CN113385666A - Preparation method of artificial ossicle made of titanium - Google Patents

Preparation method of artificial ossicle made of titanium Download PDF

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Publication number
CN113385666A
CN113385666A CN202110546138.1A CN202110546138A CN113385666A CN 113385666 A CN113385666 A CN 113385666A CN 202110546138 A CN202110546138 A CN 202110546138A CN 113385666 A CN113385666 A CN 113385666A
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China
Prior art keywords
titanium
ossicle
preparing
blank
artificial
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CN202110546138.1A
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Chinese (zh)
Inventor
陶忠
林龑
史庆
吴越
王海军
王昊飞
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Baiwei Wuhan Medical Technology Co ltd
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Baiwei Wuhan Medical Technology Co ltd
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Priority to CN202110546138.1A priority Critical patent/CN113385666A/en
Publication of CN113385666A publication Critical patent/CN113385666A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • C22C1/0458Alloys based on titanium, zirconium or hafnium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a preparation method of a titanium artificial ossicle, which comprises the following steps: mixing titanium or titanium alloy powder and a binder, and putting the mixture into a mixing roll for mixing to obtain a feed; heating the feed to a liquid state, injecting the liquid feed into a mold for preparing the ossicle through an injection machine, cooling and molding the feed to obtain a blank, and coating an anti-adhesion coating on the inner cavity of the mold; carrying out catalytic degreasing on the blank, and carrying out heating degreasing after the catalytic degreasing to obtain a dry blank; and baking the dry blank to obtain the artificial ossicle. Compared with mechanical processing, the invention does not generate cutting force and is more suitable for producing the tiny titanium auditory ossicle. The density of the ossicle prepared by the invention is more than or equal to 93 percent, and the tensile strength is more than or equal to 580 Mpa.

