CN108531864A - A kind of silver evaporation material and preparation method thereof - Google Patents
A kind of silver evaporation material and preparation method thereof Download PDFInfo
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- CN108531864A CN108531864A CN201810667971.XA CN201810667971A CN108531864A CN 108531864 A CN108531864 A CN 108531864A CN 201810667971 A CN201810667971 A CN 201810667971A CN 108531864 A CN108531864 A CN 108531864A
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of silver-colored evaporation materials and preparation method thereof, evaporation material silver is cast using continuous casting furnace first, draw silver-colored stick, then heating and thermal insulation carried out to silver-colored stick, forged using accurate swager, cold processing of swaging is carried out after the completion of forging and can be obtained silver-colored evaporation material of the present invention.The present invention processes to obtain silver-colored evaporation material using continuous casting silver stick hot-swage, technological operation is simple, production efficiency is high, realize the continuous automatic production of silver-colored evaporation material, it can ensure that interiors of products defect is few, good fluidity, quality conformance are high after melting, the quality for avoiding product is inconsistent, the bad problem of mobility.
Description
Technical field
The present invention relates to a kind of evaporation materials being used to form film, and in particular to a kind of silver evaporation material and its preparation side
Method.
Background technology
Structural evaporation coating film material is the basic material for preparing various optics, electricity etc..Evaporation material based on silver is main
For the Coating Materials of electronics industry, by heating evaporation evaporation material silver, formation silver layer film, which is supported on carrier, to be formed
The electrode material of electronic device.
The technique being deposited at present is varied, and the evaporation source that majority needs is that point evaporates, and forms point evaporation and silver granuel is needed to exist
Molten state has higher mobility, to pass through the effect glomeration of difference in height and surface tension.The vapor deposition used at present
The preparation process of material mainly has：（1）It is drawn into material after continuous casting silver bar（Under draw after method draws silver-colored bar, pass through the drawing of multi-pass
Technique prepares vapor deposition wire rod）；（2）Ingot casting is drawn into material after squeezing（After melting ingot casting, milling blank is warmed using height
Processing, carries out hot extrusion, and the bar squeezed out prepares vapor deposition wire rod using the drawing process of multi-pass）.Wherein, method（1）
The mobility of products obtained therefrom is low, glomeration energy force difference：It is poor to be primarily due to internal structure, defect is more, viscous after causing silver to melt
Property is larger；Method（2）Complex procedures, processing cost are excessively high, product quality is inhomogenous, while being readily incorporated it in process
His impurity and the stability for influencing material；Process is more, and extrusion equipment, smelting equipment input are larger.Product homogeneity difference is main
Lead to product structure inconsequent for extrusion process.
Invention content
To solve the above-mentioned problems, the present invention provides a kind of silver-colored evaporation materials and preparation method thereof.This method operation letter
Single, at low cost, efficient, the interiors of products defect that is obtained using this method is few, good fluidity, quality conformance are high after melting.
The present invention is achieved by the following technical solutions
A kind of preparation method of silver evaporation material, this approach includes the following steps：
（1）Prepare silver material, silver material is added in continuous casting furnace, inert gas is then passed through into continuous casting furnace；Inert gas is logical
After the completion of entering, by the temperature in continuous casting furnace by room temperature to 1000 ~ 1250 DEG C, and 2 ~ 10min is kept the temperature at such a temperature, heat preservation
After after complete, draw silver-colored stick；
（2）By step（1）Obtained silver-colored stick carries out heating and thermal insulation processing；
（3）Prepare accurate swager, and set temperature carries out heating and thermal insulation to the mold of accurate swager；After heating and thermal insulation is complete,
By step（2）The silver-colored stick of the heating and thermal insulation, which is delivered in the mold of accurate swager, to be forged（Under the conditions of 600 ~ 900 DEG C into
Row forging）, forge 1 ~ 5 passage；Complete forging；
（4）By step（3）The silver-colored stick for completing forging carries out that 5 ~ 10 passages are cold swages（Cold swage is carried out at room temperature）Forming,
Silver-colored evaporation material is obtained after cold forming of swaging.
