TWI480428B - A mold for partial sureface treatment of secondary optics lens on light-emitting diodes or condenser or refraction lens on solar cell - Google Patents

Description

Mould for partial surface treatment of refraction or condensing mirror for secondary optics or solar cells of light-emitting diode

The invention relates to a partial surface treatment mold suitable for a secondary optical mirror or a solar cell refractive or concentrating mirror for a light-emitting diode, which can expose a specific surface of a sample to be treated and is suitable for a specific exposed sample surface. Perform electrolysis, electropolishing, electroplating, anodizing, etching, immersion plating, pickling, caustic washing, vapor deposition, and the like.

In recent years, the development of global surface treatment is in the ascendant. Many surface treatments have successfully developed and applied to improve people's quality of life, and also created unlimited business opportunities, such as electronic product surface, communication equipment surface, and notebook computer surface, for surface treatment requirements. The quality is getting more and more stringent. Precision surface treatment is currently widely used in optical and electronic products, especially nanostructured films have the advantages of low cost process and mass production, and are favored by the industry. In the selection of mass production processes, The electrochemical process can accurately control the current density of the surface of the workpiece up to nA.cm ^-2 , so the use of electrochemical methods to improve the surface properties of the product or to fabricate nanostructured films is often a traditional industry, such as etch and electrolysis. Technology companies such as electroplating, or anodizing have entered the first step of the nanotechnology process. In order to obtain high-quality products by electrochemical methods, in order to obtain high-quality products, it is necessary to accurately control the process conditions during the manufacturing process, such as the electrolyte temperature and reaction area of the workpiece. Therefore, the sample must be clearly defined by the design of the mold. The reaction area and the design of the reaction tank accurately control the temperature of the reaction liquid.

The basic chemical treatment includes electroplating, electrolysis, anodizing, batteries, and double-layer capacitors. The electrochemical reaction system should include three parts: anode, cathode, and electrolyte. In the electrochemical system, the external metal between the two electrodes in the electrochemical system. The wire moves, and the ions are transferred by the electrolyte. The electrons move synchronously with the ions to form a basic electrochemical circuit. The reaction area of the sample is the basic parameter for evaluating the reaction rate in a chemical reaction or an electrochemical reaction. The sample reaction area needs to be clearly defined by the mold. The conventional acid-base tape can easily define the reaction area of the sample, but it is another heavy burden for the construction and tape cost, and is easy to produce tape edge leakage and The disadvantage of faster reaction rate, in order to solve the problem of strict requirements on surface treatment quality, the present invention proposes a chemical processing mold which has close contact with the surface of the sample and can accurately define the surface area of the treatment area, and can be applied to the surface of the sample. High quality surface treatment.

The anodizing treatment in electrochemical reactions is defined as a mature traditional industry, and its main applications are surface modification, such as surface corrosion resistance, coating, decoration, electrical insulation, surface plating, wear resistance, etc., due to the anodized film. The porous structure, which is subsequently subjected to a sealing treatment step, can be applied to a dense film with an aesthetic appearance and a multi-color. In recent years, due to the development of nanotechnology, the tube diameter, tube length, and tube density of the anodized film tube or nanotube structure are technically more complete. Simple anode treatment technology, which provides a low cost and fast mass production process, which can be applied to the required unit. The development of products with large surface areas, such as the development of dye-sensitized solar cells, thermal conductive sheets, and thermal insulation sheet components. Anode treatment technology, with the demand for industrial products, has been applied to the vacuum chamber of vapor deposition equipment in recent years from the early requirements for surface modification of corrosion resistance, abrasion resistance, impact resistance, and high temperature resistance of heavy industrial structures. The coating absorption layer of the part, or the barrier layer in the integrated circuit, with the development of the most popular heat dissipation materials, heat insulation materials, green building materials, and solar cells, the anodizing technology with automatic production characteristics is bound to be Become one of the processes of various industries.

The application of anodizing in industrial applications, in which the operating technology of aluminum and titanium is the most mature, when the aluminum is placed in a specific electrolyte and the appropriate anode treatment parameters are controlled, the formed oxide film has a regular cell or The structure of the nanotube, the interface between the end of the nanotube and the aluminum material forms a hemispherical barrier layer, wherein the composition of the nanotube and the barrier layer is aluminum oxide (Al ₂ O ₃ ), and the aluminum is treated at the anode. Mainly by 2Al ⁺³ +3H ₂ O→Al ₂ O ₃ +6H ⁺ reaction, therefore, it is necessary to control the pH below 4, that is, under the condition of acidic solution, and the applied voltage needs to be higher than -1.8V ( SHE) above, in which H ⁺ will generate hydrogen by H ⁺ +H ⁺ →H ₂ , which will escape from the inside of Al ₂ O ₃ , thereby causing the formation of porous alumina, thus controlling hydrogen evolution At the rate, the pores formed inside the alumina can be controlled to become an anodized aluminum film having a uniform pore size. When the aluminum is anodized, an aluminum oxide (Al ₂ O ₃ ) oxide layer is formed on the surface, and the oxide layer grows upwards in a hexagonal hole at the beginning of growth, and the arrangement of atoms around the hexagonal hole gradually increases with time. The arrangement of the disorder, so the hole gradually turns into a circular hole, and the change in the aperture can be expressed by C=mV, where C: aperture size (nm), V: anode processing voltage (V), m: constant (2~2.5).

