CN110106466B - Ultrathin heat dissipation film and preparation method and application thereof - Google Patents

Ultrathin heat dissipation film and preparation method and application thereof Download PDF

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CN110106466B
CN110106466B CN201910348619.4A CN201910348619A CN110106466B CN 110106466 B CN110106466 B CN 110106466B CN 201910348619 A CN201910348619 A CN 201910348619A CN 110106466 B CN110106466 B CN 110106466B
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李永卿
王群
金鑫
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Beijing University of Technology
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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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive 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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • 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
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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
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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Abstract

The invention provides an ultrathin heat dissipation film and a preparation method and application thereof. The ultra-thin heat dissipation film comprises a metal substrate layer and a heat radiation layer, wherein the heat radiation layer is formed by raw materials containing 65-100 wt% of CuO, and the thickness of the heat radiation layer is 0.03-3 mu m. The invention also provides a preparation method and application of the ultrathin heat dissipation film by adopting a specific sputtering mode. The ultrathin heat dissipation film material prepared by the invention is small in size, ultrathin, good in heat dissipation effect, good in adhesive force, safe, reliable, pollution-free, convenient to process and assemble, and can be applied to parts needing heat dissipation of mobile phones, computers, communication equipment and other electronic products.

Description

Ultrathin heat dissipation film and preparation method and application thereof
Technical Field
The invention relates to the technical field of heat dissipation devices, in particular to an ultrathin heat dissipation film and a preparation method and application thereof.
Background
With the rapid development of microelectronic integration, integration of high power density devices, and assembly technologies, the reliability requirements and performance indexes of electronic components are further improved, and the heat generation problems of high integration and large capacity of electronic devices are more and more serious to affect the safe use of circuits. The temperature is increased due to the heat generated by the electronic components, which causes the precision of the precision control electronic device to be reduced or unstable. According to the relevant literature, 55% of failures of electronic equipment are caused by temperature exceeding the specified value of electronic components, and heat dissipation has become a key problem in the electronic industry.
From the prior art, copper or aluminum alloy is generally used as the mainstream of the current heat dissipation technology for heat dissipation devices. The heat pipe technology is an effective means for realizing rapid heat transfer in a limited space, further increasing the heat dissipation area and greatly improving the passive heat dissipation effect. However, the heat dissipation capability of such a heat dissipation method is not strong enough, and a fan is also needed for high-end electronic products. Most of electronic devices are sealed in a sealed shell, the heat dissipation space is limited, and an auxiliary heat dissipation means cannot be adopted, so that a self-heat-discharging and temperature-reducing method of a closed heat source system needs to be researched to ensure the reliable and stable work of products.
At present, it is urgently needed to provide an ultra-thin heat dissipation device with excellent heat dissipation effect so as to solve the problem that the service life of the product is short due to poor heat dissipation of the existing electronic device.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides an ultrathin heat dissipation film and a preparation method and application thereof.
An object of the present invention is to provide a (high emissivity) ultra-thin heat dissipation film comprising a metal substrate layer and a heat radiation layer formed of a raw material containing 65 to 100 wt% of CuO, the heat radiation layer having a thickness of 0.03 to 3 μm. The ultrathin heat dissipation film material provided by the invention has the advantages of small size, thin thickness and excellent heat dissipation performance of the adopted specific heat radiation layer, can effectively reduce the temperature in an electronic instrument and improve the reliability of electronic equipment, is safe and reliable, convenient to use and simple to mount, and can be widely applied to parts of mobile phones, computers, communication equipment and other electronic products needing heat dissipation.
According to some preferred embodiments of the present invention, the heat radiating layer is formed of a raw material whose host material is a composite oxide composed of CuO and a doped transition metal oxide; the mass content of the doped transition metal oxide is 0-35%, preferably 0.1-30%; more preferably, the transition metal element in the doped transition metal oxide is selected from one or more of Mn, Fe, Co and Ni. The heat radiation layer with specific components is a submicron and micron composite oxide film obtained by deposition in a reactive sputtering mode, the composite oxide mainly comprises CuO and doped transition metal oxide, and particularly, the selected specific components and the combination thereof have high emissivity and good heat radiation effect.
