Surface treatment method of pure titanium sputtering target

Abstract

The invention discloses a surface treatment method of a pure titanium sputtering target. The treatment method comprises the steps of primary treatment, turning treatment, abrasive paper treatment, canvas treatment and flannelette treatment which are sequentially carried out. The primary treatment comprises the steps of sequentially carrying out oil removal, cleaning and drying treatment on the pure titanium target material; the turning treatment refers to turning the pure titanium target material subjected to primary treatment; the abrasive paper treatment comprises 600 # abrasive paper treatment and 800 # abrasive paper treatment which are sequentially carried out; the canvas treatment is that the pure titanium target material is subjected to canvas treatment through grinding paste with different granularities; flannelette treatment is that flannelette is adopted for polishing on a polishing disc, and a silicon dioxide polishing solution is added in the polishing process. According to the surface treatment method for the pure titanium sputtering target, the problem that the extreme value difference of the surface roughness of the sputtering target is large due to the fact that a deformation layer is easily formed and deformation twin crystals are generated in an existing surface treatment technology is solved.

Description

Technical Field

[0001] The invention belongs to the technical field of surface treatment, and in particular relates to a surface treatment method of a pure titanium sputtering target. Background Art

[0002] During the sputtering deposition process, the target is usually connected to the negative electrode and the substrate is connected to the positive electrode. A high voltage electric field is applied between the target and the substrate. The inert gas (usually argon) between the target and the substrate is ionized to form plasma under the action of the high voltage electric field. The positively charged ions bombard the target, and the atoms on the surface of the target fall off and deposit on the surface of the substrate to form a coating. If the surface roughness is too large or uneven, large particles will be generated during the sputtering process. Therefore, the surface roughness of the target has a great influence on the uniformity of the coating, especially the extreme difference of the surface roughness.

[0003] In the prior art, when pure titanium targets are subjected to surface treatment, they are usually first polished and then polished with flannel cloth. However, pure titanium is soft and has good ductility, and pure titanium is prone to form a deformation layer during the polishing process, and the deformation layer contains deformation twins. The deformation layer and the formation of twins are also important reasons for the generation of large particles during the sputtering process. In addition, for pure titanium targets, the surface roughness extreme value difference is difficult to control and the roughness extreme value difference is also difficult to measure. Summary of the invention

[0004] The purpose of the present invention is to provide a surface treatment method for a pure titanium sputtering target, which solves the problem that the existing surface treatment technology easily forms a deformation layer and produces deformation twins, resulting in a large difference in the extreme value of the sputtering target surface roughness.

[0005] The technical solution adopted by the present invention is a surface treatment method of a pure titanium sputtering target, the treatment method comprising preliminary treatment, turning treatment, sandpaper treatment, canvas treatment and flannel treatment in sequence;

[0006] The initial treatment is to degrease, clean and dry the pure titanium target in sequence;

[0007] The turning process is to turn the pure titanium target material after preliminary treatment;

[0008] Sandpaper treatment includes 600# sandpaper treatment and 800# sandpaper treatment in sequence;

[0009] The canvas treatment is to use abrasive pastes of different particle sizes to canvas the pure titanium target;

[0010] Flannel cloth treatment is to use flannel cloth to polish on the polishing disc, and add silica polishing liquid during the polishing process.

[0011] The present invention is also characterized in that:

[0012] The specific process of the preliminary treatment is: place the pure titanium target in a NaOH solution for cleaning for 5min-15min, then clean it with a hydrochloric acid solution for 5min-15min, and finally place the pure titanium target in a beaker filled with anhydrous ethanol, clean it with an ultrasonic vibrator for 2min-5min and then dry it.

[0013] The parameters of the turning process are: feed rate 0.1mm / r-0.2mm / r, turning speed 50m / min-150m / min, turning depth 0.2mm-0.4mm; the surface roughness of the target material after turning process is 0.5μm-1.2μm.

[0014] The total time for sandpaper treatment is 10min-20min, the time for 600# sandpaper treatment is 3min-7min, and the time for 800# sandpaper treatment is 7min-13min.

[0015] The total time for canvas processing is 7min-12min, and the specific process of canvas processing is:

[0016] Step 1: Use canvas to polish on the polishing disc, add diamond paste W7 during the polishing process, and the time is 4min-6min;

[0017] Step 2: Polish with canvas on the polishing disc, add diamond paste W2.5 during polishing, and the time is 2min-4min;

[0018] The third step is to use canvas to polish on the polishing disc, adding diamond paste W1 during the polishing process for 1min-2min.

