CN108754422B - Method for realizing spreading of gallium-based liquid metal on surface of solid sheet - Google Patents

Method for realizing spreading of gallium-based liquid metal on surface of solid sheet Download PDF

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CN108754422B
CN108754422B CN201810646929.XA CN201810646929A CN108754422B CN 108754422 B CN108754422 B CN 108754422B CN 201810646929 A CN201810646929 A CN 201810646929A CN 108754422 B CN108754422 B CN 108754422B
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liquid metal
gallium
based liquid
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solid sheet
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CN108754422A (en
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赵银女
闫金良
闫慧龙
李宏光
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Ludong University
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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
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
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Abstract

The invention provides a method for realizing the surface of a solid sheetA method for spreading gallium-based liquid metal belongs to the technical field of heat dissipation of electronic devices. Depositing a continuous layer of Ga on the surface of a non-wetting solid sheet2O3Film, reduction annealing Ga2O3Ga with thin film formation of inside-out structure2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer. And dripping the gallium-based liquid metal on the surface of the composite structure film, completely wetting the gallium-based liquid metal and the metal Ga layer, and spreading the liquid metal on the surface of the solid sheet. The invention avoids the electric conduction between the solid sheet and the liquid metal and realizes the infiltration and the spreading of the gallium-based liquid metal on the surface of the solid sheet.

