WO2014015767A1 - Ultra-fine grain nickel-titanium alloy root canal file and preparation method therefor - Google Patents

Ultra-fine grain nickel-titanium alloy root canal file and preparation method therefor Download PDF

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Publication number
WO2014015767A1
WO2014015767A1 PCT/CN2013/079738 CN2013079738W WO2014015767A1 WO 2014015767 A1 WO2014015767 A1 WO 2014015767A1 CN 2013079738 W CN2013079738 W CN 2013079738W WO 2014015767 A1 WO2014015767 A1 WO 2014015767A1
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Prior art keywords
titanium alloy
ultra
nickel
fine
root canal
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PCT/CN2013/079738
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French (fr)
Chinese (zh)
Inventor
郑玉峰
周慧敏
李莉
佟运祥
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哈尔滨工程大学
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Publication of WO2014015767A1 publication Critical patent/WO2014015767A1/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • 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
    • A61C5/40—Implements for surgical treatment of the roots or nerves of the teeth; Nerve needles; Methods or instruments for medication of the roots
    • A61C5/42—Files for root canals; Handgrips or guiding means therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C2201/00—Material properties
    • A61C2201/007—Material properties using shape memory effect

Definitions

  • the invention relates to a root canal and a preparation method thereof. Background technique
  • Dental root canal is one of the most frequently used instruments in the oral cavity. It is mainly used for the preparation and formation of the root canal. According to the material of the root canal, it can be divided into two types: stainless steel root canal and nickel titanium root canal. Due to the high rigidity of the stainless steel, it is not easy to bend, and the amount of elastic deformation is small. During the root canal treatment, especially when the curved root canal is prepared, the stainless steel root canal is often plastically deformed, causing accidental breakage or penetration of the tooth pulp during the treatment. The cavity brings great pain to the patient.
  • the nickel-titanium root canal has the advantages of good flexibility and high elasticity, and the root canal deviation caused by the preparation of the curved root canal is small, and the centering of the root tip is strong, and the curved root canal is
  • the preparatory aspect has obvious advantages and is increasingly favored by dentists.
  • all kinds of root canal preparation instruments made of Nitinol are constantly emerging. From traditional ISO instruments to non-ISO instruments, from hand tools to machine tools, it has gradually become the main force of root canal instruments.
  • studies have shown that nickel-titanium root canal has lower cutting efficiency than stainless steel root canal, and wear and tear in the form of cutting edge, expansion, tip deformation, rounding, etc. during clinical use. Poor wear, resulting in reduced cutting efficiency.
  • the nickel-titanium root canal will undergo fatigue fracture after repeated use, resulting in a decrease in its service life. Summary of the invention
  • the object of the present invention is to solve the technical problem of poor cutting efficiency of the existing nickel-titanium root canal, and to provide an ultrafine-crystalline nickel-titanium root canal and a preparation method thereof.
  • Ultrafine grained nickel-titanium root canal made of ultrafine grained nickel titanium alloy with a particle size of 200nm-300nm to make.
  • the preparation method of ultrafine grain nickel-titanium root canal is as follows:
  • Ultrafine grain treatment of nickel-titanium alloy A nickel-titanium alloy ingot with a percentage of Ti atoms of 48-52% is cut into round rods with a diameter of 20 mm and a length of 100 mm, and then the method of equal-angle angular pressing is adopted. The round bar has an angle of 90 through the two channels. And 120. The mold is extruded at 400-500 ° C for 4-8 passes, and then held at 300-500 ° C for 30-60 min to obtain an ultrafine-fine treated nickel-titanium alloy rod;
  • the ultrafine grain treated nickel-titanium alloy rod is made of graphite milk as a lubricant at a heating temperature of 600-700 ° C and a linear velocity of 15-25 m/s.
  • Ultrafine grained nickel-titanium alloy wire with diameter of 0.4-2.5mm is prepared under the condition of 0.04-0.01mm per pass;
  • the ultrafine-grained nickel-titanium alloy wire obtained in the second step is cut into small lengths of 21-40 mm, and then one end of the 40 mm ultrafine-grained nickel-titanium alloy wire is processed to have a taper of 0.02-0.10 and a length of 16-20 mm. a taper wire having a tip diameter of 0.15-0.4 mm, and then cutting a cutting edge on the taper wire to obtain an ultrafine grain nickel-titanium root canal precursor;
  • the ultrafine-grained nickel-titanium root canal precursor is kept at 350-650 ° C for 30-120 min, and then air-cooled to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultrafine-crystalline nickel-titanium alloy root
  • the ultrafine grain nickel-titanium alloy in the tube has a particle diameter of 200 nm to 300 nm.
  • the preparation method of ultrafine grain nickel-titanium root canal is as follows:
  • the wire with a length of 31 mm is immersed in an etching solution of 50 ⁇ 5 °C, and one end of the wire is machined to a length of 16-20 mm, a taper of 0.02-0.10, and a tip diameter of 0.15 at 35-65 °C. 0.4mm taper wire, then the taper wire is cut into a cutting edge to obtain an ultrafine grain Nitinium root canal precursor, and the etching solution is composed of HF, HN0 3 and 3 ⁇ 40, wherein HF, HN0 3 and The volume ratio of H 2 0 is 1:3:6;
  • the ultrafine-grained nickel-titanium root canal precursor is incubated at 350-650 ° C for 30-120 min to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultra-fine-crystalline nickel-titanium root canal is obtained.
  • the ultrafine grain nickel titanium alloy has a particle diameter of 200 nm to 300 nm.
  • the ultrafine-grained nickel-titanium root canal of the present invention has a phase composition at room temperature composed of martensite and austenite, and the diffraction peak is significantly broadened due to grain refinement, austenite at the use temperature, and
  • the ultrafine-grained nickel-titanium root canal prepared by the invention has good hardness and wear resistance.
  • FIG. 1 is an electron micrograph of an ultrafine-grained nickel-titanium root canal prepared in Experiment 1;
  • FIG. 2 is an XRD photograph of an ultrafine-crystalline nickel-titanium root canal prepared in Experiment 1.
  • Figure 3 is a DSC graph of the ultrafine-grained nickel-titanium root canal prepared in Experiment 1;
  • 4 is a microhardness diagram of a nickel-titanium alloy, an ultrafine-grained nickel-titanium alloy, and an ultrafine-grained nickel-titanium alloy heat-treated at 400 ° C in the first experiment, wherein 1 represents a microhardness diagram of the nickel-titanium alloy, 2 The microhardness diagram of the ultrafine grained nickel-titanium alloy is shown, and 3 represents the microhardness diagram of the ultrafine grained nickel-titanium alloy after heat treatment at 400 °C;
  • a represents a wear rate diagram of the nickel-titanium alloy, and b represents super Wear rate diagram of fine-grained nickel-titanium alloy, c represents wear rate diagram of ultra-fine-grained nickel-titanium alloy after heat treatment at 400 °C;
  • Figure 6 is a topographical view of the wear surface of Nitinol in Experiment 1;
  • Figure 7 is a topographical view of the wear surface of the ultrafine grained nickel-titanium alloy in Experiment 1;
  • Fig. 8 is a topographical view of the wear surface of the ultrafine-grained nickel-titanium alloy after heat treatment at 400 °C in Experiment 1. detailed description
  • the ultrafine-grained nickel-titanium root canal has a particle size of
  • this embodiment differs from the first embodiment in that the ultrafine-grained nickel-titanium root canal is made of an ultrafine-grained nickel-titanium alloy having a particle diameter of 260 nm. Others are the same as the first embodiment.
