CN109504969A - A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy - Google Patents
A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy Download PDFInfo
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- CN109504969A CN109504969A CN201811273417.XA CN201811273417A CN109504969A CN 109504969 A CN109504969 A CN 109504969A CN 201811273417 A CN201811273417 A CN 201811273417A CN 109504969 A CN109504969 A CN 109504969A
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- Prior art keywords
- nitinol
- minimally invasive
- endodontic treatment
- synthetic method
- berberine
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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
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C5/00—Filling or capping teeth
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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)
- General Chemical & Material Sciences (AREA)
- Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
Abstract
The invention discloses a kind of synthetic methods of minimally invasive endodontic treatment NiTi instruments control alloy, comprising the following steps: S1 Nitinol surface is without nickel；S2 Nitinol surface coating；The activation of S3 Nitinol, there are many micropores for meeting on the Nitinol handled without nickelization in the present invention by surface, after surface coating, several small cavitys are formed between Nitinol and polytetrafluoroethylene (PTFE), finally by activation step, berberine is enabled to be dipped into the cavity between Nitinol and polytetrafluoroethylene (PTFE), the berberine in cavity is able to carry out sustained release, since berberine has certain bactericidal effect, berberine can be conducive to minimally invasive endodontic treatment when being sustained.
Description
Technical field
The present invention relates to the field of medical instrument technology more particularly to a kind of minimally invasive endodontic treatment NiTi instruments control alloys
Synthetic method.
Background technique
Bio-medical Nitinol is due to widely being made with excellent mechanical performance and preferable biocompatibility
At various medical instruments.Nitinol is as biomaterial for medical purpose, due to, containing the more nickel of 50at%, working as NiTi in Nitinol
Alloy releases metallic nickel ions, and interact with biological tissue, to human body in use, corrosion process may will occur
Cause certain harm, it is therefore desirable to carry out surface to it and be modified, improve its corrosion resistance, reduce the spilling of nickel ion, change
It is apt to its and has biocompatibility, and NiTi itself does not have an effect of antibacterial, in therapeutic process, the bacterium of dental pulp depths is general
Be inconvenient to remove, influence therapeutic effect.
Berberine (berberine, BBR), also known as jamaicin are clearing heat and detoxicating drugs classical in traditional Chinese medicine,
For treating diarrhea, oneself is had more than 2,000 years history, has short treating period, curative effect fast, few side effects, action temperature and at low cost etc.
Feature.Currently, berberine has caused the concern in dentistry field, berberine not only has antibacterial action, and there are also promote bone shape
At effect.
Therefore, we have proposed a kind of minimally invasive endodontic treatment NiTi instruments synthetic methods of control alloy to be used to solve
State problem.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of minimally invasive endodontic treatment nickel proposed
The synthetic method of titanium instrument control alloy.
A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy, comprising the following steps:
S1 Nitinol surface is without nickel: Nitinol being placed in the mixed solution of potassium permanganate and hydrochloric acid, carries out alloy
Change reaction, washing is clean after completion of the reaction and is processed by shot blasting, obtains Nitinol of the surface without nickel；
S2 Nitinol surface coating: coating the aqueous solution of polytetrafluoroethylene (PTFE) on Nitinol of the surface without nickel, then will
The surface of aqueous solution coated with polytetrafluoroethylene (PTFE) is placed in 360 DEG C of -420 DEG C of environment high temperatures sintering without the Nitinol of nickel
Membranaceous coating is formed, obtains the Nitinol of overlay film after membranaceous coating is cooling；
The activation of S3 Nitinol: the Nitinol of the overlay film is immersed in berberine soak, in 80 DEG C of -90 DEG C of immersions
6h-8h is to obtain minimally invasive endodontic treatment NiTi instruments control alloy.
Preferably, in the S1, the concentration of potassium permanganate is 0.1mol/L-0.3mol/L in mixed solution, and is mixed molten
The concentration of hydrochloric acid is 0.1mol/L-0.5mol/L in liquid.
