CN114540778A - Ti-Mo alloy film and preparation method thereof - Google Patents

Ti-Mo alloy film and preparation method thereof Download PDF

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Publication number
CN114540778A
CN114540778A CN202210045084.5A CN202210045084A CN114540778A CN 114540778 A CN114540778 A CN 114540778A CN 202210045084 A CN202210045084 A CN 202210045084A CN 114540778 A CN114540778 A CN 114540778A
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China
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target
alloy film
base material
titanium
molybdenum
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潘艳
赵泉
王涛
张国君
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Xian University of Technology
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Xian 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
    • 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
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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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)
  • Electrodes Of Semiconductors (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a Ti-Mo alloy film and a preparation method thereof, wherein the Ti-Mo alloy film comprises a Ti element and a Mo element, the content of the Mo element is 20-40 wt%, and the grain size is 80-150 nm. Loading a titanium target material and a molybdenum target material into a target position of direct-current magnetron sputtering equipment, loading a base material into a workpiece frame, placing the workpiece frame in a furnace chamber, and vacuumizing the furnace chamber; introducing argon into the furnace chamber, setting a substrate bias voltage, starting a target power supply, and performing bombardment cleaning on the target and the substrate surface; adjusting the bias voltage of the base material to a preset value, setting the sputtering power of the titanium target and the molybdenum target, controlling the content of Mo element by adjusting the power of the molybdenum target, and obtaining a Ti-Mo alloy film on the surface of the base material; and cooling the furnace to room temperature, and taking out the base material to obtain the beta-phase Ti-Mo alloy film with the BCC structure. The beta-phase Ti-Mo alloy film has smooth surface, compact structure and good film adhesion; the film has good thermodynamic stability and high equilibrium potential, thereby improving the corrosion resistance of the matrix material.

