CN108531864B - Silver evaporation material and preparation method thereof - Google Patents
Silver evaporation material and preparation method thereof Download PDFInfo
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- CN108531864B CN108531864B CN201810667971.XA CN201810667971A CN108531864B CN 108531864 B CN108531864 B CN 108531864B CN 201810667971 A CN201810667971 A CN 201810667971A CN 108531864 B CN108531864 B CN 108531864B
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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
- C23C14/24—Vacuum evaporation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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Abstract
The invention discloses a silver evaporation material and a preparation method thereof. The invention adopts the hot rotary swaging processing of the continuous casting silver rod to obtain the silver evaporation material, has simple process operation and high production efficiency, realizes the continuous automatic production of the silver evaporation material, can ensure less internal defects of the product, good fluidity after melting and high quality consistency, and avoids the problems of inconsistent quality and poor fluidity of the product.
Description
Technical Field
The invention relates to an evaporation material for forming a film, in particular to a silver evaporation material and a preparation method thereof.
Background
The evaporation coating material is a basic material for preparing various optics, electrics and the like. The evaporation material based on silver is mainly used for coating materials in the electronic industry, and the evaporation material silver is evaporated by heating to form a silver layer film which is loaded on a carrier to form an electrode material of an electronic device.
At present, evaporation processes are various, most of needed evaporation sources are point evaporation, and point evaporation is formed by silver particles with high fluidity in a molten state, so that the silver particles are aggregated into balls under the action of height difference and surface tension. The preparation process of the evaporation material adopted at present mainly comprises the following steps: (1) continuously casting the silver rod, and drawing the silver rod into a material (after the silver rod is drawn out by a down-drawing method, preparing an evaporation wire by a multi-pass drawing process); (2) and (3) extruding the cast ingot and drawing the cast ingot into a material (after the cast ingot is smelted, milling a blank, performing high-temperature heat treatment, performing hot extrusion, extruding a rod material, and preparing an evaporation wire through a multi-pass drawing process). Wherein, the product obtained by the method (1) has low fluidity and poor aggregation and balling capabilities: the viscosity of the melted silver is large mainly due to poor internal structure and more defects; the method (2) has complex working procedures, overhigh processing cost and uneven product quality, and other impurities are easily introduced in the processing process to influence the stability of the material; the process is multiple, and the investment of extrusion equipment and smelting equipment is large. Poor product uniformity is mainly due to inconsistent product structure before and after extrusion process.
Disclosure of Invention
In order to solve the problems, the invention provides a silver evaporation material and a preparation method thereof. The method is simple to operate, low in cost and high in efficiency, and the product obtained by the method is few in internal defects, good in fluidity after melting and high in quality consistency.
The invention is realized by the following technical scheme
A preparation method of a silver evaporation material comprises the following steps:
(1) preparing a silver raw material, adding the silver raw material into a continuous casting furnace, and then introducing inert gas into the continuous casting furnace; after the inert gas is introduced, raising the temperature in the continuous casting furnace from room temperature to 1000-1250 ℃, preserving the heat for 2-10 min at the temperature, and leading out a silver rod after the heat preservation is finished;
(2) heating and insulating the silver rod obtained in the step (1);
(3) preparing a precision rotary forging machine, and setting the temperature to heat and preserve the temperature of a die of the precision rotary forging machine; after heating and heat preservation, conveying the silver bar subjected to heating and heat preservation in the step (2) to a die of a precision rotary forging machine for forging (forging at the temperature of 600-900 ℃), and forging for 1-5 passes; finishing forging;
(4) and (4) carrying out cold rotary swaging (cold rotary swaging at room temperature) on the forged silver rod obtained in the step (3) for 5-10 passes to form, and obtaining the silver evaporation material after cold rotary swaging forming.
In the preparation method of the silver evaporation material, the continuous casting furnace adopted in the step (1) is a horizontal continuous casting furnace (a horizontal lead-out silver rod is adopted when a horizontal lead-out continuous casting furnace is adopted) or a down-lead continuous casting furnace (a silver rod is led out from the lower part when a down-lead continuous casting furnace is adopted).
The preparation method of the silver evaporation material comprises the following steps (1): before introducing inert gas into the continuous casting machine, firstly, vacuumizing the continuous casting machine to enable the pressure inside the continuous casting machine to reach 0.1Pa, and introducing the inert gas after vacuumizing is finished.
In the preparation method of the silver evaporation material, the inert gas introduced into the continuous casting furnace in the step (1) comprises nitrogen and argon.
