CN116695118A - Infrared detection window metallization material and metallization method thereof - Google Patents

Infrared detection window metallization material and metallization method thereof Download PDF

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Publication number
CN116695118A
CN116695118A CN202310953981.0A CN202310953981A CN116695118A CN 116695118 A CN116695118 A CN 116695118A CN 202310953981 A CN202310953981 A CN 202310953981A CN 116695118 A CN116695118 A CN 116695118A
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China
Prior art keywords
metallization
infrared detection
laser
detection window
slurry
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CN202310953981.0A
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Chinese (zh)
Inventor
郝群
魏志鹏
唐鑫
陈梦璐
曹杰
李文浩
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Changchun University of Science and Technology
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Changchun University of Science and Technology
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Priority to CN202310953981.0A priority Critical patent/CN116695118A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/08Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/10Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
    • C23C24/103Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

An infrared detection window metallization material and a metallization method thereof relate to the technical field of metallization materials and solve the problems of high equipment requirement, high cost and environmental pollution of the existing metallization method. S1, preparing slurry: fully mixing metal powder and polyethylene glycol to obtain slurry for metallization; s2, laser modification: scanning a to-be-metallized area on the surface of the nonmetallic material by adopting laser focusing to realize laser modification; s3, laser metallization: the slurry is coated on the surface of a nonmetallic substrate, and the area to be metallized is scanned by laser under the protection of nitrogen, so that the solvent in the slurry volatilizes, and metal particles are fused, adhered and embedded into a microstructure of a matrix to form a metallized layer. The method can be applied to the technical field of infrared detection, can be applied to nonmetallic material metallized coating, and has the advantages of simple flow, convenient operation, environmental protection and energy conservation.

