CN112077408A - Brazing method of chromium-silicon target and copper back plate - Google Patents

Abstract

The invention relates to a brazing method for a chromium-silicon target material and a copper backplate. The density of the chromium-silicon target material is ≥5.09 g/cm ³ ; It is 12-18mm smaller than the diameter of the target material, and the depth of the solder groove is 0.2-0.3mm; the brazing method includes the following steps: sandblasting and chemical plating are performed on the welding surface of the chrome-silicon target material and the copper backplane in sequence. Nickel treatment, then brazing the treated chrome-silicon target and copper backplate; hydrochloric acid was used for activation for 15-30s in the electroless nickel plating treatment, and the pH of the nickel plating was 4.6-4.8; the average thickness of the nickel plating layer was 7 ‑12μm. In the present invention, through the redesign of the welding method, by controlling the parameters in the nickel plating process and using sandblasting, the effective welding of the chrome-silicon target and the copper backing plate is realized, the welding joint rate is ≥97%, and the single defect rate is ≤1.5 %.

Description

A kind of brazing method of chromium silicon target and copper back plate

technical field

The invention relates to the field of target material welding, in particular to a brazing method for a chromium-silicon target material and a copper backplate.

Background technique

Chromium-silicon alloy sputtering target, as a good conductor of vacuum sputtering, can be used in electronic gate material and electronic thin film field. Chromium-silicon alloy sputtering targets usually have high density, high uniformity of internal structure, low oxygen content and better machining conditions, which make chromium-silicon alloy sputtering targets in vacuum sputtering. Good performance during plating.

For example, CN207904355U discloses a rotating chromium-silicon target material, which comprises a back tube, a brazing layer is arranged outside the back tube, and a chrome-silicon alloy tube is arranged outside the brazing layer; The other end of the pipe is provided with a positioning groove and a flange. Its installation is convenient and time-saving. During the long-term work process, it can rotate stably, sputter uniformly, without arcing, and eliminate the generation of pores and accumulations; because this target uses an inner seal In this way, the back tube bears little force and hardly deforms, which avoids the cracking of the target material caused by the deformation of the back tube.

CN102251222A discloses a chromium alloy target material, which is composed of chromium and silicon, or composed of chromium and germanium, wherein the weight percentage of chromium is 5% to 95%, and when the thin film produced by the physical vapor sputtering process has a When the thickness is greater than or equal to 2 microns, the Vickers hardness values of the above-mentioned films are respectively Hv800 to Hv1200 and Hv800 to Hv1000. The above-mentioned target can be used to produce a metal material with a hard thin film, and the metal material includes a metal substrate and a chromium-silicon alloy thin film, or a metal substrate and a chromium-germanium alloy thin film.

However, due to its brittleness, chromium-silicon targets still have no suitable welding method, or the target components obtained by welding have problems such as low welding bonding rate and short service life.

SUMMARY OF THE INVENTION

In view of the problems existing in the prior art, the purpose of the present invention is to provide a brazing method for a chromium-silicon target and a copper backplate, by which the effective welding of the chromium-silicon target and the copper backplate can be achieved, and the welding bonding rate is improved. ≥97%, single defect rate ≤1.5%.

For this purpose, the present invention adopts the following technical solutions:

The invention provides a brazing method for a chromium-silicon target and a copper backplate, wherein the density of the chromium-silicon target is ≥5.09 g/cm ³ ; a solder groove is provided on the welding surface of the copper backplate, and the solder groove is The diameter is 12-18mm smaller than the diameter of the target material, and the depth of the solder groove is 0.2-0.3mm;

The brazing method includes the following steps: sequentially performing sandblasting and chemical nickel plating on the welding surface of the chromium-silicon target and the copper backplate, and then brazing the processed chromium-silicon target and the copper backplate;

In the electroless nickel plating treatment, hydrochloric acid is used for activation for 15-30s, and the pH of the nickel plating is 4.6-4.8; the average thickness of the nickel plating layer is 7-12 μm.

