JPH10259471A - Jig for vapor deposition and method for recovering noble metal from the jig for vapor deposition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To dissolve a Zn coating layer with a medicinal liquid and to easily recover the noble metals sticking to the surface of a jig for vapor deposition for which Cu or Cu alloy having a good heat radiating effect is used by successively providing the surface of the jig for vapor deposition with an Ni coating layer hardly soluble in the medicinal liquid and the Zn coating layer easily soluble therein. SOLUTION: At the time of forming a vacuum thin-film on a plastic base material, the Cu or Cu alloy is used as the jig 5 for vapor deposition for holding the base material to accelerate the heat radiation and to prevent the deformation, change of properties, etc., of the base material. The jig 5 for vapor deposition is obtd. by fixing, for example, a lower piece 1 made of Cu having mounting screws 4 and an annular upper piece 3 having an L type of sectional area made of Cu by means of these screws 4. Further, the substrate of the jig 5 is provided with the Ni coating layer 7 and the Zn coating layer 6 on the surface by plating, etc., to a thickness 1 to 30 μm and if necessary, the upper part of the Zn coating layer 6 is provided with Cu or Au strikes. After the noble metals, such as Au, Ag and Pd, are deposited by evaporation thereon, the Zn is dissolved by the medicinal liquid, as hydrochloric acid and sulfuric acid, by which the sticking noble metals are recovered in the form of foil. The surface of the remaining Ni coating layer is thereafter, coated with Zn to regenerate the 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 and the like, and more particularly to an improvement of a vapor deposition jig made of Cu or Cu alloy aiming at a heat radiation effect and a vapor deposition jig thereof. For recovering precious metals from wastewater.

[0002]

2. Description of the Related Art Vacuum thin film forming techniques typified by sputtering, ion plating, vacuum deposition and the like are widely used mainly in the semiconductor industry. When forming a vacuum thin film on a base material, it is common to mount the base material on a deposition jig called a holder and form a thin film on the base material. Since the thin film forming component, which is a vapor deposition substance, adheres to the vapor deposition jig as it is used, if the amount of the vapor deposition jig becomes unbearable for use, it will be replaced. The deposit adhered to the deposition jig is treated with a chemical solution such as a sand blast method or nitric acid to peel off the deposit, and is used again as a deposition jig.
Generally, stainless steel or titanium is used as the material of the deposition jig. However, when a thin film is formed 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 radiation and prevent deformation and deterioration of the substrate.

[0003] Stripping of a deposited material deposited on a jig for deposition of Cu or Cu alloy is performed by a sand blast method. When a noble metal such as Au or Ag or an alloy thereof (hereinafter, collectively referred to as a noble metal including a noble metal alloy) adheres to a deposition tool for Cu or a Cu alloy, if the same is peeled off by the sandblasting method, about 80% is obtained. The front and rear can be recovered as precious metal that has largely peeled off. But the remaining about 20
% Will be mixed into the emery. If the noble metal mixed into the emery is recovered, the recovery rate can be increased, but it takes much time and effort.

[0004] In order to recover all precious metals, treatment with chemicals such as aqua regia, nitric acid, and cyanide allows precious metals to be easily recovered. However, a vapor deposition jig made of Cu or a Cu alloy has no corrosion resistance to these chemicals, so that the base material also dissolves, making it impossible to reuse the vapor deposition jig. The noble metal is also an expensive material, but the vapor deposition jig is expensive, so that the former method capable of regenerating the vapor deposition jig is usually employed. In recent years, as a recovery method instead of the above two methods, using a jig provided with a protective layer made of a corrosion-resistant metal on the surface of a holder made of Cu or Cu alloy,
Various methods have been proposed in which, after use for vapor deposition, only Au, Ag, and Pd adhering to the surface are dissolved by a chemical solution to recover Au, Ag, or Pd and recycle the vapor deposition jig.
As the jig protection layer, Pt, Ni, Cr, Al, Ti,
Metals such as Ta, Nb, Rh, Ir, W, and Mo and alloys thereof are known. However, when these protective layers have fine defects such as scratches and pinholes, the chemical solution used for dissolution penetrates to the underlying portion of Cu or Cu alloy,
There are also problems such as a problem of erosion of the underlayer and a problem that the protective layer is peeled off during the deposition process and adheres to the CD due to insufficient adhesion between Au, Ag and Pd.