Description

Infrared detection window metallization material and metallization method thereof
Technical Field
The invention relates to the technical field of metallized materials, in particular to an infrared detection window metallized material and a metallization method thereof.
Background
The infrared detection device, the module and the system are widely applied in the field of army and civilian, and the material for realizing the connection part between the window and the metal shell is very important. The window materials used at present comprise calcium fluoride, barium fluoride, germanium, zinc sulfide, zinc selenide and the like, reliable airtight welding is needed to be realized with a metal shell, an infrared detection window for device, module and system packaging is formed, long-term non-leakage and stable working requirements under low-temperature, high-temperature, cold-hot conversion, high-humidity and other environments are guaranteed, and high requirements are provided for the infrared detection window.
Non-metallic materials such as ceramics, glass, semiconductors and the like with high infrared transmittance have the characteristics of high temperature resistance, high strength, high hardness, wear resistance, corrosion resistance, electric insulation and the like, but are hard and brittle, and are not suitable to be infiltrated with metal brazing solder; the metal material has excellent ductility, electrical conductivity and thermal conductivity; the advantages of nonmetal and metal are complementary and expanded, the properties of high air tightness, high heat conduction, high resistance, good mechanical strength, ideal dielectric constant and the like are realized, and the method has wide application in the fields of new energy automobiles, electronic and electric, semiconductor packaging, IGBT modules and the like. The combination of non-metals with metals is crucial to achieve reliable metallization on non-metallic surfaces.
Conventional nonmetallic materials are metallized by coating, and a metallic film is formed by depositing metallic elements on the surface of a nonmetallic substrate under high vacuum conditions by using high vacuum coating equipment such as magnetron sputtering, PVD, a coating machine and the like. However, the equipment adopted in the mode is expensive, the use and maintenance cost is high, the coating period is long, and the procedures of cleaning, masking, tooling and the like are needed, especially the local coating of the miniaturized product is time-consuming, energy-consuming and labor-consuming. The metallization of the electroless plating film needs to be subjected to the procedures of cleaning, film covering masking, roughening, activation sensitization, post-treatment and the like, so that the operation flow is complex, the types of chemical medicines are various, the chemical medicines are toxic and harmful, the waste liquid is troublesome to treat, and the method is not environment-friendly and has low efficiency; and noble metal activation processes such as palladium, silver and the like are often required in the chemical plating film, so that the cost is high, the process is complex, and the environment is polluted.
It is therefore significant to find a process that does not require a vacuum mode and does not use noble metal materials to effect the metallization of the infrared detection window.
Disclosure of Invention
The invention provides an infrared detection window metallization material and a metallization method thereof, which aim to solve the problems of high cost and environmental pollution of the existing material metallization process.
The technical scheme of the invention is as follows:
an infrared detection window metallization method comprises the following steps:
s1, preparing slurry:
fully mixing metal powder and polyethylene glycol to obtain slurry for metalizing an infrared detection window;
s2, laser modification:
scanning an infrared detection window surface to-be-metallized area by adopting laser focusing to realize laser modification;
s3, laser metallization:
coating the slurry on the surface of an infrared detection window substrate, scanning the area to be metallized by using laser under the protection of nitrogen, volatilizing the solvent in the slurry, and embedding the metal particles into a matrix microstructure by fusion adhesion to form a metallized layer.
Preferably, the mass ratio of the metal powder in the slurry is 80% -95%.
Preferably, the polyethylene glycol has a molecular weight of less than 600.
Preferably, the metal powder in the slurry is one or a mixture of at least two of nickel powder, copper powder, aluminum powder and silver powder, and can also be coated with silver materials to form an alloy.
Preferably, the particle size of the metal powder is d50=5nm to 500nm.
Preferably, the laser in step S2 is a 20W picosecond laser.
Preferably, the frequency of the laser is 50 KHz-500 KHz, the pulse width is 10Ps, and the scanning speed is 30 mm/s-100 mm/s.
Preferably, the laser in step S3 is a 5W ultraviolet laser.
Preferably, the frequency of the laser is 30 KHz-150 KHz, the pulse width is 1 us-3 us, and the scanning speed is 5 mm/s-30 mm/s.
An infrared detection window metallized material is obtained by applying the metallization method.
Compared with the prior art, the invention has the following specific beneficial effects:
1. according to the invention, the nonmetallic material of the infrared detection window is modified by laser and the metallized area is scanned, so that the vacuum coating operation is replaced, the process flow is simplified, the energy consumption is reduced, and the operation time is shortened; replaces the complex cleaning, roughening and activating procedures in the chemical plating process, simplifies the flow and replaces the use of various chemical agents; the efficiency is high, no consumable consumption and no waste material and waste material are generated; the laser can be scanned in an imaging way at will, a mask die is not needed, and the tool is simple, flexible and convenient.
2. The laser modified microstructure increases the binding force of the metallization layer, realizes normal temperature and pressure, does not need a mask, rapidly metallizes the nonmetallic nano-submicron, has low cost investment, simple operation and environmental protection, and is particularly suitable for the metallization coating application of miniaturized nonmetallic parts.
3. The invention adopts nickel, copper or a small amount of silver and other materials, polyethylene glycol is used as a mixed solvent, the components are simple, the use of noble metals is reduced, and the cost is low; the material after laser metallization can be washed with water to clean out redundant slurry, is simple and convenient, and can be reused after water is evaporated from the washed slurry at low temperature.
The method can be applied to the technical field of infrared detection, can be applied to the application of the nonmetallic material metallized film coating of the infrared detection window, and has the advantages of simple flow, convenient operation, environmental protection and energy conservation.
Drawings
FIG. 1 is a schematic diagram showing the state of a sample after test in an effect example;
