CN105887013A - Preparation method of titanium-zirconium nitride metal film for surface modification of nickel-titanium root canal file - Google Patents
Preparation method of titanium-zirconium nitride metal film for surface modification of nickel-titanium root canal file Download PDFInfo
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- CN105887013A CN105887013A CN201610404205.5A CN201610404205A CN105887013A CN 105887013 A CN105887013 A CN 105887013A CN 201610404205 A CN201610404205 A CN 201610404205A CN 105887013 A CN105887013 A CN 105887013A
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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
- C23C14/0021—Reactive sputtering or evaporation
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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
- C23C14/22—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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- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/347—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with layers adapted for cutting tools or wear applications
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Abstract
The invention discloses a preparation method of a titanium-zirconium nitride metal film for surface modification of a nickel-titanium root canal file and relates to a preparation method of a metal film. According to the method, the surface of the nickel-titanium root canal file is covered with the TiZrN film in a plated mode, outdiffusion of nickel (Ni) ions in the nickel-titanium root canal file can be effectively inhibited, the target composition, quantity and arrangement direction are determined, it is determined that a commercial high-purity titanium-zirconium alloy target is used as an arc source, a pretreatment process and a deposition process for workpieces are determined, the hardness and corrosion resistance of the surface of the nickel-titanium root canal file are improved on the basis of basically keeping original elasticity of the nickel-titanium root canal file, and therefore the use performance of the nickel-titanium root canal file can be effectively improved. The surface hardness and thickness of a film layer are guaranteed, outdiffusion of nickel (Ni) in the nickel-titanium root canal file is effectively inhibited, original elasticity of the nickel-titanium root canal file is maintained, and the corrosion resistance of the surface of the nickel-titanium root canal file is improved.
Description
Technical field
The present invention relates to the preparation method of a kind of metal film, particularly relate to the titanium zirconium for nickel-titanium instruments surface modification
The preparation method of nitrided metal film.
Background technology
Nitinol is widely used in the fields such as root canal therapy device, repair materials, implantation body and orthodontic bow-wire.NiTi
Root canal appliance has super-elasticity and superior formative memory ability, it has also become the first-selection of dental clinic root canal preparation.Nitinol
Apparatus can make root pipe keep original anatomic form when root canal preparation, still can prepare formation swimmingly for crooked root tube
Preferably tapering, decreases the formation of step and the risk of apical transportation, and can improve therapeutic efficiency.In recent years, according to horizontal stroke
The shape of section, tapering, surface process, the quantity of screw thread and the difference of cutting angle, had various different NiTi instruments
In root canal.
It is presently used for the NiTi instruments of root canal and is primarily present following shortcoming: case hardness is relatively low, nickel in root canal
The release of ion separates out, in NaOCl solution, decay resistance is strong, fracture in root canal.
Multi-arc ion coating is a kind of physical vacuum deposition technique being provided with multiple cathodic arc evaporation source that can simultaneously evaporate, tool
There are the distinguishing features such as deposition velocity is fast, morphology is fine and close, adhesive force is strong, uniformity is good.It is anti-that this technology is applicable to polynary hard
Answer the preparation of film, and obtain in terms of the preparation of the hard reaction film of titanium nitride, TiAlN, titanium nitride zirconium and more multicomponent
Successful Application.
Multi-arc ion coating titanium nitride zirconium film used by processing manufacturing industry is typically with high-speed steel and hard alloy as matrix, in plating
In membrane process, higher deposition temperature, bigger bias is generally used to carry out Bombardment and cleaning, for improving wearability and service life, film
Layer thickness is typically more than 2 microns.
Summary of the invention
It is an object of the invention to provide the system of a kind of titanium zirconium nitride metal film for nickel-titanium instruments surface modification
Preparation Method, the method is at one layer of TiZrN film of nickel-titanium instruments coating surface, it is possible to the effectively nickel (Ni) in suppression nickel-titanium instruments
Ion, to external diffusion, on the basis of the basic holding original elasticity of nickel-titanium instruments, improves the hardness on nickel-titanium instruments surface
And corrosion resistance, it is thus possible to it is effectively improved the serviceability of nickel-titanium instruments.
It is an object of the invention to be achieved through the following technical solutions:
Preparation method of the present invention includes successively:
1, deposition technique and the determination of target material composition: determining the multi-arc ion coating technology of preparing as TiZrN film, arc source target is equal
For the titanium-zirconium alloy target of purity 99.99%, the atomic ratio of titanium-zirconium alloy target is Ti:Zr=50:50.