Titanium dioxide (TiO ₂ ) produced by anodizing has been widely used in industrial and academic research because of its high-performance photocatalytic properties, high chemical stability, and low cost. Low-dimensional TiO ₂ structures, such as nanotubes, nanowires, and nano-titanium nanomaterials, have great potential in applications such as optics, electronics, catalysts, and sensors, as opposed to bulk titanium dioxide. It has a large surface area, which can absorb a large amount of photoelectrons and convert it into energy. The nanowire can detect and trace trace elements, greatly improving the sensitivity of the detector, and the catalyst with high reaction area can improve the reaction efficiency. Wait. The anodizing method can quickly obtain a high-quality anodic titanium oxide film with a nanometer tube shape, and the diameter of the tube can be made up to a diameter of 30 to 100 nm with the applied voltage, and the tube length will be electrolyzed. The liquid type is controlled to obtain a tube length of 0.1 to 1000 μm, and the nanopore density of the oxide film is between 10 ⁸ and 10 ¹⁰ pore/cm ² . An anatase anode titanium dioxide nano template having photocatalytic properties can be formed by forming an amorphous amorphous titanium oxide film on the surface through anodizing, heat treatment and the like. After the heat treatment, an anatase titanium dioxide film template of an anatase phase can be obtained.

The crystal phase of titanium dioxide (TiO ₂ ) is common, and there are anatase phase, brookite phase and rutile phase. The phase stability can be controlled by heat treatment, and the anatase phase belongs to low temperature ( 280~450°C) stable phase, while rutile phase is high temperature (580~1600°C) stable phase. The crystallized titanium dioxide has many excellent electrical and optical properties, among which the rutile phase can be used for a dielectric material of a capacitor or a high temperature oxygen partial pressure detector, and an anatase phase can be used for a photocatalyst, solar energy. Application of materials such as batteries and water repellency. When the titanium dioxide of the anatase phase is irradiated by ultraviolet light or sunlight, the electrons on the surface of the titanium dioxide absorb enough energy to escape, and an electron-hole pair (e ^- h ⁺ ) reaction can be generated on the surface. The hole oxidizes the hydroxyl group (OH ^- ) liberated from nearby water molecules (that is, it takes its electrons to become an extremely active OH radical; once the hydroxyl radical encounters an organic substance, it will The electrons will be recaptured, and the organic molecules will fall apart due to the collapse of the bond. The general pollutants or pathogens are mostly carbohydrates, and most of them will become harmless water and carbon dioxide after decomposition, so the target of decontamination and sterilization can be achieved. When the ultraviolet light wavelength is irradiated on the anatase phase of titanium dioxide, the electrons (e ^- ) in the valence band (VB) are excited by the ultraviolet energy (3.2 eV) to jump to the conduction band (CB). At this time, a positively charged hole is formed in the valence band, and a set of electron-hole pairs is formed. The titanium oxide utilizes the oxidizing power of the generated hole and the reducing power and surface contact of the electron. H ₂ O, O ₂ acts to generate a radical with strong oxidizing power. Photoexcitation of the anatase phase of titanium dioxide causes an electronic transition, and the wavelength of light required can be evaluated by this formula: E = h ν = hc / λ; where E _g : Energy gap(eV),h:planck constant=6.626×10 ^-34 (J.s), ν:Frequency(Hz),c=2.298×10 ⁸ (m/s), λ:wave length,λ=1240/ E _g (nm), TiO ₂ (anatas) E _g is 3.2eV, so λ is 387.5nm, that is, ultraviolet light with incident light wavelength less than 387.5nm, can excite titanium dioxide of anatase phase to produce photocatalytic effect .

