JPH0841624A - Deposition jig and method for reclaiming deposition jig - Google Patents

Abstract

(57) [Abstract] [Objective] Especially in vapor deposition on a plastic substrate, it is possible to satisfactorily dissipate heat, prevent deformation of the plastic substrate, and collect Au, Ag, and Pd adhering to the surface during vapor deposition. Provided is a vapor deposition jig that can be regenerated and a method for regenerating the same. [Structure] Corrosion resistant metal such as Cr, Ti, Ta, Nb, Rh, Ir, W and Mo or corrosion resistant alloy coating such as Ni alloy, Fe alloy and Cr alloy is formed on the surface of a jig for vapor deposition made of Cu or Cu alloy. A vapor deposition jig having a layer.
After using the above evaporation jig, Au, A adhered to the surface
Au or Ag or Pd by dissolving g or Pd with a chemical solution
A method for regenerating a vapor deposition jig, which comprises recovering the vapor and regenerating the vapor deposition jig.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vapor deposition jig used for sputtering, ion plating, etc., and particularly to an improvement of a vapor deposition jig made of Cu or a Cu alloy aiming at a heat dissipation effect and the vapor deposition jig. Regarding how to play.

[0002]

2. Description of the Related Art Vacuum thin film forming techniques represented by sputtering, ion plating, vacuum vapor deposition and the like are widely used mainly in the semiconductor industry. When forming a vacuum thin film on a substrate, it is common to mount the substrate on a vapor deposition jig called a holder and form the thin film on the substrate. Since a thin film forming component, which is a deposit, adheres to the evaporation jig as it is used, the evaporation jig will be replaced when the amount of adhesion becomes unusable. The vapor deposition material attached to the vapor deposition jig is treated with a chemical solution such as a sandblast method or nitric acid to remove the vapor deposition material, and is used again as the vapor deposition jig.
Generally, stainless steel or titanium is used as the material for the evaporation jig. However, when forming a thin film on a plastic substrate such as an optical disk, a vapor deposition jig made of Cu or a Cu alloy is used in order to improve heat dissipation and prevent deformation or deterioration of the substrate.

Peeling off the deposited material deposited on the Cu or Cu alloy deposition jig is performed by a sandblast method. Even when a noble metal such as Au or Ag adheres to the Cu or Cu alloy vapor deposition jig, if peeling is similarly performed by the sandblast method, about 90% can be recovered as a largely peeled noble metal. However, the remaining 10% is mixed in the emery. The recovery rate can be increased by recovering the precious metal mixed in the emery, but it takes a lot of work.

In order to recover all the precious metals, the precious metal can be easily recovered by treating the vapor deposition jig with a chemical solution such as aqua regia, nitric acid or cyan. However, since a vapor deposition jig made of Cu or a Cu alloy does not have corrosion resistance, the base material also melts, and the vapor deposition jig cannot be reused.
The precious metal is also an expensive material, but the vapor deposition jig is also expensive. Therefore, the former method is usually used because the vapor deposition jig can be regenerated.

[0005]

Therefore, the present invention solves the problem of the Cu or Cu alloy evaporation jig, and Au, Ag, or Pd is formed by chemical treatment in the same manner as the stainless or titanium evaporation jig. It is an object of the present invention to provide a vapor deposition jig and a method for regenerating the vapor deposition jig, which enables recovery of the vapor deposition jig and reuse of the vapor deposition jig.