In the present invention, through the redesign of the welding method, by controlling the parameters in the nickel plating process and using sandblasting, the effective welding of the chrome-silicon target and the copper backing plate is realized, the welding joint rate is ≥97%, and the single defect rate is ≤1.5 %.

In the present invention, the density of the chromium-silicon target material is greater than or equal to 5.09g/cm ³ , such as 5.09g/cm ³ , 5.1g/cm ³ , 5.8g/cm ³ , 6.09g/cm ³ , and 6.59g/cm 3 . ³ or 7.09 g/cm ³ , etc., but not limited to the listed values, and other unlisted values within this range are also applicable.

In the present invention, hydrochloric acid is used for activation for 15-30s in the electroless nickel plating treatment, such as 15s, 16s, 16s, 17s, 18s, 19s, 20s, 21s, 22s, 23s, 24s, 25s, 26s, 27s, 28s, 29s or 30s, etc., but not limited to the recited values, and other unrecited values within this range are also applicable.

In the present invention, the pH of nickel plating is 4.6-4.8, such as 4.6, 4.62, 4.64, 4.66, 4.68, 4.7, 4.72, 4.74, 4.76, 4.78 or 4.8, etc., but not limited to the listed values, other values within this range The same applies to non-recited values.

In the present invention, the average thickness of the nickel plating layer is 7-12 μm, such as 7 μm, 7.5 μm, 8 μm, 8.5 μm, 9 μm, 9.5 μm, 10 μm, 10.5 μm, 11 μm, 11.5 μm or 12 μm, etc., but not limited to Recited values apply equally well to other non-recited values within the range.

In the present invention, the diameter of the solder groove is 12-18mm smaller than the diameter of the target material, for example, it can be 12mm, 12.5mm, 13mm, 13.5mm, 14mm, 14.5mm, 15mm, 15.5mm, 16mm, 16.5mm, 17mm, 17.5mm or 18mm, etc., but not limited to the listed values, other unlisted values within this range are also applicable.

In the present invention, the depth of the solder groove is 0.2-0.3mm, such as 0.2mm, 0.21mm, 0.22mm, 0.23mm, 0.24mm, 0.25mm, 0.26mm, 0.27mm, 0.28mm, 0.29mm or 0.3mm mm, etc., but not limited to the recited values, and other unrecited values within the range are also applicable.

As a preferred technical solution of the present invention, the roughness of the welding surface of the chromium-silicon target and the copper backplane after the sandblasting is completed is 2-3 μm, such as 2 μm, 2.1 μm, 2.2 μm, 2.3 μm, 2.4 μm, 2.5 μm, 2.6 μm, 2.7 μm, 2.8 μm, 2.9 μm or 3 μm, etc., but not limited to the listed values, and other unlisted values within this range are also applicable.

In the present invention, by controlling the roughness of the welding surface after sandblasting, the synergistic coupling effect between the specific roughness and the thickness of the nickel-plated layer is used to improve the welding effect between the chromium-silicon target and the copper backplane, and at the same time, the chromium-silicon target is avoided. Internal stress generation after welding of silicon target and copper backplane.

As a preferred technical solution of the present invention, the mass concentration of the hydrochloric acid is 8-15%, such as 8%, 8.5%, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5% or 15%, etc., but not limited to the recited values, and other non-recited values within the range are also applicable.

As a preferred technical solution of the present invention, the temperature of the electroless nickel plating treatment is 86-90°C, such as 86°C, 86.5°C, 87°C, 87.5°C, 88°C, 88.5°C, 89°C, 89.5°C or 90°C °C, etc., but not limited to the listed numerical values, and other unlisted numerical values within this range are also applicable.

As a preferred technical solution of the present invention, the time of the electroless nickel plating treatment is 25-40min, such as 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min or 40min, etc., but not limited to the listed values, other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, in the electroless nickel plating treatment, the nickel plating solution is a mixed aqueous solution of SYC300A and SYC300B, and the concentration of nickel ions in the nickel plating solution is 4-5g/L, such as 4g/L, 4.1g /L, 4.2g/L, 4.3g/L, 4.4g/L, 4.5g/L, 4.6g/L, 4.7g/L, 4.8g/L, 4.9g/L or 5g/L, etc., but not Limitation to the recited values applies equally to other non-recited values within the range.