Preferably, in the S1, by Nitinol surface grinding after completion of the reaction be polished to roughness Ra be 0.5 μm-
1 μm。
Preferably, in the S2, the mass ratio of polytetrafluoroethylene (PTFE) and water is 1:1-1.5.
Preferably, in the S2, the partial size of polytetrafluoroethylene (PTFE) is 40 μm -60 μm.
Preferably, in the S2, the surface area of the Nitinol with surface without nickel is calculated, polytetrafluoroethylene (PTFE) it is water-soluble
The dosage of liquid is 0.01-0.05g/cm2。
Preferably, in the S3, the concentration of berberine is 0.001mol/L-0.01mol/L in berberine soak.
Preferably, it in the S3, is calculated with the surface area of the Nitinol of overlay film, the dosage of berberine soak is
0.5-1ml/cm2。
The beneficial effects of the present invention are:
1, potassium permanganate has strong oxidizing property, can corrode to nickel under acidic environment, and the potassium ion in solution can
So that titanium is passivated, so that titanium is not easy to be corroded, it may be convenient to Nitinol of the surface without nickel be made；
2, Nitinol surface coating can be improved the durability of alloy, and the thickness of overlay film is thin, does not influence the bending of alloy, becomes
Shape.
3, there are many micropores for meeting on the Nitinol handled without nickelization by surface, and after surface coating, NiTi is closed
Form several small cavitys between gold and polytetrafluoroethylene (PTFE) enables to berberine to be dipped into finally by activation step
In cavity between Nitinol and polytetrafluoroethylene (PTFE), the berberine in cavity is able to carry out sustained release, since berberine has one
Determine bactericidal effect, berberine can be conducive to minimally invasive endodontic treatment when being sustained.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
In embodiment 1
A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy, comprising the following steps:
S1 Nitinol surface is without nickel: Nitinol being placed in the mixed solution of potassium permanganate and hydrochloric acid, carries out alloy
Change reaction, washing is clean after completion of the reaction and is processed by shot blasting, obtains Nitinol of the surface without nickel；
S2 Nitinol surface coating: coating the aqueous solution of polytetrafluoroethylene (PTFE) on Nitinol of the surface without nickel, then will
The surface of aqueous solution coated with polytetrafluoroethylene (PTFE) is placed in 360 DEG C of environment high temperatures without the Nitinol of nickel and is sintered to form film
Shape coating calcines 1h, obtains the Nitinol of overlay film after membranaceous coating is cooling；
The activation of S3 Nitinol: the Nitinol of the overlay film is immersed in berberine soak, in 80 DEG C of immersion 8h with
Obtain minimally invasive endodontic treatment NiTi instruments control alloy.
In the S1, the concentration of potassium permanganate is 0.1mol/L in mixed solution, and the concentration of hydrochloric acid is in mixed solution
0.1mol/L, removal alloying reaction time are 2h.
In the S1, it is 0.5 μm that Nitinol surface grinding after completion of the reaction, which is polished to roughness Ra,.
In the S2, the mass ratio of polytetrafluoroethylene (PTFE) and water is 1:1.
In the S2, the partial size of polytetrafluoroethylene (PTFE) is 40 μm.
In the S2, the surface area of the Nitinol with surface without nickel is calculated, the use of the aqueous solution of polytetrafluoroethylene (PTFE)
Amount is 0.01g/cm2。
In the S3, the concentration of berberine is 0.001mol in berberine soak.