Description

Preparation method of artificial ossicle made of titanium
Technical Field
The invention belongs to the technical field of medical instruments, and particularly relates to a preparation method of a titanium artificial ossicle.
Background
The ossicle is the smallest bone in the human body, and each of the three ossicles of the left and right ears consists of a malleus, an incus and a stapes, and most of them are located in the upper tympanic cavity and connected by ligaments and joints to form an ossicular chain. The malleus handle is arranged on the inner side surface of the tympanic membrane and is positioned between the mucosa layer and the fiber layer. The stapes footplate is connected to the oval window by an annular ligament. Between the hammer and the stapes is the incus.
Because the auditory ossicle has an extremely small volume and has a structure with a plurality of thin walls and thin rods, if mechanical processing is carried out, precise five-axis processing equipment is needed, a cutter is small and easy to damage, and a workpiece is easy to deform and break due to insufficient strength, so that the workpiece is scrapped.
Disclosure of Invention
The invention aims to provide a preparation method of a titanium artificial ossicle. Compared with mechanical processing, the invention does not generate cutting force and is more suitable for producing the tiny titanium auditory ossicle. The density of the ossicle prepared by the invention is more than or equal to 93 percent, and the tensile strength is more than or equal to 580 Mpa.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing a titanium artificial ossicle comprises the following steps:
s1, mixing titanium or titanium alloy powder and a binder, and putting the mixture into a mixing roll for mixing to obtain a feed;
s2, heating the feed to be in a liquid state, injecting the liquid feed into a mold for preparing the ossicle through an injection machine, cooling and molding the feed to obtain a blank, and coating an anti-adhesion coating on the inner cavity of the mold;
s3, carrying out catalytic degreasing on the blank, and heating and degreasing after the catalytic degreasing to obtain a dry blank;
and S4, baking the dry blank to obtain the artificial ossicle.
As a further improvement of the technical proposal, the artificial ossicle obtained in the step S4 is further subjected to vacuum heat treatment.
Preferably, the temperature of the vacuum heat treatment is 685-695 ℃.
Preferably, in step S1, the mesh number of the titanium or titanium alloy powder is 650-2000 mesh.
Preferably, in step S1, the binder is composed of 35% polyethylene, 55% paraffin wax, and 10% stearic acid.
Preferably, in step S1, the parameters of the mixing mill are: the mixing temperature is 175 ℃ and 185 ℃, and the mixing time is 1-3 hours.
Preferably, in step S2, the anti-blocking coating is a teflon coating.
Preferably, in step S3, the specific steps of catalytic degreasing are: and (3) putting the blank into a catalytic degreasing furnace for heating, and introducing oxalic acid into the furnace.
Preferably, in step S3, the heating degreasing step is: and (4) putting the blank subjected to catalytic degreasing into a thermal degreasing furnace for heating.
Preferably, in step S4, the baking uses a vacuum baking oven.
Preferably, in step S4, the baking temperature is 1240 ℃ to 1255 ℃.
Any range recited herein is intended to include the endpoints and any number between the endpoints and any subrange subsumed therein or defined therein.
The starting materials of the present invention are commercially available, unless otherwise specified, and the equipment used in the present invention may be any equipment conventionally used in the art or may be any equipment known in the art.
Compared with the prior art, the invention has the following beneficial effects:
compared with mechanical processing, the invention does not generate cutting force and is more suitable for producing tiny titanium auditory ossicles; the density of the ossicle prepared by the invention is more than or equal to 93 percent, and the tensile strength is more than or equal to 580 Mpa.
Drawings
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings
FIG. 1 is a flow chart of the method for preparing the artificial ossicle of the invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like, as used herein, refer to an orientation or positional relationship indicated in the drawings that is solely for the purpose of facilitating the description and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and is therefore not to be construed as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1, as one aspect of the present invention, a method for preparing a titanium artificial auditory ossicle according to the present invention comprises the following steps:
s1, mixing titanium or titanium alloy powder and a binder, and putting the mixture into a mixing roll for mixing to obtain a feed;
s2, heating the feed to be in a liquid state, injecting the liquid feed into a mold for preparing the ossicle through an injection machine, cooling and molding the feed to obtain a blank, and coating an anti-adhesion coating on the inner cavity of the mold;
s3, carrying out catalytic degreasing on the blank, and heating and degreasing after the catalytic degreasing to obtain a dry blank;
and S4, baking the dry blank to obtain the artificial ossicle.
In certain preferred embodiments, the artificial ossicle obtained in step S4 is further vacuum heat treated. The stress generated in the mechanical processing is eliminated, and the vacuum heat treatment can ensure that the workpiece does not generate chemical reaction when being heated.
In certain embodiments, the temperature of the vacuum heat treatment is 685-.
In some embodiments, in step S1, the mesh size of the titanium or titanium alloy powder is 650-2000 mesh; because the artificial ossicles have small sizes, the mesh number of the powder is too small, the produced product is not compact, and the cost is increased due to too large mesh number.
In certain embodiments, in step S1, the binder is composed of 35% polyethylene, 55% paraffin wax, and 10% stearic acid.
In certain embodiments, in step S1, the parameters of the mixer are: the mixing temperature is 175 ℃ and 185 ℃, and the mixing time is 1-3 hours.
In certain embodiments, in step S2, the anti-blocking coating is a teflon coating that prevents sticking of the blank and the mold during demolding.
In certain embodiments, in step S3, the specific steps of catalytic degreasing are: and (3) putting the blank into a catalytic degreasing furnace for heating, and introducing oxalic acid into the furnace.
In some embodiments, in step S3, the heating for degreasing specifically comprises: and (4) putting the blank subjected to catalytic degreasing into a thermal degreasing furnace for heating.
In certain embodiments, in step S4, the baking uses a vacuum bake oven.
In certain embodiments, the temperature of the baking in step S4 is 1240 ℃ to 1255 ℃. Too low a temperature may result in inefficient bonding of the metal powder, and too high a temperature may result in excessive melting of the powder and failure to retain its original shape.
Example 1
A method for preparing a titanium artificial ossicle comprises the following steps:
s1, mixing titanium or titanium alloy powder and a binder, and putting the mixture into a mixing roll for mixing to obtain a feed;
s2, heating the feed to be in a liquid state, injecting the liquid feed into a mold for preparing the ossicle through an injection machine, cooling and molding the feed to obtain a blank, and coating an anti-adhesion coating on the inner cavity of the mold;
s3, carrying out catalytic degreasing on the blank, and heating and degreasing after the catalytic degreasing to obtain a dry blank;
s4, baking the dry blank to obtain an artificial ossicle;
s5, carrying out vacuum heat treatment on the artificial ossicle obtained in the step S4;
the temperature of the vacuum heat treatment is 685 ℃ ℃695 ℃;
in step S1, the mesh number of the titanium or titanium alloy powder is 650;
in step S1, the binder is composed of 35% polyethylene, 55% paraffin wax, and 10% stearic acid;
in step S1, the parameters of the mixer are: the mixing temperature is 180 ℃, and the mixing time is 2 hours.
In step S2, the anti-adhesion coating is a teflon coating;
in step S3, the catalytic degreasing specifically comprises: putting the blank into a catalytic degreasing furnace for heating, and introducing oxalic acid into the furnace;
in step S3, the heating degreasing specifically includes: putting the blank after catalytic degreasing into a thermal degreasing furnace for heating;
in step S4, the baking is performed using a vacuum baking oven;
in step S4, the baking temperature is 1240 ℃.
Through detection, the density of the artificial auditory ossicle obtained by the embodiment is 94%, the tensile strength is 581Mpa, the surface is continuous, sharp edges, burrs and attachments do not exist, and the requirements of the medical artificial auditory ossicle are met.
Example 2
Example 1 was repeated with the only difference that:
in step S1, the mesh number of the titanium or titanium alloy powder is 2000;
in step S1, the parameters of the mixer are: the mixing temperature is 175 ℃, and the mixing time is 1 hour.
In step S4, the baking temperature is 1255 ℃.
Through detection, the density of the auditory ossicle obtained by the embodiment is 95%, the tensile strength is 583Mpa, the surface is continuous, sharp edges, burrs and attachments do not exist, and the requirement of the medical artificial auditory ossicle is met.
Example 3
Example 1 was repeated with the only difference that:
in step S1, the mesh number of the titanium or titanium alloy powder is 1000;
in step S1, the parameters of the mixer are: the mixing temperature is 185 ℃, and the mixing time is 3 hours.
In step S4, the baking temperature is 1250 ℃.
Through detection, the density of the ossicle obtained by the embodiment is 97%, the tensile strength is 590Mpa, the surface is continuous, and no sharp edge, burr or attachment exists. Meets the medical requirements for artificial auditory ossicles.
Comparative example 1
Example 1 was repeated with the only difference that: in step S1, the mesh number of the titanium or titanium alloy powder is 500. Through detection, the density of the auditory ossicles obtained by the comparative example is 75%, and the tensile strength is 490 Mpa.
Comparative example 2
Example 1 was repeated with the only difference that: in step S4, the baking temperature is 1100 ℃. Through detection, the density obtained by the comparative example is 55%, and the tensile strength is 70 MPa.
Comparative example 3
Example 1 was repeated with the only difference that: in step S4, the baking temperature is 1300 ℃. Through detection, the ossicle obtained by the comparative example has excessive melting and can not keep the original shape.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.