[0019] The parameters of flannel cloth treatment are: polishing disc speed is 250r / min-600r / min, the particle size of silica polishing liquid is 0.05μm-0.15μm, and the treatment time is 2min-8min.

[0020] The beneficial effects of the present invention are:

[0021] The surface treatment method of the pure titanium sputtering target provided by the present invention adopts a combination of multiple surface treatment methods, further optimizes the treatment process, and cooperates with each other to achieve the best effect, so that the surface roughness of the target material tends to be consistent and the extreme value difference is significantly reduced, thereby improving the uniformity of sputtering. In addition, the present invention has found through multiple experiments that when the surface glossiness is between 70GU and 350GU, the extreme value difference of the roughness is between 0.02-0.06, which can well solve the problem that the extreme value difference of the roughness is difficult to measure and inaccurate, and judge whether the surface roughness of the target material tends to be consistent and the extreme value difference by detecting the surface glossiness. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a flow chart of the surface treatment method of the pure titanium sputtering target of the present invention;

[0023] Figure 2 is a test value image of the surface roughness of the pure titanium sputtering target after surface treatment in Example 4 of the present invention;

[0024] Figure 3 is a maximum value curve diagram of the surface roughness of the pure titanium sputtering target after surface treatment in Example 4 of the present invention;

[0025] Figure 4 is a microstructure diagram of the surface roughness of the pure titanium sputtering target after surface treatment in Example 4 of the present invention;

[0026] Figure 5 This is a microstructure diagram of the pure titanium sputtering target after general surface treatment in Example 4 of the present invention. DETAILED DESCRIPTION

[0027] The present invention is described in detail below with reference to the accompanying drawings and specific embodiments.

[0028] Example 1

[0029] The surface treatment method of the pure titanium sputtering target proposed in this embodiment includes preliminary treatment, turning treatment, sandpaper treatment, canvas treatment and flannel treatment in sequence;

[0030] The initial treatment is to degrease, clean and dry the pure titanium target in sequence;

[0031] The specific process of the preliminary treatment is as follows: the pure titanium target is placed in a NaOH solution for cleaning for 5 minutes, and then cleaned with a hydrochloric acid solution for 5 minutes, and finally the pure titanium target is placed in a beaker containing anhydrous ethanol, cleaned with an ultrasonic vibrator for 2 minutes, and then dried;

[0032] The turning process is to turn the pure titanium target material after preliminary treatment;

[0033] The parameters of the turning process are: feed rate 0.1mm / r, turning speed 50m / min, turning depth 0.2mm; the surface roughness of the target material after turning process is 0.5μm;

[0034] Sandpaper treatment includes 600# sandpaper treatment and 800# sandpaper treatment in sequence;

[0035] The total sandpaper treatment time is 10 minutes, the 600# sandpaper treatment time is 3 minutes, and the 800# sandpaper treatment time is 7 minutes;

[0036] The canvas treatment is to use abrasive pastes of different particle sizes to canvas the pure titanium target;

[0037] The total time of canvas processing is 7 minutes, and the specific process of canvas processing is:

[0038] Step 1: Polish with canvas on the polishing disc, add diamond paste W7 during polishing, and polish for 4 minutes;

[0039] Step 2: Polish with canvas on the polishing disc, add diamond paste W2.5 during polishing, and polish for 2 minutes;

[0040] Step 3: Polish with canvas on the polishing disc, add diamond paste W1 during polishing for 1 minute;

[0041] The flannel treatment is to use flannel on the polishing disc for polishing, and add silicon dioxide polishing liquid during the polishing process;

[0042] The parameters of the flannel treatment are: the polishing disc speed is 250 r / min, the particle size of the silica polishing liquid is 0.05 μm, and the treatment time is 2 min.

