CN108315780B - Preparation method of high-reflectivity tin-silver composite coating - Google Patents
Preparation method of high-reflectivity tin-silver composite coating Download PDFInfo
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- CN108315780B CN108315780B CN201810188241.1A CN201810188241A CN108315780B CN 108315780 B CN108315780 B CN 108315780B CN 201810188241 A CN201810188241 A CN 201810188241A CN 108315780 B CN108315780 B CN 108315780B
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- 238000000576 coating method Methods 0.000 title claims abstract description 28
- 239000011248 coating agent Substances 0.000 title claims abstract description 27
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical compound [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002310 reflectometry Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052709 silver Inorganic materials 0.000 claims abstract description 26
- 239000004332 silver Substances 0.000 claims abstract description 26
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 229960003512 nicotinic acid Drugs 0.000 claims abstract description 8
- 235000001968 nicotinic acid Nutrition 0.000 claims abstract description 8
- 239000011664 nicotinic acid Substances 0.000 claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 239000010949 copper Substances 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 7
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims abstract description 5
- 238000007747 plating Methods 0.000 claims description 44
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- 238000009713 electroplating Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 229910020836 Sn-Ag Inorganic materials 0.000 claims description 7
- 229910020988 Sn—Ag Inorganic materials 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 5
- 239000005695 Ammonium acetate Substances 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 229940043376 ammonium acetate Drugs 0.000 claims description 5
- 235000019257 ammonium acetate Nutrition 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000009792 diffusion process Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 2
- 238000005282 brightening Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000000861 blow drying Methods 0.000 claims 1
- 239000000758 substrate Substances 0.000 abstract description 8
- 239000007787 solid Substances 0.000 abstract description 4
- 238000000137 annealing Methods 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000004073 vulcanization Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 10
- 239000002905 metal composite material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012858 packaging process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- DWBPIWPCOSHWCK-UHFFFAOYSA-M silver cyanate Chemical compound [Ag+].[O-]C#N DWBPIWPCOSHWCK-UHFFFAOYSA-M 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
A preparation method of a high-reflectivity tin-silver composite coating belongs to the technical field of semiconductor illumination. The method comprises the following steps: (1) electrodepositing a tin coating on the surface of the copper substrate by using stannous sulfate and concentrated sulfuric acid; (2) electrodepositing a silver coating on the surface of the obtained tin coating by using a nicotinic acid system; (3) annealing the obtained tin-silver composite coating to enable tin-silver atoms to diffuse at a tin-silver solid-solid interface so as to obtain Ag with high reflectivity3And a Sn film. After the composite coating is annealed, the coating is uniformly distributed, the bonding strength between coatings is improved, and Ag is formed on the outermost surface of the coating3Sn film, thereby obtaining HRBE with high reflectivity, excellent oxidation resistance and excellent vulcanization performance.
Description
Technical Field
The invention belongs to the field of semiconductor lighting sources, and particularly relates to a preparation method of a high-reflectivity tin-silver composite coating.
Background
Light Emitting Diodes (LEDs) are novel solid-state Light sources that can directly convert electrical energy into Light energy with high efficiency, have the advantages of long life, small size, energy saving, high efficiency, fast response speed, shock resistance, no pollution and the like compared with conventional Light sources, are a new generation of semiconductor illumination Light sources following incandescent lamps and fluorescent lamps, and have become a green industry for promoting rapid development of economy at present. However, due to the influence of LED chip packaging, only the light emitted from the front surface is usually used effectively, and the light escaping from the bottom surface and the side surface needs to be reflected to the front surface by the reflection cup. In order to avoid the absorption of light by the die bonding material between the chip and the Reflective cup, a High Reflective Back Electrode (HRBE) can be prepared on the back surface of the chip substrate.
Currently, Ag and its alloys are the most tried as HRBE. However, experiments prove that in the subsequent packaging process, the Ag atoms at the interface are agglomerated due to the temperature rise process and the heat transfer of the interface under the working condition of the LED, so that the flatness of the interface is greatly changed to cause the diffuse reflection of photons; elements such as S existing in the environment are likely to cause a reaction at the silver interface to generate a corresponding compound, which affects the reflectance and also causes a rapid increase in contact resistance. Therefore, the protective layer is introduced into the silver electrode or other elements are doped into the silver electrode to change the thermal and chemical stability of the electrode interface, and the engineering application field has far-reaching significance.