Description

Method for realizing spreading of gallium-based liquid metal on surface of solid sheet
Technical Field
The invention relates to a method for realizing the spreading of gallium-based liquid metal on the surface of a solid sheet, belonging to the technical field of heat dissipation of electronic devices.
Background
Liquid metal refers to a metal or metal compound having a relatively low melting point. Generally, it melts to a liquid state at normal temperature or at a temperature slightly higher than normal temperature. Common liquid metals such as mercury, metallic gallium, and gallium-based metal compounds. Liquid metals are widely used in various aspects such as energy management, conversion and storage due to their high thermal and electrical conductivity. As is known, liquid metal gallium and alloy thereof have the advantages of low melting point, high thermal conductivity, good fluidity and the like, particularly the thermal conductivity of the liquid metal gallium is far higher than that of a conventional thermal interface material such as silicon oil or 1 order of magnitude of the material added with high thermal conductivity nano particles, and the liquid metal gallium and the alloy thereof are very ideal thermal interface materials. In recent years, more and more researchers have begun exploring the use of liquid metals to improve interfacial heat transfer. The liquid metal is directly used as a thermal interface material, so that the overflow phenomenon is easy to occur, and the wettability of the liquid metal and the solid heat sink is not ideal enough. FIG. 1 shows gallium-based liquid metal Ga62.5In21.5Sn16Liquid drops formed on the surface of the copper sheet indicate gallium-based liquid metal Ga62.5In21.5Sn16The surface of the copper sheet which is not specially treated is hydrophobic. Therefore, the liquid metal cannot spread well on the solid surface, and some gaps still exist on the contact surface after the interface is filled, thereby affecting the heat conductivity.
Through the search of the prior literature, the method for realizing the liquid metal spreading on the solid surface mainly focuses on improving the liquid film spreading characteristic and the heat transfer performance of the solid surface by enhancing the wettability of the liquid metal thermal interface material on the solid surface. The invention patent with application publication No. CN103131396A discloses a thermal interface material and a manufacturing method thereof, which is characterized in that metal gallium, indium, mercury, sodium, potassium, cesium or binary and multi-element alloys thereof are put in air or oxygen to be oxidized to form the thermal interface material, so that the wettability between metal-based fluid and various interfaces can be greatly improved, and the requirements of the thermal interface material can be better met. However, the thermal conductivity of the liquid metal is greatly reduced after the liquid metal is oxidized in air or oxygen, and the advantage of the liquid metal as a thermal interface material is lost. The invention patent with application publication number CN104357795A discloses a method for realizing large-area spreading of liquid by improving the wettability of liquid and solid surfaces, which is characterized in that a plurality of spherical or ellipsoidal holes are processed on a non-wetting surface, small holes with specific depths are selected, the distance of a space is limited, metal liquid drops are injected into the small holes on the non-wetting surface, and the contact angle of the obtained liquid drops is less than 90 degrees; when the metal liquid flows from top to bottom, the metal liquid drops exposed from the non-wetting surface are connected by the flowing metal liquid due to the fact that the metal liquid of the same kind is completely soaked, the flowing metal liquid and the metal liquid drops are connected into a whole liquid film and cover the surface of the non-wetting solid, and the non-wetting surface is good in wettability. The process cost for processing the spherical or ellipsoidal small hole on the solid surface is high, and the labor cost is consumed for injecting the metal liquid drop into the small hole, so that the industrial popularization is difficult.
Disclosure of Invention
The existing method for realizing the spreading of the liquid metal on the solid surface has certain defects, the wettability of the liquid metal on the solid surface is greatly enhanced after the liquid metal is oxidized in air or oxygen, the spreading of the liquid metal on the solid surface is facilitated, but the advantage of high heat conductivity of the liquid metal is lost after the liquid metal is oxidized; a plurality of spherical or ellipsoidal holes are processed on the non-wetting surface, metal liquid drops are injected into the small holes on the non-wetting surface, large-area spreading of liquid is achieved by improving the wettability of the liquid and the solid surface, the processing cost of the small holes and the labor cost for injecting the liquid drops are high, and industrial popularization is difficult.
The invention aims to overcome the defects in the prior art and provides a method for realizing the spreading of gallium-based liquid metal on the surface of a solid sheet. FIG. 2 is a schematic view showing a structure in which a gallium-based liquid metal is spread on the surface of a solid sheet according to the present invention, and a composite structure thin film 2 is formed on the surface of a solid sheet 1, the composite structure thin film 2 being formed of Ga2O3Layer 21, Ga — O mixed layer 22, and metal Ga layer 23, and gallium-based liquid metal film 3 is spread on metal Ga layer 23. The invention changes the wettability of the gallium-based liquid metal on the solid surface by coordinating the chemical components of the solid interface, and realizes the spreading of the gallium-based liquid metal on the surface of the solid sheet. The invention has simple manufacturing process and low cost, and the gallium-based liquid metal does not need to be oxidized in the process, thereby having good feasibility of implementation.
The invention provides a method for realizing the spreading of gallium-based liquid metal on the surface of a solid sheet, which is to prepare Ga on the surface of the solid sheet by using vacuum magnetron non-reactive sputtering coating2O3Film of Ga2O3Thin film reduction annealing to form Ga with structure from inside to outside2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer. When the gallium-based liquid metal is dripped on the surface of the composite structure film, the gallium-based liquid metal is spread on the surface of the solid sheet due to the fact that the gallium-based liquid metal and the metal Ga layer are completely wetted, and the spreading of the gallium-based liquid metal on the surface of the solid sheet is achieved.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a method for realizing gallium-based liquid metal spreading on the surface of a solid sheet comprises the following steps:
(1) ga of high purity2O3The target material is arranged in a water-cooling radio frequency cathode target groove in a sputtering chamber of a magnetron sputtering device, a cleaned solid sheet is fixed on a substrate holder, the substrate holder is inserted into a substrate turntable in the sputtering chamber, and the solid sheet and Ga are adjusted2O3The target distance is 60-70 mm.
(2) Vacuumizing the sputtering chamber until the base pressure of the sputtering chamber is less than 5.0 multiplied by 10-4Pa, filling high-purity Ar gas with the flow rate of 20SCCM into the sputtering chamber, and adjusting the air extraction amount to maintain the Ar gas pressure in the sputtering chamber at the high pressure0.2-2 Pa。
(3) Turn on Ga2O3The radio frequency power supply of the target material has the sputtering power density of 1.5-5.3W/cm2Opening a baffle plate after the radio frequency glow discharge is stable to prepare Ga on the surface of the solid sheet2O3Film of Ga by controlling sputtering time2O3The thickness of the film is 50-200 nm.