  • the preparation method of the ultrafine-crystalline nickel-titanium root canal in the present embodiment is as follows:
  • Ultrafine grain treatment of nickel-titanium alloy A nickel-titanium alloy ingot with a percentage of Ti atoms of 48-52% is cut into round rods with a diameter of 20 mm and a length of 100 mm, and then the method of equal-angle angular pressing is adopted. The round bar has an angle of 90 through the two channels. And 120. The mold is extruded at 400-500 ° C for 4-8 passes, and then held at 300-500 ° C for 30-60 min to obtain an ultrafine-fine treated nickel-titanium alloy rod;
  • the ultrafine grain treated nickel-titanium alloy rod is made of graphite milk as a lubricant at a heating temperature of 600-700 ° C and a linear velocity of 15-25 m/s.
  • Ultrafine grained nickel-titanium alloy wire with diameter of 0.4-2.5mm is prepared under the condition of 0.04-0.01mm per pass;
  • the ultrafine-grained nickel-titanium alloy wire obtained in the second step is cut into small lengths of 21-40 mm, and then one end of the 40 mm ultrafine-grained nickel-titanium alloy wire is processed to have a taper of 0.02-0.10 and a length of 16-20 mm. a taper wire having a tip diameter of 0.15-0.4 mm, and then cutting a cutting edge on the taper wire to obtain an ultrafine grain nickel-titanium root canal precursor;
  • the ultrafine-grained nickel-titanium root canal precursor is kept at 350-650 ° C for 30-120 min, and then air-cooled to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultrafine-crystalline nickel-titanium alloy root
  • the ultrafine grain nickel-titanium alloy in the tube has a particle diameter of 200 nm to 300 nm.
  • Embodiment 4 This embodiment differs from Embodiment 3 in the first step.
  • the nickel-titanium alloy ingot has a Ti atomic percentage of 50.8%. Others are the same as the third embodiment.
  • BEST MODE FOR CARRYING OUT THE INVENTION V This embodiment differs from the third embodiment in the first step of performing extrusion at 450 ° C for 5 passes. Others are the same as the third embodiment.
  • This embodiment differs from the third embodiment in that a taper wire having a taper of 0.04 and a length of 16 mm is machined at one end of a 31 mm-length ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
  • This embodiment differs from the third embodiment in that a taper wire having a taper of 0.06 and a length of 16 mm is machined at one end of a 25 mm-length ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
  • This embodiment differs from the third embodiment in that a taper yarn having a taper of 0.08 and a length of 16 mm is machined at one end of a 21 mm-length ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
  • This embodiment differs from the third embodiment in that a taper yarn having a taper of 0.10 and a length of 16 mm is machined at one end of a 28 mm ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
  • the preparation method of the ultrafine-crystalline nickel-titanium root canal in the present embodiment is as follows:
  • a nickel-titanium alloy rod having a Ti atomic percentage of 48-52% is drawn into a wire having a diameter of 0.4-2.5 mm and a length of 31 mm;
  • the wire with a length of 31 mm is immersed in an etching solution of 50 ⁇ 5 °C, and one end of the wire is machined to a length of 16-20 mm, a taper of 0.02-0.10, and a tip diameter of 0.15 at 35-65 °C. 0.4mm taper wire, then the taper wire is cut into a cutting edge to obtain an ultrafine grain Nitinium root canal precursor, and the etching solution is composed of HF, HN0 3 and 3 ⁇ 40, wherein HF, HN0 3 and H 2 0 Volume ratio is 1:3:6; 3.
  • the ultrafine-grained nickel-titanium root canal precursor is incubated at 350-650 ° C for 30-120 min to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultra-fine-crystalline nickel-titanium root canal is obtained.
  • the ultrafine grain nickel titanium alloy has a particle diameter of 200 nm to 300 nm.
  • the cutting edge is processed by the centerless grinding method on the tapered wire; in the second step of the embodiment, the ultrafine root canal front body processed by the cutting edge is subjected to surface electrochemical polishing.
  • the preparation method of ultrafine grain nickel-titanium root canal is as follows:
  • a nickel-titanium alloy ingot with a percentage of Ti atom of 50.8% is cut into a round rod with a diameter of 20 mm and a length of 100 mm, and then the round bar is extruded by equal-angle angular pressing.
  • the ultrafine grain treated nickel-titanium alloy rod is made of graphite milk as a lubricant at a heating temperature of 650 ° C, a linear velocity of 20 m / s, and a reduction per pass.
  • An ultrafine grain nickel titanium alloy wire having a diameter of 0.52 mm was prepared under conditions of 0.02 mm;
  • the ultrafine-grained nickel-titanium alloy wire obtained in the second step was cut into a small length of 31 mm, and then one end of the 31 mm ultrafine-grained nickel-titanium alloy wire was machined to have a taper of 0.02, a length of 16 mm, and a tip diameter of 0.2 mm. Taper wire, and then cutting the cutting edge on the taper wire to obtain an ultrafine grain nickel-titanium root canal precursor;
  • the ultrafine-grained nickel-titanium root canal precursor is incubated at 400 ° C for 60 min, and then air-cooled to obtain an ultrafine-grained nickel-titanium root canal.
  • the average grain size of the base of the nickel-titanium root canal is about 290 nm.
  • the phase composition of the ultrafine-grained nickel-titanium root canal at room temperature is composed of martensite and austenite. And the diffraction peak is significantly broadened due to grain refinement. It is seen from Fig. 3 that the ultrafine grained nickel titanium root canal (Ti-50.8 at.% Ni) is austenite at the use temperature.
  • the ultrafine-grained nickel-titanium alloy wire in the first step of the experiment was polished by SiC sandpaper and polished with A1 2 0 3 powder, and then tested for hardness and wear resistance on a microhardness tester and a ball-disk friction and wear tester, respectively.
  • the hardness and wear resistance of the conventional nickel-titanium alloy and the ultrafine-grained nickel-titanium alloy heat-treated at 400 ° C for 60 min were tested on a microhardness tester and a ball-disk friction and wear tester, respectively.
  • the nickel-titanium alloy and the ultrafine-grained nickel-titanium alloy are mainly abrasive wear, and the furrows along the rubbing direction are visible on the worn surface;
  • the crystal nickel-titanium alloy is mainly characterized by adhesive wear, and traces of peeling and plastic deformation are observed on the worn surface.
