KR101798075B1 - Hollow chain product using heat treatment process for preventing spreading of copper between two material - Google Patents
Hollow chain product using heat treatment process for preventing spreading of copper between two material Download PDFInfo
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- KR101798075B1 KR101798075B1 KR1020160004146A KR20160004146A KR101798075B1 KR 101798075 B1 KR101798075 B1 KR 101798075B1 KR 1020160004146 A KR1020160004146 A KR 1020160004146A KR 20160004146 A KR20160004146 A KR 20160004146A KR 101798075 B1 KR101798075 B1 KR 101798075B1
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- Prior art keywords
- copper
- core material
- diffusion
- heat treatment
- core
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- JXROLTCWPVDDHD-UHFFFAOYSA-N C=C=C(CN)C=C=C=C Chemical compound C=C=C(CN)C=C=C=C JXROLTCWPVDDHD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A44—HABERDASHERY; JEWELLERY
- A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
- A44C27/00—Making jewellery or other personal adornments
- A44C27/001—Materials for manufacturing jewellery
- A44C27/002—Metallic materials
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- A—HUMAN NECESSITIES
- A44—HABERDASHERY; JEWELLERY
- A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
- A44C11/00—Watch chains; Ornamental chains
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
- C22F1/057—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with copper as the next major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Electrochemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The hollow product according to an embodiment of the present invention is a hollow product manufactured by a hollow product manufacturing process including a heat treatment step of heat treating a core material made of copper and a sheath material bonded to the core material and further containing any material other than copper Wherein a diffusion preventing layer for preventing diffusion of copper from the core material to the sheathing material is formed on the surface of the core material to which the sheathing member contacts and at least one of gold, silver, platinum and platinum group elements is optional, The process includes an extrusion process and a brazing process wherein the diffusion barrier layer is formed by applying one or a combination of carbon black, graphene, graphene oxide, nano diamond, oxide powder, nitride powder and carbide powder to the surface of the core Or by oxidizing the surface of the core.
Description
The present application relates to a hollow chain product using a heat treatment method for preventing diffusion of copper between a gold alloy and a copper material.
Generally, as shown in FIG. 1, a hollow chain product is made of a gold alloy such as 14K and 18K on the surface portion. However, in order to express a volume-sensitive decorative material and lighten the weight when worn, It is a product with high added value compared to input price because it has difficulty in manufacturing process.
The manufacturing process of the hollow chain product includes a heat treatment process in which a core material of a cylindrical shape is bonded to a core material of a gold alloy and heat treatment is performed at a high temperature. In this process, since the diffusion coefficient of copper is larger, There is a problem in that the gold content of the final jacket material is lower than the target gold content ultimately. In particular, in the case of gold products, a decrease in the content of final gold products may cause serious quality problems, and a solution is needed.
With this solution, there is a method of setting the content of the noble metal shell material to be about 1% higher than the target value. For example, if you aim for a gold product of 18K with a gold content of 75%, increasing the gold content of the jacket material to 76% will enable you to produce more than 75% of 18K hollow products even after the above-mentioned heat treatment process. However, this method is not economically suitable for mass production because the gold precious metal, which is an important pricing factor in material cost, is excessively input.
It is another way to change the material of the core. There is little or no copper or gold and solubility, and it uses pure iron with a very small diffusion at about 1000 degrees. Pure iron with a low carbon content is an ideal core material because it is easy to cold work and there is no interdiffusion with gold. However, in the actual process, during the process of cutting the assembled wire, a burr is generated due to a difference in strength between the core material and the shell material having relatively softness, and the burr is cracked during the brazing process, There is a problem that defective junction can be caused.
In addition, due to the rigidity of the pure iron, a springback effect is produced in the step of bending to face the joint surface after cutting, resulting in an increase in the gap of the joint surface, which also causes a problem of joint failure. Further, in the wet removal process of core material, since core material is dissolved by using hydrochloric acid instead of nitric acid, environmental burden is increased.
For example, Korean Patent Laid-Open No. 2001-0073368 (" Method for manufacturing chains for accessories ", published on August 1, 2001) relates to technology related to the production of hollow chain products.
According to an embodiment of the present invention, it is possible to prevent the diffusion of copper generated in the heat treatment process during the production process of the hollow product, to adjust the content of the final sheathing material to the target content, and to use the heat treatment method, Products.