It in the S3, is calculated with the surface area of the Nitinol of overlay film, the dosage of berberine soak is 0.5ml/
cm2。
In embodiment 2
A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy, comprising the following steps:
S1 Nitinol surface is without nickel: Nitinol being placed in the mixed solution of potassium permanganate and hydrochloric acid, carries out alloy
Change reaction, washing is clean after completion of the reaction and is processed by shot blasting, obtains Nitinol of the surface without nickel；
S2 Nitinol surface coating: coating the aqueous solution of polytetrafluoroethylene (PTFE) on Nitinol of the surface without nickel, then will
The surface of aqueous solution coated with polytetrafluoroethylene (PTFE) is placed in 420 DEG C of environment high temperatures without the Nitinol of nickel and is sintered to form film
Shape coating calcines 30min, obtains the Nitinol of overlay film after membranaceous coating is cooling；
The activation of S3 Nitinol: the Nitinol of the overlay film is immersed in berberine soak, in 90 DEG C of immersion 6h with
Obtain minimally invasive endodontic treatment NiTi instruments control alloy.
In the S1, the concentration of potassium permanganate is 0.3mol/L in mixed solution, and the concentration of hydrochloric acid is in mixed solution
0.5mol/L, removal alloying reaction time are 1h.
In the S1, it is 1 μm that Nitinol surface grinding after completion of the reaction, which is polished to roughness Ra,.
In the S2, the mass ratio of polytetrafluoroethylene (PTFE) and water is 1:1.5.
In the S2, the partial size of polytetrafluoroethylene (PTFE) is 60 μm.
In the S2, the surface area of the Nitinol with surface without nickel is calculated, the use of the aqueous solution of polytetrafluoroethylene (PTFE)
Amount is 0.05g/cm2。
In the S3, the concentration of berberine is 0.01mol/L in berberine soak.
It in the S3, is calculated with the surface area of the Nitinol of overlay film, the dosage of berberine soak is 1ml/cm2。
In embodiment 3
A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy, comprising the following steps:
S1 Nitinol surface is without nickel: Nitinol being placed in the mixed solution of potassium permanganate and hydrochloric acid, carries out alloy
Change reaction, washing is clean after completion of the reaction and is processed by shot blasting, obtains Nitinol of the surface without nickel；
S2 Nitinol surface coating: coating the aqueous solution of polytetrafluoroethylene (PTFE) on Nitinol of the surface without nickel, then will
The surface of aqueous solution coated with polytetrafluoroethylene (PTFE) is placed in 400 DEG C of environment high temperatures without the Nitinol of nickel and is sintered to form film
Shape coating calcines 40min, obtains the Nitinol of overlay film after membranaceous coating is cooling；
The activation of S3 Nitinol: the Nitinol of the overlay film is immersed in berberine soak, in 85 DEG C of immersion 7h with
Obtain minimally invasive endodontic treatment NiTi instruments control alloy.
In the S1, the concentration of potassium permanganate is 0.2mol/L in mixed solution, and the concentration of hydrochloric acid is in mixed solution
0.3mol/L, removal alloying reaction time are 2h.
In the S1, it is 0.8 μm that Nitinol surface grinding after completion of the reaction, which is polished to roughness Ra,.
In the S2, the mass ratio of polytetrafluoroethylene (PTFE) and water is 1:1.2.
In the S2, the partial size of polytetrafluoroethylene (PTFE) is 50 μm.
In the S2, the surface area of the Nitinol with surface without nickel is calculated, the use of the aqueous solution of polytetrafluoroethylene (PTFE)
Amount is 0.03g/cm2。
In the S3, the concentration of berberine is 0.005mol/L in berberine soak.