Description

Ti-Mo alloy film and preparation method thereof
Technical Field
The invention belongs to the technical field of alloy materials, relates to a Ti-Mo alloy film and also relates to a preparation method of the Ti-Mo alloy film.
Background
The titanium alloy has high specific strength, better corrosion resistance than stainless steel in humid atmosphere and seawater medium, and great development potential in the fields of ships and marine engineering equipment. In the current practical application, the titanium material used in the field of ships in China is very small, and accounts for no more than 1% of the total weight of the ships, because the cost is high due to the fact that the titanium material is used in large quantities. If a titanium alloy coating with a certain thickness can be prepared on the surface of a part, the corrosion resistance of the material can be improved, the service life of the part can be prolonged, and the cost increase caused by using a large amount of titanium materials can be avoided. Therefore, the preparation of the corrosion-resistant titanium alloy film is an effective way for effectively reducing the cost and improving the corrosion resistance of the material.
Titanium is a metal with a strong tendency to passivate, and a stable protective film of oxidizability is rapidly formed in air and in aqueous oxidizing or neutral solutions. In order to further improve the corrosion resistance of the titanium material in seawater, the corrosion resistance can be realized by changing the kinetic control factors of the corrosion process by adding alloy elements. The ligand field theory holds that the passivation phenomenon of transition metals is related to the combination of d-layer electron vacancies and oxygen to form a passivation film. For example, Cu does not have d-layer electron vacancies and does not exhibit a passive state; and Ta, Nb, Zr, Ni, Mo, Co, Cr and other metal elements can form alloy with titanium and have d-layer electron vacancies, so that the passive film of the titanium is strengthened. The Mo element can change the kinetic control factors of the titanium corrosion process, and can also be added into the titanium alloy as a thermodynamic stability element to form a beta-phase titanium alloy with a BCC structure, so that the corrosion resistance of the titanium alloy is improved. Therefore, the beta-phase Ti-Mo alloy is considered to be a more ideal corrosion-resistant material in the titanium alloy and has good mechanical properties. At present, a beta-phase Ti-Mo alloy film with a smooth surface and a compact structure is not obtained.
Disclosure of Invention
The invention aims to provide a Ti-Mo alloy film, which solves the problem that a beta-phase Ti-Mo alloy film with a smooth surface and a compact structure cannot be prepared in the prior art.
The technical scheme adopted by the invention is that the Ti-Mo alloy film comprises a Ti element and a Mo element, wherein the content of the Mo element is 20-40 wt%, and the grain size is 80-150 nm.
Another object of the present invention is to provide a method for preparing a Ti-Mo alloy thin film.
The technical scheme adopted by the invention is that the preparation method of the Ti-Mo alloy film comprises the following steps:
step 1, loading a titanium target material and a molybdenum target material into a target position of direct-current magnetron sputtering equipment, loading a base material into a workpiece frame, placing the workpiece frame in a furnace chamber, setting the rotating speed of the workpiece frame, and vacuumizing the furnace chamber;
step 2, introducing argon into the furnace chamber, setting a base material bias voltage, starting a target material power supply, and performing bombardment cleaning on the target material and the surface of the base material;
step 3, adjusting the bias voltage of the base material to a preset value, setting the sputtering power of the titanium target and the molybdenum target, controlling the content of Mo element by adjusting the power of the molybdenum target, and obtaining a Ti-Mo alloy film on the surface of the base material;
and 4, cooling the furnace to room temperature, and taking out the base material to obtain the Ti-Mo alloy film.
The air pressure value of the furnace chamber after vacuumizing in the step 1 is less than 3 multiplied by 10-3Pa, the rotating speed of the workpiece frame is 8-10 r/min. The purity of the titanium target and the molybdenum target is 99 percent.
In the step 2, the bias voltage of the base material is-400V to-350V, and the sputtering power of the target material during cleaning is as follows: the titanium target is 1500 +/-100W, and the molybdenum target is 130W.
In step 3, the bias voltage of the base material is-125V to-75V, and the sputtering power of the target material is as follows: the titanium target is 1500 +/-100W, and the molybdenum target is 80-130W.
The invention has the beneficial effects that: according to the Ti-Mo alloy film disclosed by the invention, the content of Mo element is 20-40 wt%, a beta-phase titanium alloy with a BCC structure is formed, the thermodynamic stability of the titanium alloy is improved, the equilibrium potential of the alloy is improved, the corrosion resistance of the titanium alloy is further improved, and the Ti-Mo alloy film has good mechanical properties. According to the preparation method of the Ti-Mo alloy film, the control of the components, the grain size and the density of the Ti-Mo alloy film can be realized through the control of the process parameters; the beta-phase Ti-Mo film material with nano-scale crystal grains can be obtained, and the surface is smooth, the structure is compact, and the film adhesion is good; the corrosion resistance is excellent in 3.5% NaCl electrolyte solution, and the service life of a workpiece in a corrosive medium can be effectively prolonged; the beta-phase Ti-Mo alloy film is prepared by adopting a magnetron sputtering technology, so that the corrosion resistance of the material can be effectively improved.
Drawings
FIG. 1 is a scanning electron microscope topography of the surface and the cross section of a Ti-20Mo alloy film obtained by the preparation method of the Ti-Mo alloy film of the invention;
FIG. 2 is a surface topography of a Ti-20Mo alloy film obtained by the method for preparing the Ti-Mo alloy film according to the present invention;
FIG. 3 is a scanning electron microscope topography of the surface and the cross section of the Ti-40Mo alloy film obtained by the preparation method of the Ti-Mo alloy film of the invention;
FIG. 4 is a surface topography of a Ti-40Mo alloy film obtained by the method for preparing the Ti-Mo alloy film according to the invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The Ti-Mo alloy film comprises a Ti element and a Mo element, wherein the content of the Mo element is 20-40 wt%, and the grain size is 80-150 nm.
The preparation method of the Ti-Mo alloy film comprises the following steps:
step 1, cleaning a workpiece (substrate) and a target material by using absolute ethyl alcohol, removing stains on the surfaces of the workpiece (substrate) and the target material, and drying for later use;
step 2, adopting four targets with the same target position to carry out contraposition placement, loading 2 titanium targets and 2 molybdenum targets into the target position of the direct current magnetron sputtering equipment, wherein the purity of the titanium targets and the molybdenum targets is 99%, loading the base material into a workpiece frame, placing the workpiece frame in a furnace chamber, setting the rotating speed of the workpiece frame to be 8-10 r/min, and then vacuumizing the furnace chamber until the air pressure value is less than 3 multiplied by 10-3Pa；
And 3, introducing high-purity argon with the flow of 20sccm into the furnace chamber, setting the bias voltage of the base material to be-400V-350V, starting a target power supply, performing bombardment cleaning on the target material and the surface of the base material for 15min, wherein the sputtering power of the target material during cleaning is as follows: the titanium target is 1500 +/-100W, and the molybdenum target is 130W.
Step 4, adjusting the bias voltage of the base material to-125V to-75V, setting the sputtering power of the titanium target to 1500 +/-100W, and controlling the content of Mo element by adjusting the power of the molybdenum target, wherein the content of Mo element and the sputtering power of the molybdenum target approximately accord with the following relational expression: mo (wt%) -0.416 xp-13.2, where P is the molybdenum target power in W. The sputtering power of the molybdenum target is set to be 80-130W, the content of Mo element is changed between 20% -40%, the sputtering time is determined according to the thickness of the film, and finally the Ti-Mo alloy film is obtained on the surface of the base material.
And 5, cooling the furnace to room temperature, and taking out the base material to obtain the Ti-Mo alloy film.
Through the mode, the preparation method of the Ti-Mo alloy film adopts the pure metal target material, can flexibly control the component proportion of the alloy film, and can prepare the beta-phase Ti-Mo alloy films with different Mo contents according to the actual requirement; by regulating and controlling the sputtering power, the titanium alloy film with nano-sized crystal grains can be obtained; by regulating and controlling the bias voltage of a workpiece (base material), a titanium alloy film with a smooth surface and a compact structure can be obtained; compared with a pure titanium film, the corrosion resistance of the material can be effectively improved.
Example 1
A (100) monocrystalline silicon wafer with the size of 10mm multiplied by 0.5mm is selected as a base material, two titanium targets and two molybdenum targets are used, four targets are placed in a contraposition mode by adopting the same target, and the rotating speed of a workpiece frame is set to be 8 r/min. Adjusting the bias voltage of the substrate to-100V; the sputtering power of the target material is as follows: 1500W of titanium target and 80W of molybdenum target; the sputtering time is 55min, and the material is taken out after cooling. The prepared film has the components of Ti-20Mo (wt%) shown in figure 1, the thickness of 1.9 μm, the grain size of about 95nm, uniform and compact surface, good combination with a silicon substrate and the surface roughness of only 3.95nm shown in figure 2. The corrosion current density was measured to be 1.862. mu.A/cm in a 3.5% NaCl solution2Corrosion current density of 1.684. mu.A/cm with bulk Ti-20Mo2Basically consistent with the corrosion current density value of 9.201 mu A/cm which is far lower than that of a pure titanium film2。
Example 2
A (100) monocrystalline silicon wafer with the size of 10mm multiplied by 0.5mm is selected as a base material, two titanium targets and two molybdenum targets are used, four targets are placed in a contraposition mode by adopting the same target, and the rotating speed of a workpiece frame is set to be 8 r/min. Adjusting the bias voltage of the substrate to-100V; the sputtering power of the target material is as follows: titanium target1500W, molybdenum target 130W; the sputtering time is 40min, and the material is taken out after cooling. The prepared film has the components of Ti-40Mo (wt%), as shown in figure 3, the thickness of 1.5 μm, the grain size of about 120nm, uniform and compact surface, good combination with a silicon substrate, and the surface roughness of only 3.33nm, as shown in figure 4. The corrosion current density was measured to be 1.585. mu.A/cm in a 3.5% NaCl solution2Far lower than the corrosion current density value of 9.201 mu A/cm of the pure titanium film2。