According to the preparation method of the silver evaporation material, the speed of leading out the silver rod in the step (1) is 4-20 cm/min; the diameter of the lead-out silver rod is 6-20 mm.
The preparation method of the silver evaporation material comprises the following specific steps of (2) heating and heat-preserving the silver rod: and (3) putting the silver rod into a tunnel furnace, heating to 600-900 ℃, and preserving heat for 0.5-2 hours at the temperature of 600-900 ℃.
The preparation method of the silver evaporation material comprises the following steps of (3) heating and insulating the die: heating the die to 300-600 ℃ from room temperature, and then preserving heat for 0.5-2 hours at the temperature.
According to the preparation method of the silver evaporation material, in the step (3), the sectional area (representing the sectional area of the cylindrical silver rod) of the silver rod is contracted by 30-80% in each pass in the forging process, and the outgoing line speed is 0.5-5 m/min.
According to the preparation method of the silver evaporation material, in the step (4), in the cold rotary swaging forming process, the sectional area of the silver rod (the sectional area of the cylindrical silver rod) is contracted by 10-30% in each pass, and the outgoing line speed is 2-10 m/min.
Compared with the prior art, the invention has the following positive beneficial effects
The invention adopts the hot rotary swaging processing of the continuous casting silver rod to obtain the silver evaporation material, has simple process operation and high production efficiency, realizes the continuous automatic production of the silver evaporation material, and can ensure less internal defects of the product, good fluidity after melting and high quality consistency (avoid the problems of inconsistent quality and poor fluidity of the product);
after the silver rod is subjected to the hot rotary swaging process, the internal defects of a workpiece are reduced, the performance is uniform, and the quality consistency is high, so that the obtained silver evaporation material has good fluidity in a molten state, and can be rapidly condensed into a spherical shape to form point evaporation; the silver evaporation material obtained by the preparation method can be condensed into a ball shape in less than 1 second and become point evaporation when being melted, and the obtained film layer has good quality and better uniformity.
Detailed Description
The present invention will be described in more detail with reference to the following embodiments, but the present invention is not limited to the embodiments.
The purity of the silver used in the following examples is more than or equal to 99.99%; the horizontal continuous casting furnace and the down-leading continuous casting furnace (Shenzhen Chengyixi science and technology Limited, model: CXM-CVV) are the existing continuous casting furnaces; the precision rotary swaging machine is the existing precision rotary swaging machine;
example 1
A preparation method of a silver evaporation material comprises the following steps:
(1) preparing a silver raw material, adding the silver raw material into a horizontal continuous casting furnace, and then introducing inert gas (nitrogen) into the horizontal continuous casting furnace; after the inert gas is introduced, raising the temperature in the continuous casting furnace from room temperature to 1130 ℃, preserving the heat for 10min at the temperature, and after the heat preservation is finished, horizontally leading out a silver rod from an outlet of the horizontal continuous casting furnace at a rate of 20 cm/min; the diameter of the obtained silver rod is 6 mm;
(2) conveying the silver rod obtained in the step (1) to a tunnel furnace, then heating the temperature in the tunnel furnace from room temperature to 800 ℃, and preserving the heat for 0.5 hour at the temperature;
(3) preparing a precision rotary swaging machine, heating a die of the precision rotary swaging machine to 300 ℃ at a set temperature, and preserving heat for 0.5 hour at the temperature; after the heat preservation is finished, conveying the silver rod heated and preserved in the step (2) to a die of a precision rotary forging machine for forging, wherein the shrinkage rate of the sectional area of the silver rod in the forging is 60% in 1 pass; finishing forging after forging for one pass;
(4) and (4) carrying out cold rotary swaging forming on the forged silver rod in the step (3) for 6 passes, wherein the shrinkage rate of the sectional area of the silver rod in each pass is 20%, so as to obtain the silver evaporation material with the diameter of 1.94 mm.
The product is subjected to ultrasonic detection, the internal defect rate is 0.012 percent, and the maximum defect area is 0.06mm2。
The silver evaporation material obtained by the method is plated on a quartz crystal: after the product was melted, the agglomerated pellets formed a point of evaporation within 0.5 seconds. The film has good quality and excellent uniformity. The fluctuation range of the resistance is reduced to +1.1 to-1.9 omega, and the reduction is 18.1 percent; the frequency tolerance fluctuation range is reduced to +1.86 to-0.77 ppm, which is reduced by 10.5 percent.