2, the determination of arc source number: require according to membrane uniformity and coating chamber temperature limiting determines to be used many
Arc ion plating arc source number, i.e. for ensureing nickel-titanium instruments surface uniform plating titanium zirconium nitride film, at least select two differences
The arc sources starting the arc simultaneously deposition of orientation and one-tenth 90 degree configuration, and the whole process that nickel-titanium instruments to be ensured is in coating chamber
In, coating chamber temperature is less than 200 ° of C.
3, the pre-treatment of nickel-titanium instruments: select medical nickel-titanium instruments, before putting it into coating chamber and carrying out plated film, point
Not carrying out ultrasonic waves for cleaning with ethanol and distilled water, hair dryer slowly dries up, and is subsequently placed on the work rest of coating chamber.
4, the determination of pre-Bombardment and cleaning technique: refer to nickel-titanium instruments multi-arc ion coating before depositing Ti ZrN film
Icon bombardment cleaning technique under technology, pre-Bombardment and cleaning technique is divided into four steps to realize, and coating chamber evacuation is gone forward side by side by the first step
Row is slowly heated baking, makes back end vacuum reach 8.0 10-3More than handkerchief, temperature reach 100 ° of C；Second step, is filled with argon, makes
Coating chamber vacuum reaches 2.0 10-1To 2.3 10-1Between handkerchief, opening arc source, keep arc current at 50 amperes, bombardment is negative
Bias is-350 volts, carries out ion bom bardment, stops ion bom bardment, stop argon stream simultaneously after coating chamber temperature reaches 150 ° of C
Enter；3rd step, continues coating chamber evacuation, when coating chamber temperature returns to 100 ° of C, repeats the process of second step；4th
Step, the process of repetition the 3rd step 2 ~ 3 times.
5, the determination of depositing operation: refer to use multi sphere ion plating technology to prepare TiZrN film on nickel-titanium instruments surface
Depositing operation, coating process is divided into two stages, the first step, the deposition of TiZr alloy transition layer, i.e. by the argon in coating chamber
Air pressure is maintained at by force 2.0 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is placed in 45 ~ 50 amperes, and deposition back bias voltage is-130
~ 150 volts, start deposition, sedimentation time 3 minutes；Second step, adjusts argon flow amount so that it is partial pressure reaches 0.8 10-1Handkerchief, with
Time in coating chamber, be passed through nitrogen, make mixed gas total pressure reach 2.5 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is equal
Being placed in 45 ~ 50 amperes, deposition back bias voltage is set as-100 ~ 110 volts, starts deposition, after 5 minutes, increases nitrogen flow, makes mixing
Gas total pressure is increased to 3.0 10-1Handkerchief, the arc current in holding titanium-zirconium alloy target arc source is constant simultaneously, deposition back bias voltage is constant,
Continue deposition, 12 ~ 15 minutes time, and keep coating chamber temperature less than 200 ° of C.
6, work rest rotates: is slowly heated baking at coating chamber evacuation carrying out, nickel-titanium instruments carries out ion bangs
Hit, TiZr alloy transition layer deposition, TiZrN film deposition whole during be always maintained at work rest rotate, rotating speed is 6 revs/min
Clock.
According to the proposed by the invention TiZrN film for nickel-titanium instruments surface modification using titanium-zirconium alloy target to prepare
Preparation method, it is possible to obtain above-mentioned TiZrN film, this TiZrN film can suppress the nickel (Ni) in nickel-titanium instruments to extending out
Dissipate, keep the original elasticity of nickel-titanium instruments to be basically unchanged, improve the hardness on nickel-titanium instruments surface, wearability and anticorrosive
Property, and the service life of nickel-titanium instruments can be effectively improved.
Advantages of the present invention with effect is:
Target material composition, quantity and configuration orientation are present invention determine that, it is determined that commercial high-purity titanium zircaloy target is as arc source, really
Determine workpiece pre-treating technology and depositing operation, it is ensured that the hardness of film surface, thicknesses of layers, effectively inhibit NiTi root pipe
Nickel (Ni) in file, to external diffusion, maintains original elasticity of nickel-titanium instruments, improves the corrosion-resistant of nickel-titanium instruments surface
Property.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
In medical nickel-titanium instruments (S series, specification SX, length 19mm) coating surface titanium zirconium nitride (TiZrN) film, its method
It is:
1, deposition technique and the determination of target material composition: determining the multi-arc ion coating technology of preparing as TiZrN film, arc source target is equal
For the titanium-zirconium alloy target of purity 99.99%, the atomic ratio of titanium-zirconium alloy target is Ti:Zr=50:50.