Claims (6)

  1. The Ti-Mo alloy film comprises a Ti element and a Mo element, and is characterized in that the content of the Mo element is 20-40 wt%, and the grain size is 80-150 nm.
  2. A preparation method of a Ti-Mo alloy film is characterized by comprising the following steps:
    step 1, loading a titanium target material and a molybdenum target material into a target position of direct-current magnetron sputtering equipment, loading a base material into a workpiece frame, placing the workpiece frame in a furnace chamber, setting the rotating speed of the workpiece frame, and vacuumizing the furnace chamber;
    step 2, introducing argon gas into the furnace chamber, setting a substrate bias voltage, starting a target power supply, and performing bombardment cleaning on the target and the substrate surface;
    step 3, adjusting the bias voltage of the base material to a preset value, setting the sputtering power of the titanium target and the molybdenum target, controlling the content of Mo element by adjusting the power of the molybdenum target, and obtaining a Ti-Mo alloy film on the surface of the base material;
    and 4, cooling the furnace to room temperature, and taking out the base material to obtain the Ti-Mo alloy film.
  3. 3. The method of claim 2, wherein the pressure in the furnace chamber after the evacuation in step 1 is less than 3X 10-3Pa, the rotating speed of the workpiece frame is 8-10 r/min.
  4. 4. The method of claim 2, wherein the purity of the titanium target and the molybdenum target is 99%.
  5. 5. The method for preparing a Ti-Mo alloy film according to claim 2, wherein in step 2, the bias voltage of the substrate is-400V to-350V, and the sputtering power of the target during cleaning is as follows: the titanium target is 1500 +/-100W, and the molybdenum target is 130W.
  6. 6. The method for preparing a Ti-Mo alloy film according to claim 2, wherein in step 3, the substrate bias is-125V to-75V, and the target sputtering power is: the titanium target is 1500 +/-100W, and the molybdenum target is 80-130W.
CN202210045084.5A 2022-01-14 2022-01-14 Ti-Mo alloy film and preparation method thereof Pending CN114540778A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005029862A (en) * 2003-07-10 2005-02-03 Hitachi Metals Ltd Sputtering target for thin film deposition
CN101360576A (en) * 2005-10-20 2009-02-04 H.C.施塔克公司 Methods of making molybdenum titanium sputtering plates and targets
CN102115872A (en) * 2009-12-30 2011-07-06 沈阳天贺新材料开发有限公司 Preparation method for magnetron sputtering TiMo film on titanium alloy surface
CN104602438A (en) * 2014-12-29 2015-05-06 中国原子能科学研究院 Preparation method of tritium impregnated target slice

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005029862A (en) * 2003-07-10 2005-02-03 Hitachi Metals Ltd Sputtering target for thin film deposition
CN101360576A (en) * 2005-10-20 2009-02-04 H.C.施塔克公司 Methods of making molybdenum titanium sputtering plates and targets
CN102115872A (en) * 2009-12-30 2011-07-06 沈阳天贺新材料开发有限公司 Preparation method for magnetron sputtering TiMo film on titanium alloy surface
CN104602438A (en) * 2014-12-29 2015-05-06 中国原子能科学研究院 Preparation method of tritium impregnated target slice

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
GANG LIU ET AL.: "The phase, morphology and surface characterization of Ti–Mo alloy films prepared by magnetron sputtering", RSC ADVANCES, no. 7, pages 52597 - 52598 *

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