CN106756784A - Nb/NbN multilayer corrosion-resistant conductive film and preparation method thereof - Google Patents
Nb/NbN multilayer corrosion-resistant conductive film and preparation method thereof Download PDFInfo
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- CN106756784A CN106756784A CN201611215047.5A CN201611215047A CN106756784A CN 106756784 A CN106756784 A CN 106756784A CN 201611215047 A CN201611215047 A CN 201611215047A CN 106756784 A CN106756784 A CN 106756784A
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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
- C23C14/0641—Nitrides
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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
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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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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Abstract
The invention discloses a Nb/NbN multilayer corrosion-resistant conductive film and a preparation method thereof, and the Nb/NbN multilayer corrosion-resistant conductive film comprises Nb layers and NbN layers which are alternately deposited on a substrate, wherein the Nb layer is close to the substrate, the NbN layer is arranged on the outermost layer, and the interface phase at the junction of the Nb layer and the NbN layer is Nb with a hexagonal structure2N phase, the Nb layers alternating with NbN layers being deposited at least 10 times. The Nb/NbN multilayer film is adopted, and the layer close to the substrate is a metal Nb layer, so that the Nb/NbN multilayer film can be well combined with the substrate, and the good binding force of the film and the substrate is ensured; the multilayer structure of the film effectively blocks the path of corrosive medium entering the film, and the film mainly comprises NbN and Nb phases2The N phase and the Nb phase are corrosion-resistant phases, so that the corrosion resistance of the film is improved; conduction using metallic NbThe conductivity of the film is improved, the influence of the increase of the body resistance caused by excessive layers is avoided according to the multilayer film prepared by the process conditions, and the conductivity of the film is not influenced; the multi-layer film is deposited by utilizing the multi-arc ion plating technology, the working efficiency is improved, the process is simple and feasible, and the large-scale industrial production is facilitated.
Description
Technical field
It is anti-corrosion the present invention relates to ganoine thin film prepared by a kind of multi-arc ion coating, more particularly to a kind of Nb/NbN multilayers
Conductive film and preparation method thereof.
Background technology
Multi-arc ion coating has the spy that ionization level is high, film forming speed is fast as one kind of physical vapour deposition (PVD) (PVD) technology
Point, can obtain outstanding, the homogeneous ganoine thin film of film-substrate cohesion, be compared to magnetron sputtering, be more beneficial for extensive
Industrialized production, it is cost-effective, it is one of surface peening means for being widely used now.
Transition metal nitride ganoine thin film has had developing history very long because its high rigidity, friction resistant ability high,
It is rotten that the features such as outstanding high-temperature stability and good chemical stability, is widely used in machine-building, Tool in Cutting, ocean
The every field such as erosion, wherein multi-element film again with TiN, CrN and based on this is most commonly seen.
Compared to common individual layer ganoine thin film, the ganoine thin film with sandwich construction is often because of the compound action of its structure
Embody more superior performance.Wu Bo et al. is plated in bipolar plate of stainless steel surface by arc ions, and to be prepared for CrN respectively mono-
Tunic, Cr/CrN duplicatures and Cr/CrN/Cr sandwich structure films, compare its corrosion resistance and electric conductivity, find sandwich knot
The film of structure is advantageous on properties.Thus, it is to improve film corrosion resistance and electric conductivity one kind to have to prepare multilayer hard
The method of effect.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of Nb/NbN multilayers corrosion-resistant conductive film and
Its preparation method, the decay resistance and electric conductivity of film are improve using sandwich construction.
The present invention is achieved by the following technical solutions, and the present invention includes the Nb on matrix layers and NbN of alternating deposit
Layer, near matrix is Nb layers, and outermost layer is NbN layers, and described Nb layers is mutually hexagonal structure with the interface of NbN layers of intersection
Nb2N phases, described Nb layers with NbN layers of alternating deposit at least 10 times.
As one of preferred embodiment of the invention, described Nb layers with NbN layers of alternating deposit 10~20 times.Alternating deposit number of times
It is too small can be because of the excessively thin influence corrosion resistance of film；Alternating deposit number of times is crossed at most because internal stress increase and bulk resistance increase influence film
Base junction is made a concerted effort and electric conductivity.
The thickness of the film is 1.2~1.8 μm.The thickness of film is able to ensure that electric conductivity and corrosion resistance.