Disclosure of Invention
Aiming at the defects of the prior HRBE technology for preparing Ag and the alloy thereof, the invention aims to provide a novel high-reflectivity metal composite coating which has simple preparation process and good stability and can be produced in a large scale and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a high-reflectivity metal composite coating, which comprises the following steps
(1) Preparing a plating solution:
dissolving a certain amount of concentrated sulfuric acid serving as a complexing agent in water, fully stirring, and sequentially adding a certain amount of tin salt and a brightening agent to obtain a tinning liquid;
dissolving a certain amount of nicotinic acid serving as a complexing agent in water, fully stirring, sequentially adding a certain amount of silver nitrate, ammonium acetate, potassium hydroxide and potassium carbonate, and dripping a proper amount of ammonia water to obtain the silver plating solution.
(2) Preparing a plating layer:
the tin plating solution is placed in an electrolytic bath, a metal workpiece commonly used in the field of illumination is used as a cathode after being cleaned, derusted and dried, a tin sheet is used as an anode, and a direct current deposition mode is adopted for electroplating to obtain a tin plating layer.
Secondly, placing the silver plating solution in an electrolytic bath, cleaning and drying the workpiece with the tin plating layer obtained by electroplating to be used as a cathode, and electroplating by using a direct current deposition mode by using a silver sheet as an anode to obtain the silver plating layer.
Thirdly, vacuum diffusion heat treatment: placing the electrodeposited Sn-Ag composite coating sample in a vacuum resistance furnace, heating to 125-225 ℃ along with the furnace, keeping the temperature for 2-30 minutes at the heating speed of 5-7 ℃/minute, and cooling to room temperature in the air;
as a further preferable mode of the invention for the above scheme, the content of each component of the tin plating solution in the step (1) is: 30-40 g/L stannous sulfate, 180-220 g/L concentrated sulfuric acid and 30mL/L brightener.
As a further preferable mode of the invention for the above scheme, the content of each component of the silver plating solution in the step (1) is: 42-50 g/L of silver nitrate, 90-110 g/L of nicotinic acid, 77g/L of ammonium acetate, 45-55 g/L of potassium hydroxide, 70-82 g/L of potassium carbonate and 32mL/L of ammonia water.
In a further preferred embodiment of the present invention, the area ratio of the cathode to the anode should be 1: 1.
As a further preferable mode of the present invention to the above-mentioned embodiment, the pH of the silver plating solution is adjusted to 9.0 to 9.5 by using acetic acid or potassium hydroxide.
As a further preferable mode of the present invention for the above aspect, the metal workpiece in the step (2) is a pure copper workpiece.
As a further preferable mode of the present invention to the above-mentioned scheme, the cathode current density in the electroplating process in step (2) is controlled to be 0.5 to 2A/dm2(tin plating) and 0.2-0.4A/dm2And (silver plating), wherein the temperature of the plating solution is controlled to be 10-30 ℃, and the plating time is respectively 10 minutes (tin plating) and 30-300 seconds (silver plating).
The invention has the beneficial effects that:
the method comprises the following steps: (1) electrodepositing a tin coating on the surface of the copper substrate by using stannous sulfate and concentrated sulfuric acid; (2) electrodepositing a silver coating on the surface of the obtained tin coating by using a nicotinic acid system; (3) annealing the obtained tin-silver composite coating to enable tin-silver atoms to diffuse at a tin-silver solid-solid interface so as to obtain Ag with high reflectivity3And a Sn film.
(1) The prepared plating layer mainly contains tin and silver elements, the plating layer has high reflectivity and excellent oxidation resistance and sulfuration resistance, and the tin element is introduced into the silver electrode to change the thermal stability and chemical stability of an electrode interface, so that the plating layer can be effectively used for an LED packaging process.
(2) The invention utilizes a direct current electroplating method to prepare a large-area metal composite coating on the surface of a metal material. The required equipment is simple, the technological process is stable and controllable, and the method can be used for large-area production and is suitable for engineering application.
(3) The invention can realize the preparation of the high-reflectivity composite coating by using the methods of electrodeposition and heat treatment, and the preparation process without using toxic substances and organic matter modification simplifies the preparation process and ensures the stability of the coating. The traditional cyanate silver plating method is abandoned in the silver plating process, and a nicotinic acid system is adopted for silver plating, so that the damage to the environment and the human body is greatly reduced.
(4) After the Sn-Ag composite plating layer prepared by the invention is subjected to vacuum diffusion heat treatment at 125-225 ℃ for 1-60 minutes, Ag meeting the design requirement of HRBE is obtained on a Sn-Ag solid-solid interface3Sn film, and obviously improves the uniformity of plating compositions and the interface bonding strength of the plating and the substrate.
Drawings
The invention is further illustrated with reference to the following figures and examples.
Fig. 1 is a schematic diagram of a tin-silver composite plating layer. In fig. 1, 1 is silver plating, 2 is tin plating, and 3 is copper substrate.