As a preferred technical solution of the present invention, the volume ratio of SYC300A and SYC300B is 1:(1.5-2.5), for example, it can be 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, 1:1:1. 2, 1:2.1, 1:2.2, 1:2.3, 1:2.4 or 1:2.5, etc., but not limited to the listed values, and other unlisted values within this range are also applicable.

As a preferred technical solution of the present invention, the temperature of the brazing is 200-220°C, such as 200°C, 202°C, 204°C, 206°C, 208°C, 210°C, 212°C, 214°C, 216°C , 218°C or 220°C, etc., but are not limited to the listed values, and other unlisted values within this range are also applicable.

Preferably, the solder in the brazing is indium solder.

As a preferred technical solution of the present invention, after the brazing is completed, pressure cooling is carried out with the furnace.

Preferably, physical pressurization is used in the pressurized cooling with the furnace.

Preferably, the mass of the briquette in the physical press is 45-50kg, for example, it can be 45kg, 46kg, 47kg, 48kg, 49kg or 50kg, etc., but is not limited to the listed numerical values, and other unlisted numerical values within this range The same applies.

As a preferred technical solution of the present invention, the density of the chromium-silicon target material is greater than or equal to 5.09g/cm ³ ; the soldering surface of the copper backplane is provided with a solder groove, and the diameter of the solder groove is 12-18mm smaller than the diameter of the target material, The depth of the solder groove is 0.2-0.3mm;

The brazing method includes the following steps: sequentially performing sandblasting and chemical nickel plating on the welding surface of the chromium-silicon target and the copper backplate, and then brazing the processed chromium-silicon target and the copper backplate;

After sandblasting, the roughness of the welding surface of the chrome-silicon target and the copper backplate is 2-3μm;

In the electroless nickel plating treatment, hydrochloric acid is used for activation for 15-30s, and the pH of the nickel plating is 4.6-4.8; the average thickness of the nickel plating layer is 7-12 μm.

Compared with the prior art solutions, the present invention at least has the following beneficial effects:

(1) In the present invention, through the redesign of the welding method, the effective welding of the chrome-silicon target and the copper backplate is realized by controlling the parameters in the nickel plating process and using sandblasting, the welding bonding rate is ≥97%, and a single defect rate≤1.5%.

(2) In the present invention, by controlling the roughness of the welding surface after sandblasting, the synergistic coupling effect between the specific roughness and the thickness of the nickel plating layer is used to improve the welding effect between the chromium-silicon target and the copper backplane, and at the same time It avoids the generation of internal stress after welding of the chrome-silicon target and the copper backplane.

Detailed ways

In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, typical but non-limiting examples of the present invention are as follows:

Example 1

This embodiment provides a brazing method for a chrome-silicon target and a copper backplate, wherein the density of the chrome-silicon target is 5.09 g/cm ³ ; a solder groove is provided on the welding surface of the copper backplate, and the solder groove The diameter is 15mm smaller than the diameter of the target, and the depth of the solder groove is 0.25mm;

The brazing method includes the following steps: sequentially performing sandblasting and chemical nickel plating on the welding surface of the chromium-silicon target and the copper backplate, and then brazing the processed chromium-silicon target and the copper backplate;

After sandblasting, the roughness of the welding surface of the chromium-silicon target and the copper backing plate is 2μm;

In the electroless nickel plating treatment, hydrochloric acid with a mass concentration of 11% was used for activation for 22 s, the pH of the nickel plating was 4.7, the temperature was 88 °C, the nickel plating time was 32 minutes, and the average thickness of the nickel plating layer was 9 μm;

In the chemical nickel plating treatment, the nickel plating solution is a mixed aqueous solution of SYC300A and SYC300B, the concentration of nickel ions in the nickel plating solution is 4.5g/L, and the volume ratio of SYC300A and SYC300B is 1:2;

The temperature of the brazing was 210° C., and the solder in the brazing was indium solder. After the brazing was completed, the furnace was pressurized and cooled, and physical pressure was used. The mass of the compact in the physical pressure was 47kg.