[0006]

A vapor deposition jig of the present invention for solving the above-mentioned problems comprises a holder made of Cu or a Cu alloy on the surface of which a corrosion resistant metal (excluding Ni and Pt) or a corrosion resistant alloy is formed. It is characterized in that a coating layer is provided. It is particularly suitable for forming a vacuum thin film on a plastic substrate which is easily deformed by heat. The corrosion-resistant metals include Cr, Ti, Ta, Nb, Rh, Ir, W and Mo, and the corrosion-resistant alloys include Ni alloy, Fe alloy and Cr.
Although alloys and the like are used, a coating layer of Cr or Ni-P alloy gives good results. When the Cr coating is used, the thickness is preferably 2 μm to 100 μm, and when the Ni—P alloy coating is used, the thickness is
It is preferably 0.5 μm to 50 μm. Further, an Ni-plated intermediate plating layer may be provided between the corrosion-resistant metal or corrosion-resistant alloy coating layer and Cu or Cu alloy to improve the adhesion and corrosion resistance. In addition, in the method for recycling the vapor deposition jig of the present invention, after the vapor deposition jig of the present invention is used, Au, Ag or Pd adhering to the surface is dissolved with a chemical solution to recover Au, Ag or Pd. Along with this, the vapor deposition jig is regenerated. The chemical solution is preferably a cyan compound solution or an iodine compound solution.

[0007]

As described above, the vapor deposition jig of the present invention is made of Cu or a Cu alloy. Therefore, in vapor deposition on a plastic substrate, heat is radiated favorably and deformation or deterioration of the substrate is prevented. Further, in the vapor deposition jig of the present invention, a coating layer of a corrosion-resistant metal or a corrosion-resistant alloy is provided on the surface of Cu or a Cu alloy, and in the recycling method of the present invention after use, Au deposited on the surface is used. , Ag or Pd is dissolved by a chemical solution,
When recovering u, Ag or Pd, the coating layer of the corrosion resistant metal or the corrosion resistant alloy acts as a protective film of the Cu or Cu alloy base material. Since the vapor deposition jig is not attacked by the chemical liquid and corrosion is prevented, the vapor deposition jig is regenerated. Further, especially in the case of the Cr coating layer and the Ni-P coating layer, since they have abrasion resistance, they are effective in preventing the abrasion of the jig when the jig is frequently attached and detached.

When the surface of the evaporation jig is a Cr coating layer, nitric acid, aqua regia, cyanide compound solution, iodine compound solution or the like can be used as a chemical solution for dissolving Au, Ag or Pd. However, since the Cr coating layer formed by chrome plating has many defects such as cracks, it is somewhat weak against nitric acid and aqua regia, and more preferably a cyan compound solution or an iodine compound solution. When a Ni-P layer is used, nitric acid, a cyanide compound solution, an iodine compound solution or the like can be used as a chemical liquid to be used, but a solution such as aqua regia or hydrochloric acid and chlorine gas dissolves the Ni-P layer Cannot be used as it will attack the material. The use of nitric acid is effective when the vapor deposition component is Ag or Pd or its alloy composition, but it cannot be applied to Au because it does not dissolve in nitric acid. Ni is not soluble in concentrated nitric acid, but is attacked by dilute nitric acid. Therefore, even when the Ni-P coating layer is used, a cyan compound solution or an iodine compound solution is more preferable. In the case of a cyan compound solution, it is easy to use a cyan-based gold solution. Commercially available products include Concentrate N (manufactured by Japan Electroplating Engineers) and Enstrip S (manufactured by Japan Metal Co.). Those to which a reaction accelerator is added can be dissolved quickly. . Further, it may be dissolved by using air or hydrogen peroxide in a potassium cyanide solution as in the bluing method used for refining gold or silver. The cyan solution can dissolve any of Au, Ag, and Pd, and has a wide range of application. The iodine compound solution also dissolves Au, Ag, and Pd similarly to the cyan compound solution. Although it is easy to dissolve with a commercially available iodine etching solution, Au in a solution containing potassium iodide and iodine,
Ag or Pd can be dissolved.