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According to another embodiment of the present invention, there is provided a hollow product manufactured by a hollow product manufacturing process including a core material made of copper and a heat treatment step of heat-treating a jacket material bonded to the core material and further containing any material other than copper And a diffusion preventive layer for preventing copper from diffusing from the core material to the jacket material is formed on the surface of the core material to which the jacket material abuts, and the optional material includes at least one of gold, silver, platinum and platinum group elements Wherein the heat treatment process comprises an extrusion process and a brazing process, wherein the diffusion barrier layer comprises one or a combination of carbon black, graphene, graphene oxide, nano diamond, oxide powder, nitride powder and carbide powder The surface of the core material is coated or the surface of the core material is oxidized. The right product is provided.
According to one embodiment of the present invention, diffusion preventing layer for preventing diffusion of copper is formed on the surface of the core material, and heat treatment of the joined core material and the sheathing material prevents diffusion of copper, And can solve environmental problems.
BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a diagram of a hollow chain product in accordance with an embodiment of the present invention.
2A to 2I are diagrams illustrating a production process of a hollow chain product according to an embodiment of the present invention.
3 is a diagram for explaining an experimental method according to an embodiment of the present invention,
FIG. 4 is an enlarged view of a specific portion of the joined material in the experiment conducted according to FIG.
DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. However, the embodiments of the present invention can be modified into various other forms, and the scope of the present invention is not limited to the embodiments described below. The shape and the size of the elements in the drawings may be exaggerated for clarity and the same elements are denoted by the same reference numerals in the drawings.
2A to 2I are diagrams illustrating a production process of a hollow chain product according to an embodiment of the present invention.
Hereinafter, the production process of the hollow chain product will be described with reference to FIGS. 2A to 2I.
2A, three grooves H are formed in a cylinder-
next. 2B shows a noble metal shell material 203 (also referred to as a "second material") prepared in the noble metal shell preparation step. The
Next, FIG. 2C shows a process of joining and assembling the
Next, Fig. 2 (d) is an extrusion process, which extrudes a wire of the desired size and shape through a plurality of extrusion processes. In this case, a heat treatment process at 580 ° C. for 30 minutes is required for hot extrusion processing.
Next, Fig. 2e shows the cutting and chaining process, in which the extruded wire is cut and bent to the desired length and machined into a donut-shaped chain element. At this time, the gap is controlled so that the two opposing surfaces coincide.
Next, in FIG. 2F, the brazing process is carried out using a reflow material or a heat treatment adapter of about 890 to about 10 minutes so that the contacts of the processed chain elements are brazed.
Next, FIG. 2H is a process for selectively removing core material, which selectively removes only cores made of copper having a high corrosion rate using nitric acid. This completes the chain of precious metals with only a hollow envelope.
Finally, Fig. 2 (i) is a post-treatment step, in which a final product is completed and shipped through tumbling and finishing to improve the surface smoothness. The final product is shown in Figure 2i.
In the case of FIGS. 2d and 2f in which a high temperature heat treatment process is required during the production process of the hollow chain product described above, since the diffusion coefficient of copper is large, copper of the core material diffuses into the sheath material, and ultimately, the content of the final sheath material is lower .
To this end, according to one embodiment of the present invention, in order to prevent copper from diffusing from the surface of a core material (also referred to as a 'first material') to a sheath material (also referred to as a 'second material') during a heat treatment process, The diffusion preventive layer can be formed in advance on the surface of the core material.
The diffusion preventing layer can oxidize the surface of the core to form an oxide layer. Here, the oxidation may be performed by any one of thermal oxidation, anodizing and sputtering.
Alternatively, the diffusion barrier layer may be produced by applying one or a combination of carbon black, graphene, graphene oxide, nano diamond, oxide powder, nitride powder and carbide powder to the surface of the core. Hereinafter, a specific material or a specific method is exemplarily described for the formation of the diffusion preventing layer, but this is only for the understanding of the invention, and is not limited thereto.
A. Example One - In core material Diffusion prevention layer formation
FIG. 3 is a view for explaining an experimental method according to an embodiment of the present invention, and FIG. 4 is an enlarged view of a specific part of a bonded material in an experiment performed according to FIG.
