CN114214620A - Preparation method of root canal file nano TiN coated film - Google Patents

Preparation method of root canal file nano TiN coated film Download PDF

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Publication number
CN114214620A
CN114214620A CN202111551498.7A CN202111551498A CN114214620A CN 114214620 A CN114214620 A CN 114214620A CN 202111551498 A CN202111551498 A CN 202111551498A CN 114214620 A CN114214620 A CN 114214620A
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China
Prior art keywords
root canal
nano tin
environment
coated film
preparation
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CN202111551498.7A
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Chinese (zh)
Inventor
高淑春
郑碧霄
宋东峰
李家旺
王秋实
张少骞
李艳君
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Shenyang Boya Biotechnology Co ltd
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Shenyang Boya Biotechnology Co ltd
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Priority to CN202111551498.7A priority Critical patent/CN114214620A/en
Publication of CN114214620A publication Critical patent/CN114214620A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding

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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)
  • Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)

Abstract

The invention belongs to the technical field of biomedical metal products, and particularly relates to a preparation method of a root canal file nano TiN coated film. The preparation method of the root canal file nano TiN coated film comprises the following steps: treating the environment to a certain vacuum degree, and adsorbing Ti atoms on the surface of the material; introducing nitrogen to increase the environment to normal atmospheric pressure; and nitriding the activated Ti to obtain the compact nano TiN coating. The film coating method adopted by the application has the advantages of simple process, excellent film coating effect, tight combination of TiN and the matrix, maintenance of the mechanical property of the matrix, smooth surface and no crack or shedding in hyperelastic deformation. Can completely adapt to the recoverable deformation of 8-10% of the large-deformation matrix nickel-titanium alloy, and has no biological toxicity.