Example 2
A preparation method of a silver evaporation material comprises the following steps:
(1) preparing a silver raw material, adding the silver raw material into a horizontal continuous casting furnace, and then introducing inert gas (argon) into the horizontal continuous casting furnace; after the inert gas is introduced, raising the temperature in the continuous casting furnace from room temperature to 1250 ℃, preserving the heat for 3min at the temperature, and horizontally leading out a silver rod from an outlet of the horizontal continuous casting furnace after the heat preservation is finished, wherein the leading-out speed is 8 cm/min; the diameter of the obtained silver rod is 10 mm;
(2) conveying the silver rod obtained in the step (1) to a tunnel furnace, then heating the temperature in the tunnel furnace from room temperature to 800 ℃, and preserving the heat for 0.5 hour at the temperature;
(3) preparing a precision rotary swaging machine, heating a die of the precision rotary swaging machine to 400 ℃ at a set temperature, and preserving heat for 0.5 hour at the temperature; after the heat preservation is finished, conveying the silver rod heated and heat preserved in the step (2) to a die of a precision rotary forging machine for forging, wherein 2 times of forging are carried out, and the shrinkage rate of the sectional area of the silver rod in each time is 50%; finishing forging after two passes of forging;
(4) and (4) carrying out cold rotary swaging forming on the forged silver rod in the step (3) for 5 passes, wherein the shrinkage rate of the sectional area of the silver rod in each pass is 25%, so as to obtain the silver evaporation material with the diameter of 2.4 mm.
Ultrasonic testing of the productThe internal defect rate is 0.015 percent, and the maximum defect area is 0.07mm2。
The silver evaporation material obtained by the method is plated on a quartz crystal, and when the film is plated: after the product is melted, the product is condensed into balls in 0.9 second, and the formed points are evaporated. The film has good quality and excellent uniformity. The fluctuation range of the resistance is reduced to +1.2 to-2.5 omega, and the reduction is 22.1 percent; the frequency tolerance fluctuation range is reduced to +2.16 to-0.8 ppm, and the reduction is 13.3 percent.
Example 3
A preparation method of a silver evaporation material comprises the following steps:
(1) preparing a silver raw material, adding the silver raw material into a down-drawing continuous casting furnace, and then introducing inert gas (argon) into the down-drawing continuous casting furnace; after the inert gas is introduced, heating the temperature in the down-drawing continuous casting furnace from room temperature to 1120 ℃, preserving the heat for 7min at the temperature, and after the heat preservation is finished, downwards drawing out a silver rod from an outlet of the down-drawing continuous casting furnace at the speed of 5 cm/min; the diameter of the silver rod is 20 mm;
(2) conveying the silver rod obtained in the step (1) to a tunnel furnace, then heating the temperature in the tunnel furnace from room temperature to 700 ℃, and preserving the heat for 1 hour at the temperature;
(3) preparing a precision rotary swaging machine, heating a die of the precision rotary swaging machine to 500 ℃ at a set temperature, and preserving heat for 1 hour at the temperature; after the heat preservation is finished, conveying the silver rod heated and heat preserved in the step (2) to a die of a precision rotary forging machine for forging, wherein the shrinkage rate of the sectional area of the silver rod in each pass is 50 percent; finishing forging after three passes of forging;
(4) and (4) carrying out cold rotary swaging forming on the forged silver rod in the step (3) for 6 passes, wherein the shrinkage rate of the sectional area of the silver rod in each pass is 20%, so as to obtain the silver evaporation material with the diameter of 3.6 mm.
Ultrasonic detection is carried out on the product, the internal defect rate of the product is 0.015 percent, and the maximum defect area is 0.075mm2。
The silver evaporation material obtained by the method is used for quartz resonators: after the product is melted, the product is condensed into balls within 1.0 second, and the formed points are evaporated. The film has good quality and excellent uniformity. The fluctuation range of the resistance is reduced to +1.42 to-2.65 omega, and the reduction is 19.8 percent; the frequency tolerance fluctuation range is reduced to +2.53 to-1.2 ppm, and the reduction is 16.4 percent.