All the experiments were performed by laminating two
In general, pure copper is easily oxidized to a thermal oxidation of 400 degrees or an aqueous alkali solution to form a dense oxide film on the surface. The red oxide copper oxide film composed of the mixed phase of Cu 2 O (I) and CuO (II) forms is stable up to 1200 ° C. and stable in the heat treatment conditions of 890 ° C. and 10 minutes required in the present invention It can prevent diffusion.
In order to confirm this, a specimen of 18K plate (1 × 1 cm 2 ) was put on a pure copper plate, and the specimen was set in a vacuum furnace with a weight of 100 g at 3 × 10 -3 torr and heat treated at 900 ° C. for 10 minutes. As a result, these specimens underwent interdiffusion and bonding, but Cu 2 O was formed by heating the pure copper plate with a torch at 1100 ° C for 1 minute. In the same experiment, it was easily separated without mutual diffusion.
In order to confirm the above example, six kinds ((1) to (6)) were experimentally confirmed as described below. All 25 × 25 × 0.3 mm pure copper was used. All copper plates were immersed in alcohol and acetone before washing and ultrasonically cleaned.
(1) Copper plates - Copper plates
As a result of the experiment according to FIG. 3, it can be seen that complete bonding between the gold alloy and the copper material occurred due to diffusion (see (1) in FIG. 4).
(2) Copper plate - copper plate with 20 second torch heating copper oxide
The copper oxide film was formed by placing a copper plate in the center of the alumina crucible in the atmosphere and heating the crucible with a torch for 20 seconds to form a uniform oxide film of 1 μm thickness on the surface of the conductive path. As a result of the experiment according to FIG. 3, it can be seen that complete bonding between the gold alloy and the copper material occurred (see (2) in FIG. 4).
(3) Copper plate - copper plate with 60 seconds torch heating copper oxide
- The copper oxide film of the specimen was a copper plate placed in the center of the alumina crucible in the atmosphere and the crucible was heated with a torch for 60 seconds to produce a 3 μm thick uniform oxide film on the surface of the conduction furnace. Here, the thickness of the copper oxide film may range from 0.1 to 500 mu m. As a result of the experiment according to FIG. 3, it can be seen that partial bonding occurred between the gold alloy and the copper material (see (3) in FIG. 4).
(4) Copper plates - Copper plates with carbon black
- Carbon black of the specimen was coated by adding 0.5 g of carbon black powder having a particle size of 45 nm to 15 ml of ethanol and ultrasonic wave was added for 5 minutes and the mixture was accelerated for 10 seconds at 1000 rpm using a spin coater and maintained for 10 seconds Uniformly applied to a copper plate with a thickness of 45 nm. Here, the thickness condition of the carbon black may be 45 nm to 100 占 퐉. As a result of the experiment according to FIG. 3, it can be seen that the joining between the gold alloy and the copper material occurred (see (4) in FIG. 4). That is, it can be seen that the non-bonding is caused by the gap D1 between the gold alloy and the copper material.
(5) Copper plates - Copper plates coated with graphene oxide
- Application of the graphene oxide of the specimen was accelerated by spin coating at 1000 rpm for 10 seconds using graphene oxide (Graphene supermarket HC-Gpraphene Oxide model) product with a flake particle size of 0.5-5 ㎛, To a copper plate uniformly at a thickness of 1 mu m. Here, the thickness condition of the graphene oxide may be 1 nm to 100 탆. As a result of the experiment according to FIG. 3, it can be seen that the joining between the gold alloy and the copper material occurred (see (5) in FIG. 4). That is, it can be seen that the non-bonding was caused by the gap D2 between the gold alloy and the copper material.
(6) Copper plate - Copper plate coated with SiC powder
- SiC coating of specimen was carried out by mixing 0.2 g of SiC powder (particle size of 100 탆) in 15 ml of ethanol solution, accelerating the mixture solution at 1000 rpm for 10 seconds by a spin coating method, holding it for 10 seconds, Respectively. As a result of the experiment according to FIG. 3, it can be seen that the joining between the gold alloy and the copper material occurred (see (6) in FIG. 4). That is, it can be seen that the non-bonding is caused by the gap D3 between the gold alloy and the copper material.