It is an object of the present invention to provide a partial surface treatment mold suitable for a secondary optical mirror or a solar cell refracting or concentrating mirror of a light-emitting diode, which can be electrolyzed, electrolytically polished, and plated by a mold assisting a specific region of the sample. Chemical reactions such as anodizing and etching. The invention patent considers the operation convenience and service life of the mold Long, and commercial value, therefore, the use of low-material cost polymer, metal, metal surface insulation materials such as insulating materials, engineering plastics, polymers, or acrylic to make a chemical processing mold and apply wet chemistry In the processing environment, the mold structure for the chemical treatment has characteristics such as simple production and large area variability, and is suitable for industrial mass production. The structure of the chemical processing mold is as shown in Fig. 1, comprising: a conductive wire 101; a silicone sleeve 102; a conductive wire waterproof cover 13; a conductive wire waterproof seat 104; a conductive wire waterproof seat O-ring 105; Conductive bar 106; mold lower seat 107; mold lower seat O-ring 108; conductive sheet 109; upper cover waterproof gasket 110; working sample 111; mold upper cover 112; open reaction area 113 of working sample.

Figure 2 further illustrates a three-dimensional assembly structure of the mold 20, the structure comprising a conductive line 201 connected between the working sample and the conductive rod; the rubber sleeve 202 for preventing water seepage, the conductive waterproof cover 203, the conductive line waterproof a seat 204, a conductive waterproof seat O-ring 205; a mold lower seat 206 for fixing the conductive sheet and the working test piece; a mold lower seat O-ring 207 for preventing water seepage; for defining an open reaction area of the working sample The upper cover 208. 3 is a view showing a mold lower seat-conductive wire-conductive bar assembly structure, including a mold lower seat 301; a mold lower seat O-ring 302 for preventing water from seeping between the lower seat 301 and the upper cover; and a conductive wire 306 for preventing the conductive wire 306. A conductive waterproofing base 303, a conductive waterproof cover 304, and a silicone sleeve 305, which are in contact with the lower seat 301, are connected to the conductive wire 306 between the conductive rod 307 and the power supply. Figure 4 is a view showing the structure of the conductive sheet. The conductive sheet is an integrally formed or bonded conductor. The first surface 401 has a larger diameter and can be placed in the upper cover of the mold. The second surface 402 has a smaller diameter and can be placed. In the lower seat of the mold, the second surface is further provided with a conductive rod fixing hole 403 for increasing the contact stability of the conductive rod on the conductive sheet.

Figure 5 illustrates the structure of the upper cover of the mold, the structure of which includes the outer diameter 501 of the upper cover of the mold; the inner diameter 502 of the upper cover of the mold provides the first surface for fixing the conductive sheet; the contact surface 503 of the upper cover and the lower seat of the mold provides the waterproof film placement; The upper cover female teeth 504 are used to bond the mold lower seat male teeth; the upper mold cover waterproof film holder 505 is used to prevent liquid from penetrating into the mold upper cover female teeth 504 from the open reaction area 506 of the working sample. Figure 6 is a view showing the structure of the lower seat of the mold, the structure including the lower seat male tooth 601 for joining the upper cover tooth of the mold; the lower seat torque assisting hole 602 for assisting the application of a torsion force to combine the lower seat male tooth with the upper cover male tooth The tightness; the conductive wire waterproof seat O-ring groove 603 is used to prevent liquid from penetrating into the conductive piece of the mold lower seat 601 by the conductive wire; the lower seat female tooth 604 is used for bonding the conductive wire waterproof seat male tooth.

Hereinafter, each embodiment of a mold for chemical treatment according to the present invention will be described in detail using Figs. 1 to 15 . In the description of the drawings, the same elements or elements having the same function are denoted by the same reference numerals, and the description thereof will not be repeated.

[Example 1]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. The size of the anodized electrolyte is 1~10 vol.% sulfuric acid or Phosphoric acid, or 1~8wt.% of oxalic acid, anodizing conditions of 10~200 volts (V), -5~30 °C, 1 minute~24 hours, Figure 7 shows the use of 3wt.% (by weight) aqueous oxalic acid solution The electrolyte, plus 40 volts DC voltage, anode treatment time of 5 minutes, electrolyte temperature of 25 ° C, can completely react the aluminum metal film into a transparent aluminum oxide film, so the surface of the silicon wafer is brownish black. primary color.

[Example 2]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. The size, using 5wt.% (% by weight) aqueous solution of oxalic acid as electrolyte, plus 30 volts DC voltage, electrolyte temperature of 25 ° C, anode treatment time of 5 minutes, can completely react the metal aluminum film into a transparent aluminum oxide film Therefore, the surface of the wafer is brownish black and the original color of the wafer.

[Example 3]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The area of the surface of the aluminum film is limited by the opening range of the mold, so that the surface of the aluminum film is porous after being anodized. Aluminium oxide film, and using the applied voltage and electrolyte composition to control the distribution of pore density and the size of the pores, using 3wt.% (by weight) aqueous solution of oxalic acid as electrolyte, plus 60 volts DC voltage, electrolyte temperature At 10 ° C and an anodic treatment time of 3 minutes, the aluminum metal film can be completely reacted into a transparent aluminum oxide film, so that the surface of the ruthenium wafer has a brownish black enamel wafer primary color.