  • the preparation method of ultrafine grain nickel-titanium root canal is as follows:
  • a nickel-titanium alloy rod having a Ti atom content of 50.8% is drawn into a wire having a diameter of 2.5 mm and a length of 40 mm;
  • the etching solution consists of HF, HN0 3 and 3 ⁇ 40, wherein the volume ratio of HF, HN0 3 to 3 ⁇ 40 is 1:3:6;
  • the ultrafine-crystalline Nitinol root canal precursor is incubated at 500 ° C for 30 min to obtain an ultrafine-crystalline nickel-titanium root canal.

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Abstract

Disclosed are an ultra-fine grain nickel-titanium alloy root canal file and a preparation method therefor. The ultra-fine grain nickel-titanium alloy root canal file is made of an ultra-fine grain nickel-titanium alloy having a particle size of 200 nm to 300 nm. The preparation method therefor comprises: 1, ultra-fine grain treatment on a nickel-titanium alloy; 2, preparation of an ultra-fine grain nickel-titanium alloy wire; 3, machining and surface treatment on a root canal file cutting edge; and 4, heat treatment on an ultra-fine grain nickel-titanium alloy root canal file. The ultra-fine grain nickel-titanium alloy root canal file is in martensite and austenite phases at room temperature, and a diffraction peak broadens obviously due to grain refinement; however, the ultra-fine grain nickel-titanium alloy root canal file is in austenite phase at usage temperature. The ultra-fine grain nickel-titanium alloy root canal file solves technical problems that the existing nickel-titanium root canal file is low in cutting efficiency and prone to bending and intra-root-canal fracture. Compared with the existing nickel-titanium root canal file, the ultra-fine grain nickel-titanium alloy root canal file has good hardness and good wear resistance, and significantly increases cutting efficiency in clinical use.

Description

超细晶镍钛合金根管锉及其制备方法 技术领域  Ultrafine grain nickel-titanium root canal and preparation method thereof
本发明涉及一种根管锉及其制备方法。 背景技术  The invention relates to a root canal and a preparation method thereof. Background technique
齿科根管锉是口腔临床中使用最为频繁的器械之一， 主要用于牙齿根 管的预备、 成形。 根据根管锉的材质可以将其分为不锈钢根管锉和镍钛根 管锉两种。 由于不锈钢刚性大， 不易弯曲， 弹性变形量小， 在根管治疗过 程中， 尤其是弯曲根管预备时， 常常使不锈钢根管锉发生塑性变形， 引发 治疗过程中的意外折断或穿透牙齿髓腔， 给患者带来很大痛苦。 相比较而 言， 镍钛根管锉具有柔韧性好、 弹性大等优点， 预备弯曲根管时引起的根 管偏移较小， 而且在根尖部位的对中性较强， 在弯曲根管的预备方面有着 明显的优势， 越来越多地受到口腔医生们的青睐。 目前， 镍钛合金制作的 各类根管预备器械不断涌出， 从传统的 ISO器械到非 ISO器械， 从手用器 械到机用器械， 已逐渐成为根管器械的主力军。 但是， 研究表明， 与不锈 钢根管锉相比， 镍钛根管锉的切削效率较低， 临床使用过程中会发生切割 刃的开槽、 展开、 尖部变形、 变圆等形式的磨损， 耐磨性较差， 导致切削 效率下降。 另外， 对于机用镍钛根管锉， 在高速旋转载荷下， 镍钛根管锉 经多次使用后， 会发生疲劳断裂， 导致其使用寿命下降。 发明内容  Dental root canal is one of the most frequently used instruments in the oral cavity. It is mainly used for the preparation and formation of the root canal. According to the material of the root canal, it can be divided into two types: stainless steel root canal and nickel titanium root canal. Due to the high rigidity of the stainless steel, it is not easy to bend, and the amount of elastic deformation is small. During the root canal treatment, especially when the curved root canal is prepared, the stainless steel root canal is often plastically deformed, causing accidental breakage or penetration of the tooth pulp during the treatment. The cavity brings great pain to the patient. In comparison, the nickel-titanium root canal has the advantages of good flexibility and high elasticity, and the root canal deviation caused by the preparation of the curved root canal is small, and the centering of the root tip is strong, and the curved root canal is The preparatory aspect has obvious advantages and is increasingly favored by dentists. At present, all kinds of root canal preparation instruments made of Nitinol are constantly emerging. From traditional ISO instruments to non-ISO instruments, from hand tools to machine tools, it has gradually become the main force of root canal instruments. However, studies have shown that nickel-titanium root canal has lower cutting efficiency than stainless steel root canal, and wear and tear in the form of cutting edge, expansion, tip deformation, rounding, etc. during clinical use. Poor wear, resulting in reduced cutting efficiency. In addition, for the machined nickel-titanium root canal, under high-speed rotational load, the nickel-titanium root canal will undergo fatigue fracture after repeated use, resulting in a decrease in its service life. Summary of the invention
本发明的目的是为了解决现有镍钛根管锉切削效率较差的技术问题， 提供了一种超细晶镍钛合金根管锉及其制备方法。  The object of the present invention is to solve the technical problem of poor cutting efficiency of the existing nickel-titanium root canal, and to provide an ultrafine-crystalline nickel-titanium root canal and a preparation method thereof.
超细晶镍钛合金根管锉由粒径为 200nm-300nm 的超细晶镍钛合金制 成。 Ultrafine grained nickel-titanium root canal made of ultrafine grained nickel titanium alloy with a particle size of 200nm-300nm to make.