Description

Preparation method of root canal file nano TiN coated film
Technical Field
The invention belongs to the technical field of biomedical metal products, and particularly relates to a preparation method of a root canal file nano TiN coated film.
Background
Root canal treatment is the primary treatment of endodontic and periapical diseases, in which root canal preparation is one of the key factors in determining the success or failure of root canal treatment, and the effectiveness of root canal preparation is largely related to the selection of appropriate root canal preparation instruments. In the case of file selection, a stiffer file can easily cause a step, a lateral puncture, or a root tip pull-apart, leading to failure; the file that elasticity is good gets into crooked root canal more easily, need not the root to pressurization, and doctor's operation is lighter, and the comfort level is high, reduces hand fatigue, both protects the doctor, can guarantee better treatment quality moreover.
In recent years, the nickel titanium root canal preparation instrument has developed most rapidly with its remarkable advantages of good flexibility, formability, unique memory property and the like. Because of the requirement of complex root canal to metal large deformation, the intensity and the wear resistance are not enough, and the root canal is not cleaned completely.
The superelastic recoverable deformation of nickel titanium shape memory alloys is 8-10%, and TiN as a bioceramic has little plasticity. Therefore, the nanometer TiN coated film can adapt to the super-elastic change of the matrix nickel-titanium alloy through the nanometer micromolecule effect. Not only can meet the requirements of the nickel-titanium shape memory alloy on biological functionality and biocompatibility, but also can meet the requirement of wear resistance. The TiN coated film enables the nickel-titanium alloy root canal file to fully exert the performance in use.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a preparation method of a root canal file nano TiN coated film. The TiN coated film ensures that the nickel-titanium shape memory alloy root canal file has biocompatibility and biological functionality and can also improve the wear resistance.
In order to achieve the above object, the present invention provides the following technical solutions.
A preparation method of a root canal file nano TiN coated film comprises the following steps:
step 1, treating the environment to a certain vacuum degree, and adsorbing Ti atoms on the surface of the material.
And 2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure.
And 3, nitriding the Ti activated in the step 2 to obtain the compact nano TiN coating.
Further, the material in the step 1 is nickel titanium shape memory alloy.
Further, the vacuum degree in the step 1 is 10-2-10-3And (4) supporting.
Further, the nitriding condition in the step 3 is 200-700 ℃ for 2-10 minutes.
Compared with the prior art, the invention has the beneficial effects of.
1. The TiN film coating process increases the firmness of the film layer.
2. The nano TiN film covers the ceramic, so that the brittleness of the ceramic is changed. The compact film prevents nickel ions from being separated out, and ensures the biocompatibility of the NiTi shape memory alloy.
3. The safety and the practicability are good. The biological functionality and the mechanical property of the NiTi shape memory alloy are suitable for human bodies. And the compact TiN coated film is a biological ceramic and has excellent biocompatibility.
4. The film coating method adopted by the application has the advantages of simple process, excellent film coating effect, tight combination of TiN and the matrix, maintenance of the mechanical property of the matrix, smooth surface and no crack or shedding in hyperelastic deformation. Can completely adapt to the recoverable deformation of 8-10% of the large-deformation matrix nickel-titanium alloy, and has no biological toxicity.
5. Titanium and titanium alloy have good corrosion resistance and biocompatibility, and can fully and fully react with oxygen, nitrogen and the like to obtain stable compounds mainly because of the activity of Ti. The titanium and the nitrogen have strong affinity, and a stable TiN film can be quickly formed on the surface in the nitrogen-containing environment, and the TiN film is more than TiO2The film is harder and more wear resistant. So that it exhibits excellent corrosion resistance. The TiN coating on the surface of the nickel titanium has the main advantages that: the TiN coating is a ceramic material and has no toxicity; secondly, the solubility of the TiN coating in water is very low; the TiN coating has good wear resistance and improves the cutting performance of the root canal file. The TiN coating can improve the corrosion resistance and blood compatibility of the matrix and prevent nickel ions from being separated out.
Drawings
FIG. 1A root canal file with a nano TiN film prepared in example 1.
Detailed Description
The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
A preparation method of a root canal file nano TiN coated film comprises the following steps:
step 1, treating the environment to a certain vacuum degree, and adsorbing Ti atoms on the surface of the material.
And 2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure.
And 3, nitriding the Ti activated in the step 2 to obtain the compact nano TiN coating.
Further, the material in the step 1 is nickel titanium shape memory alloy.
Further, the vacuum degree in the step 1 is 10-2-10-3And (4) supporting.
Further, the nitriding condition in the step 3 is 200-700 ℃ for 2-10 minutes.
Example 1.
Step 1, the environment is brought to vacuum 10-2And (3) supporting Ti atoms to be adsorbed on the surface of the material of the root canal file 2506.
And 2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure.
And 3, nitriding the activated Ti within the temperature range of 300 ℃ for 3 minutes to obtain the compact nano TiN coating.
Example 2.
Step 1, the environment is brought to vacuum 10-2And (3) supporting Ti atoms to be adsorbed on the surface of the root canal file type 2004 material.
And 2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure.
And 3, nitriding the activated Ti within the temperature range of 500 ℃ for 2 minutes to obtain the compact nano TiN coating.
Example 3.
Step 1, the environment is brought to vacuum 10-3And (3) supporting, and adsorbing Ti atoms on the surface of the straightening arch wire material of 0.12x 0.12.
And 2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure.
And 3, nitriding the activated Ti within the temperature range of 580 ℃ for 6 minutes to obtain the compact nano TiN coating.
Comparative example 1.
Preparation of TiO by PVD method2Coating film (2):
step 1, the environment is brought to vacuum 10-3And (4) supporting.
Step 2, depositing activated Ti atoms and activated oxygen atoms on the surface of the root canal file at the same time.
And 3, adopting mechanical rotation to achieve uniform coating.
Step 4, depositing for 2min to form TiO2Coating and taking out the coating machine in a shutdown mode.
Table 1 table of test results of examples 1 to 3 and comparative example 1.
Serial number Uniformity of coating 90 DEG fatigue 1000 times, No. 1000 sand paper, 5N pressure grinding for 10 seconds. Placing the alloy in an acidic corrosive liquid to test Ni2+And (4) precipitating.
Example 1 Even TiN coating Free of Ni2+The coating is good and has no crack. And (3) wear resistance.
Example 2 Even TiN coating Free of Ni2+The coating is good and has no crack. And (3) wear resistance.
Example 3 Even TiN coating Free of Ni2+The coating is good and has no crack. And (3) wear resistance.
Comparative example 1 TiO2Coating unevenness Small amount of Ni2+And a small amount of cracks are precipitated after fatigue.
The file after TiN coating presents dark yellow.

