invention, titanium refers to pure titanium or titanium alloys, etc.

[0038] In this invention, stamping refers to applying external force to sheet metal, strip metal, tube metal, and profile metal using a press and a die to shape the material into the desired form. The specific die used in stamping can be rationally designed based on the required shape. The die design should be based on conventional requirements in this field. For example, pot-shaped stamping... Figure 1 As shown, flange stamping is as follows Figure 2 As shown.

[0039] The stamping method of the pot shape includes: cold stamping.

[0040] The insulation temperature of the insulation treatment is 550-600℃, for example, it can be 550℃, 555℃, 560℃, 565℃, 570℃, 575℃, 580℃, 585℃, 590℃, 595℃ or 600℃, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0041] The heat preservation time is 60-120 min, for example, it can be 60 min, 66 min, 72 min, 78 min, 84 min, 90 min, 96 min, 102 min, 108 min, 114 min or 120 min, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0042] The flange stamping method includes hot stamping.

[0043] In this invention, hot stamping refers to stamping directly after the product has been heat-treated and removed from the furnace.

[0044] Ultrasonic treatment is used in the heat preservation process.

[0045] The frequency of the ultrasound is 20-40kHz, for example, it can be 20kHz, 22kHz, 24kHz, 26kHz, 28kHz, 30kHz, 32kHz, 34kHz, 36kHz, 38kHz or 40kHz, but is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0046] The power density of the ultrasound is 10-40 W / cm². 2 For example, it could be 10W / cm 2 13W / cm 2 16W / cm 2 19W / cm 2 22W / cm 2 25W / cm 2 28W / cm 2 31W / cm 2 34W / cm 2 37W / cm 2 Or 40W / cm 2 The values ​​may include, but are not limited to, the listed values; other unlisted values ​​within this range also meet the requirements.

[0047] In this invention, the ultrasound in the heat preservation process refers to non-contact ultrasound, that is, the material is placed in an ultrasonic field during the heat preservation process.

[0048] In this invention, the titanium blank can be directly purchased from commercially available plates according to the required size, or it can be obtained by processing titanium materials. For example, the process of obtaining the titanium blank includes:

[0049] The titanium material is subjected to forging, first annealing, air cooling, cold rolling, second annealing and air cooling in sequence to obtain a titanium billet.

[0050] In this invention, the titanium blank obtained during the acquisition process can be better matched with the stamping method of this invention, ensuring that a pot-shaped target material with superior performance can be obtained.

[0051] Before forging begins, the titanium material is preheated at 600-800℃ for 30-60 minutes. The preheating temperature can be, for example, 600℃, 620℃, 640℃, 660℃, 680℃, 700℃, 720℃, 740℃, 760℃, 780℃, or 800℃, and the time can be, for example, 30 minutes, 33 minutes, 36 minutes, 39 minutes, 42 minutes, 45 minutes, 48 ​​minutes, 51 minutes, 54 minutes, 57 minutes, or 60 minutes, but is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0052] The deformation during forging is controlled to be 60-80%, for example, it can be 60%, 62%, 64%, 66%, 68%, 70%, 72%, 74%, 76%, 78% or 80%, etc., but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0053] The holding temperature for the first annealing is 500-700℃, for example, it can be 500℃, 520℃, 540℃, 560℃, 580℃, 600℃, 620℃, 640℃, 660℃, 680℃ or 700℃, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0054] The holding time for the first annealing is 60-120 min, for example, it can be 60 min, 66 min, 72 min, 78 min, 84 min, 90 min, 96 min, 102 min, 108 min, 114 min or 120 min, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0055] The total deformation during cold rolling is controlled to be 50-70%, for example, it can be 50%, 52%, 54%, 56%, 58%, 60%, 62%, 64%, 66%, 68% or 70%, etc., but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0056] The holding temperature for the second annealing is 500-700℃, for example, it can be 500℃, 520℃, 540℃, 560℃, 580℃, 600℃, 620℃, 640℃, 660℃, 680℃ or 700℃, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0057] The holding time for the second annealing is 90-120 min, for example, it can be 90 min, 93 min, 96 min, 99 min, 102 min, 105 min, 108 min, 111 min, 114 min, 117 min or 120 min, but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0058] In this invention, the forging and rolling endpoints can be designed based on the titanium material and the required billet dimensions according to conventional requirements in the field.

[0059] II. This embodiment provides an integrally molded pot-shaped target material, which is prepared by the stamping forming method described in the first aspect.