超细晶镍钛合金根管锉的制备方法如下：  The preparation method of ultrafine grain nickel-titanium root canal is as follows:
一、镍钛合金超细晶处理： 将 Ti原子百分含量为 48-52%的镍钛合金铸 锭切割成直径为 20mm、 长度为 100mm的圆棒， 然后采用等径角挤压的方 法将圆棒分别通过两通道夹角为 90。 和 120。 的模具，在 400-500°C进行 4-8 道次的挤压， 然后在 300-500°C下保温 30-60min, 得到超细晶处理后的镍钛 合金棒；  1. Ultrafine grain treatment of nickel-titanium alloy: A nickel-titanium alloy ingot with a percentage of Ti atoms of 48-52% is cut into round rods with a diameter of 20 mm and a length of 100 mm, and then the method of equal-angle angular pressing is adopted. The round bar has an angle of 90 through the two channels. And 120. The mold is extruded at 400-500 ° C for 4-8 passes, and then held at 300-500 ° C for 30-60 min to obtain an ultrafine-fine treated nickel-titanium alloy rod;
二、 超细晶镍钛合金丝的制备方法： 将超细晶处理后的镍钛合金棒以 石墨乳为润滑剂， 在加热温度为 600-700°C、 线速度为 15-25m/s、 每道次压 下量 0.04-0.01mm的条件下，制备成直径为 0.4-2.5mm的超细晶镍钛合金丝； 三、 超细晶镍钛合金丝锥度制备与根管锉切割刃成型处理：  2. Preparation method of ultrafine grained nickel-titanium alloy wire: The ultrafine grain treated nickel-titanium alloy rod is made of graphite milk as a lubricant at a heating temperature of 600-700 ° C and a linear velocity of 15-25 m/s. Ultrafine grained nickel-titanium alloy wire with diameter of 0.4-2.5mm is prepared under the condition of 0.04-0.01mm per pass; 3. Preparation of taper of ultrafine grained nickel-titanium alloy and forming process of root canal cutting blade :
将步驟二得到的超细晶镍钛合金丝剪成长度为 21-40mm的小段， 然后 将长度为 40mm超细晶镍钛合金丝的一端加工出锥度为 0.02-0.10、 长为 16-20mm、 尖端直径为 0.15-0.4mm的锥度丝， 然后在锥度丝上切削加工出 切刃， 得到超细晶镍钛合金根管锉前驱体；  The ultrafine-grained nickel-titanium alloy wire obtained in the second step is cut into small lengths of 21-40 mm, and then one end of the 40 mm ultrafine-grained nickel-titanium alloy wire is processed to have a taper of 0.02-0.10 and a length of 16-20 mm. a taper wire having a tip diameter of 0.15-0.4 mm, and then cutting a cutting edge on the taper wire to obtain an ultrafine grain nickel-titanium root canal precursor;
四、 将超细晶镍钛合金根管锉前驱体在 350-650°C保温 30-120 min, 然 后空冷， 即得超细晶镍钛合金根管锉， 所得的超细晶镍钛合金根管锉中超 细晶镍钛合金粒径为 200nm-300nm。  4. The ultrafine-grained nickel-titanium root canal precursor is kept at 350-650 ° C for 30-120 min, and then air-cooled to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultrafine-crystalline nickel-titanium alloy root The ultrafine grain nickel-titanium alloy in the tube has a particle diameter of 200 nm to 300 nm.
超细晶镍钛合金根管锉的制备方法如下：  The preparation method of ultrafine grain nickel-titanium root canal is as follows:
一、 将 Ti 原子百分含量为 48-52%的镍钛合金棒拉拔成直径为 1. Pull the nickel-titanium alloy rod with a percentage of Ti atoms of 48-52% into a diameter of
0.4-2.5mm、 长度为 31mm的丝材； 0.4-2.5mm wire with a length of 31mm;
二、 将长度为 31mm的丝材浸入 50 ± 5 °C的腐蚀溶液中， 在 35-65 °C将 丝材的一端加工出长度为 16-20mm、 锥度为 0.02-0.10 , 尖端直径为 0.15-0.4mm 的锥度丝， 然后将锥度丝切削加工出切刃， 得到超细晶镍钛合 金根管锉前驱体， 腐蚀溶液由 HF、 HN03和 ¾0组成， 其中 HF、 HN03与 H20的体积比为 1:3:6; 2. The wire with a length of 31 mm is immersed in an etching solution of 50 ± 5 °C, and one end of the wire is machined to a length of 16-20 mm, a taper of 0.02-0.10, and a tip diameter of 0.15 at 35-65 °C. 0.4mm taper wire, then the taper wire is cut into a cutting edge to obtain an ultrafine grain Nitinium root canal precursor, and the etching solution is composed of HF, HN0 3 and 3⁄40, wherein HF, HN0 3 and The volume ratio of H 2 0 is 1:3:6;
三、 将超细晶镍钛合金根管锉前驱体在 350-650°C下保温 30-120min, 即得超细晶镍钛合金根管锉， 所得的超细晶镍钛合金根管锉中超细晶镍钛 合金粒径为 200nm-300nm。  3. The ultrafine-grained nickel-titanium root canal precursor is incubated at 350-650 ° C for 30-120 min to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultra-fine-crystalline nickel-titanium root canal is obtained. The ultrafine grain nickel titanium alloy has a particle diameter of 200 nm to 300 nm.
本发明的超细晶镍钛根管锉室温下的相组成由马氏体和奥氏体组成， 并且衍射峰由于晶粒细化而明显宽化， 在使用温度下为奥氏体， 并且本发 明制备的超细晶镍钛合金根管锉的硬度和耐磨性较好。 附图说明  The ultrafine-grained nickel-titanium root canal of the present invention has a phase composition at room temperature composed of martensite and austenite, and the diffraction peak is significantly broadened due to grain refinement, austenite at the use temperature, and The ultrafine-grained nickel-titanium root canal prepared by the invention has good hardness and wear resistance. DRAWINGS
图 1是实验一制备的超细晶镍钛合金根管锉的电子显微镜照片； 图 2是实验一制备的超细晶镍钛合金根管锉的 XRD照片；  1 is an electron micrograph of an ultrafine-grained nickel-titanium root canal prepared in Experiment 1; FIG. 2 is an XRD photograph of an ultrafine-crystalline nickel-titanium root canal prepared in Experiment 1.
图 3是实验一制备的超细晶镍钛合金根管锉的 DSC曲线图；  Figure 3 is a DSC graph of the ultrafine-grained nickel-titanium root canal prepared in Experiment 1;
图 4是实验一中镍钛合金、超细晶镍钛合金和经 400°C热处理后的超细 晶镍钛合金的显微硬度图， 图中 1表示镍钛合金的显微硬度图， 2表示超细 晶镍钛合金的显微硬度图， 3表示经 400°C热处理后的超细晶镍钛合金的显 微硬度图；  4 is a microhardness diagram of a nickel-titanium alloy, an ultrafine-grained nickel-titanium alloy, and an ultrafine-grained nickel-titanium alloy heat-treated at 400 ° C in the first experiment, wherein 1 represents a microhardness diagram of the nickel-titanium alloy, 2 The microhardness diagram of the ultrafine grained nickel-titanium alloy is shown, and 3 represents the microhardness diagram of the ultrafine grained nickel-titanium alloy after heat treatment at 400 °C;
图 5是实验一中镍钛合金、超细晶镍钛合金和经 400°C热处理后的超细 晶镍钛合金的磨损速率图， 图中 a表示镍钛合金的磨损速率图， b表示超细 晶镍钛合金的磨损速率图， c表示经 400°C热处理后的超细晶镍钛合金的磨 损速率图；  5 is a wear rate diagram of a nickel-titanium alloy, an ultrafine-grained nickel-titanium alloy, and an ultrafine-grained nickel-titanium alloy heat-treated at 400 ° C in the first experiment, wherein a represents a wear rate diagram of the nickel-titanium alloy, and b represents super Wear rate diagram of fine-grained nickel-titanium alloy, c represents wear rate diagram of ultra-fine-grained nickel-titanium alloy after heat treatment at 400 °C;
图 6是实验一中镍钛合金磨损表面形貌图；  Figure 6 is a topographical view of the wear surface of Nitinol in Experiment 1;
图 7是实验一中超细晶镍钛合金磨损表面形貌图；  Figure 7 is a topographical view of the wear surface of the ultrafine grained nickel-titanium alloy in Experiment 1;
图 8是实验一中经 400°C热处理后的超细晶镍钛合金磨损表面形貌图。 具体实施方式  Fig. 8 is a topographical view of the wear surface of the ultrafine-grained nickel-titanium alloy after heat treatment at 400 °C in Experiment 1. detailed description
本发明技术方案不局限于以下所列举具体实施方式， 还包括各具体实 施方式间的任意组合。 The technical solution of the present invention is not limited to the specific embodiments listed below, and includes specific embodiments. Any combination between the modes.