[Embodiment 4]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. The size, using 10vol.% (volume percent) sulfuric acid aqueous solution as electrolyte, plus 20 volts DC voltage, electrolyte temperature 10 ° C, anode treatment time 3 minutes, can completely react the metal aluminum film into a transparent aluminum oxide film Therefore, the surface of the wafer is brownish black and the original color of the wafer.

[Embodiment 5]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The area of the surface of the aluminum film is limited by the opening range of the mold, so that the surface of the aluminum film is porous after being anodized. Aluminium oxide film, and using the applied voltage and electrolyte composition to control the pore density distribution and pore size, using 10vol.% (volume percent) sulfuric acid aqueous solution as electrolyte, plus 10 volts DC voltage, electrolyte temperature At 5 ° C and an anode treatment time of 5 minutes, the aluminum metal film can be completely reacted into a transparent aluminum oxide film, so that the surface of the germanium wafer is brownish black and the original color of the wafer.

[Embodiment 6]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. The size, using 10vol.% (volume percent) sulfuric acid aqueous solution as electrolyte, plus 5 volts DC voltage, electrolyte temperature 0 ° C, anode treatment time 10 minutes, can completely react the metal aluminum film into a transparent aluminum oxide film Therefore, the surface of the wafer is brownish black and the original color of the wafer.

[Embodiment 7]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The area of the surface of the aluminum film is limited by the opening range of the mold, so that the surface of the aluminum film is porous after being anodized. Aluminium oxide film, and using the applied voltage and electrolyte composition to control the pore density distribution and pore size, using 1vol.% (volume percent) phosphoric acid aqueous solution as electrolyte, plus 120 volts DC voltage, electrolyte temperature At 3 ° C, the anode treatment time is 3 minutes, the metal aluminum film can be completely reacted into a transparent aluminum oxide film, so the surface of the germanium wafer is brownish black and the original color of the wafer.

[Embodiment 8]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. Size, using 1vol.% (volume percent) aqueous phosphoric acid solution as electrolyte, plus 180 volts DC voltage, electrolyte temperature -1 ° C, anode treatment time 2 minutes, can completely react aluminum metal film into transparent aluminum oxide The film, so the surface of the wafer is brownish black and the original color of the wafer.

[Embodiment 9]

The anode treatment of the aluminum film on the surface of the 6-inch wafer was carried out by the mold body of Fig. 1. In this example, an aluminum film having a thickness of 1 μm is vapor-deposited on the surface of the wafer, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The area of the surface of the aluminum film is limited by the opening range of the mold, so that the surface of the aluminum film is porous after being anodized. The aluminum oxide film, using the applied voltage and electrolyte composition to control the pore density distribution and pore size, using 1vol.% (volume percent) phosphoric acid aqueous solution as electrolyte, plus 205 volts DC voltage, electrolyte temperature At -5 ° C, the anode treatment time of 1 minute, the metal aluminum film can be completely reacted into a transparent aluminum oxide film, so the surface of the germanium wafer is brownish black and the original color of the wafer.

[Embodiment 10]

The anode treatment of the aluminum film on the surface of the 4 吋 glass was carried out by the mold body of Fig. 1. The glass surface of this sample is vapor-deposited with an aluminum film having a thickness of 1 μm, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. The size, the anodized electrolyte is mainly sulfuric acid, phosphoric acid, or oxalic acid. Figure 8 shows the use of 3wt.% (by weight) aqueous oxalic acid solution as electrolyte, plus 40 volts DC voltage, anode treatment time 5 minutes, electrolyte At a temperature of 25 ° C, the aluminum metal film can be completely reacted into a transparent aluminum oxide film, so that the reaction zone is in the form of a transparent glass.

[Embodiment 11]

The anode treatment of the aluminum film on the surface of the 4 吋 glass was carried out by the mold body of Fig. 1. The glass surface of this sample is vapor-deposited with an aluminum film having a thickness of 1 μm, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. Use the opening range of the mold The area to be treated on the surface of the aluminum film is such that the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the size of the pore, and the anode is treated. The electrolyte is mainly composed of sulfuric acid, phosphoric acid, or oxalic acid. The 10 vol.% (volume percent) aqueous solution of sulfuric acid is used as the electrolyte, plus 20 volts DC voltage, the anode treatment time is 3 minutes, and the electrolyte temperature is 10 ° C. The film is completely reacted into a transparent aluminum oxide film, so the reaction zone is in the form of a transparent glass.