The brazed target assembly has a welding bonding rate of 98%, a single defect rate of 1.2%, and no internal stress.

Example 2

This embodiment provides a brazing method for a chromium-silicon target and a copper backplate, wherein the density of the chromium-silicon target is 6.09 g/cm ³ ; a solder groove is provided on the welding surface of the copper backplate, and the solder groove is The diameter is 12mm smaller than the diameter of the target, and the depth of the solder groove is 0.3mm;

The brazing method includes the following steps: sequentially performing sandblasting and chemical nickel plating on the welding surface of the chromium-silicon target and the copper backplate, and then brazing the processed chromium-silicon target and the copper backplate;

After sandblasting, the roughness of the welding surface of the chrome-silicon target and the copper backing plate is 3 μm;

In the electroless nickel plating treatment, hydrochloric acid with a mass concentration of 8% was used for activation for 30 s, the pH of the nickel plating was 4.6, the temperature was 90 °C, the nickel plating time was 25 minutes, and the average thickness of the nickel plating layer was 12 μm;

In the chemical nickel plating treatment, the nickel plating solution is a mixed aqueous solution of SYC300A and SYC300B, the concentration of nickel ions in the nickel plating solution is 4g/L, and the volume ratio of SYC300A and SYC300B is 1:1.5;

The temperature of the brazing was 218° C., and the solder in the brazing was indium solder. After the brazing was completed, the furnace was pressurized and cooled, and physical pressure was used. The mass of the compact in the physical pressure was 50 kg.

The brazed target assembly has a welding bonding rate of 97%, a single defect rate of 1.5%, and no internal stress.

Example 3

This embodiment provides a brazing method for a chromium-silicon target and a copper backplane, wherein the density of the chromium-silicon target is ≥6.59 g/cm ³ ; a solder groove is provided on the welding surface of the copper backplane, and the solder groove is The diameter is 18mm smaller than that of the target, and the depth of the solder groove is 0.2mm;

The brazing method includes the following steps: sequentially performing sandblasting and chemical nickel plating on the welding surface of the chromium-silicon target and the copper backplate, and then brazing the processed chromium-silicon target and the copper backplate;

After sandblasting, the roughness of the welding surface of the chromium-silicon target and the copper backing plate is 2.4 μm;

In the electroless nickel plating treatment, hydrochloric acid with a mass concentration of 15% was used for activation for 15s, the pH of the nickel plating was 4.8, the temperature was 86 °C, the nickel plating time was 38 minutes, and the average thickness of the nickel plating layer was 7.3 μm;

In the chemical nickel plating treatment, the nickel plating solution is a mixed aqueous solution of SYC300A and SYC300B, the concentration of nickel ions in the nickel plating solution is 4.8g/L, and the volume ratio of SYC300A and SYC300B is 1:2.4;

The temperature of the brazing was 202° C., and the solder in the brazing was indium solder. After the brazing was completed, the furnace was pressurized and cooled, and physical pressure was used. The mass of the compact in the physical pressure was 45kg.

The brazed target assembly has a welding bonding rate of 98%, a single defect rate of 1.1%, and no internal stress.

Comparative Example 1

The only difference from Example 1 is that the density of the chromium-silicon target is 4.09 g/cm ³ , the brazed target assembly has a welding bonding rate of 90%, a single defect rate of 2%, and local internal stress is generated. .

Comparative Example 2

The only difference from Example 1 is that the average thickness of the nickel-plated layer is 5 μm, the brazed target assembly has a welding bonding rate of 93%, a single defect rate of 1.8%, and local internal stress.

Comparative Example 3

The only difference from Example 1 is that the average thickness of the nickel-plated layer is 15 μm, the brazed target assembly has a welding bond rate of 92%, a single defect rate of 1.9%, and local internal stress.