fig. 2 is a partial enlarged view of fig. 1.
Detailed Description
In order to make the technical solution of the present invention clearer, the technical solution of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention, and it should be noted that the following embodiments are only used for better understanding of the technical solution of the present invention, and should not be construed as limiting the present invention.
Example 1.
In this example, a semiconductor zinc selenide sheet was metallized, and the size of the zinc selenide sheet was as follows: diameter 25.4mm and thickness 2.5mm.
And (3) slurry preparation: fully mixing d50=100 nm nickel powder (85 percent by mass) and polyethylene glycol (molecular weight 400, 15 percent by mass) to obtain nickel slurry;
20W picosecond laser (frequency 200KHz, pulse width 10Ps, scanning speed 50 mm/s) is adopted to focus and scan the side and bottom peripheral (inner diameter 21mm, outer diameter 25.4 mm) areas of the zinc selenide sheet, the surface morphology of the modified substrate material is induced and activated, the roughness and activity of the surface area of the material are changed, so that the surface of the zinc selenide sheet forms a micro-nano structure, the hydrophilicity of a local area is enhanced, the surface roughening and sensitization are realized, and the adhesiveness of the coating slurry material on the surface of the substrate is improved;
the slurry is sprayed and coated on the surface of a zinc selenide sheet substrate, the thickness is controlled to be 500nm, a 5W ultraviolet laser (with the frequency of 150KHz, the pulse width of 3us and the annular filling scanning speed of 30 mm/s) is adopted to scan a target metallization area under the protection of nitrogen, so that the solvent in the slurry volatilizes, nickel metal particles are melted, adhered and embedded into the microstructure of the zinc selenide sheet substrate, and the nickel metal particles are melted and connected into a metal film layer.
And (3) cleaning the metallized zinc selenide sheet by deionized water, removing slurry in the area which is not scanned by laser, and cleaning to obtain the zinc selenide sheet with metallized outer rings on the side surfaces and the bottom surface.
Example 2.
In this embodiment, the germanium sheet is metallized, and the dimensions of the germanium sheet are as follows: diameter 25.4mm and thickness 2.5mm.
And (3) slurry preparation: fully mixing d50=300 nm nickel powder (80 mass percent) and polyethylene glycol (molecular weight 400, 20 mass percent) to obtain nickel slurry;
focusing and scanning the side and bottom peripheral (inner diameter 21mm, outer diameter 25.4 mm) areas of the germanium sheet by adopting 20W picosecond laser (frequency 400KHz, pulse width 10Ps, scanning speed 80 mm/s), inducing activation to modify the surface morphology of the matrix material, changing the roughness and activity of the surface area of the material, enabling the surface of the germanium sheet to form a micro-nano structure, enhancing the hydrophilicity of a local area, realizing surface roughening and sensitization, and improving the adhesiveness of a coating slurry material on the surface of the matrix;
the slurry is sprayed and coated on the surface of a germanium sheet substrate, the thickness is controlled to be 500nm, a 5W ultraviolet laser (with the frequency of 50KHz, the pulse width of 1us and the annular filling scanning speed of 10 mm/s) is adopted to scan a target metallization area under the protection of nitrogen, so that the solvent in the slurry volatilizes, nickel metal particles are melted, adhered and embedded into the microstructure of the germanium sheet substrate, and the metal film layer is formed by fusion connection.
And (3) cleaning the metallized germanium sheet by deionized water, removing slurry in the non-laser scanning area, and cleaning to obtain the germanium sheet with side and bottom surface outer ring metallization.
Example 3.
In this embodiment, a zinc sulfide material of a certain infrared detection window is metallized, and the size of the zinc sulfide material is as follows: 25mm long, 20mm wide and 6mm thick.
And (3) slurry preparation: fully mixing d50=200 nm copper powder (90 mass percent) and polyethylene glycol (molecular weight 400, 10 mass percent) to obtain copper slurry;
20W picosecond laser (frequency 250KHz, pulse width 10Ps, scanning speed 60 mm/s) is adopted to focus and scan the areas of 5mm on the side surface and the bottom periphery of the zinc sulfide material, the surface morphology of the modified matrix material is induced and activated, the roughness and activity of the surface area of the material are changed, so that the surface of the zinc sulfide material forms a micro-nano structure, the hydrophilicity of a local area is enhanced, the surface roughening and sensitization are realized, and the adhesiveness of the coating slurry material on the surface of the matrix is improved;
the slurry is sprayed and coated on the surface of a zinc sulfide material substrate, the thickness is controlled to be 500nm, a 5W ultraviolet laser (with the frequency of 120KHz, the pulse width of 2.5us, the annular filling scanning and the speed of 20 mm/s) is adopted to scan a target metallization area under the protection of nitrogen, so that the solvent in the slurry volatilizes, nickel metal particles are melted, adhered and embedded into a zinc sulfide material substrate microstructure, and the metal film layer is formed by fusion connection.
And (3) cleaning the metallized zinc sulfide material with deionized water, removing slurry in the non-laser scanning area, and cleaning to obtain the zinc sulfide material with side and bottom surface outer ring metallization.
Effect example.
The metallized samples of examples 1-3 were tested separately using the method disclosed in ISO 2409:
using a knife back of a surgical knife or a designated cross knife to scratch at least two scratches vertically on the metallized layer on the surface of the substrate, and brushing the substrate for 5 times along the scratch direction; the 3M tape 600 was applied to the substrate surface and pressed with a finger tip to ensure good adhesion to the metallization layer and was peeled off from one end of the tape at a 60 ° angle for 0.5s in 5 min. If no shedding is marked as 5B, the shedding amount is marked as 4B between 0% and 5%, 3B between 5% and 15%, 2B between 15% and 35%, 1B between 35% and 65%, and 0B above 65%.
The graph of the tested sample is shown in fig. 1, and the local enlargement of the outer ring metallization layer is shown in fig. 2. It can be seen that the surface metallization does not fall off at all.
The test results are shown in the following table:
it can be seen that the infrared detection window metallization method provided by the invention is adopted to metalize the surface of the nonmetallic substrate, and the binding force between the metalizing layer and the substrate is very reliable. Therefore, the method can be widely applied to the technical field of infrared detection, meets the requirements of the metallized coating of the infrared detection window, and has the advantages of simple flow, convenient operation, environmental protection and energy conservation.