2, the determination of arc source number: select two different azimuth and become the arc source starting the arc simultaneously deposition of 90 degree of configurations, simultaneously
During ensureing whole in coating chamber of nickel-titanium instruments, coating chamber temperature is less than 200 ° of C.
3, the pre-treatment of nickel-titanium instruments: select medical nickel-titanium instruments (S series, specification SX, length 19mm), by it
Putting into before coating chamber carries out plated film, carry out ultrasonic waves for cleaning with ethanol and distilled water respectively, hair dryer slowly dries up, and is subsequently placed in
On the work rest of coating chamber.
4, the determination of pre-Bombardment and cleaning technique: refer to nickel-titanium instruments multi-arc ion coating before depositing Ti ZrN film
Icon bombardment cleaning technique under technology, pre-Bombardment and cleaning technique is divided into four steps to realize, and coating chamber evacuation is gone forward side by side by the first step
Row is slowly heated baking, makes back end vacuum reach 7.8 10-3Handkerchief, temperature reach 100 ° of C；Second step, is filled with argon, makes plated film
Room vacuum reaches 2.0 10-1Handkerchief, opens arc source, keeps arc current at 50 amperes, and bombardment back bias voltage is-350 volts, carries out ion
Bombardment, stops ion bom bardment after coating chamber temperature reaches 150 ° of C, stops argon simultaneously and flows into；3rd step, continues coating chamber
Evacuation, when coating chamber temperature returns to 100 ° of C, repeats the process of second step；4th step, the process of repetition the 3rd step 2 times.
5, the determination of depositing operation: refer to use multi sphere ion plating technology to prepare TiZrN film on nickel-titanium instruments surface
Depositing operation, coating process is divided into two stages, the first step, the deposition of TiZr alloy transition layer, i.e. by the argon in coating chamber
Air pressure is maintained at by force 2.0 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is placed in 45 amperes, and deposition back bias voltage is-130 volts,
Start deposition, sedimentation time 3 minutes；Second step, adjusts argon flow amount so that it is partial pressure reaches 0.8 10-1Handkerchief, simultaneously to plating
Film indoor are passed through nitrogen, make mixed gas total pressure reach 2.5 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is placed in 50
Ampere, deposition back bias voltage is set as-100 volts, starts deposition, after 5 minutes, increases nitrogen flow, makes mixed gas total pressure liter
High to 3.0 10-1Handkerchief, the arc current in holding titanium-zirconium alloy target arc source is constant simultaneously, deposition back bias voltage is constant, continues deposition, time
Between 12 minutes, and keep coating chamber temperature less than 200 ° of C.
6, work rest rotates: is slowly heated baking at coating chamber evacuation carrying out, nickel-titanium instruments carries out ion bangs
Hit, TiZr alloy transition layer deposition, TiZrN film deposition whole during be always maintained at work rest rotate, rotating speed is 6 revs/min
Clock.
To making the TiZrN film prepared in aforementioned manners test, this TiZrN film is firmly combined with nickel-titanium instruments, film
Layer thickness is 0.4 micron, covers complete, it is possible to the nickel after external diffusion, plated film of nickel (Ni) ion in suppression nickel-titanium instruments
Titanium root canal file anti-folding number of times reaches the 98% of original non-plated film nickel-titanium instruments, and the nickel-titanium instruments case hardness after plated film reaches
HV2350, the corrosion resistance in NaOCl solution improves, and pitting potential is higher than uncoated nickel-titanium instruments, and is easily formed
Secondary passivity district.
Embodiment 2
In medical nickel-titanium instruments (F series, specification F2, length 21mm) coating surface titanium zirconium nitride (TiZrN) film, its method
It is:
1, deposition technique and the determination of target material composition: determining the multi-arc ion coating technology of preparing as TiZrN film, arc source target is equal
For the titanium-zirconium alloy target of purity 99.99%, the atomic ratio of titanium-zirconium alloy target is Ti:Zr=50:50.