[0060] III. To illustrate the excellent properties of the pot-shaped target material obtained by the stamping method provided by the present invention, the following example is used for explanation:

[0061] Example 1

[0062] This embodiment provides a stamping forming method for a titanium pot-shaped target, the stamping forming method comprising:

[0063] Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium billet (purity of 99.999%).

[0064] The process of obtaining the titanium billet includes: sequentially forging, first annealing, air cooling, cold rolling, second annealing, and air cooling to obtain the titanium billet; the titanium material is preheated at 700℃ for 40 minutes before forging; the deformation is controlled at 70% during forging; the holding temperature of the first annealing is 600℃; the holding time of the first annealing is 80 minutes; the total deformation is controlled at 60% during cold rolling; the holding temperature of the second annealing is 600℃; the holding time of the second annealing is 110 minutes.

[0065] The stamping method for the pot shape includes: cold stamping;

[0066] The heat preservation treatment is performed at a temperature of 560℃; the heat preservation time is 80 minutes; the heat preservation treatment is supplemented with ultrasound; the frequency of the ultrasound is 30kHz; and the power density of the ultrasound is 20W / cm². 2 ;

[0067] The flange stamping method includes: hot stamping.

[0068] Example 2

[0069] This embodiment provides a stamping forming method for a titanium pot-shaped target, the stamping forming method comprising:

[0070] Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium billet (purity of 99.999%).

[0071] The process of obtaining the titanium billet includes: sequentially forging, first annealing, air cooling, cold rolling, second annealing, and air cooling to obtain the titanium billet; the titanium material is preheated at 750℃ for 50 minutes before forging; the deformation is controlled at 75% during forging; the holding temperature of the first annealing is 650℃; the holding time of the first annealing is 100 minutes; the total deformation is controlled at 55% during cold rolling; the holding temperature of the second annealing is 550℃; the holding time of the second annealing is 100 minutes.

[0072] The pot shape is stamped by cold stamping.

[0073] The heat preservation treatment is performed at a temperature of 580℃; the heat preservation time is 100 minutes; the heat preservation treatment is supplemented with ultrasound; the frequency of the ultrasound is 36 kHz; and the power density of the ultrasound is 30 W / cm². 2 ;

[0074] The flange is stamped using hot stamping.

[0075] Example 3

[0076] This embodiment provides a stamping forming method for a titanium pot-shaped target, the stamping forming method comprising:

[0077] Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium billet (purity of 99.999%).

[0078] The process of obtaining the titanium billet includes: sequentially forging, first annealing, air cooling, cold rolling, second annealing, and air cooling to obtain the titanium billet; the titanium material is preheated at 600℃ for 30 minutes before forging; the deformation is controlled at 60% during forging; the holding temperature of the first annealing is 700℃; the holding time of the first annealing is 120 minutes; the total deformation is controlled at 70% during cold rolling; the holding temperature of the second annealing is 500℃; the holding time of the second annealing is 90 minutes.

[0079] The pot shape is stamped by cold stamping.

[0080] The heat preservation treatment is performed at a temperature of 550℃; the heat preservation time is 60 minutes; the heat preservation treatment is supplemented with ultrasound; the frequency of the ultrasound is 20kHz; and the power density of the ultrasound is 40W / cm². 2 ;

[0081] The flange is stamped using hot stamping.

[0082] Example 4

[0083] This embodiment provides a stamping forming method for a titanium pot-shaped target, the stamping forming method comprising:

[0084] Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium billet (purity of 99.999%).

[0085] The process of obtaining the titanium billet includes: sequentially forging, first annealing, air cooling, cold rolling, second annealing, and air cooling to obtain the titanium billet; the titanium material is preheated at 800℃ for 60 minutes before forging; the deformation is controlled at 80% during forging; the holding temperature of the first annealing is 500℃; the holding time of the first annealing is 60 minutes; the total deformation is controlled at 50% during cold rolling; the holding temperature of the second annealing is 700℃; the holding time of the second annealing is 120 minutes.

[0086] The pot shape is stamped by cold stamping.

[0087] The heat preservation treatment is performed at a temperature of 600℃; the heat preservation time is 120 minutes; the heat preservation treatment is supplemented with ultrasound; the frequency of the ultrasound is 40kHz; and the power density of the ultrasound is 10W / cm². 2 ;

[0088] The flange is stamped using hot stamping.