具体实施方式一： 本实施方式中超细晶镍钛合金根管锉由粒径为 DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS First: In this embodiment, the ultrafine-grained nickel-titanium root canal has a particle size of
200nm-300nm的超细晶镍钛合金制成。 Made of 200nm-300nm ultra-fine grain nickel-titanium alloy.
具体实施方式二： 本实施方式与具体实施方式一不同的是所述超细晶 镍钛合金根管锉由粒径为 260nm的超细晶镍钛合金制成。 其它与具体实施 方式一相同。  BEST MODE FOR CARRYING OUT THE INVENTION Secondly, this embodiment differs from the first embodiment in that the ultrafine-grained nickel-titanium root canal is made of an ultrafine-grained nickel-titanium alloy having a particle diameter of 260 nm. Others are the same as the first embodiment.
具体实施方式三： 本实施方式中超细晶镍钛合金根管锉的制备方法如 下：  DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT 3: The preparation method of the ultrafine-crystalline nickel-titanium root canal in the present embodiment is as follows:
一、镍钛合金超细晶处理： 将 Ti原子百分含量为 48-52%的镍钛合金铸 锭切割成直径为 20mm、 长度为 100mm的圆棒， 然后采用等径角挤压的方 法将圆棒分别通过两通道夹角为 90。 和 120。 的模具，在 400-500°C进行 4-8 道次的挤压， 然后在 300-500°C下保温 30-60min, 得到超细晶处理后的镍钛 合金棒；  1. Ultrafine grain treatment of nickel-titanium alloy: A nickel-titanium alloy ingot with a percentage of Ti atoms of 48-52% is cut into round rods with a diameter of 20 mm and a length of 100 mm, and then the method of equal-angle angular pressing is adopted. The round bar has an angle of 90 through the two channels. And 120. The mold is extruded at 400-500 ° C for 4-8 passes, and then held at 300-500 ° C for 30-60 min to obtain an ultrafine-fine treated nickel-titanium alloy rod;
二、 超细晶镍钛合金丝的制备方法： 将超细晶处理后的镍钛合金棒以 石墨乳为润滑剂， 在加热温度为 600-700°C、 线速度为 15-25m/s、 每道次压 下量 0.04-0.01mm的条件下，制备成直径为 0.4-2.5mm的超细晶镍钛合金丝； 三、 超细晶镍钛合金丝锥度制备与根管锉切割刃成型处理：  2. Preparation method of ultrafine grained nickel-titanium alloy wire: The ultrafine grain treated nickel-titanium alloy rod is made of graphite milk as a lubricant at a heating temperature of 600-700 ° C and a linear velocity of 15-25 m/s. Ultrafine grained nickel-titanium alloy wire with diameter of 0.4-2.5mm is prepared under the condition of 0.04-0.01mm per pass; 3. Preparation of taper of ultrafine grained nickel-titanium alloy and forming process of root canal cutting blade :
将步驟二得到的超细晶镍钛合金丝剪成长度为 21-40mm的小段， 然后 将长度为 40mm超细晶镍钛合金丝的一端加工出锥度为 0.02-0.10、 长为 16-20mm、 尖端直径为 0.15-0.4mm的锥度丝， 然后在锥度丝上切削加工出 切刃， 得到超细晶镍钛合金根管锉前驱体；  The ultrafine-grained nickel-titanium alloy wire obtained in the second step is cut into small lengths of 21-40 mm, and then one end of the 40 mm ultrafine-grained nickel-titanium alloy wire is processed to have a taper of 0.02-0.10 and a length of 16-20 mm. a taper wire having a tip diameter of 0.15-0.4 mm, and then cutting a cutting edge on the taper wire to obtain an ultrafine grain nickel-titanium root canal precursor;
四、 将超细晶镍钛合金根管锉前驱体在 350-650°C保温 30-120 min, 然 后空冷， 即得超细晶镍钛合金根管锉， 所得的超细晶镍钛合金根管锉中超 细晶镍钛合金粒径为 200nm-300nm。  4. The ultrafine-grained nickel-titanium root canal precursor is kept at 350-650 ° C for 30-120 min, and then air-cooled to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultrafine-crystalline nickel-titanium alloy root The ultrafine grain nickel-titanium alloy in the tube has a particle diameter of 200 nm to 300 nm.
具体实施方式四： 本实施方式与具体实施方式三不同的是步驟一中所 述的镍钛合金铸锭的 Ti原子百分含量为 50.8%。 其它与具体实施方式三相 同。 Specific Embodiment 4: This embodiment differs from Embodiment 3 in the first step. The nickel-titanium alloy ingot has a Ti atomic percentage of 50.8%. Others are the same as the third embodiment.
具体实施方式五： 本实施方式与具体实施方式三不同的是步驟一中在 450°C进行 5道次的挤压。 其它与具体实施方式三相同。  BEST MODE FOR CARRYING OUT THE INVENTION V: This embodiment differs from the third embodiment in the first step of performing extrusion at 450 ° C for 5 passes. Others are the same as the third embodiment.
具体实施方式六： 本实施方式与具体实施方式三不同的是步驟三中将 长度为 31mm超细晶镍钛合金丝的一端加工出锥度为 0.04、 长为 16mm的 锥度丝。 其它与具体实施方式三相同。  DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Sixth embodiment: This embodiment differs from the third embodiment in that a taper wire having a taper of 0.04 and a length of 16 mm is machined at one end of a 31 mm-length ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
具体实施方式七： 本实施方式与具体实施方式三不同的是步驟三中将 长度为 25mm超细晶镍钛合金丝的一端加工出锥度为 0.06、 长为 16mm的 锥度丝。 其它与具体实施方式三相同。  BEST MODE FOR CARRYING OUT THE INVENTION Seventh Embodiment: This embodiment differs from the third embodiment in that a taper wire having a taper of 0.06 and a length of 16 mm is machined at one end of a 25 mm-length ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
具体实施方式八： 本实施方式与具体实施方式三不同的是步驟三中将 长度为 21mm超细晶镍钛合金丝的一端加工出锥度为 0.08、 长为 16mm的 锥度丝。 其它与具体实施方式三相同。  BEST MODE FOR CARRYING OUT THE INVENTION Eighth: This embodiment differs from the third embodiment in that a taper yarn having a taper of 0.08 and a length of 16 mm is machined at one end of a 21 mm-length ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
具体实施方式九： 本实施方式与具体实施方式三不同的是步驟三中将 长度为 28mm超细晶镍钛合金丝的一端加工出锥度为 0.10、 长为 16mm的 锥度丝。 其它与具体实施方式三相同。  BEST MODE FOR CARRYING OUT THE INVENTION Nineth Embodiment: This embodiment differs from the third embodiment in that a taper yarn having a taper of 0.10 and a length of 16 mm is machined at one end of a 28 mm ultrafine-grained nickel-titanium alloy wire in the third step. Others are the same as the third embodiment.