The preparation method of the silver-colored evaporation material, step（1）The continuous casting furnace used is horizontal continuous casting furnace（Using flat
When drawing formula continuous casting furnace silver-colored stick is drawn to be horizontal）Draw formula continuous casting furnace under or（It uses down silver-colored to be drawn by lower section when drawing formula continuous casting furnace
Stick）.
The preparation method of the silver-colored evaporation material, step（1）Further include：Be passed through into conticaster inert gas it
Before, conticaster is vacuumized first, the pressure inside conticaster is made to reach 0.1Pa, inert gas is passed through after the completion of vacuumizing.
The preparation method of the silver-colored evaporation material, step（1）The inert gas being passed through in continuous casting furnace includes nitrogen
And argon gas.
The preparation method of the silver-colored evaporation material, step（1）Rate when the extraction silver stick is 4 ~ 20cm/min；Institute
State a diameter of 6 ~ 20mm for drawing silver-colored stick.
The preparation method of the silver-colored evaporation material, step（2）It is described to be specially to the progress heating and thermal insulation processing of silver-colored stick：It will
Silver-colored stick is put into continuous tunnel furnace, is heated to 600 ~ 900 DEG C, and keep the temperature 0.5 ~ 2 hour under the conditions of 600 ~ 900 DEG C.
The preparation method of the silver evaporation material, step（3）It is described to be to mold progress heating and thermal insulation：By mold by room temperature
300 ~ 600 DEG C are heated to, then keeps the temperature 0.5 ~ 2 hour at such a temperature.
The preparation method of the silver evaporation material, step（3）Each passage makes the section of silver-colored stick in the forging process
Product（Indicate the cross-sectional area of cylinder silver stick）30% ~ 80% is shunk, it is 0.5 ~ 5m/min to go out linear velocity.
The preparation method of the silver evaporation material, step（4）Each passage makes silver-colored stick in the cold forming journey of swaging
Sectional area（The cross-sectional area of cylinder silver stick）10% ~ 30% is shunk, it is 2-10m/min to go out linear velocity.
Compared with prior art, the present invention has following positive beneficial effect
The present invention processes to obtain silver-colored evaporation material using continuous casting silver stick hot-swage, and technological operation is simple, production efficiency is high, realizes
The continuous automatic production of silver-colored evaporation material, it can be ensured that interiors of products defect is few, good fluidity, quality conformance are high after melting
（The quality for avoiding product is inconsistent, the bad problem of mobility）；
Silver stick of the present invention is after the hot-swage technique of the present invention so that inside workpiece defect is reduced, and performance is uniform, matter
It is high to measure consistency, therefore obtained silver-colored evaporation material has good mobility in molten state, can quickly be condensed into spherical shape
And form point evaporation；The silver-colored evaporation material that preparation method obtains through the invention, in fusing, in the time less than 1 second
It is condensed into spherical and is evaporated as point, obtained film quality is fine, has preferable uniformity.
Specific implementation mode
The present invention is described in more details below by specific implementation mode, but is not intended to restrict the invention
Protection domain.