Comparative Example 4

The only difference from Example 1 is that the roughness of the welding surface of the chrome-silicon target and the copper backing plate after sandblasting is 1 μm, the welding bonding rate of the brazed target assembly is 90%, and the single defect rate is 1.8%. , local internal stress is generated.

Comparative Example 5

The only difference from Example 1 is that the roughness of the welding surface of the chromium-silicon target and the copper backing plate after sandblasting is 5 μm, the welding bonding rate of the brazed target assembly is 91%, and the single defect rate is 1.7%. , local internal stress is generated.

From the results of the above examples and comparative examples, it can be seen that in the present invention, through the redesign of the welding method, the effective welding of the chrome-silicon target and the copper backplate is realized by controlling the parameters in the nickel plating process and using sandblasting. The bonding rate is ≥97%, and the single defect rate is ≤1.5%.

The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must rely on the above detailed structural features to be implemented. Those skilled in the art should understand that any improvement to the present invention, the equivalent replacement of the selected components of the present invention, the addition of auxiliary components, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims (10)

1. The brazing method of the chromium-silicon target and the copper back plate is characterized in that the density of the chromium-silicon target is more than or equal to 5.09g/cm³(ii) a The welding surface of the copper back plate is provided with a solder groove, the diameter of the solder groove is 12-18mm smaller than that of the target material, and the depth of the solder groove is 0.2-0.3 mm;

the brazing method comprises the following steps: carrying out sand blasting and chemical nickel plating treatment on the welding surfaces of the chromium-silicon target material and the copper back plate in sequence, and then carrying out braze welding on the treated chromium-silicon target material and the copper back plate;

activating with hydrochloric acid for 15-30s in chemical nickel plating treatment, wherein the pH of nickel plating is 4.6-4.8; the average thickness of the nickel plating layer is 7-12 μm.

2. The brazing method according to claim 1, wherein the roughness of the welding surface of the chromium silicon target and the copper backing plate after the sand blasting is finished is 2-3 μm.

3. The brazing method according to claim 1 or 2, wherein the hydrochloric acid is present in a concentration of 8 to 15% by mass.

4. The brazing method according to any one of claims 1 to 3, wherein the electroless nickel plating treatment is carried out at a temperature of 86 to 90 ℃.

5. The brazing method according to any one of claims 1 to 4, wherein the electroless nickel plating treatment is carried out for 25 to 40 min.

6. The brazing method according to any one of claims 1 to 5, wherein the nickel plating solution in the electroless nickel plating treatment is a mixed aqueous solution of SYC300A and SYC300B, and the concentration of nickel ions in the nickel plating solution is 4 to 5 g/L.

7. The brazing method according to claim 6, wherein the volume ratio of SYC300A to SYC300B is 1 (1.5-2.5).

8. The brazing method according to any one of claims 1 to 7, wherein the temperature of the brazing is 200 ℃ to 220 ℃;

preferably, the solder in the soldering joint is indium solder.

9. The brazing method according to any one of claims 1 to 8, wherein furnace pressure cooling is performed after the brazing is completed;

preferably, physical pressurization is adopted in the furnace pressurization cooling;

preferably, the mass of the briquettes in the physical pressing is 45-50 kg.

10. The welding method according to any one of claims 1 to 9, wherein the density of the chromium-silicon target is not less than 5.09g/cm³(ii) a The welding surface of the copper back plate is provided with a solder groove, the diameter of the solder groove is 12-18mm smaller than that of the target material, and the depth of the solder groove is 0.2-0.3 mm;

the brazing method comprises the following steps: carrying out sand blasting and chemical nickel plating treatment on the welding surfaces of the chromium-silicon target material and the copper back plate in sequence, and then carrying out braze welding on the treated chromium-silicon target material and the copper back plate;

after the sand blasting is finished, the roughness of the welding surface of the chromium-silicon target and the copper back plate is 2-3 mu m;

activating with hydrochloric acid for 15-30s in chemical nickel plating treatment, wherein the pH of nickel plating is 4.6-4.8; the average thickness of the nickel plating layer is 7-12 μm.