2, the determination of arc source number: select two different azimuth and become the arc source starting the arc simultaneously deposition of 90 degree of configurations, simultaneously
During ensureing whole in coating chamber of nickel-titanium instruments, coating chamber temperature is less than 200 ° of C.
3, the pre-treatment of nickel-titanium instruments: select medical nickel-titanium instruments (F series, specification F2, length 21mm), by it
Putting into before coating chamber carries out plated film, carry out ultrasonic waves for cleaning with ethanol and distilled water respectively, hair dryer slowly dries up, and is subsequently placed in
On the work rest of coating chamber.
4, the determination of pre-Bombardment and cleaning technique: refer to nickel-titanium instruments multi-arc ion coating before depositing Ti ZrN film
Icon bombardment cleaning technique under technology, pre-Bombardment and cleaning technique is divided into four steps to realize, and coating chamber evacuation is gone forward side by side by the first step
Row is slowly heated baking, makes back end vacuum reach 7.8 10-3Handkerchief, temperature reach 100 ° of C；Second step, is filled with argon, makes plated film
Room vacuum reaches 2.0 10-1Handkerchief, opens arc source, keeps arc current at 50 amperes, and bombardment back bias voltage is-350 volts, carries out ion
Bombardment, stops ion bom bardment after coating chamber temperature reaches 150 ° of C, stops argon simultaneously and flows into；3rd step, continues coating chamber
Evacuation, when coating chamber temperature returns to 100 ° of C, repeats the process of second step；4th step, the process of repetition the 3rd step 3 times.
5, the determination of depositing operation: refer to use multi sphere ion plating technology to prepare TiZrN film on nickel-titanium instruments surface
Depositing operation, coating process is divided into two stages, the first step, the deposition of TiZr alloy transition layer, i.e. by the argon in coating chamber
Air pressure is maintained at by force 2.0 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is placed in 50 amperes, and deposition back bias voltage is-150 volts,
Start deposition, sedimentation time 3 minutes；Second step, adjusts argon flow amount so that it is partial pressure reaches 0.8 10-1Handkerchief, simultaneously to plating
Film indoor are passed through nitrogen, make mixed gas total pressure reach 2.5 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is placed in 45
Ampere, deposition back bias voltage is set as-110 volts, starts deposition, after 5 minutes, increases nitrogen flow, makes mixed gas total pressure liter
High to 3.0 10-1Handkerchief, the arc current in holding titanium-zirconium alloy target arc source is constant simultaneously, deposition back bias voltage is constant, continues deposition, time
Between 15 minutes, and keep coating chamber temperature less than 200 ° of C.
6, work rest rotates: is slowly heated baking at coating chamber evacuation carrying out, nickel-titanium instruments carries out ion bangs
Hit, TiZr alloy transition layer deposition, TiZrN film deposition whole during be always maintained at work rest rotate, rotating speed is 6 revs/min
Clock.
To making the TiZrN film prepared in aforementioned manners test, this TiZrN film is firmly combined with nickel-titanium instruments, film
Layer thickness is 0.5 micron, covers complete, it is possible to the nickel after external diffusion, plated film of nickel (Ni) ion in suppression nickel-titanium instruments
Titanium root canal file anti-folding number of times reaches the 96% of original non-plated film nickel-titanium instruments, and the nickel-titanium instruments case hardness after plated film reaches
HV2450, the corrosion resistance in NaOCl solution improves, and pitting potential is higher than uncoated nickel-titanium instruments, and is easily formed
Secondary passivity district.
Claims (4)
1. it is used for the preparation method of the titanium zirconium nitride metal film of nickel-titanium instruments surface modification, it is characterised in that described method
Including procedure below:
Preparation method of the present invention includes successively:
The determination of a, deposition technique and target material composition: determining the multi-arc ion coating preparation scheme as TiZrN film, arc source target is equal
For the titanium-zirconium alloy target of purity 99.99%, the atomic ratio of titanium-zirconium alloy target is Ti:Zr=50:50；
B, the determination of arc source number: according to membrane uniformity require and coating chamber temperature limiting determine multi sphere to be used from
Son plating arc source number；
C, the pre-treatment of nickel-titanium instruments: select medical nickel-titanium instruments, before putting it into coating chamber and carrying out plated film, use respectively
Ethanol and distilled water carry out ultrasonic waves for cleaning, and hair dryer slowly dries up, and is subsequently placed on the work rest of coating chamber；
D, the determination of pre-Bombardment and cleaning technique: refer to nickel-titanium instruments multi sphere ion plating technology before depositing Ti ZrN film
Under icon bombardment cleaning technique；
E, the determination of depositing operation: refer to use multi sphere ion plating technology to prepare the heavy of TiZrN film on nickel-titanium instruments surface
Long-pending technique, coating process is divided into two stages；
F, work rest rotate: coating chamber evacuation carrying out be slowly heated baking, nickel-titanium instruments is carried out ion bom bardment,
TiZr alloy transition layer deposition, TiZrN film deposition whole during be always maintained at work rest rotate, rotating speed is 6 revs/min.