具体实施方式十： 本实施方式中超细晶镍钛合金根管锉的制备方法如 下：  DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Tenth Embodiment: The preparation method of the ultrafine-crystalline nickel-titanium root canal in the present embodiment is as follows:
一、 将 Ti 原子百分含量为 48-52%的镍钛合金棒拉拔成直径为 0.4-2.5mm、 长度为 31mm的丝材；  1. A nickel-titanium alloy rod having a Ti atomic percentage of 48-52% is drawn into a wire having a diameter of 0.4-2.5 mm and a length of 31 mm;
二、 将长度为 31mm的丝材浸入 50±5 °C的腐蚀溶液中， 在 35-65 °C将 丝材的一端加工出长度为 16-20mm、 锥度为 0.02-0.10 , 尖端直径为 0.15-0.4mm 的锥度丝， 然后将锥度丝切削加工出切刃， 得到超细晶镍钛合 金根管锉前驱体， 腐蚀溶液由 HF、 HN03和 ¾0组成， 其中 HF、 HN03与 H20的体积比为 1 :3:6; 三、 将超细晶镍钛合金根管锉前驱体在 350-650°C下保温 30-120min, 即得超细晶镍钛合金根管锉， 所得的超细晶镍钛合金根管锉中超细晶镍钛 合金粒径为 200nm-300nm。 2. The wire with a length of 31 mm is immersed in an etching solution of 50±5 °C, and one end of the wire is machined to a length of 16-20 mm, a taper of 0.02-0.10, and a tip diameter of 0.15 at 35-65 °C. 0.4mm taper wire, then the taper wire is cut into a cutting edge to obtain an ultrafine grain Nitinium root canal precursor, and the etching solution is composed of HF, HN0 3 and 3⁄40, wherein HF, HN0 3 and H 2 0 Volume ratio is 1:3:6; 3. The ultrafine-grained nickel-titanium root canal precursor is incubated at 350-650 ° C for 30-120 min to obtain ultra-fine-grained nickel-titanium root canal, and the obtained ultra-fine-crystalline nickel-titanium root canal is obtained. The ultrafine grain nickel titanium alloy has a particle diameter of 200 nm to 300 nm.
本实施方式步驟二中在锥度丝上采用无心研磨的方法加工出切刃； 本 实施方式步驟二中加工出切削刃的超细晶根管锉前躯体进行了表面电化学 抛光。  In the second step of the embodiment, the cutting edge is processed by the centerless grinding method on the tapered wire; in the second step of the embodiment, the ultrafine root canal front body processed by the cutting edge is subjected to surface electrochemical polishing.
采用下述实验验证本发明效果：  The effects of the present invention were verified by the following experiments:
实验一：  experiment one:
超细晶镍钛合金根管锉的制备方法如下：  The preparation method of ultrafine grain nickel-titanium root canal is as follows:
一、 镍钛合金超细晶处理： 将 Ti原子百分含量为 50.8%的镍钛合金铸 锭切割成直径为 20mm、 长度为 100mm的圆棒， 然后采用等径角挤压的方 法将圆棒分别通过两通道夹角为 90度和 120度的模具， 在 450°C进行 6道 次的挤压， 然后在 400°C下保温 50min, 得到超细晶处理后的镍钛合金棒； 二、 超细晶镍钛合金丝的制备方法： 将超细晶处理后的镍钛合金棒以 石墨乳为润滑剂， 在加热温度为 650°C、 线速度为 20m/s、 每道次压下量 1. Ultrafine grain treatment of nickel-titanium alloy: A nickel-titanium alloy ingot with a percentage of Ti atom of 50.8% is cut into a round rod with a diameter of 20 mm and a length of 100 mm, and then the round bar is extruded by equal-angle angular pressing. Through two molds with angles of 90 degrees and 120 degrees, 6 times of extrusion at 450 ° C, and then held at 400 ° C for 50 min, to obtain ultra-fine grain treated Nitinol rod; Preparation method of ultrafine grained nickel-titanium alloy wire: The ultrafine grain treated nickel-titanium alloy rod is made of graphite milk as a lubricant at a heating temperature of 650 ° C, a linear velocity of 20 m / s, and a reduction per pass.
0.02mm的条件下， 制备成直径为 0.52mm的超细晶镍钛合金丝； An ultrafine grain nickel titanium alloy wire having a diameter of 0.52 mm was prepared under conditions of 0.02 mm;
三、 超细晶镍钛合金丝锥度制备与根管锉切割刃成型处理：  Third, ultra-fine grain nickel-titanium alloy taper preparation and root canal cutting edge forming process:
将步驟二得到的超细晶镍钛合金丝剪成长度为 31mm的小段， 然后将 长度为 31mm超细晶镍钛合金丝的一端加工出锥度为 0.02、长为 16mm、尖 端直径为 0.2mm的锥度丝， 然后在锥度丝上切削加工出切刃， 得到超细晶 镍钛合金根管锉前驱体；  The ultrafine-grained nickel-titanium alloy wire obtained in the second step was cut into a small length of 31 mm, and then one end of the 31 mm ultrafine-grained nickel-titanium alloy wire was machined to have a taper of 0.02, a length of 16 mm, and a tip diameter of 0.2 mm. Taper wire, and then cutting the cutting edge on the taper wire to obtain an ultrafine grain nickel-titanium root canal precursor;
四、 将超细晶镍钛合金根管锉前驱体在 400°C保温 60min, 然后空冷， 即得超细晶镍钛合金根管锉。  4. The ultrafine-grained nickel-titanium root canal precursor is incubated at 400 ° C for 60 min, and then air-cooled to obtain an ultrafine-grained nickel-titanium root canal.
从图 1看出镍钛根管锉的基体平均晶粒尺寸为 290nm左右。  It can be seen from Fig. 1 that the average grain size of the base of the nickel-titanium root canal is about 290 nm.
从图 2看出室温下超细晶镍钛根管锉的相组成由马氏体和奥氏体组成， 并且衍射峰由于晶粒细化而明显宽化。 从图 3 看出超细晶镍钛根管锉 ( Ti-50.8at.%Ni )在使用温度下为奥氏体。 It can be seen from Fig. 2 that the phase composition of the ultrafine-grained nickel-titanium root canal at room temperature is composed of martensite and austenite. And the diffraction peak is significantly broadened due to grain refinement. It is seen from Fig. 3 that the ultrafine grained nickel titanium root canal (Ti-50.8 at.% Ni) is austenite at the use temperature.
