CN114561622B - Gradient structure Ti-Nb alloy film and preparation method thereof - Google Patents
Gradient structure Ti-Nb alloy film and preparation method thereof Download PDFInfo
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- CN114561622B CN114561622B CN202210043689.0A CN202210043689A CN114561622B CN 114561622 B CN114561622 B CN 114561622B CN 202210043689 A CN202210043689 A CN 202210043689A CN 114561622 B CN114561622 B CN 114561622B
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- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000010936 titanium Substances 0.000 claims abstract description 32
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 230000008859 change Effects 0.000 claims abstract description 4
- 239000010955 niobium Substances 0.000 claims description 55
- 239000000758 substrate Substances 0.000 claims description 25
- 229910052758 niobium Inorganic materials 0.000 claims description 24
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 24
- 238000004544 sputter deposition Methods 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 13
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 9
- 230000007423 decrease Effects 0.000 abstract 1
- 239000000956 alloy Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 229910000734 martensite Inorganic materials 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
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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
- C23C14/06—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
-
- 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
- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
-
- 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
- C23C14/3492—Variation of parameters during 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/548—Controlling the composition
-
- 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
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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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)
Abstract
The invention discloses a gradient structure Ti-Nb alloy film and a preparation method thereof, wherein the gradient structure Ti-Nb alloy film comprises four layers of films with equal thickness, which are composed of Ti elements and Nb elements, the content of the Nb elements gradually decreases from outside to inside layer by layer, and the phase composition shows gradient change. The first layer of film from outside to inside is beta phase, the Nb element content is 30-34 at%, the second layer of film is beta phase or alpha+beta phase, the Nb element content is 21-26 at%, the third layer of film is +beta phase, the Nb element content is 14-17 at%, and the fourth layer of film is pure titanium; the grain size of the Ti-Nb alloy film is 70-130 nm. The performance advantages of titanium alloy film materials with different Nb contents can be combined, and the matching of mechanical properties and corrosion resistance can be achieved.
Description
Technical Field
The invention belongs to the technical field of alloy materials, relates to a gradient structure Ti-Nb alloy film and also relates to a preparation method of the gradient structure Ti-Nb alloy film.
Background
Ti-Nb alloy films have great application potential in the field of artificial implant materials due to good biocompatibility, high corrosion resistance, excellent superelasticity and nontoxicity, and are commonly used for surface modification of materials such as stainless steel, pure titanium, magnesium alloy and the like. In the titanium alloy, the alpha phase is of a HCP structure, the beta phase is of a BCC structure, and compared with the alpha phase and the alpha+beta phase titanium alloy, the beta phase titanium alloy has good mechanical property, corrosion resistance and better biocompatibility. With the increase of the content of the beta phase stabilizing element, the phase composition of the titanium alloy is changed from alpha phase to alpha+beta phase to beta phase, and the mechanical behavior and the corrosion resistance of the titanium alloy are also changed. The beta-phase Ti-Nb alloy film with high Nb content has high hardness and strong corrosion resistance and wear resistance; the beta phase or alpha+beta two-phase Ti-Nb alloy film with inferior Nb content generates superelasticity due to martensitic transformation; the Ti-Nb alloy film with low Nb content has an alpha+beta two-phase structure; pure titanium is an alpha phase and has better binding force with a substrate material of a HCP structure, for example, pure titanium or magnesium alloy is used as the substrate material. Therefore, how to combine the performance advantages of Ti-Nb alloy films or pure titanium film materials with different Nb contents to achieve the matching of mechanical properties and corrosion resistance becomes a difficult problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a gradient structure Ti-Nb alloy film, which solves the problem that the mechanical property and the corrosion resistance are difficult to match in the prior art.
The technical scheme adopted by the invention is that the gradient structure Ti-Nb alloy film comprises four layers of films with equal thickness composed of Ti element and Nb element, the content of the Nb element is gradually decreased from outside to inside layer by layer, and the phase composition shows gradient change. The first layer film from outside to inside is beta phase, the Nb element content is 30-34 at%, the second layer film is beta phase or alpha+beta phase, the Nb element content is 21-26 at%, the third layer film is alpha+beta phase, the Nb element content is 14-17 at%, and the fourth layer film is pure titanium; the grain size of the Ti-Nb alloy film is 70-130 nm.