It is >=99.99% that the purity of silver used is used in following embodiment；Horizontal continuous casting furnace used and under draw formula continuous casting
Stove（Shenzhen Chengyixin Technology Co., Ltd., model：CXM-CVV）It is existing continuous casting furnace；Precision swager used is existing
Accurate swager；
Embodiment 1
A kind of preparation method of silver evaporation material, this approach includes the following steps：
（1）Prepare silver material, silver material is added in horizontal continuous casting furnace, inert gas is then passed through into horizontal continuous casting furnace（Nitrogen
Gas）；After the completion of inert gas is passed through, by the temperature in continuous casting furnace by room temperature to 1130 DEG C, and keep the temperature at such a temperature
10min, draws silver-colored stick after the completion of heat preservation, by the outlet level of horizontal continuous casting furnace, rate when extraction is 20cm/min；Gained silver
A diameter of 6mm of stick；
（2）By step（1）Obtained silver-colored stick is delivered in continuous tunnel furnace, then the temperature in continuous tunnel furnace by room temperature to 800 DEG C,
And keep the temperature 0.5 hour at such a temperature；
（3）Prepare accurate swager, and set temperature heats the mold of accurate swager, is heated to 300 DEG C, and at this
At a temperature of keep the temperature 0.5 hour；After the completion of heat preservation, by step（2）The silver-colored stick of the heating and thermal insulation is delivered to the mould of accurate swager
It is forged in tool, 1 passage of forging, the shrinking percentage of silver-colored stick sectional area is 60% in the passage；It is completed after forging a passage
Forging；
（4）By step（3）The silver-colored stick for completing forging carries out the cold forming of swaging of 6 passages, silver-colored stick sectional area in every time
Shrinking percentage is 20%, obtains the silver-colored evaporation material of diameter 1.94mm.
Ultrasound examination is carried out to the product, internal defects rate is 0.012%, and greatest drawback area is 0.06mm2。
The silver-colored evaporation material that this method obtains is plated in above quartz crystal：After product has melted, balling-up is agglomerated in 0.5 second
Form point evaporation.Film quality is good, excellent in uniformity.Resistance fluctuation range is down to+1.1 ~ -1.9 Ω, reduces 18.1%；
Frequency tolerance fluctuation range is down to+1.86 ~ -0.77ppm, reduces 10.5%.
Embodiment 2
A kind of preparation method of silver evaporation material, this approach includes the following steps：
（1）Prepare silver material, silver material is added in horizontal continuous casting furnace, inert gas is then passed through into horizontal continuous casting furnace（Argon
Gas）；After the completion of inert gas is passed through, by the temperature in continuous casting furnace by room temperature to 1250 DEG C, and keep the temperature at such a temperature
3min, draws silver-colored stick after the completion of heat preservation, by the outlet level of horizontal continuous casting furnace, rate when extraction is 8cm/min；Gained silver stick
A diameter of 10mm；
（2）By step（1）Obtained silver-colored stick is delivered in continuous tunnel furnace, then the temperature in continuous tunnel furnace by room temperature to 800 DEG C,
And keep the temperature 0.5 hour at such a temperature；
（3）Prepare accurate swager, and set temperature heats the mold of accurate swager, is heated to 400 DEG C, and at this
At a temperature of keep the temperature 0.5 hour；After the completion of heat preservation, by step（2）Silver-colored stick after the heating and thermal insulation is delivered to accurate swager
It is forged in mold, 2 passages of forging, the shrinking percentage of silver-colored stick sectional area is 50% in each passage；It is after forging two passages
Complete forging；
（4）By step（3）The silver-colored stick for completing forging carries out the cold forming of swaging of 5 passages, silver-colored stick sectional area in every time
Shrinking percentage is 25%, obtains the silver-colored evaporation material of 2.4 mm of diameter.
Ultrasound examination is carried out to the product, internal defects rate is 0.015%, and greatest drawback area is 0.07mm2。
The silver-colored evaporation material that this method obtains is plated in above quartz crystal, when carrying out plated film：After product has melted,
Balling-up is agglomerated in 0.9 second, forms point evaporation.Film quality is good, excellent in uniformity.Resistance fluctuation range is down to+1.2 ~ -2.5
Ω reduces 22.1%；Frequency tolerance fluctuation range is down to+2.16 ~ -0.8ppm, reduces 13.3%.