[Embodiment 12]

The anode treatment of the aluminum film on the surface of the 4 吋 glass was carried out by the mold body of Fig. 1. The glass surface of this sample is vapor-deposited with an aluminum film having a thickness of 1 μm, and the aluminum film is reacted to form a porous aluminum oxide film by anodization. The opening area of the mold is used to define the area to be treated on the surface of the aluminum film, and the surface of the aluminum film is treated with a porous aluminum oxide film after the anode treatment, and the applied voltage and electrolyte composition are used to control the distribution of the pore density and the pores. The size and anode treated electrolyte are mainly sulfuric acid, phosphoric acid, or oxalic acid. The 1vol.% (volume percent) phosphoric acid aqueous solution is used as the electrolyte, plus 120 volts DC voltage, the anode treatment time is 4 minutes, and the electrolyte temperature is -1. °C, the metal aluminum film can be completely reacted into a transparent aluminum oxide film, so the reaction zone is transparent glass.

[Example 13]

The anodizing treatment of the surface of the 4 Å aluminum sheet was carried out by the mold body of Fig. 1. In this example, the surface of the mechanically ground aluminum sheet is anodized to react the aluminum sheet into a porous aluminum oxide film. Using the opening range of the mold to define the surface of the aluminum sheet The area of the aluminum sheet is made of a film of aluminum oxide which is porous after being anodized, and the applied voltage and electrolyte composition are used to control the distribution of pore density and the size of the pore. The electrolyte treated by the anode is mainly sulfuric acid. Phosphoric acid or oxalic acid is the main one. Figure 9 shows that the surface of the metal aluminum sheet can be made by using 3wt.% (by weight) aqueous oxalic acid solution as electrolyte, 40 volt DC voltage, 1 hour anodic treatment time and 25 °C electrolyte temperature. The reaction produces a transparent aluminum oxide film, and the residual aluminum substrate is removed by using a saturated copper chloride solution to obtain a porous transparent aluminum oxide film, and the microstructure image thereof is shown in FIG.

[Embodiment 14]

The anodizing treatment of the surface of the 4 Å aluminum sheet was carried out by the mold body of Fig. 1. In this example, the surface of the mechanically ground aluminum sheet is anodized to react the aluminum sheet into a porous aluminum oxide film. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the surface of the aluminum sheet is treated with anodized aluminum oxide film, and the applied voltage and electrolyte composition are used to control the distribution of pore density and the pores. The size, anode treated electrolyte is mainly sulfuric acid, phosphoric acid, or oxalic acid, using 10vol.% (by volume) sulfuric acid aqueous solution as electrolyte, plus 20 volts DC voltage, anode treatment time 1 hour, electrolyte temperature 15 °C The surface of the metal aluminum sheet can be reacted to produce a transparent aluminum oxide film, and the residual aluminum substrate can be removed by using a saturated copper chloride solution to obtain a transparent aluminum oxide film.

[Example 15]

The anodizing treatment of the surface of the 4 Å aluminum sheet was carried out by the mold body of Fig. 1. In this example, the surface of the mechanically ground aluminum sheet is anodized to react the aluminum sheet into a porous aluminum oxide film. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the surface of the aluminum sheet is treated with anodized aluminum oxide film, and the applied voltage and electrolyte composition are used to control the distribution of pore density and the pores. The size and anode treated electrolyte are mainly sulfuric acid, phosphoric acid, or oxalic acid. The 1vol.% (volume percent) phosphoric acid aqueous solution is used as the electrolyte, plus 180 volts DC voltage, the anode treatment time is 1 hour, and the electrolyte temperature is -3. °C, the surface of the metal aluminum sheet can be reacted to produce a transparent aluminum oxide film, and the residual aluminum substrate is removed by using a saturated copper chloride solution to obtain a transparent aluminum oxide film.

[Example 16]

The anode treatment of the surface of the 6-inch titanium sheet was carried out in the mold body of Fig. 1. In this example, the surface of the mechanically ground titanium sheet is anodized to react the titanium sheet into a porous titanium dioxide film. The opening area of the mold is used to define the area to be treated on the surface of the titanium sheet, and the surface of the titanium sheet and the titanium oxide film which is porous after the anode treatment are used, and the distribution of the pore density and the size of the pore are controlled by the applied voltage and the electrolyte composition, and the anode is used. The treated electrolyte is mainly fluorinated ammonia or hydrofluoric acid, and Figure 11 shows the use of 0.4 wt.% NH ₄ F (fluorinated ammonia) + 2 vol.% H ₂ O + 98 vol.% Ethyl glycol (ethylene glycol) For the electrolyte, an external DC voltage of 60 volts, an anodic treatment time of 1 hour, and an electrolyte temperature of 25 ° C, the surface of the titanium metal sheet can be reacted to produce a porous transparent titanium oxide film, and the microstructure image thereof is as shown in FIG.

