CN108220878A - It is a kind of that there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film - Google Patents

It is a kind of that there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film Download PDF

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Publication number
CN108220878A
CN108220878A CN201611128761.0A CN201611128761A CN108220878A CN 108220878 A CN108220878 A CN 108220878A CN 201611128761 A CN201611128761 A CN 201611128761A CN 108220878 A CN108220878 A CN 108220878A
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Prior art keywords
high heat
nitrogen
heat conduction
matrix
preparation
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CN201611128761.0A
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Inventor
吴学坤
许壮志
薛健
张明
初小葵
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LIAONING FAKU COUNTY CERAMIC ENGINEERING TECHNOLOGY RESEARCH CENTER
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LIAONING FAKU COUNTY CERAMIC ENGINEERING TECHNOLOGY RESEARCH CENTER
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Priority to CN201611128761.0A priority Critical patent/CN108220878A/en
Publication of CN108220878A publication Critical patent/CN108220878A/en
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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
    • C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating

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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)
  • Physical Vapour Deposition (AREA)
  • Laminated Bodies (AREA)

Abstract

It is a kind of that there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film, this method selects fine aluminium as cathode targets, the purity of aluminium target is 99.99%, reaction gas uses pure nitrogen gas, the purity of nitrogen is 99.999%, reacts to form A1N high heat conduction films with nitrogen by the aluminium ion of ionization out.Realize step：1) it is put into sample room, is vacuumized after first workpiece substrate is cleaned and dried, in order to obtain high quality aluminium nitride coating, vacuum degree must be controlled 9 × 10‑3Below Pa；2) it is passed through high-purity Ar gas and sputter clean is carried out to matrix；3) then lead to argon gas, open arc plus back bias voltage, lead to nitrogen, nitrogen pressure is 1~3 × 10‑1Pa, pre- Bombardment and cleaning carry out 10~180min under 250v~650V back bias voltages.The present invention can deposit on complex sample surface, become one of most widely used film layer preparation method of field of engineering technology.Its method is simple, and easy to operate and technique is practical, is suitable for industrialized production.The nitrogen aluminium thick film ratio of preparation is consistent, oxygen-containing few, and thermal conductivity is high.