[0005]

Therefore, the present invention solves the problem of the conventional jig for vapor deposition of Cu or Cu alloy, and recovers the noble metal by chemical solution treatment similarly to the jig for vapor deposition of stainless steel or titanium. An object of the present invention is to provide a vapor deposition jig and a method of recovering a noble metal from the vapor deposition jig.

[0006]

According to a first aspect of the present invention, there is provided a vapor deposition jig comprising: a holder made of Cu or a Cu alloy; and a Ni coating layer and a Zn coating layer sequentially provided on the surface of the holder. It is a feature. Particularly, it is suitable for forming a vacuum thin film on a plastic substrate which is easily deformed by heat.
In addition, the method for recovering noble metals from the jig for vapor deposition of the present invention is such that after using the jig for vapor deposition of the present invention, Zn is dissolved with a chemical solution such as hydrochloric acid to remove Au, Ag, and Pd adhering to the jig surface. It is characterized by being recovered in the form of metal foil.

As described above, since the base of the vapor deposition jig of the present invention is made of Cu or Cu alloy having excellent heat conductivity,
Upon vapor deposition on the plastic substrate, good heat radiation is performed, and deformation and deterioration of the substrate are prevented. Further, the jig for vapor deposition of the present invention comprises a Ni coating layer and a Z
Since the n coating layer is provided in order, in the noble metal recovery method of the present invention after use, Zn is dissolved by a chemical solution,
When recovering Au, Ag, or Pd, the insoluble jig coating layer prevents the jig for vapor deposition of Cu or Cu alloy from being attacked by the chemical solution, thereby preventing corrosion. As a result, after the recovery processing, the Ni-coated vapor deposition is performed. Tool is obtained. By coating this jig again with Zn, the jig for vapor deposition of the present invention is regenerated.

[0008]

DESCRIPTION OF THE PREFERRED EMBODIMENTS As a method for forming a Zn coating layer and a Ni coating layer, there are a wet coating such as electroplating, a dry plating such as vacuum evaporation and sputtering, a paste coating method, a metal foil sticking method, and the like. Can be used,
The electroplating method is most suitable in consideration of productivity applicable to a jig having a complicated shape, adhesion to a base, and thermal conductivity. The thickness of the Zn coating layer and the Ni coating layer in the jig for vapor deposition of the present invention is preferably 1 μm or more, and it is effective that the thickness is 5 μm or more when troubles such as scratches are included. There is no problem if it is too thick, but the upper limit is 30 μm in terms of cost.

In order to enhance the adhesion to the noble metal to be deposited, a Cu strike and / or A
A u strike may be provided. In that case, the strike may have a thickness of 0.01 μm to 1.0 μm.

As a chemical solution used for dissolving Zn, sulfuric acid or hydrochloric acid having a concentration of 1 to 35% can be used.
A solution such as aqua regia or hydrochloric acid and chlorine gas cannot be used because it dissolves Ni and attacks the base material.

[0011]

[Embodiment 1] An embodiment of a vapor deposition jig and a recovery method using the vapor deposition jig of the present invention will be described. Prior to the specific examples, the material test will be described.
A sample piece made of Cu having a thickness of 20 mm, a width of 20 mm, and a thickness of 0.5 mm was prepared. Each of the sample pieces was immersed in 10% hydrochloric acid for 2 minutes, and the solution was subjected to ICP analysis. Ni and Cu in the solution were both 0.1 mg or less, and neither the base material Cu nor the Ni coating was dissolved. I understood. In addition, it turned out that Zn melt | dissolved completely from the weight reduction of a sample piece.

[0012]

Example 2 The same test piece as in Example 1 was immersed in 10% hydrochloric acid for 1 hour at room temperature to conduct a dissolution test. Dissolve the solution
After CP analysis, Ni and Cu in the solution were 5.3 mg each,
1.6 mg. When this amount of dissolution is converted into thickness, Ni
Is 0.07 μm and Cu corresponds to a decrease in thickness of 0.03 μm.
It was found from the dimensions of the deposition jig that the amount of film reduction was such that no problem occurred.