[Example 17]

The anode treatment of the surface of the 6-inch titanium sheet was carried out in the mold body of Fig. 1. In this example, the surface of the mechanically ground titanium sheet is anodized to react the titanium sheet into a porous titanium dioxide film. The opening area of the mold is used to define the area to be treated on the surface of the titanium sheet, and the surface of the titanium sheet and the titanium oxide film which is porous after the anode treatment are used, and the distribution of the pore density and the size of the pore are controlled by the applied voltage and the electrolyte composition, and the anode is used. The treated electrolyte is mainly fluorinated ammonia or hydrofluoric acid. Figure 11 shows the use of 0.4 vol.% HF (hydrofluoric acid) aqueous solution as electrolyte, plus 20 volt DC voltage, anode treatment time 20 minutes, electrolyte temperature At 25 ° C, the surface of the titanium metal sheet can be reacted to produce a porous transparent titanium oxide film.

[Embodiment 18]

The surface of the aluminum material was electropolished with the mold body of Fig. 1. In this example, the surface of the aluminum material after pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the applied voltage and electrolyte composition are used to control the quality of the electropolishing. The conditions of the electropolishing are: 5-20% perchloric acid (HClO ₄ ) + 5~20 % monobutyl ether ethylene diester (CH ₃ (CH ₂ ) ₃ OCH ₂ CH ₂ OH) + 85 ~ 95% ethanol (C ₂ H ₆ O), electrolyte temperature is 2 ~ 40 ° C, electrolysis voltage is 5 ~ 50 Volt, electropolishing time is 1~10 minutes, Figure 13 shows the best electropolishing operation condition is 15% perchloric acid (HClO ₄ ) + 15% monobutyl ether ethylene diester (CH ₃ (CH ₂ ) ₃ OCH ₂ CH ₂ OH)+70% ethanol (C ₂ H ₆ O), the electrolyte temperature is 25 ° C, the electrolysis voltage is 40 volts, the electropolishing time is 1.5 minutes, and the surface of the aluminum plate treated with the mold has an optical grade reflection. The plane, its metallographic microstructure is shown in Figure 14.

[Example 19]

The surface of the aluminum material was electropolished with the mold body of Fig. 1. In this example, the surface of the aluminum material after pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the quality of the electropolishing is controlled by the applied voltage and the electrolyte composition. The electropolishing operation condition is 15% perchloric acid (HClO ₄ ) + 15% monobutyl ether B Diester (CH ₃ (CH ₂ ) ₃ OCH ₂ CH ₂ OH) + 70% ethanol (C ₂ H ₆ O), the electrolyte temperature is 10 ° C, the electrolysis voltage is 40 volts, and the electropolishing time is 5 minutes. The surface of the aluminum plate after the mold treatment has an optical level of reflection plane.

[Example 20]

The surface of the aluminum material was electropolished with the mold body of Fig. 1. In this example, the surface of the aluminum material after pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the quality of the electropolishing is controlled by the applied voltage and the electrolyte composition. The electropolishing operation condition is 15% perchloric acid (HClO ₄ ) + 15% monobutyl ether B Diester (CH ₃ (CH ₂ ) ₃ OCH ₂ CH ₂ OH) + 70% ethanol (C ₂ H ₆ O), electrolyte temperature is 35 ° C, electrolysis voltage is 40 volts, electropolishing time is 1 minute, using this The surface of the aluminum plate after the mold treatment has an optical level reflection plane, and the flat surface can be used as a secondary optical mirror of a light-emitting diode or a refraction or condensing mirror of a solar cell.

[Example 21]

Electrolytic polishing of the surface of the titanium material is carried out using the mold body of Fig. 1. In this example, the surface of the titanium material after acid pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The area of the surface of the titanium sheet is limited by the opening range of the mold, and the quality of the electropolishing is controlled by the applied voltage and the electrolyte composition. The conditions of the electropolishing are: 5-20% perchloric acid (HClO ₄ ) + 5~20 % monobutyl ether ethylene diester (CH ₃ (CH ₂ ) ₃ OCH ₂ CH ₂ OH) + 85 ~ 95% methanol (CH ₃ OH), the electrolyte temperature is 2 ~ 40 ° C, the electrolysis voltage is 5 ~ 60 volts, The electropolishing time is 1 to 10 minutes, and the preferred electropolishing operation conditions are 5% perchloric acid (HClO ₄ ) + 53% ethylene glycol monobutylether (HOCH ₂ CH ₂ OC ₄ H ₉ ) + 42% methanol (CH ₃ OH) The electrolyte temperature was 25 ° C, the electrolysis voltage was 52 volts, and the electropolishing time was 3 minutes. The surface of the titanium plate treated by the mold has an optical level reflection plane.