According to some preferred embodiments of the present invention, the heat radiating layer is made of CuO and MnOx、FeOy、CoOmAnd NiOnWherein x is at least one of 1, 1.5 and 2, y is 1 and/or 1.5, m is 1 and/or 1.5, and n is 1 and/or 1.5. The heat radiation layer is a high-emissivity material, the radiation heat dissipation effect is obvious, and the emissivity of the heat radiation layer can reach 0.98. The oxides in the heat-radiating layer in the present invention mainly utilize the +2 and +3 valences of the transition metal. Mixed oxides of different valence states may be present simultaneously.
According to some preferred embodiments of the present invention, further comprising an intermediate transition layer between the metal base layer and the heat radiating layer; preferably, the intermediate transition layer is formed by gradually transiting a metal phase and an oxide phase from the metal substrate layer to the surface heat radiation layer in sequence; the metal phase is a mixture formed by Cu and the doped transition metal element; the oxide phase is a mixture formed by copper oxide and the transition metal doped oxide; more preferably, an intermediate transition metal layer is formed on one side of the metal substrate layer by the metal phase; and/or forming an intermediate transition oxide layer between the intermediate transition metal layer and the heat radiating layer from the oxide phase. The film material consists of a metal substrate layer, an intermediate transition layer and a surface heat radiation layer. The specific intermediate transition layer is adopted as the intermediate matching of the substrate and the heat radiation layer, so that the bonding force of the substrate and the heat radiation layer can be greatly improved, and meanwhile, the heat radiation layer has higher heat conductivity and improves the heat radiation efficiency.
According to some preferred embodiments of the invention, the metal base layer has a thickness of 5 to 300 μm; preferably, the metal substrate layer is a copper foil, an aluminum foil, a copper sheet or an aluminum sheet. The metal basal layer can be electrolytic copper foil, aluminum foil or copper sheet, and can also be on the metal surface of the existing electronic product and other parts needing heat dissipation, the invention is preferably electrolytic copper foil, aluminum foil or copper sheet, has good heat conduction function, and the specific metal basal layer and the intermediate transition layer are matched to effectively improve the binding force of the metal basal layer and the surface heat radiation layer, and also has the advantages of safety, reliability, no pollution, convenient processing and convenient assembly, and can be pasted on the mobile phone, the computer, the communication equipment and other parts needing heat dissipation of the electronic product.
According to some preferred embodiments of the present invention, a thickness ratio of the heat radiation layer to the intermediate transition layer is (500nm-2.5 μm): (250nm-700 nm); the invention adopts the ultrathin heat dissipation film material with specific thickness ratio to have excellent heat dissipation performance, the heat generated by the electronic component can be quickly conducted to the surface heat radiation layer through the metal basal layer and the intermediate transition layer, the heat is dissipated to the surrounding environment space by the high emissivity of the surface radiation layer, and the layers have high adhesive force.
According to some preferred embodiments of the present invention, the metal substrate layer is a copper foil with a thickness of 30-70 μm, and the intermediate transition layer is composed of one or more metals of Cu, Mn, Fe, Co and Ni and their lower oxides with a thickness of 250nm-700 nm; the heat radiation layer is made of CuO and MnOx、FeOy、CoOmAnd NiOnWherein x is at least one of 1, 1.5 and 2, y is 1 and/or 1.5, m is 1 and/or 1.5, n is 1 and/or 1.5, and the thickness is 500nm to 2.5 μm.