将实验一步驟二中的超细晶镍钛合金丝经 SiC砂纸研磨和 A1203粉抛光 后，分别在显微硬度计和球-盘式摩擦磨损试验机上进行硬度和耐磨性测试， 为了进行比较，将常规镍钛合金和 400°C保温 60min热处理后的超细晶镍钛 合金分别在显微硬度计和球-盘式摩擦磨损试验机上进行硬度和耐磨性测 试。 The ultrafine-grained nickel-titanium alloy wire in the first step of the experiment was polished by SiC sandpaper and polished with A1 2 0 3 powder, and then tested for hardness and wear resistance on a microhardness tester and a ball-disk friction and wear tester, respectively. For comparison, the hardness and wear resistance of the conventional nickel-titanium alloy and the ultrafine-grained nickel-titanium alloy heat-treated at 400 ° C for 60 min were tested on a microhardness tester and a ball-disk friction and wear tester, respectively.
由图 4和图 5可知与常规镍钛合金相比， 超细晶处理后的镍钛合金和 经 400°C保温 60min热处理后的超细晶镍钛合金的硬度和耐磨性均有所提 高。 400°C保温 60min热处理后， 镍钛合金中形成细小弥散分布的析出相， 因而超细晶镍钛合金的硬度和耐磨性会进一步提高。  It can be seen from Fig. 4 and Fig. 5 that the hardness and wear resistance of the ultrafine grained nickel-titanium alloy and the ultrafine grained nickel-titanium alloy after heat treatment at 400 ° C for 60 minutes are improved compared with the conventional nickel-titanium alloy. . After heat treatment at 400 ° C for 60 minutes, a fine dispersion phase of the precipitated phase is formed in the nickel-titanium alloy, so that the hardness and wear resistance of the ultrafine grain nickel-titanium alloy are further improved.
从图 6、 图 7和图 8中可以看出，镍钛合金和超细晶镍钛合金以磨粒磨 损为主， 磨损表面上可见明显的沿摩擦方向的犁沟； 而热处理后的超细晶 镍钛合金以粘着磨损为主， 磨损表面上可见剥离和塑性变形的痕迹。  It can be seen from Fig. 6, Fig. 7 and Fig. 8 that the nickel-titanium alloy and the ultrafine-grained nickel-titanium alloy are mainly abrasive wear, and the furrows along the rubbing direction are visible on the worn surface; The crystal nickel-titanium alloy is mainly characterized by adhesive wear, and traces of peeling and plastic deformation are observed on the worn surface.
实验二：  Experiment 2:
超细晶镍钛合金根管锉的制备方法如下：  The preparation method of ultrafine grain nickel-titanium root canal is as follows:
一、 将 Ti原子百分含量为 50.8%的镍钛合金棒拉拔成直径为 2.5mm、 长度为 40mm的丝材；  1. A nickel-titanium alloy rod having a Ti atom content of 50.8% is drawn into a wire having a diameter of 2.5 mm and a length of 40 mm;
二、将丝材浸入腐蚀溶液中，在 50 °C将丝材的一端加工出长度为 16mm、 锥度为 0.04, 尖端直径为 0.2mm的锥度丝， 然后将锥度丝切削加工出切刃， 得到超细晶镍钛合金根管锉前驱体， 腐蚀溶液由 HF、 HN03和 ¾0组成， 其中 HF、 HN03与 ¾0的体积比为 1:3:6; 2. Dip the wire into the etching solution, and machine the taper wire with a length of 16mm, a taper of 0.04 and a tip diameter of 0.2mm at one end of the wire at 50 °C, and then cut the taper wire to produce a cutting edge. a fine-grained nickel-titanium root canal precursor, the etching solution consists of HF, HN0 3 and 3⁄40, wherein the volume ratio of HF, HN0 3 to 3⁄40 is 1:3:6;
三、 将超细晶镍钛合金根管锉前驱体在 500°C下保温 30min, 即得超细 晶镍钛合金根管锉。  3. The ultrafine-crystalline Nitinol root canal precursor is incubated at 500 ° C for 30 min to obtain an ultrafine-crystalline nickel-titanium root canal.

Claims

权利要求书 claims
1、 超细晶镍钛合金根管锉， 其特征在于超细晶镍钛合金根管锉由粒径 为 200nm-300nm的超细晶镍钛合金制成。 1. Ultra-fine-grained nickel-titanium alloy root canal file, which is characterized in that the ultra-fine-grained nickel-titanium alloy root canal file is made of ultra-fine-grained nickel-titanium alloy with a particle size of 200nm-300nm.
2、 根据权利要求 1所述超细晶镍钛合金根管锉， 其特征在于所述超细 晶镍钛合金根管锉由粒径为 290nm的超细晶镍钛合金制成。 2. The ultra-fine-grained nickel-titanium alloy root canal file according to claim 1, characterized in that the ultra-fine-grained nickel-titanium alloy root canal file is made of ultra-fine-grained nickel-titanium alloy with a particle size of 290 nm.
3、 权利要求 1所述超细晶镍钛合金根管锉的制备方法， 其特征在于超 细晶镍钛合金根管锉的制备方法如下： 3. The preparation method of the ultra-fine-grained nickel-titanium alloy root canal file according to claim 1, which is characterized in that the preparation method of the ultra-fine-grained nickel-titanium alloy root canal file is as follows:
一、镍钛合金超细晶处理： 将 Ti原子百分含量为 48-52%的镍钛合金铸 锭切割成直径为 20mm、 长度为 100mm的圆棒， 然后采用等径角挤压的方 法将圆棒分别通过两通道夹角为 90。 和 120。 的模具，在 400-500 °C进行 4-8 道次的挤压， 然后在 300-500 °C下保温 30-60min, 得到超细晶处理后的镍钛 合金棒； 1. Ultra-fine grain processing of nickel-titanium alloy: Cut the nickel-titanium alloy ingot with a Ti atomic percentage of 48-52% into round rods with a diameter of 20mm and a length of 100mm, and then use the method of equal diameter and angular extrusion. The angle between the round rods passing through the two channels is 90°. and 120. Use the mold to perform 4-8 passes of extrusion at 400-500 °C, and then keep it at 300-500 °C for 30-60 minutes to obtain an ultra-fine grained nickel-titanium alloy rod;
二、 超细晶镍钛合金丝的制备方法： 将超细晶处理后的镍钛合金棒以 石墨乳为润滑剂， 在加热温度为 600-700° (：、 线速度为 15-25m/s、 每道次压 下量 0.04-0.01mm的条件下，制备成直径为 0.4-2.5mm的超细晶镍钛合金丝； 三、 超细晶镍钛合金丝锥度制备与根管锉切割刃成型处理： 2. Preparation method of ultra-fine grained nickel-titanium alloy wire: Use graphite emulsion as lubricant to prepare ultra-fine-grained nickel-titanium alloy rods at a heating temperature of 600-700° (:) and a linear speed of 15-25m/s , Under the conditions of 0.04-0.01mm reduction per pass, prepare ultra-fine grained nickel-titanium alloy wire with a diameter of 0.4-2.5mm; 3. Preparation of ultra-fine-grained nickel-titanium alloy taper and root canal file cutting edge shaping deal with:
将步驟二得到的超细晶镍钛合金丝剪成长度为 21-40mm的小段， 然后 将长度为 21-40mm超细晶镍钛合金丝的一端加工出锥度为 0.02-0.10、 长为 16-20mm、 尖端直径为 0.15-0.4mm的锥度丝， 然后在锥度丝上切削加工出 切刃， 得到超细晶镍钛合金根管锉前驱体； Cut the ultra-fine grained nickel-titanium alloy wire obtained in step 2 into small sections with a length of 21-40mm, and then process one end of the ultra-fine-grained nickel-titanium alloy wire with a length of 21-40mm to have a taper of 0.02-0.10 and a length of 16- 20mm, a tapered wire with a tip diameter of 0.15-0.4mm, and then cutting a cutting edge on the tapered wire to obtain an ultra-fine-grained nickel-titanium alloy root canal file precursor;
四、 将超细晶镍钛合金根管锉前驱体在 350-650°C保温 30-120 min, 然 后空冷， 即得超细晶镍钛合金根管锉， 所得的超细晶镍钛合金根管锉中超 细晶镍钛合金粒径为 200nm-300nm。 4. The ultra-fine-grained nickel-titanium alloy root canal file precursor is kept at 350-650°C for 30-120 minutes, and then air-cooled to obtain an ultra-fine-grained nickel-titanium alloy root canal file. The obtained ultra-fine-grained nickel-titanium alloy root canal file is The particle size of ultra-fine-grained nickel-titanium alloy in pipe files is 200nm-300nm.