Used as one of preferred embodiment of the invention, each Nb layers of thickness is 50.5~78.5nm in the film, each
NbN layers of thickness is 39.5~61.5nm.
As one of preferred embodiment of the invention, according to atomicity percentages, including Nb50~65% in the film,
N35~50%.
A kind of preparation method of Nb/NbN multilayers corrosion-resistant conductive film, comprises the following steps：
(1) vacuum chamber is put into after matrix ultrasonic wave is cleaned, then argon ion bombardment cleaning is carried out to matrix,；
(2) metal Nb targets are opened, Nb layers is deposited, sedimentation time is 8~10min, completes single Nb layers deposition；
(3) holding substrate temperature, bias, partial pressure, pivoted frame speed are constant, and Ar throughputs reduce to 15~25sccm, plus
Nitrogen charging throughput is 280~300sccm, deposits NbN layers, and sedimentation time is 7~9min, completes single NbN layers deposition；
(4) repeat step (2) and step (3), Nb layers and NbN layers on alternating deposit on base material.
In the step (1), vacuum is 2 × 10-3Pa~3.5 × 10-3Pa, argon flow amount is 80~100sccm, argon
The Ion Cleaning time is 5~20min, and pressure is 0.2Pa, and back bias voltage is 700~1000V, and substrate temperature is 300~350 DEG C, is turned
Frame speed is 3~5 turns/min.
In the step (2), the condition of Nb layers of deposition is：Keep substrate temperature at 300~350 DEG C, argon flow amount is reduced to
50~60sccm, partial pressure is 0.4~0.5Pa, and it is 80~100V to bias, and pivoted frame speed is 2~5 turns/min.
Alternate cycles 10~20 times, total time is 150~180min, completes Nb layers with the NbN layers of deposition on matrix.
NbN films are influenceed by metal Nb compact structures, and compared with the film such as TiN, CrN, film surface is more smooth
Densification, particle is smaller, it is possible to prevente effectively from corrosive medium enters inside film, so as to improve the decay resistance of film.
The content of Nb and N is controlled, Nb metallic voids can be reduced, corrosion resistance can be improved, Nb layers can have preferably
Electric conductivity.The appropriate deposition number of plies, disclosure satisfy that the requirement of corrosion resistance.
The present invention has advantages below compared to existing technology：The present invention uses Nb/NbN plural layers, and nearly base layer is gold
Nb layers of category, can be with matrix good combination, it is ensured that film and the good adhesion of matrix；Film multi-layer structures effectively hinder
The path that corrosive medium enters inside film, and film mainly constitutes phase NbN, Nb2N and Nb phases are corrosion-resistant phase, improve
The decay resistance of film；The electric conductivity of film is improve using the electric conductivity of metal Nb, according to process conditions prepare it is many
Layer film, it is to avoid because the number of plies excessively makes the increased influence of bulk resistance, it is ensured that film conductivity is unaffected；Using many
Arc ion plating technique deposits plural layers, improves operating efficiency, simple for process, is conducive to large-scale industrial production.
Brief description of the drawings
Fig. 1 is Nb/NbN multi-layer film structures schematic diagram obtained in the present invention；
Fig. 2 is Nb/NbN plural layers obtained by embodiment 1 in 10%H2SO4Tafel polarization curves in solution.
Specific embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed implementation method and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
Stainless steel base after polishing is respectively washed 15min by acetone and alcohol, vacuum chamber pivoted frame is put into after drying
On pallet.Open vavuum pump and the base vacuum of vacuum chamber is extracted into 3 × 10-3Pa, vacuum room temperature rises to 300 DEG C.Open Ar gas
Holding flow is 100sccm, and pressure is adjusted to 0.2Pa, and back bias voltage is adjusted to 700V, and pivoted frame speed is 3 turns/min, and matrix surface is entered
Row Ions Bombardment 10min, removes surface irregularities and oxide layer；Vacuum degree in vacuum chamber and temperature-resistant is kept, Ar throughputs are subtracted
To 60sccm, pressure rises to 0.4Pa, and bias is adjusted to 80V, and pivoted frame speed is 2 turns/min, opens 4 pieces of Nb targets, and target current is
200A, Nb single thin films are deposited in matrix surface, and sedimentation time is 9 minutes；Keep vacuum, temperature, gas pressure intensity, bias,
Pivoted frame speed, target current are constant, and Ar throughputs are reduced into 20sccm, plus filling N2 makes flow reach 280sccm, in Nb single thin films
Upper deposition NbN films, sedimentation time is 7min；Nb single thin films and NbN thin-film techniques parameter totally 10 times are repeated, Nb/NbN is obtained
Plural layers；Process cycles terminate rear coupons and cool to room temperature with the furnace, open vacuum chamber room door, take out print.