[0043] Example 2

[0044] The surface treatment method of the pure titanium sputtering target proposed in this embodiment includes preliminary treatment, turning treatment, sandpaper treatment, canvas treatment and flannel treatment in sequence;

[0045] The initial treatment is to degrease, clean and dry the pure titanium target in sequence;

[0046] The specific process of the preliminary treatment is as follows: the pure titanium target is placed in a NaOH solution for cleaning for 10 minutes, and then cleaned with a hydrochloric acid solution for 10 minutes, and finally the pure titanium target is placed in a beaker containing anhydrous ethanol, cleaned with an ultrasonic vibrator for 4 minutes, and then dried;

[0047] The turning process is to turn the pure titanium target material after preliminary treatment;

[0048] The parameters of turning treatment are: feed rate 0.15mm / r, turning speed 100m / min, turning depth 0.3mm; the surface roughness of the target material after turning treatment is 0.8μm;

[0049] Sandpaper treatment includes 600# sandpaper treatment and 800# sandpaper treatment in sequence;

[0050] The total sandpaper treatment time is 15 minutes, the 600# sandpaper treatment time is 5 minutes, and the 800# sandpaper treatment time is 10 minutes;

[0051] The canvas treatment is to use abrasive pastes of different particle sizes to canvas the pure titanium target;

[0052] The total time of canvas processing is 9 minutes, and the specific process of canvas processing is:

[0053] Step 1: Polish with canvas on the polishing disc, add diamond paste W7 during polishing, and polish for 5 minutes;

[0054] Step 2: Polish with canvas on the polishing disc, add diamond paste W2.5 during polishing, and polish for 3 minutes;

[0055] Step 3: Polish with canvas on the polishing disc, add diamond paste W1 during polishing for 1 minute;

[0056] The flannel treatment is to use flannel on the polishing disc for polishing, and add silicon dioxide polishing liquid during the polishing process;

[0057] The parameters of the flannel treatment are: the polishing disc speed is 400 r / min, the particle size of the silica polishing liquid is 0.1 μm, and the treatment time is 5 min.

[0058] Example 3

[0059] The surface treatment method of the pure titanium sputtering target proposed in this embodiment includes preliminary treatment, turning treatment, sandpaper treatment, canvas treatment and flannel treatment in sequence;

[0060] The initial treatment is to degrease, clean and dry the pure titanium target in sequence;

[0061] The specific process of the preliminary treatment is as follows: the pure titanium target is placed in a NaOH solution for cleaning for 15 minutes, and then cleaned with a hydrochloric acid solution for 15 minutes, and finally the pure titanium target is placed in a beaker containing anhydrous ethanol, cleaned with an ultrasonic vibrator for 5 minutes, and then dried;

[0062] The turning process is to turn the pure titanium target material after preliminary treatment;

[0063] The parameters of turning treatment are: feed rate 0.2mm / r, turning speed 150m / min, turning depth 0.4mm; the surface roughness of the target material after turning treatment is 1.2μm;

[0064] Sandpaper treatment includes 600# sandpaper treatment and 800# sandpaper treatment in sequence;

[0065] The total sandpaper treatment time is 20 minutes, the 600# sandpaper treatment time is 7 minutes, and the 800# sandpaper treatment time is 13 minutes;

[0066] The canvas treatment is to use abrasive pastes of different particle sizes to canvas the pure titanium target;

[0067] The total time for canvas processing is 12 minutes, and the specific process of canvas processing is:

[0068] Step 1: Polish with canvas on the polishing disc, add diamond paste W7 during polishing, and polish for 6 minutes;

[0069] Step 2: Polish with canvas on the polishing disc, add diamond paste W2.5 during polishing, and polish for 4 minutes;

[0070] Step 3: Polish with canvas on the polishing disc, add diamond paste W1 during polishing for 2 minutes;

[0071] The flannel treatment is to use flannel on the polishing disc for polishing, and add silicon dioxide polishing liquid during the polishing process;

[0072] The parameters of the flannel treatment are: the polishing disc speed is 600 r / min, the particle size of the silica polishing liquid is 0.15 μm, and the treatment time is 8 min.

[0073] Example 4

[0074] The surface treatment method of the pure titanium sputtering target proposed in this embodiment includes preliminary treatment, turning treatment, sandpaper treatment, canvas treatment and flannel treatment in sequence. Figure 1 As shown;

[0075] The initial treatment was to place the sample in 400 ml / L 10% NaOH solution for 10 min to remove the surface oil, then use 400 ml / L hydrochloric acid solution for 10 min to remove the surface oxide film, and finally place the sample in a beaker containing anhydrous ethanol, use an ultrasonic vibrator to clean for 3 min and then dry;

[0076] The turning process is to turn the pure titanium target after preliminary treatment; the feed rate during turning is 0.15mm / r, the turning speed is 100m / min, and the turning depth is 0.2mm. The surface roughness of the target after treatment is 0.8μm;