The other purpose of the invention is to provide a preparation method of the ultrathin heat dissipation film, wherein the heat radiation layer is deposited on the metal substrate layer in a reactive sputtering mode; or depositing an intermediate transition layer and the heat radiation layer on the metal substrate layer in a reactive sputtering manner. At present, for the oxide mixing mode, such as spraying and solid-phase sintering, the oxide coating prepared by the methods is thick, generally more than tens of microns, and is not beneficial to being used in the limited space of electronic components with small capacity. The thickness of the ultrathin film prepared by the magnetron sputtering method is in the range of submicron to several microns, and the use is convenient. Preferably, the deposition process in the present invention uses a sputtering target composed of copper and the transition metal, wherein the content of copper is 70-100%, preferably 70-98%, and the content of the transition metal is 0-30%, preferably 2-30%, based on the total weight of the sputtering target. According to the ultrathin heat dissipation film material with the single-phase structure, which is formed in the magnetron sputtering codeposition process, CuO is used as a main crystal phase, the CuO crystal lattice is distorted through a doping method, for example, as an XRD (XRD) of a Cu alloy reaction sputtering product is shown in figure 3, the peak position is shifted to the left, and the crystal lattice constant is increased. Due to the valence-change characteristic of the transition metal, different oxides are generated due to different oxygen introducing amounts and different sputtering time, the lattice distortion and the crystal structure symmetry are reduced due to the valence change of elements and the doping of different elements, the lattice vibration absorption is enhanced, and the heat radiation characteristic of the material is improved. The ultrathin heat dissipation film material prepared by the process mode has the characteristic of high heat radiation. The film thicknesses of the prepared film materials are different due to different control parameters such as sputtering components, sputtering time, sputtering power and the like, and the emissivity of the material in a wave band range of 1-22 mu m is as high as 0.88-0.98.
According to some preferred embodiments of the invention, comprising:
step (1), introducing argon, and controlling Ar and O2The flow ratio of (1: 0) and the sputtering time of 1-5 min, and forming the intermediate transition metal layer on the metal substrate layer;
step (2), introducing argon and a small amount of oxygen, and controlling Ar and O2The flow ratio of (1: 0) -0.25, the sputtering time is 10-20min, and the intermediate transition metal oxide layer is formed on the intermediate transition metal layer;
step (3), introducing argon and oxygen, and controlling Ar and O2The flow ratio of (1: 0.25) to (1), the sputtering time is 20 to 60min, and the heat radiation layer is formed on the intermediate transition metal oxide layer.
According to a large number of experimental studies, the inventors surprisingly found that: because the copper has multi-valence state, the reaction sputtering lasts for about 3min, and the product is Cu2O; sputtering for about 6min to obtain Cu product4O3(ii) a The reactive sputtering time for forming the copper oxide layer is controlled to be 10min or more because the resultant is CuO after the reactive sputtering is carried out for 8min or more, and the control time of the reactive resultant is slightly different according to the ratio of oxygen to argon and the sputtering power. The invention obtains the heat radiation layer with the synergistic effect of the specific valence composite transition metal oxide by controlling time and other sputtering conditions, greatly improves the radiation characteristic of the heat radiation layer, and simultaneously has the characteristics ofExcellent adhesion.
The invention also aims to provide the application of the ultrathin heat dissipation film obtained by the preparation method or the ultrathin heat dissipation film obtained by the preparation method as a heat dissipation material in an electronic product; the electronic product is preferably a microelectronic component, a mobile phone, a computer, an internet communication device, a high-low voltage electric appliance, an air-conditioning refrigeration device or a wind power generator.
The invention has the beneficial effects that: the ultrathin heat dissipation film material prepared by the invention is small in size, ultrathin, good in heat dissipation effect, good in adhesive force, safe, reliable, pollution-free, convenient to process and assemble, and can be applied to parts needing heat dissipation of mobile phones, computers, communication equipment and other electronic products.
Drawings
FIG. 1 is an SEM image of a cross section of an ultra-thin heat spreader film material in an embodiment of the invention.
Fig. 2 is a schematic view of the structure of the ultra-thin heat dissipation film material in the embodiment of the invention.
Fig. 3 is a schematic view illustrating the structure of each layer of the ultra-thin heat dissipation film according to the embodiment of the present invention.
Fig. 4 is a graph illustrating the content of metal and oxide in the intermediate transition layer according to an embodiment of the present invention.
FIG. 5 is an XRD pattern of a reaction sputtered thermal radiation layer of a CuNi alloy in an embodiment of the present invention.
Reference numerals: 1. a metal substrate; 2. an intermediate transition metal layer; 3. an intermediate transition metal oxide layer; 4. a heat radiation layer; 5. and an intermediate transition layer.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention.
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials added in the examples are commercially conventional raw materials unless otherwise specified.