[0013]

Embodiment 3 Next, a specific embodiment and a conventional example will be described. As shown in FIG. 1, a plurality of mounting screw pins 2 are mounted on the lower surface of a circular Cu lower piece 1 having a diameter of 140 mm and a thickness of 12 mm. Is fixed to the outer periphery of the upper surface, and an annular upper Cu piece 3 having an inverted L-shaped cross section 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 is fixed from below with a set screw 4, A Cu deposition jig 5 is formed. As a working example, a coating layer 7 of Ni plating was applied to the surface of the jig 5 made of Cu at 5 μm, and then a coating layer 6 of Zn plating was applied at 5 μm, and further, a Cu strike and an Au strike were performed. As a conventional example, C
Al is formed on the surface of the u deposition jig 5 by sputtering.
1 μm was applied.

A donut-shaped substrate 9 having a circular hole 8 having an inner diameter of 15 mm at the center as shown in FIG. 2 is mounted on the two jigs for vapor deposition as shown in FIG. Was deposited at about 1 μm. As a result, as shown in FIG. 4, Au10 adheres to the outer peripheral surface, the upper surface and the inner peripheral surface of the upper piece 3, and the center of the upper surface of the lower piece 1 which are exposed after the substrate is mounted. However, in the conventional vapor deposition jig, when Au adhered to about 0.5 μm, peeling occurred, and A
Sputtering was stopped because the adhesion of u did not work well.

The jig for vapor deposition of the embodiment to which Au was adhered was immersed in the same hydrochloric acid solution as above at room temperature and subjected to a dissolution treatment, whereby the foil-like Au and the jig were separated cleanly.

[0016]

As described above, the vapor deposition jig of the present invention is made of Cu or a Cu alloy having a Ni coating layer and a Zn coating layer on its surface. Heat is dissipated and deformation of the plastic substrate is prevented. Further, since the adhesiveness is excellent, an improvement in productivity can be sufficiently expected. Furthermore, the method for regenerating the jig for vapor deposition of the present invention,
Cu or C with Ni coating layer and Zn coating layer on the surface
After the use of the vapor deposition jig made of a u-alloy, Au, Ag or Pd can be recovered in the form of a metal foil by dissolving the Zn coating layer with a chemical solution, and the Cu or C
Since the u-alloy jig for vapor deposition is not immersed in the solution and corrosion is prevented, the jig for vapor deposition can be easily regenerated and can be used semipermanently repeatedly.

[Brief description of the drawings]

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

FIG. 2 is a view showing a donut-shaped substrate on which Au is deposited.

FIG. 3 is a view showing a state where the substrate of FIG. 2 is mounted on the vapor deposition jig of FIG. 1;

FIG. 4 is a view showing a state in which Au adheres to the vapor deposition jig when Au is vapor-deposited on a substrate mounted on the vapor deposition jig of FIG. 3;

[Explanation of symbols]

 5 Deposition jig 6 Zn coating layer 7 Ni coating layer

Claims (6)

[Claims] 1. A vapor deposition jig comprising: a vapor deposition jig made of Cu or a Cu alloy; and a Ni coating layer and a Zn coating layer sequentially provided on a surface of the vapor deposition jig. 2. The deposition jig according to claim 1, wherein said deposition jig is for forming a vacuum thin film on a plastic substrate. 3. The thickness of the Ni coating layer and the Zn coating layer is 1 μm.
The vapor deposition jig according to claim 1 or 2, wherein the thickness is from 30 to 30 µm. 4. The vapor deposition jig according to claim 1, wherein a Cu strike and / or an Au strike are provided on the Zn coating layer. 5. The method according to claim 1, wherein after using the vapor deposition jig, Zn is dissolved with a chemical solution to recover at least one of noble metals such as Au, Ag, and Pd or alloys thereof. Noble metal recovery method from jig for vapor deposition. 6. The method according to claim 5, wherein the chemical is hydrochloric acid or sulfuric acid.
A method for recovering precious metals from the above described jig for vapor deposition.