[0077] The sandpaper treatment includes 600# sandpaper treatment and 800# sandpaper treatment in sequence; the total sandpaper treatment time is 15 minutes, the 600# sandpaper treatment time is 5 minutes, and the 800# sandpaper treatment time is 10 minutes;

[0078] The total time for canvas processing is 10 minutes, including three steps:

[0079] Step 1: Polish with canvas on the polishing disc, add diamond paste W7 during polishing, and polish for 5 minutes;

[0080] Step 2: Polish with canvas on the polishing disc, add diamond paste W2.5 during polishing, and polish for 3 minutes;

[0081] Step 3: Polish with canvas on the polishing disc, add diamond paste W1 during polishing for 2 minutes;

[0082] The flannel cloth treatment is to use flannel cloth to polish on the polishing disc, add silicon dioxide polishing liquid with a particle size of 0.05 μm during the polishing process, the treatment time is 6 minutes, and the rotation speed of the polishing disc during the treatment is 450 r / min; the process parameters of the surface treatment in Example 4 are shown in Table 1.

[0083] Table 1 Surface treatment process parameters

[0084]

[0085] When it is necessary to further improve the surface gloss or remove the deformation layer caused by cutting, put the mechanically polished sample into the vibration polishing fixture, add two counterweights, and put it into the vibration polishing pool containing OP-S polishing liquid and hydrogen peroxide mixed polishing liquid. Vibration polish for 30 minutes, then take out the sample and ultrasonically clean it with anhydrous ethanol for 15 minutes.

[0086] The difference between Comparative Example 1 and Sample 1 of Example 4 is that the feed rate during turning is 0.25 mm / r, the turning speed is 100 m / min, and the turning depth is 0.2 mm. The surface roughness of the target material after turning is 1.7 μm. Even if the flannel treatment is repeated 5 times, the surface gloss is still 420 GU, and the extreme difference in roughness is 0.35 μm. The subsequent increase in the number of flannel treatments has little effect on the surface gloss and the extreme difference in roughness. The reason is that the surface roughness of the target material after turning is 1.5 μm, and the traces of turning treatment are too large to be eliminated in subsequent treatments.

[0087] The difference between Comparative Example 2 and Sample 1 of Example 4 is that 800# sandpaper was used directly for 14 minutes instead of 600# sandpaper. Even if the flannel treatment was repeated more than 4 times, the surface glossiness was still 415GU, and the extreme value difference of roughness was 0.28μm. The subsequent increase in the number of flannel treatments had little effect on the surface glossiness and the extreme value difference of roughness.

[0088] The difference between Comparative Example 3 and Sample 1 of Example 4 is that before the 600# sandpaper treatment, the 400# sandpaper treatment was used for 3 minutes. Even if the flannel treatment was repeated for more than 6 times, the surface glossiness was still 520GU, and the extreme difference of roughness was 0.43μm. The subsequent increase in the number of flannel treatments had little effect on the surface glossiness and the extreme difference of roughness, because the rough scratches and deformation layer caused by the 400# sandpaper were difficult to eliminate later.

[0089] The difference between Comparative Example 4 and Sample 1 of Example 4 is that no diamond paste is used in the canvas processing.

[0090] The difference between Comparative Example 5 and Sample 1 of Example 4 is that no silica polishing liquid is used during the flannel treatment.

[0091] The difference between Comparative Example 6 and Sample 1 of Example 4 is that the canvas is replaced with a scouring pad, specifically:

[0092] The total time for the scouring pad treatment is 10 minutes, including three steps:

[0093] Step 1: Use a scouring pad to polish on the polishing disc, add diamond paste W7 during the polishing process, and polish for 5 minutes;

[0094] Step 2: Polishing with a scouring pad on the polishing disc, adding diamond paste W2.5 during the polishing process for 3 minutes;

[0095] Step 3: Use a scouring pad to polish on the polishing disc, add diamond paste W1 during the polishing process, and polish for 2 minutes.

[0096] The difference between Comparative Example 7 and Sample 1 of Example 4 is that diamond abrasive paste W1 is used in the flannel processing.

[0097] The evaluation of the sputtering surface of the target material after the surface treatment of Example 4 and Comparative Examples 1-7 is shown in Table 2, and the glossiness is measured according to the 20 degree glossiness standard.