Description

It is a kind of that there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film
Technical field
There is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film the present invention relates to a kind of, this method is suitable for The multiple fields such as electronic measuring instrument, computer equipment, TT＆C system, aircraft, arms of precision.Belong to face coat to prepare and answer Use technical field.
Background technology
With being constantly progressive for science and technology, electronic equipment, computer and household electrical appliance emerge in multitude with it is widely available so that Electronic device Highgrade integration, high capacity have influenced the safe handling of circuit increasingly severely.In particular with work The extension of time causes temperature to increase due to device heating, and temperature rise easily causes electronic device operating temperature and rises rapidly There is job insecurity phenomenon, and then also contribute to the accurate of entire instrument in high, accurate control electronic device accuracy decline Control ability.Due also to the rigorous of electronic device, most of device is enclosed in the housing environment of sealing, heat-dissipating space ten It is point limited, the auxiliary heat dissipations means such as additional ventilation, water cooling can not be used, it is therefore desirable to study closed heat system from heat extraction drop Warm method, to ensure the reliable and stable work of product.
Aluminium nitride film by lattice wave or heat wave can be carried out the transmission of heat, led by the vibration of dot matrix or lattice Heat, heat dissipation performance are very good, are widely used in heat conducting coating field.At present, the A1N films that market is prepared are mostly inclined Thin, when the film of aluminium nitride is more than 1 μm, binding force becomes excessively poor, and deposition velocity is slow, efficiency is very low, occurs The problem of being difficult to commercialization.
Invention content
The present invention is provided a kind of with high heat conduction, high heat dispersion for the purpose of solving above-mentioned the deficiencies in the prior art The preparation method of aluminium nitride thick film.This method mainly solve the prior art cannot prepare aluminium nitride thick film and deposition velocity slowly and The problems such as being difficult to commercialization.
To achieve the above object, the present invention uses following technical proposals：One kind has high heat conduction, high heat dispersion aluminium nitride The preparation method of thick film, involved basis material can be the metals such as stainless steel, iron, copper, aluminium or pottery in this method The inorganic non-metallic materials such as porcelain, glass can also be the macromolecules organic polymer such as epoxy resin, polyimides.
The preparation method is that realized by following processing steps：It is good in order to make to have between film layer and matrix Binding force first has to be surface-treated basis material, and surface treatment directly affects film base binding performance and performance And reliability.Matrix surface is polished using mechanical polishing method first for metal material, is then chemically treated, makes surface Cleaning is bright.Chemical cleaning will be carried out for inorganic non-metallic material and organic material.
Further, process mechanism of the invention is to select fine aluminium the purity of aluminium target is as cathode targets 99.99%, reaction gas uses pure nitrogen gas, and the purity of nitrogen is 99.999%, and the aluminium ion and nitrogen come out by ionization is anti- A1N high heat conduction films should be formed.
In order to which film layer is made to have high thermal conductivity, technological parameter of the invention is just particularly important, and is the present invention below Preparation process.
1) it is put into sample room, is vacuumized after first workpiece substrate is cleaned and dried, in order to obtain high quality aluminium nitride Coating, vacuum degree must be controlled 9 × 10-3Below Pa；
2) it is passed through high-purity Ar gas and sputter clean is carried out to matrix；
3) then lead to argon gas, open arc plus back bias voltage, lead to nitrogen, nitrogen pressure is 1~3 × 10-1Pa.Pre- Bombardment and cleaning exists 10~180min is carried out under 250v~650V back bias voltages.
The method have the characteristics that：The aluminium nitride thick film prepared using present invention process, coating nitrogen al proportion are consistent, oxygen-containing Few, thermal conductivity is high, and the A1N high heat conduction film thicknesses of layers that this method is prepared is up to 3~10 μm, binding force between film layer and matrix Greatly, heat conductivility is good.It can particularly be deposited on complex sample surface, become the most widely used film layer system of field of engineering technology One of Preparation Method.Its method is simple, and easy to operate and technique is practical, is suitable for industrialized production.The nitrogen aluminium thick film ratio one of preparation It causes, is oxygen-containing few, thermal conductivity is high.
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It should be understood that these implementation be merely to illustrate the present invention and It is not used in and limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art The present invention can be made various changes or modifications, such equivalent forms equally fall within what the application the appended claims were limited Range.
Embodiment 1
Sputter clean：4×10-3Under Pa under vacuum state, it is passed through high-purity Ar gas and sputter clean is carried out to matrix.Plate A1N films： It first has to carry out matrix 100 DEG C of heating, the distance between target and matrix are 200mm, and the variation range for setting back bias voltage is 300V, cathode current 58A, nitrogen partial pressure 4 × 10-2Pa, sedimentation time 30 minutes obtain 3 μm of high heat conduction A1N films.
Embodiment 2
Sputter clean：6×10-3Under Pa under vacuum state, it is passed through high-purity Ar gas and sputter clean is carried out to matrix.Plate A1N films： It first has to carry out matrix 100 DEG C of heating, the distance between target and matrix are 200mm, and the variation range for setting back bias voltage is 500V, cathode current 60A, nitrogen partial pressure 5 × 10-2Pa, sedimentation time 60 minutes obtain 5 μm of high heat conduction A1N films.
Embodiment 3
Sputter clean：6×10-3Under Pa under vacuum state, it is passed through high-purity Ar gas and sputter clean is carried out to matrix.Plate A1N films： It first has to carry out matrix 100 DEG C of heating, the distance between target and matrix are 200mm, and the variation range for setting back bias voltage is 600V, cathode current 65A, nitrogen partial pressure 8 × 10-2Pa, sedimentation time 150 minutes obtain 9 μm of high heat conduction A1N films.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention Any modification made within refreshing and principle, equivalent replacement and improvement etc., should all be included in the protection scope of the present invention.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention Any modification made within refreshing and principle, equivalent replacement and improvement etc., should all be included in the protection scope of the present invention.