4、 根据权利要求 3所述超细晶镍钛合金根管锉的制备方法， 其特征在 于步驟一中所述的镍钛合金铸锭的 Ti原子百分含量为 50.8%。 4. The method for preparing ultra-fine-grained nickel-titanium alloy root canal files according to claim 3, characterized in that the Ti atomic percentage of the nickel-titanium alloy ingot described in step one is 50.8%.
5、 根据权利要求 3所述超细晶镍钛合金根管锉的制备方法， 其特征在 于步驟一中在 450 °C进行 6道次的挤压。 5. The method for preparing ultra-fine-grained nickel-titanium alloy root canal files according to claim 3, characterized in that in step one, 6 passes of extrusion are performed at 450°C.
6、 根据权利要求 3所述超细晶镍钛合金根管锉的制备方法， 其特征在 于步驟三中将长度为 31mm超细晶镍钛合金丝的一端加工出锥度为 0.04、 长为 16mm的锥度丝。 6. The method for preparing an ultra-fine-grained nickel-titanium alloy root canal file according to claim 3, characterized in that in step three, one end of an ultra-fine-grained nickel-titanium alloy wire with a length of 31 mm is processed to have a taper of 0.04 and a length of 16 mm. Tapered wire.
7、 根据权利要求 3所述超细晶镍钛合金根管锉的制备方法， 其特征在 于步驟三中将长度为 25mm超细晶镍钛合金丝的一端加工出锥度为 0.06、 长为 16mm的锥度丝。 7. The method for preparing an ultra-fine-grained nickel-titanium alloy root canal file according to claim 3, characterized in that in step three, one end of an ultra-fine-grained nickel-titanium alloy wire with a length of 25 mm is processed to have a taper of 0.06 and a length of 16 mm. Tapered wire.
8、 根据权利要求 3所述超细晶镍钛合金根管锉的制备方法， 其特征在 于步驟三中将长度为 21mm超细晶镍钛合金丝的一端加工出锥度为 0.08、 长为 16mm的锥度丝。 8. The method for preparing an ultra-fine-grained nickel-titanium alloy root canal file according to claim 3, characterized in that in step three, one end of an ultra-fine-grained nickel-titanium alloy wire with a length of 21 mm is processed to have a taper of 0.08 and a length of 16 mm. Tapered wire.
9、 根据权利要求 3所述超细晶镍钛合金根管锉的制备方法， 其特征在 于步驟三中将长度为 28mm超细晶镍钛合金丝的一端加工出锥度为 0.10、 长为 16mm的锥度丝。 9. The method for preparing an ultra-fine-grained nickel-titanium alloy root canal file according to claim 3, characterized in that in step three, one end of an ultra-fine-grained nickel-titanium alloy wire with a length of 28 mm is processed to have a taper of 0.10 and a length of 16 mm. Tapered wire.
10、 权利要求 1 所述超细晶镍钛合金根管锉的制备方法， 其特征在于 超细晶镍钛合金根管锉的制备方法如下： 10. The preparation method of the ultra-fine-grained nickel-titanium alloy root canal file described in claim 1, characterized in that the preparation method of the ultra-fine-grained nickel-titanium alloy root canal file is as follows:
一、 将 Ti 原子百分含量为 48-52%的镍钛合金棒拉拔成直径为 0.4-2.5mm、 长度为 40mm的丝材； 1. Draw a nickel-titanium alloy rod with a Ti atomic percentage of 48-52% into a wire with a diameter of 0.4-2.5mm and a length of 40mm;
二、 将长度为 31mm的丝材浸入 50±5°C的腐蚀溶液中， 在 35-65 °C将 丝材的一端加工出长度为 16-20mm、 锥度为 0.02-0.10 , 尖端直径为 2. Immerse the wire with a length of 31mm into the corrosive solution at 50±5°C, and process one end of the wire at 35-65°C to a length of 16-20mm, a taper of 0.02-0.10, and a tip diameter of
0.15-0.4mm 的锥度丝， 然后将锥度丝切削加工出切刃， 得到超细晶镍钛合 金根管锉前驱体， 腐蚀溶液由 HF、 HN03和 ¾0组成， 其中 HF、 HN03与 H20的体积比为 1 :3:6; 0.15-0.4mm taper wire, and then the taper wire is cut to form a cutting edge to obtain an ultra-fine-grained nickel-titanium alloy root canal file precursor. The corrosion solution is composed of HF, HN0 3 and ¾0, in which HF, HN0 3 and H 2 The volume ratio of 0 is 1:3:6;
三、 将超细晶镍钛合金根管锉前驱体在 350-650°C下保温 30-120min, 即得超细晶镍钛合金根管锉， 所得的超细晶镍钛合金根管锉中超细晶镍钛 合金粒径为 200nm-300nm。 3. Keep the ultra-fine-grained nickel-titanium alloy root canal file precursor at 350-650°C for 30-120 minutes to obtain an ultra-fine-grained nickel-titanium alloy root canal file. The obtained ultra-fine-grained nickel-titanium alloy root canal file contains Ultra-fine grained nickel titanium The alloy particle size is 200nm-300nm.
PCT/CN2013/079738 2012-07-24 2013-07-19 Ultra-fine grain nickel-titanium alloy root canal file and preparation method therefor WO2014015767A1 (en)

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