In conclusion, if the conventional process is performed to fabricate the above-described hollow-gold alloy product, the relative content of gold in the final gold product is inevitably in error due to interdiffusion of copper components. Therefore, it is preferable to produce a copper oxide film, and effective diffusion of copper can be prevented even by applying economically inexpensive graphite powder (carbon black). Likewise, nanomaterials such as graphene oxide can sufficiently prevent diffusion. Since copper and non-solid SiC can be completely prevented from diffusing, nitriding materials such as AlN, TiN, TaN, BN, and c-BN are applied to the core as well as oxide powders containing the same Al 2 O 3 , SiO 2 and MgO In addition, it was possible to successfully improve the manufacturing process without any change in the final gold content (without the diffusion of the actual copper component).
B. Example 2 - In addition to spread prevention Employment rate High Oxide film Hire
PbO powder can also be adopted as a diffusion preventive layer for solving the above problem. PbO is solid at normal temperature and changes into a liquid state at 800 ° C or higher. At this time, PbO has a high solubility with main alloying elements such as copper, silver and zinc, which have no solubility and stable activity with stable gold element. Therefore, PbO powders having a solid particle size of 1 ㎛ were mixed with alcohol as a diffusion preventing layer, and the resulting mixture was coated on the surface of copper core with a thickness of 0.1 탆 to 30 탆 and subjected to a hollow chain process.
At this time, during the heat treatment process, copper was solved in PbO from the noble metal sheathing sheet, and it was possible to relatively increase the gold content of the noble metal sheath by 0.2%. Therefore, if our gold content target is 75.0wt%, the final product can be made 75.0wt% even if you use 74.8wt% low-fat material, which reduces the gold content. have. Therefore, it is possible to employ a material having a high solubility selectively for elements other than gold as the diffusion preventing layer.
As described above, according to the embodiment of the present invention, diffusion preventing layer for preventing diffusion of copper is formed on the surface of the core material, heat treatment of the joined core material and the sheathing material prevents diffusion of copper, The content can be adjusted to the target content, and the problem of bonding failure between the gold alloy and the copper material and the environmental problem can be solved.
The present invention is not limited to the above-described embodiments and the accompanying drawings. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. It will be self-evident.
201, 202: core material
203:
300: Crucible
311: diffusion prevention layer
310: second material
320: First material
400: enlarged region
Claims (10)
A diffusion barrier layer for preventing diffusion of copper from the core material to the jacket material is formed on a surface of the core material to which the jacket material contacts,
Wherein the optional material comprises at least one of gold, silver, platinum and platinum group elements,
The heat treatment process includes an extrusion process and a brazing process,
The diffusion preventive layer may be formed by applying one or a combination of carbon black, graphene, graphene oxide, nano diamond, oxide powder, nitride powder, and carbide powder to the surface of the core material or by oxidizing the surface of the core material product.
Preferably,
Hollow products by any one of thermal oxidation, anodizing, and sputtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020160004146A KR101798075B1 (en) | 2016-01-13 | 2016-01-13 | Hollow chain product using heat treatment process for preventing spreading of copper between two material |
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020160004146A KR101798075B1 (en) | 2016-01-13 | 2016-01-13 | Hollow chain product using heat treatment process for preventing spreading of copper between two material |
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| Publication Number | Publication Date |
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| KR20170084824A KR20170084824A (en) | 2017-07-21 |
| KR101798075B1 true KR101798075B1 (en) | 2017-11-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102269246B1 (en) | 2020-12-14 | 2021-06-24 | 박해남 | Hollow chain manufacturing method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005270479A (en) * | 2004-03-26 | 2005-10-06 | Citizen Watch Co Ltd | Ornament with gold coating film and manufacturing method thereof |
| KR100980039B1 (en) * | 2008-02-01 | 2010-09-06 | 포항공과대학교 산학협력단 | Manufacturing method of thin film for diffusion barrier and thin film for diffusion barrier produced thereby |
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- 2016-01-13 KR KR1020160004146A patent/KR101798075B1/en active IP Right Grant
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005270479A (en) * | 2004-03-26 | 2005-10-06 | Citizen Watch Co Ltd | Ornament with gold coating film and manufacturing method thereof |
| KR100980039B1 (en) * | 2008-02-01 | 2010-09-06 | 포항공과대학교 산학협력단 | Manufacturing method of thin film for diffusion barrier and thin film for diffusion barrier produced thereby |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102269246B1 (en) | 2020-12-14 | 2021-06-24 | 박해남 | Hollow chain manufacturing method |
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| KR20170084824A (en) | 2017-07-21 |
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