(4) Ga (b) is2O3Film at H2Annealing in an Ar-mixed gas, H2H in-Ar gas mixture25-15% of volume fraction, 480-550 ℃ of annealing temperature and 10-15 minutes of annealing time; ga2O3Thin film reduction annealing to form Ga from inside to outside2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer.
(5) In Ga2O3And injecting gallium-based liquid metal liquid drops on the composite structure film of the layer/Ga-O mixed layer/metal Ga layer, wherein the gallium-based liquid metal is completely wetted with the metal Ga and can be expanded along the surface of the solid sheet and attached to the surface of the solid sheet, so that the gallium-based liquid metal is spread on the surface of the solid sheet.
The solid piece in the step (1) is a silicon chip or a copper sheet
In the step (5), the gallium-based liquid metal is Ga62.5In21.5Sn16、Ga68.5In21.5Sn10、Ga75.5In24.5One kind of (1).
The invention has the beneficial effects or characteristics that:
the invention forms Ga with a structure from inside to outside on the surface of a solid sheet2O3The composite structure film of the layer/Ga-O mixed layer/metal Ga layer realizes the spreading of the gallium-based liquid metal on the surface of the solid sheet. Ga2O3The layer avoids electrical conduction between the solid piece and the liquid metal. Compared with the prior art that the wettability between the metal-based fluid and various interfaces is improved mainly by using the oxidized liquid metal, the gallium-based liquid metal in the invention does not need to be oxidized in air or oxygen, and the advantage of high thermal conductivity of the gallium-based liquid metal is kept. Compared with the reported method for processing a plurality of spheres on the surface of a solid orThe invention has the advantages of relatively economic process cost and labor cost, simple process and strong feasibility of industrialized popularization.
Drawings
FIG. 1 shows gallium-based liquid metal Ga62.5In21.5Sn16Droplets formed on the surface of the copper sheet, wherein: 1. a copper sheet; 2. gallium-based liquid metal Ga62.5In21.5Sn16；
FIG. 2 is a schematic illustration of the structure of the gallium-based liquid metal spread on the surface of a solid sheet after treatment according to the present invention;
in the figure: 1. a solid tablet; 2. a composite structural film; 21. ga2O3A layer; 22. a Ga-O mixed layer; 23. a metal Ga layer; 3. a gallium-based liquid metal film.
FIG. 3 shows gallium-based liquid metal Ga62.5In21.5Sn16The surface of the copper sheet was spread after the treatment, in the figure: 1. a copper sheet; 2. gallium-based liquid metal Ga62.5In21.5Sn16。
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
(1) Ga of high purity2O3The target material is arranged in a water-cooling radio frequency cathode target groove in a sputtering chamber of the magnetron sputtering device, the cleaned copper sheet is fixed on a substrate holder, the substrate holder is inserted into a substrate turntable in the sputtering chamber, and the copper sheet and Ga are adjusted2O3The target distance was 60 mm.
(2) Vacuumizing the sputtering chamber until the base pressure of the sputtering chamber is less than 5.0 multiplied by 10-4Pa, filling high-purity Ar gas with the flow rate of 20SCCM into the sputtering chamber, and adjusting the air extraction amount to maintain the Ar gas pressure of the sputtering chamber at 2 Pa.
(3) Turn on Ga2O3The radio frequency power supply of the target material has the sputtering power density of 1.5W/cm2Opening the barrier after the radio frequency glow discharge is stabilizedPreparation of Ga on surface of copper sheet by using board2O3Film of Ga by controlling sputtering time2O3The thickness of the film is 50 nm.
(4) Ga (b) is2O3Film at H2Annealing in an Ar-mixed gas, H2H in-Ar gas mixture2The volume fraction is 5 percent, the annealing temperature is 480 ℃, and the annealing time is 10 minutes; ga2O3Thin film reduction annealing to form Ga from inside to outside2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer.
(5) In Ga2O3Injecting gallium-based liquid metal Ga on the composite structure film of layer/Ga-O mixed layer/metal Ga layer62.5In21.5Sn16Liquid droplets due to gallium-based liquid metal Ga62.5In21.5Sn16Completely wet with metal Ga, gallium-based liquid metal Ga62.5In21.5Sn16Will expand along the surface of the copper sheet and attach to the surface of the copper sheet to realize the Ga-based liquid metal Ga62.5In21.5Sn16Spread on the surface of a copper sheet, FIG. 3 shows gallium-based liquid metal Ga62.5In21.5Sn16The surface of the copper sheet spreads after the treatment.
Example 2
(1) Ga of high purity2O3The target material is arranged in a water-cooling radio frequency cathode target groove in a sputtering chamber of a magnetron sputtering device, a cleaned silicon wafer is fixed on a substrate holder, the substrate holder is inserted into a substrate turntable in the sputtering chamber, and the silicon wafer and Ga are adjusted2O3The target distance was 70 mm.
(2) Vacuumizing the sputtering chamber until the base pressure of the sputtering chamber is less than 5.0 multiplied by 10-4Pa, filling high-purity Ar gas with the flow rate of 20SCCM into the sputtering chamber, and adjusting the air extraction amount to maintain the Ar gas pressure of the sputtering chamber at 0.2 Pa.
(3) Turn on Ga2O3The radio frequency power supply of the target material has the sputtering power density of 5.3W/cm2Opening the baffle plate after the radio frequency glow discharge is stable to prepare Ga on the surface of the silicon wafer2O3Film of Ga by controlling sputtering time2O3The thickness of the film is 200nm。
(4) Ga (b) is2O3Film at H2Annealing in an Ar-mixed gas, H2H in-Ar gas mixture2The volume fraction is 15 percent, the annealing temperature is 550 ℃, and the annealing time is 15 minutes; ga2O3Thin film reduction annealing to form Ga from inside to outside2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer.
(5) In Ga2O3Injecting gallium-based liquid metal Ga on the composite structure film of layer/Ga-O mixed layer/metal Ga layer75.5In24.5Liquid droplets due to gallium-based liquid metal Ga75.5In24.5Completely wet with metal Ga, gallium-based liquid metal Ga75.5In24.5Will expand along the surface of the silicon chip and attach to the surface of the silicon chip to realize gallium-based liquid metal Ga75.5In24.5Spread on the surface of the silicon wafer.
Example 3
(1) Ga of high purity2O3The target material is arranged in a water-cooling radio frequency cathode target groove in a sputtering chamber of the magnetron sputtering device, the cleaned copper sheet is fixed on a substrate holder, the substrate holder is inserted into a substrate turntable in the sputtering chamber, and the copper sheet and Ga are adjusted2O3The target distance was 65 mm.
(2) Vacuumizing the sputtering chamber until the base pressure of the sputtering chamber is less than 5.0 multiplied by 10-4Pa, filling high-purity Ar gas with the flow rate of 20SCCM into the sputtering chamber, and adjusting the air extraction amount to maintain the Ar gas pressure of the sputtering chamber at 0.5 Pa.
(3) Turn on Ga2O3The radio frequency power supply of the target material has the sputtering power density of 2.5W/cm2Opening a baffle plate after the radio frequency glow discharge is stable to prepare Ga on the surface of the copper sheet2O3Film of Ga by controlling sputtering time2O3The thickness of the film is 100 nm.
(4) Ga (b) is2O3Film at H2Annealing in an Ar-mixed gas, H2H in-Ar gas mixture2The volume fraction is 10 percent, the annealing temperature is 500 ℃, and the annealing time is 12 minutes; ga2O3Thin film reduction annealing to form Ga from inside to outside2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer.
(5) In Ga2O3Injecting gallium-based liquid metal Ga on the composite structure film of layer/Ga-O mixed layer/metal Ga layer68.5In21.5Sn10Liquid droplets due to gallium-based liquid metal Ga68.5In21.5Sn10Completely wet with metal Ga, gallium-based liquid metal Ga68.5In21.5Sn10Will expand along the surface of the copper sheet and attach to the surface of the copper sheet to realize the Ga-based liquid metal Ga68.5In21.5Sn10Spread on the surface of the copper sheet.