When a Cr coating layer is used in the vapor deposition jig of the present invention, its thickness is slightly thicker. The thickness is preferably 2 μm or more, and 5 μm or more is effective in consideration of any troubles such as scratches. There is no problem if it is too thick, but from the viewpoint of labor, the upper limit is 100 μm. The Cr coating is most conveniently formed by chrome plating. Various chrome plating baths have been reported, so the bath should be selected appropriately. Further, dry plating is more preferable because it forms a coating with fewer defects than chromium plating, but it is expensive. When a Ni-P coating layer is used, its thickness is
It is preferably 0.5 μm or more, more preferably 1.0 μm.
It is effective to have m or more. There is no problem if it is too thick,
From the aspect of labor, the upper limit is 50 μm. The Ni-P coating can be easily formed by Ni-P electroless plating.
An amorphous coating having a composition of ˜98% by weight and P2 to 15% by weight is obtained. It is known as an amorphous coating and has excellent corrosion resistance and wear resistance. There is also a method of forming by dry plating like Cr. Other corrosion-resistant metals or corrosion-resistant alloys such as Rh and Fe alloys can be formed by electrolytic plating.
The i, Ta, Nb, Ir, W, Mo, Cr alloy and the like are formed by a method such as sputtering. A binder such as Ni plating may be provided on the base of the corrosion-resistant metal or corrosion-resistant alloy coating layer to enhance the adhesion and further improve the corrosion resistance. In that case, the corrosion resistance may be worse than the case where the corrosion-resistant metal or corrosion-resistant alloy coating layer is directly provided depending on the conditions such as thickness and local battery action. Therefore, the condition setting is appropriately selected. The thickness of the intermediate Ni coating layer is preferably 0.5 μm or more, and there is no problem if it is too thick, but the upper limit is 50 μm.

[0010]

[Embodiment 1] An embodiment of a vapor deposition jig and a method for recycling the vapor deposition jig of the present invention will be described. Prior to a concrete example, the material test will be described. Length 40 mm, width 20 m
A Cu sample piece having a thickness of 0.5 mm and a thickness of 0.5 mm was prepared, and as an example, prior to Cr plating and Ni—P plating, Cu strike plating was previously performed as an intermediate layer and then nickel plating was performed to a thickness of 5 μm. Then Cr plating 2μm, 10μ
m and Ni-P electroless plating 1.0μm, 5μ
Prepared one. As a conventional example, pure C
A u-made sample piece was prepared. Each of the above sample pieces was immersed in a cyan gold solution (containing 5% of potassium cyanide and a reaction accelerator) at room temperature, and air was blown into the solution to check the weight change. The results shown in Table 1 below were obtained. Obtained.

[0011]

[Table 1]

As is clear from Table 1 above, the Cr-plated or Ni-P-plated sample pieces had no base material (Cu) dissolved in the cyan gold solution, but the pure sample pieces were
It completely dissolved in 1.5 hours.

In the case of Cr plating (2 μm), swelling occurred between the nickel intermediate layer and the chromium layer,
Others were unchanged.

[0014]

[Example 2] A test piece made of brass having a length of 40 mm, a width of 20 mm and a thickness of 0.5 mm was made, Cr and Ni-P plating were applied to 5 μm, and two test pieces which were dry plated with gold of 10 μm and silver were used.
Two 10 μm dry-plated test pieces were prepared. The test pieces were immersed in a concentrated nitric acid solution and an iodine compound solution (containing 20% potassium iodide and 5% iodine) at room temperature for 1 hour.
When the state after r was examined, the results shown in Table 2 below were obtained.

[0015]

[Table 2]

It can be clearly seen from Table 2 above that when concentrated nitric acid is used, both Ni--P and Cr coatings are slightly weak. On the contrary, with the iodine compound solution, both Au and Ag could be recovered and the base material was not attacked.

[0017]

[Embodiment 3] Next, a specific embodiment and a conventional example will be described. As shown in FIG. 1, a plurality of screw pins 2 for attachment are attached to the lower surface of a circular Cu lower piece 1 having a diameter of 140 mm and a thickness of 12 mm. Is fixed, and an annular Cu upper piece 3 having an upper inner diameter of 115 mm, a lower inner diameter of 120 mm, an outer diameter of 140 mm, and a height of 8 mm, which has an inverted L-shaped cross section, is fixed from the lower side with a set screw 4, A Cu vapor deposition jig 5 was formed, and as an example, the Cu vapor deposition jig 5 was subjected to Cu strike plating, Ni underlayer plating to 10 μm, and Ni—P plating to 5 μm.