The equipment adopted by the invention is high-vacuum multifunctional magnetron sputtering coating equipment, and the gas is high-purity argon and high-purity oxygen. The emissivity is detected by an IR-2 dual-waveband emissivity measuring instrument.
The preparation method of the ultrathin heat dissipation film material of the following embodiment comprises the following steps: sputtering target materials (copper or copper alloy, mainly composed of copper and other transition metals) and a metal substrate layer 1 are placed in the high-vacuum multifunctional magnetron sputtering coating equipment. Before sputtering the metal substrate, respectively performing ultrasonic treatment in deionized water and absolute ethyl alcohol for 15min, drying, and placing on a coating equipment base. The sputtering process is as follows:
introducing high-purity argon by adopting a direct current or power frequency power supply, wherein the sputtering time is 1-5 min, and the thickness of a deposited film (the intermediate transition metal layer 2) is 50-200 nm;
introducing high-purity argon and a small amount of oxygen, Ar and O2The flow ratio of (1) to (0-0.25), the sputtering time is 10-20min, and the thickness of the deposition film (the intermediate transition metal oxide layer 3) is 200-500 nm;
introducing high-purity argon and oxygen, Ar and O2The flow ratio of (1) to (0.25-1), the sputtering time of 20-60min, and the thickness of the deposited film (heat radiation layer 4) of 500nm-2.5 μm.
The generated metal, oxide or composite oxide film is deposited on the metal substrate by the three-stage reactive sputtering mode to form the ultrathin heat dissipation film. Fig. 1 to 3 show a metal substrate layer 1, an intermediate transition layer 5 and a heat radiation layer 4 in the ultra-thin heat dissipation film prepared. Fig. 4 is a graph showing the variation of the metal and oxide contents in the intermediate transition layer in the example. FIG. 5 is an XRD pattern of a reaction sputtered thermal radiation layer of a CuNi alloy in an example.
Example 1
The metal substrate in this example was an electrolytic copper foil 50 μm thick, and the target was a 99.99% copper target. The sputtering power is 90W, the working pressure is 0.5Pa, and argon is introduced for sputtering for 5 min; then introducing a small amount of oxygen, and sputtering for 10 min; finally, the ratio of argon to oxygen is stabilized to be 4:1, and the sputtering time is 35 min. The total sputtering time was 50min, and the thickness of the resulting thin film material was about 1.6. mu.m.
Example 2
The metal substrate in this example is an electrolytic copper sheet with a thickness of 20 μm, and the target is an alloy target of Cu80Ni 20. When the sputtering power is 100W and the working pressure is 0.6Pa, argon is introduced for sputtering for 2 min; then introducing a small amount of oxygen, and sputtering for 10 min; finally, the ratio of argon to oxygen is stabilized to be 4:1, and the sputtering time is 20 min. The total sputtering time was 32min, and the thickness of the resulting thin film material was about 1.1. mu.m.
Example 3
The metal substrate in this example was an electrolytic copper foil 15 μm thick, and the target was a Cu90Mn10 alloy target. When the sputtering power is 100W and the working pressure is 0.6Pa, introducing argon for sputtering for 5 min; then introducing a small amount of oxygen, and sputtering for 10 min; finally, the ratio of argon to oxygen is stabilized to be 4:2, and the sputtering time is 30 min. The total sputtering time was 45min, and the thickness of the resulting thin film material was about 1.6. mu.m.
Example 4
The metal substrate in this example was an electrolytic copper foil having a thickness of 70 μm, and the target was a Cu70Ni20Mn10 alloy target. When the sputtering power is 80W and the working pressure is 0.5Pa, introducing argon for sputtering for 5 min; then introducing a small amount of oxygen, and sputtering for 10 min; finally, the ratio of argon to oxygen is stabilized to be 4:2, and the sputtering time is 20 min. The total sputtering time was 35min, and the thickness of the resulting thin film material was about 0.9. mu.m.
Example 5
The metal substrate in this example was an electrolytic copper foil 9 μm thick, and the target was an alloy target of Cu70Ni15Fe 15. When the sputtering power is 90W and the working pressure is 0.5Pa, introducing argon for sputtering for 5 min; then introducing a small amount of oxygen, and sputtering for 20 min; finally, the ratio of argon to oxygen is stabilized to be 4:1, and the sputtering time is 60 min. The total sputtering time was 85min, and the thickness of the resulting thin film material was about 2.7 μm.