Claims (7)

1. A preparation method of a root canal file nano TiN coated film is characterized by comprising the following steps:
step 1, treating the environment to a certain vacuum degree, and adsorbing Ti atoms on the surface of a material;
2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure;
and 3, nitriding the Ti activated in the step 2 to obtain the compact nano TiN coating.
2. The method for preparing a nano TiN coated film of an endodontic file according to claim 1, wherein the material in the step 1 is a nickel titanium shape memory alloy.
3. The method for preparing a nano TiN coated film of an endodontic file according to claim 1, wherein the degree of vacuum in step 1 is 10-2-10-3And (4) supporting.
4. The method for preparing the nano TiN coated film of the root canal file according to claim 1, wherein the nitriding condition in the step 3 is 200-700 ℃ for 2-10 minutes.
5. A preparation method of a root canal file nano TiN coated film is characterized by comprising the following steps:
step 1, the environment is brought to vacuum 10-2A support, which is used for adsorbing Ti atoms on the surface of the material of the root canal file 2506;
2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure;
and 3, nitriding the activated Ti within the temperature range of 300 ℃ for 3 minutes to obtain the compact nano TiN coating.
6. A preparation method of a root canal file nano TiN coated film is characterized by comprising the following steps:
step 1, the environment is brought to vacuum 10-2A support, Ti atoms are adsorbed on the surface of a root canal file type 2004 material;
2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure;
and 3, nitriding the activated Ti within the temperature range of 500 ℃ for 2 minutes to obtain the compact nano TiN coating.
7. A preparation method of a root canal file nano TiN coated film is characterized by comprising the following steps:
step 1, the environment is brought to vacuum 10-3Supporting, adsorbing Ti atoms on the surface of a correction arch wire material of 0.12x 0.12;
2, introducing nitrogen at the speed of 200ml/s to increase the environment to normal atmospheric pressure;
and 3, nitriding the activated Ti within the temperature range of 580 ℃ for 6 minutes to obtain the compact nano TiN coating.
CN202111551498.7A 2021-12-17 2021-12-17 Preparation method of root canal file nano TiN coated film Pending CN114214620A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008064517A1 (en) * 2006-11-27 2008-06-05 Lifetech Scientific (Shenzhen) Co., Ltd. Method for preparing a coating on the surface of medical devices made of nickel-titanium alloy
CN101988182A (en) * 2010-12-08 2011-03-23 沈阳工业大学 Surface modification method for wear-resisting orthodontic arch wire and obtained wear-resisting arch wire
CN103096830A (en) * 2010-06-21 2013-05-08 耶达研究及发展有限公司 Endodontic files and method of preparation thereof
CN103233219A (en) * 2013-03-22 2013-08-07 常州大学 Metal TiN ceramic coating preparation process method
CN108220900A (en) * 2018-01-15 2018-06-29 沈阳大学 A kind of method of dental nickel-titanium instruments coating surface nitridation titanium compound film
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008064517A1 (en) * 2006-11-27 2008-06-05 Lifetech Scientific (Shenzhen) Co., Ltd. Method for preparing a coating on the surface of medical devices made of nickel-titanium alloy
CN103096830A (en) * 2010-06-21 2013-05-08 耶达研究及发展有限公司 Endodontic files and method of preparation thereof
CN101988182A (en) * 2010-12-08 2011-03-23 沈阳工业大学 Surface modification method for wear-resisting orthodontic arch wire and obtained wear-resisting arch wire
CN103233219A (en) * 2013-03-22 2013-08-07 常州大学 Metal TiN ceramic coating preparation process method
CN108220900A (en) * 2018-01-15 2018-06-29 沈阳大学 A kind of method of dental nickel-titanium instruments coating surface nitridation titanium compound film
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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