A doughnut-shaped substrate 8 having a circular hole 7 having an inner diameter of 15 mm in the central portion as shown in FIG. 2 was mounted on both of these evaporation jigs as shown in FIG. Was vapor-deposited. As a result, the outer peripheral surface exposed after mounting the vapor deposition jig on the substrate, the upper surface and the inner peripheral surface of the upper piece 3,
Au was attached to the central portion of the upper surface of the lower piece 1 as shown in FIG.

The vapor deposition jigs of the examples were treated by blowing air into both of the vapor deposition jigs to which Au had adhered, while immersing them in the same cyan gold solution as described above at room temperature to dissolve the adhered Au. Only Au was completely dissolved.

[0020]

As described above, since the vapor deposition jig of the present invention is made of Cu or a Cu alloy having a Cr or Ni-P coating layer on its surface, it is particularly suitable for vapor deposition on a plastic substrate. It is suitable for vapor deposition of compact discs, MO discs, etc. Further, the method for regenerating a vapor deposition jig of the present invention is such that after the vapor deposition jig made of Cu or a Cu alloy having a Cr or Ni-P coating layer on the surface is used, Au, Ag or Pd attached to the surface is used. Is dissolved in a chemical solution, Au, Ag, or Pd can be recovered, and the Cr or Ni-P coating layer does not immerse the Cu or Cu alloy vapor deposition jig in the chemical solution and thus prevents corrosion.
The evaporation jig can be regenerated and can be used semi-permanently repeatedly.

[Brief description of drawings]

FIG. 1 is a diagram showing a vapor deposition jig of the present invention.

FIG. 2 is a diagram showing a doughnut-shaped substrate on which Au is deposited.

FIG. 3 is a diagram showing a state in which the substrate of FIG. 2 is mounted on the evaporation jig of FIG.

4 is a diagram showing a state in which Au is attached to a vapor deposition jig when Au is vapor-deposited on a substrate mounted on the vapor deposition jig shown in FIG.

[Explanation of symbols]

 5 Deposition jig 6 Pt coating layer

Claims (11)

[Claims] 1. A vapor deposition jig comprising a coating layer of a corrosion resistant metal (excluding Pt and Ni) or a corrosion resistant alloy provided on the surface of a vapor deposition jig made of Cu or a Cu alloy. 2. The evaporation jig according to claim 1, wherein the evaporation jig is for forming a vacuum thin film on a plastic substrate. 3. The corrosion resistant metal is Cr, Ti, Ta, N.
It is one of b, Rh, Ir, W or Mo.
Or the jig for vapor deposition according to 2. 4. The vapor deposition jig according to claim 1, wherein the corrosion-resistant metal is Cr. 5. The vapor deposition jig according to claim 1, wherein the corrosion resistant alloy is any one of a Ni alloy, a Fe alloy and a Cr alloy. 6. The jig for vapor deposition according to claim 1, wherein the corrosion resistant alloy is a Ni—P alloy. 7. The Cr coating layer has a thickness of 2 μm to 100 μm.
The jig for vapor deposition according to claim 4, which has a thickness of μm. 8. The vapor deposition jig according to claim 6, wherein the Ni-P coating layer has a thickness of 0.5 μm to 50 μm. 9. An intermediate plating layer of Ni plating is provided between the Cu or Cu alloy and the corrosion-resistant metal or corrosion-resistant alloy coating layer.
The jig for vapor deposition according to 5, 6, 7 or 8. 10. The Au or Ag deposited on the surface after the use of the vapor deposition jig according to any one of claims 1 to 9.
Or, Pd is dissolved by a chemical solution, and Au, Ag, or Pd is dissolved.
And a method for remanufacturing a jig for vapor deposition, which comprises reclaiming the jig. 11. The method for regenerating a deposition jig according to claim 10, wherein the chemical solution is a cyan compound solution or an iodine compound solution.