The invention further aims to provide a preparation method of the gradient structure Ti-Nb alloy film.
The other technical scheme adopted by the invention is that the preparation method of the gradient structure Ti-Nb alloy film comprises the following steps:
Step 1, loading a titanium target and a niobium target into a target position of a direct current magnetron sputtering device, 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 substrate bias voltage, starting a target power supply, and carrying out bombardment cleaning on the surfaces of the target and the substrate;
step 3, regulating the substrate bias voltage to a preset value, setting sputtering power of a titanium target and a niobium target, controlling Nb element contents in different layers of the film by regulating the power of the niobium target, and performing layer-by-layer sputtering to obtain a gradient structure Ti-Nb alloy film on the surface of the substrate;
and step 4, cooling the furnace temperature to room temperature, and taking out the base material to obtain the Ti-Nb alloy film.
The air pressure value of the furnace chamber after the vacuum pumping in the step 1 is less than 3 multiplied by 10 -3 Pa, and the rotating speed of the workpiece frame is 8-10 r/min. The purity of the titanium target and the niobium target is 99.99 percent.
In the step 2, the substrate bias voltage is-400V, and the sputtering power of the target during cleaning is as follows: 1500+ -100W for titanium target, 220W for niobium target.
In the step 3, the substrate bias voltage is-125V to-75V, and the sputtering power of the target is as follows: titanium target 1500+ -100W, niobium target 130-220W of first layer to third layer film from outside to inside, niobium target 0W of fourth layer film.
The beneficial effects of the invention are as follows: the gradient structure Ti-Nb alloy film is of a four-layer equal-thickness gradient structure, the outermost layer is beta phase, the content of Nb element is 30-34 at%, the hardness is high, and the corrosion resistance and the wear resistance are strong; the secondary outer layer is beta phase or alpha+beta phase, the content of Nb element is 21-26 at%, and martensitic transformation is facilitated to generate superelasticity; the secondary inner layer is an alpha+beta phase, the Nb element content is 14-17 at%, and the secondary inner layer is used as a transition layer for coordinating the beta phase layer and the alpha phase layer; the innermost layer is alpha-phase pure titanium, and has better binding force for a substrate material of a HCP structure; the performance advantages of titanium alloy film materials with different Nb contents can be combined, and the matching of mechanical properties and corrosion resistance can be achieved. According to the preparation method of the gradient structure Ti-Nb alloy film, the pure metal target is adopted, so that the component proportion of the gradient structure alloy film can be flexibly controlled; the Ti-Nb alloy film with a smooth surface and a compact structure can be obtained by regulating and controlling the substrate bias voltage; compared with a single-component Ti-Nb film, the high-performance film material with good film base binding force and better matching mechanical property and corrosion resistance is beneficial to be obtained, so that the diversified requirements on the performance of the Ti-Nb alloy film material are met.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The gradient structure Ti-Nb alloy film comprises four layers of films with equal thickness, wherein the films consist of Ti element and Nb element, the content of the Nb element is gradually decreased from outside to inside layer by layer, and the phase composition shows gradient change; the first layer of film from outside to inside is beta phase, nb element content is 30-34 at%, the second layer of film is beta phase or alpha+beta phase, nb element content is 21-26 at%, the third layer of film is alpha+beta phase, nb element content is 14-17 at%, and the fourth layer of film is alpha phase, pure titanium; the grain size of the Ti-Nb alloy film is 70-130 nm.
The preparation method of the gradient structure Ti-Nb alloy film comprises the following steps:
Step 1, cleaning a base material and a target material by using absolute ethyl alcohol, removing stains on the surfaces of the base material and the target material, and drying for later use;
Step 2, adopting four targets to be placed in the same target alignment, loading 2 titanium targets and 2 niobium targets into the targets of the direct current magnetron sputtering equipment, wherein the purities of the titanium targets and the niobium targets are 99.99%, loading a 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 vacuumizing the furnace chamber until the air pressure value is less than 3X 10 -3 Pa;
Step 3, introducing high-purity argon with the flow of 20sccm into the furnace chamber, setting the bias voltage of the substrate to be-400V, starting a target power supply, and carrying out bombardment cleaning on the surfaces of the target and the substrate for 15min, wherein the sputtering power of the target during cleaning is as follows: 1500+ -100W for titanium target, 130W for niobium target.