Embodiment 3
A kind of preparation method of silver evaporation material, this approach includes the following steps：
（1）Prepare silver material, silver material is added down and is drawn in formula continuous casting furnace, then draws downwards in formula continuous casting furnace and is passed through inert gas
（Argon gas）；After the completion of inert gas is passed through, the temperature in formula continuous casting furnace is drawn by under by room temperature to 1120 DEG C, and in the temperature
Silver-colored stick is drawn downwards in lower heat preservation 7min, the outlet that formula continuous casting furnace is drawn after the completion of heat preservation, by down, and rate when extraction is 5cm/min；
A diameter of 20mm of gained silver stick；
（2）By step（1）Obtained silver-colored stick is delivered in continuous tunnel furnace, then the temperature in continuous tunnel furnace by room temperature to 700 DEG C,
And keep the temperature 1 hour at such a temperature；
（3）Prepare accurate swager, and set temperature heats the mold of accurate swager, is heated to 500 DEG C, and at this
At a temperature of keep the temperature 1 hour；After the completion of heat preservation, by step（2）Silver-colored stick after the heating and thermal insulation is delivered to the mould of accurate swager
It is forged in tool, 3 passages of forging, the shrinking percentage of silver-colored stick sectional area is 50% in each passage；It is i.e. complete after three passages of forging
At forging；
（4）By step（3）The silver-colored stick for completing forging carries out the cold forming of swaging of 6 passages, silver-colored stick sectional area in every time
Shrinking percentage is 20%, obtains the silver-colored evaporation material of 3.6 mm of diameter.
Ultrasound examination is carried out to the product, internal defects rate is 0.015%, and greatest drawback area is 0.075mm2。
The silver-colored evaporation material that this method obtains is used for quartz resonator：After product has melted, in 1.0 seconds agglomerate balling-up,
Form point evaporation.Film quality is good, excellent in uniformity.Resistance fluctuation range is down to+1.42 ~ -2.65 Ω, reduces
19.8%；Frequency tolerance fluctuation range is down to+2.53 ~ -1.2ppm, reduces 16.4%.
Embodiment 4
A kind of preparation method of silver evaporation material, this approach includes the following steps：
（1）Prepare silver material, silver material is added down and is drawn in formula continuous casting furnace, formula continuous casting furnace is then drawn under and carries out vacuumizing place
Reason, it is 0.1Pa to make the pressure in stove, draws downwards in formula continuous casting furnace after vacuumizing and is passed through inert gas（Nitrogen）；Inert gas
After the completion of being passed through, the temperature in formula continuous casting furnace is drawn by under by room temperature to 1200 DEG C, and keep the temperature 5min at such a temperature, kept the temperature
After the completion, silver-colored stick is drawn downwards in the outlet for drawing formula continuous casting furnace by down, and rate when extraction is 10cm/min；The diameter of gained silver stick
For 15mm；
（2）By step（1）Obtained silver-colored stick is delivered in continuous tunnel furnace, then the temperature in continuous tunnel furnace by room temperature to 600 DEG C,
And keep the temperature 2 hours at such a temperature；
（3）Prepare accurate swager, and set temperature heats the mold of accurate swager, is heated to 400 DEG C, and at this
At a temperature of keep the temperature 0.5 hour；After the completion of heat preservation, by step（2）Silver-colored stick after the heating and thermal insulation is delivered to accurate swager
It is forged in mold, 3 passages of forging, the shrinking percentage of silver-colored stick sectional area is 60% in each passage；It is after forging three passages
Complete forging；
（4）By step（3）The silver-colored stick for completing forging carries out the cold forming of swaging of 10 passages, silver-colored stick sectional area in every time
Shrinking percentage is 10%, obtains the silver-colored evaporation material of diameter 2.24mm.
Ultrasound examination is carried out to the product, internal defects rate is 0.01%, and greatest drawback area is 0.05mm2。
The silver-colored evaporation material that this method obtains is for being plated in above quartz crystal：After product has melted, agglomerated in 0.6 second
Balling-up forms point evaporation.Film quality is good, excellent in uniformity.Resistance fluctuation range is down to+0.9 ~ -2.0 Ω, reduces
17.9%；Frequency tolerance fluctuation range is down to+1.85 ~ -0.7ppm, reduces 9.8%.