[0098] Table 2 Evaluation of target sputtering surface after surface treatment

[0099]

[0100] The surface treatment methods commonly used in the prior art are not effective for pure titanium targets, especially the target surface roughness extreme value difference is difficult to control and difficult to measure. The present invention has found through multiple experiments that when the surface gloss is between 70GU and 350GU, the roughness extreme value difference is between 0.02-0.06. Therefore, the present invention can well solve the problem that the roughness extreme value difference is difficult to measure and is inaccurate, and judge whether the target surface roughness tends to be consistent and the extreme value difference by detecting the surface gloss.

[0101] By comparing Sample 1 of Example 4 with Comparative Examples 1-6, it can be seen that the surface roughness of the target material after turning, the choice of sandpaper, and the choice of polishing cloth, polishing liquid and grinding paste during polishing all have an important influence on the final roughness. Taking Comparative Example 1 as an example, the surface roughness of the target material after turning is 1.7μm. Even if the number of flannel cloth treatments is continuously increased, the effect on the surface gloss and roughness extreme value difference is not significant. The reason is that the surface roughness of the target material after turning is 1.7μm, and the traces of turning treatment are too large to be eliminated in subsequent treatments. At the same time, the surface roughness test value of Sample 1 of Example 4 is tested using a surface roughness meter, as shown in FIG. Figure 2 As shown in the figure, the calculated surface roughness extreme value difference is 0.058; the curve diagram of the maximum roughness in this test is as follows Figure 3 As shown in FIG. 1 , it is shown that the surface undulation of the pure titanium after treatment is small and the surface roughness is low. Figure 4 As shown, the SEM photo of the sample of Comparative Example 1 is as follows: Figure 5 As shown in the figure, it can be seen that after general surface treatment, there are micropores and fine scratches on the surface of the pure titanium target material. After the surface treatment proposed by the present invention, the surface of the pure titanium target material is smooth and clean, without micropores and scratches. It can be seen that the sample 1 of Example 4 achieves the best effect through the cooperation of various steps, so that the surface roughness of the target material tends to be consistent and the extreme value difference is significantly reduced.

Claims

1. A method for treating a pure titanium sputtering target surface, characterized in that: The treatment method includes preliminary treatment, turning treatment, sandpaper treatment, canvas treatment and flannel treatment performed in sequence; The preliminary treatment is to sequentially perform degreasing, cleaning and drying treatments on the pure titanium target; The turning process is to turn the pure titanium target material after preliminary treatment; The sandpaper treatment includes 600# sandpaper treatment and 800# sandpaper treatment performed sequentially; The canvas treatment is to perform canvas treatment on the pure titanium target material by using abrasive pastes of different particle sizes; The flannel cloth treatment is to use flannel cloth to perform polishing on the polishing disc, and add silicon dioxide polishing liquid during the polishing process.

2. The surface treatment method of a pure titanium sputtering target according to claim 1, characterized in that: The specific process of the preliminary treatment is: place the pure titanium target in a NaOH solution for cleaning for 5min-15min, then use a hydrochloric acid solution for cleaning for 5min-15min, and finally place the pure titanium target in a beaker containing anhydrous ethanol, use an ultrasonic vibrator to clean for 2min-5min and then dry.

3. The surface treatment method of the pure titanium sputtering target according to claim 1, characterized in that: The parameters of the turning process are: feed rate 0.1mm / r-0.2mm / r, turning speed 50m / min-150m / min, turning depth 0.2mm-0.4mm; the surface roughness of the target material after the turning process is 0.5μm-1.2μm.

4. The surface treatment method of a pure titanium sputtering target according to claim 1, characterized in that: The total time of the sandpaper treatment is 10 min-20 min, the time of the 600# sandpaper treatment is 3 min-7 min, and the time of the 800# sandpaper treatment is 7 min-13 min.

5. The surface treatment method of a pure titanium sputtering target according to claim 1, characterized in that: The total time of the canvas processing is 7min-12min, and the specific process of the canvas processing is: Step 1: Use canvas to polish on the polishing disc, add diamond paste W7 during the polishing process, and the time is 4min-6min; Step 2: Polish with canvas on the polishing disc, add diamond paste W2.5 during polishing, and the time is 2min-4min; The third step is to use canvas to polish on the polishing disc, adding diamond paste W1 during the polishing process for 1min-2min.

6. The surface treatment method of a pure titanium sputtering target according to claim 1, characterized in that: The parameters of the flannel treatment are: the polishing disc speed is 250r / min-600r / min, the particle size of the silicon dioxide polishing liquid is 0.05μm-0.15μm, and the treatment time is 2min-8min.

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