And 4, adjusting the substrate bias voltage to-125V to-75V, setting the sputtering power of the titanium target to 1500+/-100W, and controlling the Nb element content by adjusting the power of the niobium target, wherein the Nb element content and the sputtering power of the niobium target approximately accord with the following relation: nb (at%) =0.243×p-17.81, where P is the niobium target power in W. The sputtering power of the niobium targets of the first layer to the third layer films is 130 to 220W, the Nb element is 30 to 34at percent, 21 to 26at percent and 14 to 17at percent from outside to inside in sequence, and the sputtering power of the niobium targets of the fourth layer film is 0W. And sputtering layer by layer to make the thickness of each layer equal, wherein the sputtering time is determined according to the thickness of the film, and finally obtaining the gradient structure Ti-Nb alloy film on the surface of the substrate.
And 5, cooling the furnace to room temperature, and taking out the base material to obtain the Ti-Nb alloy film.
Through the mode, the gradient structure Ti-Nb alloy film is a film with a 4-layer uniform thickness gradient structure, the outermost layer is beta phase, the Nb element content is 30-34 at%, the hardness is high, and the corrosion resistance and the wear resistance are strong; the secondary outer layer is beta phase or alpha+beta phase, the content of Nb element is 21-26 at%, and martensitic transformation is facilitated to generate superelasticity; the secondary inner layer is an alpha+beta phase, the Nb element content is 14-17 at%, and the secondary inner layer is used as a transition layer for coordinating the beta phase layer and the alpha phase layer; the innermost layer is alpha-phase pure titanium, and has better binding force for a substrate material of a HCP structure; the performance advantages of titanium alloy film materials with different Nb contents can be combined, and the matching of mechanical properties and corrosion resistance can be achieved. According to the preparation method of the gradient structure Ti-Nb alloy film, the pure metal target is adopted, so that the component proportion of the gradient structure alloy film can be flexibly controlled; the Ti-Nb alloy film with a smooth surface and a compact structure can be obtained by regulating and controlling the substrate bias voltage; compared with a single-component Ti-Nb film, the high-performance film material with good film base binding force and better matching mechanical property and corrosion resistance is beneficial to be obtained, so that the diversified requirements on the performance of the Ti-Nb alloy film material are met.
Examples
A (100) monocrystalline silicon wafer substrate material with the size of 10mm multiplied by 0.5mm is selected, and the silicon wafer is subjected to ultrasonic cleaning by absolute ethyl alcohol. Two titanium targets and two niobium targets are used, the four targets are placed in alignment with the same targets, and the rotating speed of the workpiece frame is set to be 10r/min. Adjusting the substrate bias to-100V; the sputtering power of the titanium target is as follows: 1500W; the sputtering power of the niobium target is set to be respectively, from the outside to the inside, a first layer 210W, a second layer 170W, a third layer 140W and a fourth layer 0W. The corresponding sputtering time is respectively 70min for the first layer, 72min for the second layer, 75min for the third layer and 90min for the fourth layer. And taking out after cooling. The components of the prepared film are from outside to inside: the first layer of Ti-33Nb (at%), the second layer of Ti-23Nb (at%), the third layer of Ti-15Nb (at%) and the fourth layer of pure titanium, wherein each layer of pure titanium has a thickness of about 2.5 mu m, the grain size of about 105nm, and the surface is uniform and compact, and is well combined with a silicon substrate.