Embodiment 2
Matrix after polishing is respectively washed 15min by acetone and alcohol, is put into after drying on vacuum chamber pivoted frame pallet.
Open vavuum pump and the base vacuum of vacuum chamber is extracted into 2 × 10-3Pa, vacuum room temperature rises to 350 DEG C.Open Ar gas and keep flow
It is 180sccm, pressure is adjusted to 0.2Pa, and back bias voltage is adjusted to 1000V, and pivoted frame speed is 5 turns/min, and ion is carried out to matrix surface
Bombardment 20min, removes surface irregularities and oxide layer；Vacuum degree in vacuum chamber and temperature-resistant is kept, Ar throughputs are reduced to
50sccm, pressure rises to 0.5Pa, and bias is adjusted to 100V, and pivoted frame speed is 5 turns/min, opens 4 pieces of Nb targets, and target current is
200A, Nb single thin films are deposited in matrix surface, and sedimentation time is 8 minutes；Keep vacuum, temperature, gas pressure intensity, bias,
Pivoted frame speed, target current are constant, and Ar throughputs are reduced into 25sccm, plus filling N2 makes flow reach 300sccm, in Nb single thin films
Upper deposition NbN films, sedimentation time is 9min；Nb single thin films and NbN thin-film techniques parameter totally 15 times are repeated, Nb/NbN is obtained
Plural layers；Process cycles terminate rear coupons and cool to room temperature with the furnace, open vacuum chamber room door, take out print.
Embodiment 3
In the present embodiment, Nb single thin films sedimentation time is 4.5min, and NbN single thin films sedimentation time is 3.5min, weight
Multiple Nb single thin films and NbN thin-film techniques parameter totally 20 times, obtain Nb/NbN plural layers.Other technological processes and parameter and reality
Apply example 1 identical.
As shown in figure 1, wherein near matrix is Nb layers, outermost layer is NbN layers for the structure of gained Nb/NbN plural layers.
Electro-chemical test is carried out to embodiment 1,2 gained Nb/NbN plural layers and stainless steel base, is tested 10%
H2SO4Carried out under the conditions of solution room temperature.Test gained Tafel polarization curves as shown in Fig. 2 fitting data as shown in table 1, as a result
Show, the film corrosion potential E of embodiment 1corr=0.003V, corrosion current icorr=2.43 × 10-6A·cm-2, polarization electricity
Resistance Rp=1.78 × 104Ω·cm2, the film corrosion potential E of embodiment 3corr=-0.022V, corrosion current icorr=2.40
×10-6A·cm-2, polarization resistance Rp=1.53 × 104Ω·cm2.Embodiment gained film is certainly rotten compared with stainless steel base
Erosion electric current improves an order of magnitude with polarization resistance, and corrosion potential also has very big lifting, enhances the corrosion resisting property of matrix.
The embodiment Tafel of table 1 polarization test fitting data
Contact resistance (ICR) test, any 3rd area of piece of materialsing are carried out to gained Nb/NbN plural layers in embodiment 1,3
Domain, acquired results are as shown in table 2.Embodiment 1 is in 78.5Ncm-2Under pressure, average area resistance is 18.317m Ω cm2,
In 117.75Ncm-2Under pressure, average area resistance 12.102m Ω cm2；Embodiment 3 is in 78.5Ncm-2Under pressure, put down
Equal area resistance is 20.934m Ω cm2, in 117.75Ncm-2Under pressure, average area resistance 13.410m Ω cm2, with
Stainless steel base compares (ICR is substantially improved under the same conditions(78.5N·cm-2)＞ 200m Ω cm2, ICR(117.75N·cm-2)
＞ 150m Ω cm2)。
The Nb/NbN plural layers contact resistance of table 2 is tested
Comparative example 1 and 3, and 9min and 7min, Nb single thin film and NbN are respectively when Nb the and NbN monolayer deposition times
During thin-film technique parameter cyclic 10 times, the corrosion resistance and electric conductivity of film layer are optimal, therefore, the technological parameter corresponding to embodiment 1
It is optimum process.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (9)
1. a kind of Nb/NbN multilayers corrosion-resistant conductive film, it is characterised in that Nb layers including alternating deposit on matrix and NbN
Layer, near matrix is Nb layers, and outermost layer is NbN layers, and described Nb layers is mutually hexagonal structure with the interface of NbN layers of intersection
Nb2N phases, described Nb layers with NbN layers of alternating deposit at least 10 times.