Claims (5)

1. a kind of have high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film, it is characterised in that：Fine aluminium is selected as the moon Pole target, the purity of aluminium target is 99.99%, and reaction gas uses pure nitrogen gas, and the purity of nitrogen is 99.999%, passes through ionization Aluminium ion out reacts to form A1N high heat conduction films with nitrogen, implements step：
1) it is put into sample room, is vacuumized after first workpiece substrate is cleaned and dried, in order to obtain high quality aluminium nitride coating, Vacuum degree must be controlled 9 × 10-3Below Pa；
2) it is passed through high-purity Ar gas and sputter clean is carried out to matrix；
3) then lead to argon gas, open arc plus back bias voltage, lead to nitrogen, nitrogen pressure is 1~3 × 10-1Pa, pre- Bombardment and cleaning is in 250v 10~180min is carried out under~650V back bias voltages.
2. there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film as described in claim 1, it is characterised in that： The workpiece substrate material is using stainless steel, iron, copper, aluminum metal or ceramics, glass inorganic nonmetallic materials or asphalt mixtures modified by epoxy resin Fat, polyimides macromolecule organic polymer.
3. there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film as described in claim 1, it is characterised in that： Sputter clean：4×10-3Under Pa under vacuum state, it is passed through high-purity Ar gas and sputter clean is carried out to matrix, plate A1N films：It first has to pair Matrix carries out 100 DEG C of heating, and the distance between target and matrix are 200mm, and the variation range for setting back bias voltage is 300V, and cathode is electric Flow 58A, nitrogen partial pressure 4 × 10-2Pa, sedimentation time 30 minutes obtain 3 μm of high heat conduction A1N films.
4. there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film as described in claim 1, it is characterised in that： Sputter clean：6×10-3Under Pa under vacuum state, it is passed through high-purity Ar gas and to matrix sputter clear, plating A1N films：It first has to base Body carry out heating 100 DEG C, the distance between target and matrix be 200mm, set back bias voltage variation range be 500V, cathode current 60A, nitrogen partial pressure 5 × 10-2Pa, sedimentation time 60 minutes obtain 5 μm of high heat conduction A1N films.
5. there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film as described in claim 1, it is characterised in that： Sputter clean：6×10-3Under Pa under vacuum state, it is passed through high-purity Ar gas and to matrix sputter clear, plating A1N films：It first has to base Body carry out heating 100 DEG C, the distance between target and matrix be 200mm, set back bias voltage variation range be 600V, cathode current 65A, nitrogen partial pressure 8 × 10-2Pa, sedimentation time 150 minutes obtain 9 μm of high heat conduction A1N films.
CN201611128761.0A 2016-12-09 2016-12-09 It is a kind of that there is high heat conduction, the preparation method of high heat dispersion aluminium nitride thick film Withdrawn CN108220878A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101775585A (en) * 2010-02-11 2010-07-14 厦门大学 Preparation method of high hardness zirconium nitride hard coat
CN101948999A (en) * 2010-09-26 2011-01-19 华南理工大学 Low-temperature-doped luminescent aluminum nitride thin film and preparation method thereof
CN103173727A (en) * 2011-12-22 2013-06-26 辽宁法库陶瓷工程技术研究中心 Preparation method of high-heat-conduction aluminum nitride thick film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101775585A (en) * 2010-02-11 2010-07-14 厦门大学 Preparation method of high hardness zirconium nitride hard coat
CN101948999A (en) * 2010-09-26 2011-01-19 华南理工大学 Low-temperature-doped luminescent aluminum nitride thin film and preparation method thereof
CN103173727A (en) * 2011-12-22 2013-06-26 辽宁法库陶瓷工程技术研究中心 Preparation method of high-heat-conduction aluminum nitride thick film

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