Claims (2)
1. The gradient structure Ti-Nb alloy film is characterized by comprising four layers of films with equal thickness, wherein the films comprise Ti element and Nb element, the content of the Nb element is gradually decreased from outside to inside layer by layer, and the phase composition shows gradient change; the first layer of film from outside to inside is beta phase, the Nb element content is 30-34 at%, the second layer of film is beta phase or alpha+beta phase, the Nb element content is 21-26 at%, the third layer of film is alpha+beta phase, the Nb element content is 14-17 at%, and the fourth layer of film is pure titanium; the grain size of the Ti-Nb alloy film is 70-130 nm;
the preparation method of the gradient structure Ti-Nb alloy film comprises the following steps:
Step 1, loading a titanium target and a niobium target into a target position of a direct current magnetron sputtering device, 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 substrate bias voltage, starting a target power supply, and carrying out bombardment cleaning on the surfaces of the target and the substrate;
step 3, regulating the substrate bias voltage to a preset value, setting sputtering power of a titanium target and a niobium target, controlling Nb element contents in different layers of the film by regulating the power of the niobium target, and performing layer-by-layer sputtering to obtain a gradient structure Ti-Nb alloy film on the surface of the substrate;
step 4, cooling the furnace to room temperature, and taking out the base material to obtain a Ti-Nb alloy film;
In the step2, the substrate bias voltage is-400V, and the sputtering power of the target during cleaning is as follows: titanium target 1500±100W, niobium target 220W;
In the step3, the substrate bias voltage is minus 125V to minus 75V, and the sputtering power of the target is as follows: titanium target 1500+/-100W, niobium target 130-220W of the first layer to the third layer film from outside to inside, and niobium target 0W of the fourth layer film;
The air pressure value of the furnace chamber after the vacuum pumping in the step 1 is smaller than 3 multiplied by 10 -3 Pa, and the rotating speed of the workpiece frame is 8-10 r/min.
2. The gradient structure Ti-Nb alloy film according to claim 1, wherein the purity of the titanium target and the niobium target is 99.99%.
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Citations (8)
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| JP2001110751A (en) * | 1999-05-24 | 2001-04-20 | Lucent Technol Inc | Titanium-tantalum barrier thin film and formation method therefor |
| CN1321790A (en) * | 2000-04-28 | 2001-11-14 | 大连理工大学 | Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film |
| WO2002014576A1 (en) * | 2000-08-15 | 2002-02-21 | Honeywell International Inc. | Sputtering target |
| CN109207952A (en) * | 2018-10-25 | 2019-01-15 | 北京航空航天大学 | Using the method for high-throughput techniques preparation gradient Nb-Si base alloy film |
| CN109735869A (en) * | 2018-11-28 | 2019-05-10 | 清华大学 | A kind of corrosion-resistant conductive alloy film layer and its preparation method and application |
| CN109930124A (en) * | 2019-04-12 | 2019-06-25 | 大连理工大学 | One kind being applied to anti-corrosion Ti-Nb-Ta alloy film material of detecting head surface high-temperature electric conduction and preparation method thereof |
| CN110965024A (en) * | 2019-10-29 | 2020-04-07 | 南京航空航天大学 | Biomedical material and preparation method thereof |
| CN111979541A (en) * | 2020-08-21 | 2020-11-24 | 中南大学 | Titanium alloy with Ti-Nb alloy coating and preparation method and application thereof |
-
2022
- 2022-01-14 CN CN202210043689.0A patent/CN114561622B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001110751A (en) * | 1999-05-24 | 2001-04-20 | Lucent Technol Inc | Titanium-tantalum barrier thin film and formation method therefor |
| CN1321790A (en) * | 2000-04-28 | 2001-11-14 | 大连理工大学 | Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film |
| WO2002014576A1 (en) * | 2000-08-15 | 2002-02-21 | Honeywell International Inc. | Sputtering target |
| CN109207952A (en) * | 2018-10-25 | 2019-01-15 | 北京航空航天大学 | Using the method for high-throughput techniques preparation gradient Nb-Si base alloy film |
| CN109735869A (en) * | 2018-11-28 | 2019-05-10 | 清华大学 | A kind of corrosion-resistant conductive alloy film layer and its preparation method and application |
| CN109930124A (en) * | 2019-04-12 | 2019-06-25 | 大连理工大学 | One kind being applied to anti-corrosion Ti-Nb-Ta alloy film material of detecting head surface high-temperature electric conduction and preparation method thereof |
| CN110965024A (en) * | 2019-10-29 | 2020-04-07 | 南京航空航天大学 | Biomedical material and preparation method thereof |
| CN111979541A (en) * | 2020-08-21 | 2020-11-24 | 中南大学 | Titanium alloy with Ti-Nb alloy coating and preparation method and application thereof |
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