Claims (10)
1. a kind of preparation method of silver evaporation material, which is characterized in that this approach includes the following steps：
（1）Prepare silver material, silver material is added in conticaster, inert gas is then passed through into conticaster；Inert gas is logical
After the completion of entering, by the temperature in conticaster by room temperature to 1000 ~ 1250 DEG C, and 2 ~ 10min is kept the temperature at such a temperature, heat preservation
After the completion, silver-colored stick is drawn；
（2）By step（1）Obtained silver-colored stick carries out heating and thermal insulation processing；
（3）Prepare accurate swager, and set temperature carries out heating and thermal insulation to the mold of accurate swager；Heating and thermal insulation is completed
Afterwards, by step（2）The silver-colored stick of the heating and thermal insulation, which is delivered in the mold of accurate swager, to be forged, and 1 ~ 5 passage is forged；
Complete forging；
（4）By step（3）The silver-colored stick for completing forging carries out the cold forming of swaging of 5 ~ 10 passages, after cold forming of swaging to obtain the final product
To silver-colored evaporation material.
2. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（1）The continuous casting of the use
Stove be horizontal continuous casting furnace or under draw formula continuous casting furnace.
3. the preparation method of silver evaporation material according to claim 1 or claim 2, which is characterized in that step（1）Further include：To
It is passed through before inert gas in conticaster, vacuumize process is carried out to conticaster first, the pressure inside conticaster is made to reach
0.1Pa is passed through inert gas again after the completion of vacuumizing.
4. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（1）It is described to be passed through continuous casting furnace
Interior inert gas includes nitrogen and argon gas.
5. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（1）When the extraction silver stick
Rate be 4 ~ 20cm/min；A diameter of 6 ~ the 20mm for drawing silver-colored stick.
6. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（2）It is described that silver-colored stick is carried out
Heating and thermal insulation is handled：Silver-colored stick is put into continuous tunnel furnace, is heated to 600 ~ 900 DEG C, and kept the temperature under the conditions of 600 ~ 900 DEG C
0.5 ~ 2 hour.
7. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（3）It is described that mold is carried out
Heating and thermal insulation is：Mold is heated to 300 ~ 600 DEG C by room temperature, then keeps the temperature 0.5 ~ 2 hour at such a temperature.
8. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（3）It is described to be forged to process
In each passage make the sectional area of silver-colored stick shrink 30% ~ 80%, it is 0.5 ~ 5m/min to go out linear velocity.
9. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that the purity of the silver material >=
99.99%。
10. the preparation method of silver-colored evaporation material according to claim 1, which is characterized in that step（4）In the cold journey of swaging
Each passage makes the sectional area of silver-colored stick shrink 10% ~ 30%, and it is 2 ~ 10m/min to go out linear velocity.
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| CN201810667971.XA CN108531864B (en) | 2018-06-26 | 2018-06-26 | Silver evaporation material and preparation method thereof |
Applications Claiming Priority (1)
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|---|---|---|---|
| CN201810667971.XA CN108531864B (en) | 2018-06-26 | 2018-06-26 | Silver evaporation material and preparation method thereof |
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| CN108531864B CN108531864B (en) | 2020-10-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111215839A (en) * | 2018-11-23 | 2020-06-02 | 宁波江丰电子材料股份有限公司 | Forming method of coating material |
| CN111485138A (en) * | 2020-04-23 | 2020-08-04 | 中国科学院金属研究所 | Preparation method of cold-processed cobalt-based alloy rod wire |
| CN112872077A (en) * | 2021-01-29 | 2021-06-01 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111215839A (en) * | 2018-11-23 | 2020-06-02 | 宁波江丰电子材料股份有限公司 | Forming method of coating material |
| CN111485138A (en) * | 2020-04-23 | 2020-08-04 | 中国科学院金属研究所 | Preparation method of cold-processed cobalt-based alloy rod wire |
| CN112872077A (en) * | 2021-01-29 | 2021-06-01 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity silver evaporation material |
| 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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| CN108531864B (en) | 2020-10-23 |
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