[Example 22]

The metal surface is discolored by the mold body of Fig. 1. The metal plate used in the metal surface discoloration treatment of this example is titanium metal. The opening area of the mold is used to define the area to be treated of the titanium metal surface, so that the surface of the titanium metal and the titanium dioxide film formed by the anodizing process have an interference effect with the titanium substrate, and the thickness of the film is controlled by the applied voltage, along with the thickness of the titanium dioxide film. The surface of the changed titanium metal interferes with different colors. The electrolyte treated by the anode is a chemical solution containing no fluorine, chlorine, bromine or iodine. The anode treatment conditions are 1~100 volts (V), 0~30 °C, 1~. 60 seconds, of which the preferred anode treatment strip The material is 10 vol.% sulfuric acid aqueous solution, plus 10, 20, 40, 60, 80 volts DC voltage, and the anode treatment time is 2 seconds, respectively, and the interference films of gold, blue, yellow, green, and pink can be respectively obtained, and the mold is used. The surface of the treated titanium plate has a color interference film, which can be used for decorative or material marking applications.

[Example 23]

The metal surface is discolored by the mold body of Fig. 1. The metal plate used in the metal surface discoloration treatment of this example is titanium metal. The opening area of the mold is used to define the area to be treated of the titanium metal surface, so that the surface of the titanium metal and the titanium dioxide film formed by the anodizing process have an interference effect with the titanium substrate, and the thickness of the film is controlled by the applied voltage, along with the thickness of the titanium dioxide film. The surface of the changed titanium metal interferes with different colors. The electrolyte treated by the anode is a chemical solution containing no fluorine, chlorine, bromine or iodine. The anode treatment conditions are 1~100 volts (V), 0~30 °C, 1~. 60 seconds, when the anode treatment operating conditions are 10 vol.% sulfuric acid aqueous solution, plus 100 volts DC voltage, and the anode treatment time is 2 seconds, a purple interference film can be obtained, the microstructure of which is a partially broken interference film, so 100 volts DC is applied. The voltage is the limiting voltage at which the interference film grows.

[Example 24]

The metal surface is discolored by the mold body of Fig. 1. The metal plate used in the metal surface discoloration treatment of this example is titanium metal. The opening area of the mold is used to define the area to be treated of the titanium metal surface, so that the surface of the titanium metal and the titanium oxide film formed by the anodization have an interference effect with the titanium substrate, and the thickness of the film is controlled by an applied voltage. As the thickness of the titanium dioxide film changes, the surface of the titanium metal interferes with different colors. The electrolyte treated by the anode is a chemical solution containing no fluorine, chlorine, bromine or iodine. The anode treatment condition is 1~100 volts (V), 0. ~30 ° C, 1 ~ 60 seconds, when the anode treatment operating conditions are 10vol.% sulfuric acid aqueous solution, plus 60 volts DC voltage, anode treatment time of 2 seconds, can produce a colored mosaic appearance on the surface of the electro-polished titanium material. The reason is that the crystal planes of the crystal grains are different in the growth rate of the film under constant voltage conditions, and the interference film of different thicknesses on the surface of each crystal plane is caused, and the microscopic image is as shown in Fig. 15.

10‧‧‧Molding structure decomposition diagram for chemical treatment

101, 201, 306‧‧‧ conductive lines

102, 202, 305‧ ‧ 矽 rubber casing

103, 203, 304‧‧‧ conductive waterproof cover

104, 204, 303‧‧‧ conductive line waterproof seat

105,205‧‧‧Electrical line waterproof seat O-ring

106‧‧‧ Conductive rod

107, 206, 301‧‧‧ mold lower seat

108, 207, 302‧‧‧ mold lower seat O-ring

109‧‧‧Conductor

110‧‧‧Top cover waterproof gasket

111‧‧‧Work samples

112, 208, 50‧‧‧ mold cover

Opening reaction area of 113, 506‧‧ working samples

20‧‧‧Mold processing combined structure diagram

30‧‧‧Mechanical treatment mold lower seat-conducting wire-conductive rod combination structure diagram

40‧‧‧Conductor sheet structure for chemical processing molds

401‧‧‧First surface of conductive sheet

402‧‧‧Second surface of conductive sheet

403‧‧‧ Conductive rod fixing hole

501‧‧‧Mold cover outer diameter

502‧‧‧Mold cover inner diameter

503‧‧‧Contact surface of the mold upper cover and the lower seat

504‧‧‧Mold upper cover

505‧‧‧Mold cover with waterproof enamel film holder

60‧‧‧Under the mold for chemical treatment

601‧‧‧The lower teeth

602‧‧‧Lower torque assist hole

603‧‧‧Electrical line waterproof seat O-ring groove

604‧‧‧The lower teeth

Fig. 1 is a structural view of a mold for chemical processing.

Fig. 2 is a structural diagram of a combination of molds for chemical processing.

Fig. 3 The structure of the lower part of the chemical processing mold-conducting wire-conductive bar.