It in the S3, is calculated with the surface area of the Nitinol of overlay film, the dosage of berberine soak is 0.7ml/
cm2。
The control alloy prepared in embodiment 1-3 is analyzed below with reference to experimental data, will be prepared in embodiment 1-3
Good control alloy is placed into the culture dish equipped with Porphyromonas endodontalis in vitro, and depositing for Porphyromonas endodontalis in vitro is observed after 30min
Motility rate, experimental result are as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Survival rate % | 12.3 | 9.6 | 11.4 |
By experimental data as can be seen that the control alloy of embodiment 1-3 preparation have the effect of it is certain, in the minimally invasive dental pulp of progress
When treatment, control alloy can sterilize the dead angle of dental pulp depths, improve therapeutic efficiency.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy, which comprises the following steps:
S1 Nitinol surface is without nickel: Nitinol being placed in the mixed solution of potassium permanganate and hydrochloric acid, carries out alloy
Change reaction, washing is clean after completion of the reaction and is processed by shot blasting, obtains Nitinol of the surface without nickel；
S2 Nitinol surface coating: coating the aqueous solution of polytetrafluoroethylene (PTFE) on Nitinol of the surface without nickel, then will
The surface of aqueous solution coated with polytetrafluoroethylene (PTFE) is placed in 360 DEG C of -420 DEG C of environment high temperatures sintering without the Nitinol of nickel
Membranaceous coating is formed, obtains the Nitinol of overlay film after membranaceous coating is cooling；
The activation of S3 Nitinol: the Nitinol of the overlay film is immersed in berberine soak, in 80 DEG C of -90 DEG C of immersions
6h-8h is to obtain minimally invasive endodontic treatment NiTi instruments control alloy.
2. a kind of synthetic method of the minimally invasive endodontic treatment NiTi instruments according to claim 1 with control alloy, feature
It is, in the S1, the concentration of potassium permanganate is 0.1mol/L-0.3mol/L, and hydrochloric acid in mixed solution in mixed solution
Concentration is 0.1mol/L-0.5mol/L.
3. a kind of synthetic method of the minimally invasive endodontic treatment NiTi instruments according to claim 1 with control alloy, feature
It is, in the S1, it is 0.5 μm -1 μm that Nitinol surface grinding after completion of the reaction, which is polished to roughness Ra,.
4. a kind of synthetic method of the minimally invasive endodontic treatment NiTi instruments according to claim 1 with control alloy, feature
It is, in the S2, the mass ratio of polytetrafluoroethylene (PTFE) and water is 1:1-1.5.
5. a kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy according to claim 1 or 4, special
Sign is, in the S2, the partial size of polytetrafluoroethylene (PTFE) is 40 μm -60 μm.
6. a kind of synthetic method of the minimally invasive endodontic treatment NiTi instruments according to claim 1 with control alloy, feature
It is, in the S2, the surface area of the Nitinol with surface without nickel is calculated, and the dosage of the aqueous solution of polytetrafluoroethylene (PTFE) is
0.01-0.05g/cm2。
7. a kind of synthetic method of the minimally invasive endodontic treatment NiTi instruments according to claim 1 with control alloy, feature
It is, in the S3, the concentration of berberine is 0.001mol/L-0.01mol/L in berberine soak.
8. a kind of synthetic method of the minimally invasive endodontic treatment NiTi instruments according to claim 1 with control alloy, feature
It is, in the S3, calculated with the surface area of the Nitinol of overlay film, the dosage of berberine soak is 0.5-1ml/cm2。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811273417.XA CN109504969A (en) | 2018-10-30 | 2018-10-30 | A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy |
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| CN201811273417.XA CN109504969A (en) | 2018-10-30 | 2018-10-30 | A kind of synthetic method of minimally invasive endodontic treatment NiTi instruments control alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114351235A (en) * | 2022-02-14 | 2022-04-15 | 淮阴工学院 | Preparation method of Ni-free functional microporous structure on surface of nickel-titanium alloy |
-
2018
- 2018-10-30 CN CN201811273417.XA patent/CN109504969A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114351235A (en) * | 2022-02-14 | 2022-04-15 | 淮阴工学院 | Preparation method of Ni-free functional microporous structure on surface of nickel-titanium alloy |
| CN114351235B (en) * | 2022-02-14 | 2023-02-28 | 淮阴工学院 | Preparation method of Ni-free functional microporous structure on surface of nickel-titanium alloy |
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Application publication date: 20190322 |
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