FIG. 2 is a schematic diagram of the Sn-Ag composite coating after annealing treatment (150 ℃ C., 5 minutes). 4.Ag in FIG. 23Sn film, 5 tin coating and 6 copper substrate.
Detailed Description
Example 1
(1) 3g of stannous sulfate, 18g of concentrated sulfuric acid and 3mL of brightener are added into deionized water to prepare 100mL of tinning liquid.
In this example, pure copper was used as the cathode substrate, and electroplating was performed by direct current deposition after polishing and cleaning, with a cathode current density of 2A/dm2The plating time was 10 minutes.
(2) 4.2g of silver nitrate, 9g of nicotinic acid, 7.7g of ammonium acetate, 4.5g of potassium hydroxide, 7g of potassium carbonate and 3.2mL of light ammonia water are added into deionized water to prepare 100mL of silver plating solution.
In this example, the test using the deposited tin coatingThe sample is a cathode substrate, washed by acetone and alcohol, dried and electroplated by a direct current deposition method, and the cathode current density is 0.4A/dm2And the electroplating time is 1 minute, so that the tin-silver composite coating is obtained, as shown in figure 1.
(3) Placing the electrodeposited Sn-Ag composite coating sample in a vacuum resistance furnace, heating to 150 ℃ along with the furnace, keeping the temperature for 2-30 minutes at the heating speed of 5-7 ℃/minute, and cooling to room temperature along with the furnace; as shown in FIG. 2, there is a layer of Ag about 0.8 μm thick at the Sn-Ag solid interface3And a Sn film.
Claims (1)
1. A preparation method of a high-reflectivity tin-silver composite coating is characterized by comprising the following steps:
(1) placing the tin plating solution in an electrolytic bath, taking a metal workpiece subjected to cleaning, derusting and blow-drying as a cathode, taking a tin sheet as an anode, and electroplating by adopting a direct current deposition mode to obtain a tin plating layer, wherein the area ratio of the cathode to the anode is 1: 1; dissolving concentrated sulfuric acid as a complexing agent in water, fully stirring, and sequentially adding a tin salt and a brightening agent to obtain a tinning liquid; the tin plating solution comprises the following components in percentage by weight: 30-40 g/L of stannous sulfate, 180-220 g/L of concentrated sulfuric acid and 30mL/L of brightener; the metal workpiece is a pure copper workpiece;
in the process of tin plating, the cathode current density is controlled to be 0.5-2A/dm2Controlling the temperature of the plating solution at 10-30 ℃ and the electroplating time at 10 minutes;
(2) placing the silver plating solution in an electrolytic bath, cleaning and drying a workpiece with a tin plating layer obtained by electroplating to obtain a cathode, taking a silver sheet as an anode, and electroplating by adopting a direct current deposition mode to obtain a silver plating layer, wherein the area ratio of the cathode to the anode is 1: 1; dissolving nicotinic acid as a complexing agent in water, fully stirring, sequentially adding silver nitrate, ammonium acetate, potassium hydroxide and potassium carbonate, and dripping ammonia water to obtain a silver plating solution; the silver plating solution comprises the following components in percentage by weight: 42-50 g/L of silver nitrate, 90-110 g/L of nicotinic acid, 77g/L of ammonium acetate, 45-55 g/L of potassium hydroxide, 70-82 g/L of potassium carbonate and 32mL/L of ammonia water; adjusting the pH value of the silver plating solution to 9.0-9.5 by using acetic acid or potassium hydroxide;
in the silver plating process, the cathode current density is controlled to be 0.2-0.4A/dm2Controlling the temperature of the plating solution to be 10-30 ℃ and the electroplating time to be 30-300 seconds;
(3) vacuum diffusion heat treatment: and (3) placing the electrodeposited Sn-Ag composite coating sample in a vacuum resistance furnace, heating to 125-225 ℃ along with the furnace, keeping the temperature for 2-30 minutes at the heating speed of 5-7 ℃/minute, and cooling to room temperature in the air.
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| CN201810188241.1A CN108315780B (en) | 2018-03-07 | 2018-03-07 | Preparation method of high-reflectivity tin-silver composite coating |
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| CN201810188241.1A CN108315780B (en) | 2018-03-07 | 2018-03-07 | Preparation method of high-reflectivity tin-silver composite coating |
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| JP5313773B2 (en) * | 2009-06-04 | 2013-10-09 | 三菱伸銅株式会社 | Plated copper strip and method for producing the same |
| CN105358741B (en) * | 2013-06-10 | 2018-04-20 | 东方镀金株式会社 | The manufacture method and plating laminated body of plating laminated body |
| WO2014207975A1 (en) * | 2013-06-24 | 2014-12-31 | オリエンタル鍍金株式会社 | Method for producing plated material, and plated material |
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