Figure 4 Conductive sheet of a mold for chemical processing.

Figure 5 The chemical treatment is covered with a mold.

Figure 6 The lower seat of the chemical processing mold.

Figure 7 Sixth image of the wafer surface film after processing.

Figure 8 Image of a four-glass glass surface treated film.

Figure 9 Image of the anodized aluminum plate surface after anodizing.

Figure 10 Microstructured image of the surface of the four-inch aluminum plate after anodizing.

Figure 11 Image of the anodized surface of the titanium dioxide plate.

Figure 12 Microstructured image of the surface of the titanium dioxide plate after anodizing.

Figure 13 Image of the surface of the aluminum block after electropolishing.

Figure 14 Surface microscopic image of the surface of the aluminum block after electropolishing.

Figure 15 A mosaic microscopic image of the surface of a titanium plate after anodization.

1O‧‧‧Decomposition structure diagram for chemical treatment

101‧‧‧Flexible wire

102‧‧‧矽 rubber casing

103‧‧‧Flexible waterproof cover

104‧‧‧Electrical line waterproof seat

105‧‧‧Electrical line waterproof seat O-ring

106‧‧‧ Conductive rod

107‧‧‧Mold lower seat

108‧‧‧Mould lower seat O-ring

109‧‧‧Conductor

110‧‧‧Top cover waterproof gasket

111‧‧‧Work samples

112‧‧‧Mold cover

113‧‧‧Open reaction area of working samples

Claims (9)

A partial surface treatment mold suitable for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, the structure comprising: a conductive rod for connecting a conductive sheet and a conductive line; and for connecting the conductive rod with a conductive sheet between the samples; a conductive line connected between the conductive rod and the power supply; a conductive waterproof seat for preventing water from penetrating between the conductive line and the lower seat; a conductive waterproof cover, and a silicone sleeve; The O-ring groove for preventing the liquid from infiltrating into the lower seat of the mold by the conductive wire; the O-ring; the lower seat of the mold for fixing the conductive sheet and the working test piece; Tooth; used to bond the conductive teeth to the lower teeth of the male teeth. A partial surface treatment mold suitable for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, comprising: a method for assisting application of a torsion force to a lower male tooth and a upper male tooth Combined with the tightness of the seat under the auxiliary hole; the upper cover of the mold lower seat O-ring for preventing water seepage is used to define the open reaction area of the working sample; the mold lower seat O-ring for preventing water seepage between the lower seat and the upper cover The conductive sheet upper cover waterproof gasket used to fix the working sample. A refraction of a secondary optic or solar cell suitable for a light-emitting diode, as in claim 1 Or a partial surface treatment mold of the concentrating mirror, wherein the mold upper cover structure comprises an outer diameter of the upper cover of the mold; the inner diameter of the upper cover of the mold provides a first surface for fixing the conductive sheet; the contact surface of the upper cover and the lower seat of the mold provides a waterproof enamel film placement; The tooth is used to bond the lower teeth of the mold; the upper cover of the mold is used to prevent liquid from penetrating into the upper teeth of the mold cover by the open reaction area of the working sample. The partial surface treatment mold for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, wherein the reaction area of the upper cover sample may be a specific area of a single number or a plurality of shapes. A partial surface treatment mold suitable for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, wherein the mold lower seat structure comprises a lower seat male tooth for bonding the upper cover of the mold; The torque assisting hole is used to assist the application of a torsion force to make the lower seat male teeth and the upper cover male teeth tightly combined; the conductive wire waterproof seat O-ring groove is used to prevent the liquid from penetrating into the conductive piece in the lower seat of the mold; The mother teeth are used to bond the conductive waterproof seat male teeth. A partial surface treatment mold suitable for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, wherein the conductive sheet is an integrally formed or bonded conductor having a diameter of a first surface thereof It can be placed in the upper cover of the mold, and the smaller diameter of the second surface can be placed in the lower seat of the mold, and the second surface is more A conductive rod fixing hole is provided for increasing the contact stability of the conductive rod on the conductive sheet. A partial surface treatment mold suitable for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, wherein the sample is subjected to electrolysis, electrolytic polishing, electroplating, anodizing, etching, immersion plating, Pickling, caustic washing, evaporation, etc. prevent liquid or vapor from penetrating into the surface outside the specific exposed area. A partial surface treatment mold suitable for a secondary optical mirror of a light-emitting diode or a refractive or condensing mirror of a solar cell, wherein the material of the mold comprises metal, ceramic, glass, polymer, or metal surface is insulated. Handling of insulating materials. One of the claims 1 is suitable for a secondary optical mirror of a light-emitting diode or a partial surface treatment mold for a refractive or condensing mirror of a solar cell, wherein the gasket property comprises an insulating, waterproof, compressible material.