Claims (4)

1. A method for realizing the spreading of gallium-based liquid metal on the surface of a solid sheet is characterized in that the method prepares Ga on the surface of the solid sheet by vacuum magnetron non-reactive sputtering coating2O3A film; ga is mixed with2O3The film is placed in H2Volume fraction of 5-15% of H2Annealing in-Ar mixed gas at 480-550 ℃ for 10-15 minutes to form Ga from inside to outside2O3A composite structure film of layer/Ga-O mixed layer/metal Ga layer; the gallium-based liquid metal liquid drop spreads along the surface of the composite structure film and spreads on the surface of the solid sheet.
2. The method for realizing gallium-based liquid metal spreading on the surface of a solid sheet according to claim 1, wherein the Ga is subjected to radio frequency magnetron sputtering in an Ar gas atmosphere2O3Preparation of Ga from target material2O3Film, solid sheet and Ga2O3The target distance is 60-70mm, the Ar gas pressure of the sputtering chamber is 0.2-2 Pa, and the sputtering power density is 1.5-5.3W/cm2，Ga2O3The thickness of the film is 50-200 nm.
3. The method for realizing gallium-based liquid metal spreading on the surface of a solid sheet according to claim 1, wherein the solid sheet is a silicon wafer or a copper sheet.
4. The method of claim 1The method for spreading the gallium-based liquid metal on the surface of the solid sheet is characterized in that the gallium-based liquid metal is Ga62.5In21.5Sn16、Ga68.5In21.5Sn10、Ga75.5In24.5One kind of (1).
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