Claims (10)

1. The infrared detection window metallization method is characterized by comprising the following steps of:
s1, preparing slurry:
fully mixing metal powder and polyethylene glycol to obtain slurry for metallization;
s2, laser modification:
scanning a to-be-metallized area on the surface of the nonmetallic material of the infrared detection window by adopting laser focusing to realize laser modification;
s3, laser metallization:
coating the slurry on the surface of a nonmetallic substrate of an infrared detection window, scanning an area to be metallized by using laser under the protection of nitrogen, volatilizing a solvent in the slurry, and fusing, adhering and embedding metal particles into a microstructure of a matrix to form a metallized layer.
2. The method for metalizing an infrared detection window according to claim 1, wherein the mass ratio of the metal powder in the slurry is 80% -95%.
3. The method of claim 1, wherein the polyethylene glycol has a molecular weight of less than 600.
4. The method for metallizing an infrared detection window according to claim 1, wherein the metal powder in the slurry is one or a mixture of at least two of nickel powder, copper powder, aluminum powder and silver powder.
5. The method for metallizing an infrared detection window according to claim 1, wherein the particle size of the metal powder is d50=5nm to 500nm.
6. The method of claim 1, wherein the laser light in step S2 is a 20W picosecond laser light.
7. The method for metallizing an infrared detection window according to claim 6, wherein the laser has a frequency of 50 khz-500 khz, a pulse width of 10Ps and a scanning speed of 30 mm/s-100 mm/s.
8. The method of claim 1, wherein the laser light in step S3 is a 5W uv laser light.
9. The method for metallizing an infrared detection window according to claim 8, wherein the laser has a frequency of 30 khz-150 khz, a pulse width of 1 us-3 us and a scanning speed of 5 mm/s-30 mm/s.
10. An infrared detection window metallization material, which is characterized in that the infrared detection window metallization material is obtained by applying the metallization method according to any one of claims 1-9.
CN202310953981.0A 2023-08-01 2023-08-01 Infrared detection window metallization material and metallization method thereof Pending CN116695118A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1576263A (en) * 2003-07-21 2005-02-09 Abb研究有限公司 Laser-irradiated metallized electroceramic
JP2008216174A (en) * 2007-03-07 2008-09-18 Showa Optronics Co Ltd Infrared detector and method of manufacturing the same
CN106653630A (en) * 2017-01-22 2017-05-10 大连大学 Silicon surface metallization method
CN107737937A (en) * 2017-11-27 2018-02-27 南通金源智能技术有限公司 A kind of aluminium powder for 3D printing and preparation method thereof
CN111172532A (en) * 2020-02-18 2020-05-19 重庆理工大学 Method for preparing medium-entropy alloy coating on surface of pure titanium plate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1576263A (en) * 2003-07-21 2005-02-09 Abb研究有限公司 Laser-irradiated metallized electroceramic
JP2008216174A (en) * 2007-03-07 2008-09-18 Showa Optronics Co Ltd Infrared detector and method of manufacturing the same
CN106653630A (en) * 2017-01-22 2017-05-10 大连大学 Silicon surface metallization method
CN107737937A (en) * 2017-11-27 2018-02-27 南通金源智能技术有限公司 A kind of aluminium powder for 3D printing and preparation method thereof
CN111172532A (en) * 2020-02-18 2020-05-19 重庆理工大学 Method for preparing medium-entropy alloy coating on surface of pure titanium plate

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Application publication date: 20230905