[0089] Example 5

[0090] The only difference from Example 1 is that the titanium blank is made of commercially available TA1 pure titanium plate.

[0091] Example 6

[0092] The only difference from Example 1 is that the same heat preservation treatment is performed before the pot is stamped.

[0093] Example 7

[0094] The only difference from Example 1 is that ultrasound is not used in the heat preservation process.

[0095] Example 8

[0096] The only difference from Example 1 is that the frequency of the ultrasound is 10 kHz.

[0097] Example 9

[0098] The only difference from Example 1 is that the frequency of the ultrasound is 50 kHz.

[0099] Example 10

[0100] The only difference from Example 1 is that the ultrasonic power density is 5 W / cm². 2 .

[0101] Example 11

[0102] The only difference from Example 1 is that the ultrasonic power density is 50 W / cm². 2 .

[0103] Comparative Example 1

[0104] The only difference from Example 1 is that no heat preservation treatment is performed.

[0105] Comparative Example 2

[0106] The only difference from Example 1 is that the heat preservation temperature is 400°C.

[0107] Comparative Example 3

[0108] The only difference from Example 1 is that the heat preservation temperature is 700°C.

[0109] Comparative Example 4

[0110] The only difference from Example 1 is that after heat preservation treatment, the flange is cooled to room temperature of 25°C in the furnace before flange stamping.

[0111] The grain properties of the titanium pot-shaped targets obtained in the above embodiments and comparative examples were analyzed, and the results are shown in Table 1 below.

[0112] Table 1

[0113]

[0114] In the table: the average grain size is tested according to GB / T 6394-2017. At the same time, the standard deviation of the grains in the measurement area is obtained by software, and the grain uniformity is obtained by dividing it by the average grain size in the measurement area.

[0115] As shown in Table 1, in the solution provided by the present invention, the flange and the pot body are integrally formed by two stamping processes, which ensures the reliability and stability of the connection between the flange and the pot body. At the same time, the heat preservation treatment introduced between the two stamping processes can significantly refine the grains and optimize the grain distribution, which is beneficial to improving the performance of the pot-shaped target material. Furthermore, the welding process is eliminated, which improves the production efficiency. In addition, the introduction of ultrasound in the heat preservation process can further optimize the grain distribution behavior of the pot-shaped target material and improve the performance of the target material. The average grain size of the resulting pot-shaped target material is ≤55μm, and the grain distribution uniformity is ≤0.87%. Under the preferred scheme, the average grain size is ≤26μm, and the grain distribution uniformity is ≤0.25%.

[0116] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0117] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

[0118] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. A method for stamping a titanium pot-shaped target, characterized in that, The stamping method includes: Titanium pot-shaped target material is obtained by sequentially performing pot-shaped stamping, heat preservation treatment and flange stamping on titanium billet; The insulation temperature for the insulation treatment is 550-600℃.

2. The stamping forming method as described in claim 1, characterized in that, The stamping method for the pot shape includes: cold stamping; Preferably, the heat preservation time is 60-120 minutes; Preferably, the flange stamping method includes hot stamping.

3. The stamping forming method as described in claim 1, characterized in that, Ultrasound is used in the heat preservation process; Preferably, the frequency of the ultrasound is 20-40 kHz; Preferably, the power density of the ultrasound is 10-40 W / cm². 2 .

4. The stamping forming method as described in claim 1, characterized in that, The process of obtaining the titanium billet includes: The titanium material is subjected to forging, first annealing, air cooling, cold rolling, second annealing and air cooling in sequence to obtain a titanium billet.

5. The stamping forming method as described in claim 4, characterized in that, Before the forging begins, the titanium material is preheated at 600-800℃ for 30-60 minutes.

6. The stamping forming method as described in claim 4, characterized in that, The deformation during forging is controlled at 60-80%.

7. The stamping forming method as described in claim 4, characterized in that, The holding temperature for the first annealing is 500-700℃; Preferably, the holding time for the first annealing is 60-120 minutes.

8. The stamping forming method as described in claim 4, characterized in that, The total deformation during cold rolling is controlled at 50-70%.

9. The stamping forming method as described in claim 4, characterized in that, The holding temperature for the second annealing is 500-700℃; Preferably, the holding time for the second annealing is 90-120 minutes.

10. A one-piece molded pot-shaped target material, characterized in that, The integrally molded pot-shaped target material is prepared by the stamping forming method as described in any one of claims 1-9.

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