Example 4
A preparation method of a silver evaporation material comprises the following steps:
(1) preparing a silver raw material, adding the silver raw material into a down-drawing continuous casting furnace, then vacuumizing the down-drawing continuous casting furnace to enable the pressure in the furnace to be 0.1Pa, and introducing inert gas (nitrogen) into the down-drawing continuous casting furnace after vacuumizing; after the inert gas is introduced, heating the temperature in the down-drawing continuous casting furnace from room temperature to 1200 ℃, preserving the heat for 5min at the temperature, and after the heat preservation is finished, downwards leading out a silver rod from an outlet of the down-drawing continuous casting furnace at a speed of 10 cm/min; the diameter of the obtained silver rod is 15 mm;
(2) conveying the silver rod obtained in the step (1) to a tunnel furnace, then heating the temperature in the tunnel furnace from room temperature to 600 ℃, and preserving the heat for 2 hours at the temperature;
(3) preparing a precision rotary swaging machine, heating a die of the precision rotary swaging machine to 400 ℃ at a set temperature, and preserving heat for 0.5 hour at the temperature; after the heat preservation is finished, conveying the silver rod heated and heat preserved in the step (2) to a die of a precision rotary forging machine for forging, wherein the shrinkage rate of the sectional area of the silver rod in each pass is 60 percent; finishing forging after three passes of forging;
(4) and (4) carrying out cold rotary swaging forming on the forged silver rod in 10 passes, wherein the shrinkage of the sectional area of the silver rod in each pass is 10%, so as to obtain the silver evaporation material with the diameter of 2.24 mm.
The product is subjected to ultrasonic detection, the internal defect rate of the product is 0.01 percent, and the maximum defect area is 0.05mm2。
The silver evaporation material obtained by the method is used for plating on the quartz crystal: after the product is melted, the product is condensed into balls in 0.6 second, and the formed points are evaporated. The film has good quality and excellent uniformity. The fluctuation range of the resistance is reduced to +0.9 to-2.0 omega, and the reduction is 17.9 percent; the frequency tolerance fluctuation range is reduced to +1.85 to-0.7 ppm, and the frequency tolerance fluctuation range is reduced by 9.8 percent.
Claims (7)
1. The preparation method of the silver evaporation material is characterized by comprising the following steps:
(1) preparing a silver raw material, adding the silver raw material into a continuous casting machine, and then introducing inert gas into the continuous casting machine; after the inert gas is introduced, raising the temperature in the continuous casting machine from room temperature to 1000-1250 ℃, preserving the heat for 2-10 min at the temperature, and leading out a silver rod after the heat preservation is finished;
the speed of leading out the silver rod is 4-20 cm/min; the diameter of the lead-out silver rod is 6-20 mm;
(2) heating and insulating the silver rod obtained in the step (1); the heating and heat preservation treatment of the silver rod comprises the following specific steps: putting the silver rod into a tunnel furnace, heating to 600-900 ℃, and preserving heat for 0.5-2 hours at the temperature of 600-900 ℃;
(3) preparing a precision rotary forging machine, and setting the temperature to heat and preserve the temperature of a die of the precision rotary forging machine; after heating and heat preservation are finished, conveying the silver bar subjected to heating and heat preservation in the step (2) to a die of a precision rotary forging machine for forging for 1-5 passes; finishing forging; in the forging process, the sectional area of the silver rod is contracted by 30-80% in each pass, and the wire outlet speed is 0.5-5 m/min;
(4) and (4) carrying out cold rotary swaging forming on the forged silver rod in the step (3) for 5-10 passes, and obtaining the silver evaporation material after cold rotary swaging forming.
2. The method of claim 1, wherein the continuous casting machine in step (1) is a horizontal continuous casting furnace or a down-draw continuous casting furnace.
3. The method for preparing silver vapor deposition material according to claim 1 or 2, wherein the step (1) further comprises: before introducing inert gas into the continuous casting machine, firstly, vacuumizing the continuous casting machine to enable the pressure inside the continuous casting machine to reach 0.1Pa, and then introducing the inert gas after vacuumizing.
4. The method of claim 1, wherein the inert gas introduced into the continuous casting machine in step (1) comprises nitrogen and argon.
5. The method for preparing silver evaporation materials according to claim 1, wherein the step (3) of heating and maintaining the temperature of the die of the precision rotary swaging machine comprises the following steps: heating the die to 300-600 ℃ from room temperature, and then preserving heat for 0.5-2 hours at the temperature.
6. The method of claim 1, wherein the purity of the silver source material is greater than or equal to 99.99%.
7. The method for preparing the silver evaporation material according to claim 1, wherein in the step (4), the sectional area of the silver rod is shrunk by 10-30% in each pass of the cold swaging process, and the outgoing line speed is 2-10 m/min.
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| CN111485138B (en) * | 2020-04-23 | 2021-07-23 | 中国科学院金属研究所 | Preparation method of cold-processed cobalt-based alloy rod wire |
| CN112872077B (en) * | 2021-01-29 | 2022-12-02 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity silver evaporation material |
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