2. a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 1, it is characterised in that described Nb layers and NbN
Layer alternating deposit 10~20 times.
3. a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 1, it is characterised in that the thickness of the film
It is 1.2~1.8 μm.
4. a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 1, it is characterised in that in the film each
Nb layers of thickness is 50.5~78.5nm, and each NbN layers of thickness is 39.5~61.5nm.
5. a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 1, it is characterised in that in the film according to
Atomicity percentages, including Nb50~65%, N35~50%.
6. a kind of preparation method of the Nb/NbN multilayers corrosion-resistant conductive film as described in any one of Claims 1 to 5, its feature exists
In comprising the following steps：
(1) vacuum chamber is put into after matrix ultrasonic wave is cleaned, then argon ion bombardment cleaning is carried out to matrix,；
(2) metal Nb targets are opened, Nb layers is deposited, sedimentation time is 8~10min, completes single Nb layers deposition；
(3) holding substrate temperature, bias, partial pressure, pivoted frame speed are constant, and Ar throughputs reduce to 15~25sccm, plus nitrogen charging
Throughput is 280~300sccm, deposits NbN layers, and sedimentation time is 7~9min, completes single NbN layers deposition；
(4) repeat step (2) and step (3), Nb layers and NbN layers on alternating deposit on base material.
7. the preparation method of a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 6, it is characterised in that described
In step (1), vacuum is 2 × 10-3Pa~3.5 × 10-3Pa, argon flow amount is 80~100sccm, argon ion scavenging period
It is 5~20min, pressure is 0.2Pa, and back bias voltage is 700~1000V, and substrate temperature is 300~350 DEG C, and pivoted frame speed is 3~5
Turn/min.
8. the preparation method of a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 6, it is characterised in that described
In step (2), the condition of Nb layers of deposition is：Keep substrate temperature at 300~350 DEG C, argon flow amount reduces to 50~60sccm, gas
Body partial pressure is 0.4~0.5Pa, and it is 80~100V to bias, and pivoted frame speed is 2~5 turns/min.
9. the preparation method of a kind of Nb/NbN multilayers corrosion-resistant conductive film according to claim 6, it is characterised in that alternately
Circulation 10~20 times, total time is 150~180min, completes Nb layers with the NbN layers of deposition on matrix.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254032A (en) * | 1999-11-24 | 2000-05-24 | 上海交通大学 | Superhard nanometer multi-layer film and its making process |
| US20070128829A1 (en) * | 2005-12-01 | 2007-06-07 | National Institute Of Information And Communications Technology, Incorporated | Method for fabricating thin layer device |
| KR100884610B1 (en) * | 2008-07-18 | 2009-02-23 | 한국과학기술연구원 | Multilayer structure having high spin injection ratio using conductive nitride as a spacer and the fabrication method thereof |
-
2016
- 2016-12-26 CN CN201611215047.5A patent/CN106756784B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254032A (en) * | 1999-11-24 | 2000-05-24 | 上海交通大学 | Superhard nanometer multi-layer film and its making process |
| US20070128829A1 (en) * | 2005-12-01 | 2007-06-07 | National Institute Of Information And Communications Technology, Incorporated | Method for fabricating thin layer device |
| KR100884610B1 (en) * | 2008-07-18 | 2009-02-23 | 한국과학기술연구원 | Multilayer structure having high spin injection ratio using conductive nitride as a spacer and the fabrication method thereof |
Non-Patent Citations (1)
| Title |
|---|
| RUIZ, E. ET AL: "Tribocorrosion Behaviour of Niobium Nitride/Niobium Multilayer in Contact with Ringer Lactate", 《INTERNATIONAL JOURNAL OF ELECTROCHEMICAL SCIENCE》 * |
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