The preparation method of the titanium zirconium nitride metal film for nickel-titanium instruments surface modification the most according to claim 1,
It is characterized in that, described multi-arc ion coating arc source number, i.e. for ensureing nickel-titanium instruments surface uniform plating titanium zirconium nitride
Film, at least selects two different azimuth and becomes the arc source starting the arc simultaneously deposition of 90 degree of configurations, and nickel-titanium instruments to be ensured
During whole in coating chamber, coating chamber temperature is less than 200 ° of C.
The preparation method of the titanium zirconium nitride metal film for nickel-titanium instruments surface modification the most according to claim 1,
It is characterized in that, described pre-Bombardment and cleaning technique is divided into four steps to realize, and the first step, to coating chamber evacuation and be slowly heated
Baking, makes back end vacuum reach 8.0 10-3More than handkerchief, temperature reach 100 ° of C；Second step, is filled with argon, makes coating chamber vacuum
Degree reaches 2.0 10-1To 2.3 10-1Between handkerchief, opening arc source, keep arc current at 50 amperes, bombardment back bias voltage is-350
Volt, carries out ion bom bardment, stops ion bom bardment after coating chamber temperature reaches 150 ° of C, stops argon simultaneously and flows into；3rd step,
Continue coating chamber evacuation, when coating chamber temperature returns to 100 ° of C, repeat the process of second step；4th step, repeats the 3rd
The process of step 2 ~ 3 times.
The preparation method of the titanium zirconium nitride metal film for nickel-titanium instruments surface modification the most according to claim 1,
It is characterized in that, described coating process is divided into two stages: first stage, the deposition of TiZr alloy transition layer, i.e. by coating chamber
Interior ar pressure is maintained at 2.0 10-1Handkerchief, the arc current in titanium-zirconium alloy target arc source is placed in 45 ~ 50 amperes, deposits back bias voltage
For-130 ~ 150 volts, start deposition, sedimentation time 3 minutes；Second stage, adjusts argon flow amount so that it is partial pressure reaches 0.8
10-1Handkerchief, is passed through nitrogen in coating chamber simultaneously, makes mixed gas total pressure reach 2.5 10-1Handkerchief, titanium-zirconium alloy target arc source
Arc current be placed in 45 ~ 50 amperes, deposition back bias voltage be set as-100 ~ 110 volts, start deposition, after 5 minutes, increase nitrogen
Flow, makes mixed gas total pressure be increased to 3.0 10-1Handkerchief, simultaneously keep titanium-zirconium alloy target arc source arc current constant, deposition
Back bias voltage is constant, continues deposition, 12 ~ 15 minutes time, and keeps coating chamber temperature less than 200 ° of C.
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| CN201610404205.5A CN105887013A (en) | 2016-06-12 | 2016-06-12 | Preparation method of titanium-zirconium nitride metal film for surface modification of nickel-titanium root canal file |
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| CN201610404205.5A CN105887013A (en) | 2016-06-12 | 2016-06-12 | Preparation method of titanium-zirconium nitride metal film for surface modification of nickel-titanium root canal file |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN108251809A (en) * | 2018-01-15 | 2018-07-06 | 沈阳大学 | A kind of method of dental stainless steel root canal file coating surface nitridation titanium compound film |
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| CN117684134A (en) * | 2023-12-12 | 2024-03-12 | 利兰生物科技(苏州)有限公司 | Preparation method of nickel-titanium alloy bracket biological ceramic coating |
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| CN110497163A (en) * | 2019-09-26 | 2019-11-26 | 江苏盛玛特新材料科技有限公司 | A kind of lamination combined type root canal file and its processing technology |
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