Example 6
The metal substrate in this example is an ultra-thin aluminum foil with a thickness of 6 μm, and the target material is a Cu80Ni10Co10 alloy target. When the sputtering power is 100W and the working pressure is 0.5Pa, introducing argon for sputtering for 5 min; then introducing a small amount of oxygen, and sputtering for 10 min; finally, the ratio of argon to oxygen is stabilized to be 4:1, and the sputtering time is 30 min. The total sputtering time was 45min, and the thickness of the resulting thin film material was about 1.5. mu.m.
Example 7
The metal substrate in this example was an electrolytic copper foil 30 μm thick, and the target was an alloy target of Cu80Ni5Co5Mn5Fe 5. When the sputtering power is 100W and the working pressure is 0.5Pa, introducing argon for sputtering for 5 min; then introducing a small amount of oxygen, and sputtering for 10 min; finally, the ratio of argon to oxygen is stabilized to be 4:2, and the sputtering time is 40 min. The total sputtering time was 55min, and the thickness of the resulting thin film material was about 2.0. mu.m.
Experimental example 1
The emissivity performance of the thin film materials obtained in the above examples 1 to 7 in the wavelength band of 1 to 22 μm is measured, and the thickness of the thin film materials is obtained by means of SEM cross section, and the measurement results are shown in the following table 1:
TABLE 1 test results of film materials
Figure BDA0002043203460000081
Figure BDA0002043203460000091
The detection result shows that the ultrathin film prepared by the invention can reach micron or submicron level and has high emissivity.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (4)

1. The preparation method of the ultrathin heat dissipation film is characterized in that the ultrathin heat dissipation film comprises a metal substrate layer, a heat radiation layer and an intermediate transition layer, wherein the intermediate transition layer is positioned between the metal substrate layer and the heat radiation layer;
the intermediate transition layer is formed by gradually transiting a metal phase and an oxide phase from the metal substrate layer to the heat radiation layer in sequence; the intermediate transition layer is composed of metals of Cu, Mn, Fe, Co and Ni and low-valence oxides thereof, and the thickness is 250nm-700 nm;
the heat radiation layer is made of CuO and MnOx、FeOy、CoOmAnd NiOnWherein x is at least one of 1, 1.5 and 2, y is 1 and/or 1.5, m is 1 and/or 1.5, n is 1 and/or 1.5, and the thickness is 500nm to 2.5 [ mu ] m;
the metal basal layer is a copper foil;
depositing an intermediate transition layer and the heat radiation layer on the metal substrate layer in a reactive sputtering mode, wherein a sputtering target composed of copper and transition metal is used in the deposition process, the content of the copper is 70-98% and the content of the transition metal is 2-30% based on the total weight of the sputtering target, and the preparation of the ultrathin heat dissipation film comprises the following steps:
step (1), introducing argon, and controlling Ar and O2The flow ratio of (1: 0) and the sputtering time of 1-5 min, and forming the intermediate transition metal layer on the metal substrate layer;
step (2), introducing argon and a small amount of oxygen, and controlling Ar and O2The flow ratio of (1: 0) -0.25, the sputtering time is 10-20min, and the intermediate transition metal oxide layer is formed on the intermediate transition metal layer;
step (3), introducing argon and oxygen, and controlling Ar and O2The flow ratio of (1: 0.25) to (1), the sputtering time is 20 to 60min, and the heat radiation layer is formed on the intermediate transition metal oxide layer.
2. The method for preparing the ultra-thin heat dissipation film as recited in claim 1, wherein the metal substrate layer has a thickness of 5 to 300 μm.
3. The ultra-thin heat dissipation film obtained by the method for preparing the ultra-thin heat dissipation film according to any one of claims 1 or 2.
4. Use of the ultra-thin heat-dissipating film according to claim 3 or the ultra-thin heat-dissipating film obtained by the manufacturing method according to claim 1 or 2 as a heat-dissipating material in an electronic product.
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