Claims (10)

1. A preparation method of a titanium artificial ossicle is characterized by comprising the following steps:
s1, mixing titanium or titanium alloy powder and a binder, and putting the mixture into a mixing roll for mixing to obtain a feed;
s2, heating the feed to be in a liquid state, injecting the liquid feed into a mold for preparing the ossicle through an injection machine, cooling and molding the feed to obtain a blank, and coating an anti-adhesion coating on the inner cavity of the mold;
s3, carrying out catalytic degreasing on the blank, and heating and degreasing after the catalytic degreasing to obtain a dry blank;
and S4, baking the dry blank to obtain the artificial ossicle.
2. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: and (4) carrying out vacuum heat treatment on the artificial ossicle obtained in the step S4.
3. The method for preparing an artificial ossicle made of titanium as claimed in claim 2, characterized in that: the temperature of the vacuum heat treatment is 685-695 ℃.
4. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S1, the mesh number of the titanium or titanium alloy powder is 650-2000 mesh.
5. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S1, the adhesive is composed of 35% polyethylene, 55% paraffin wax, and 10% stearic acid.
6. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S1, the parameters of the mixer are: the mixing temperature is 175 ℃ and 185 ℃, and the mixing time is 1-3 hours.
7. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S2, the anti-blocking coating is a teflon coating.
8. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S3, the catalytic degreasing specifically comprises: and (3) putting the blank into a catalytic degreasing furnace for heating, and introducing oxalic acid into the furnace.
9. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S3, the heating degreasing specifically includes: and (4) putting the blank subjected to catalytic degreasing into a thermal degreasing furnace for heating.
10. The method for preparing an artificial ossicle made of titanium as claimed in claim 1, characterized in that: in step S4, the baking is performed using a vacuum baking oven;
preferably, in step S4, the baking temperature is 1240 ℃ to 1255 ℃.
CN202110546138.1A 2021-05-19 2021-05-19 Preparation method of artificial ossicle made of titanium Pending CN113385666A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06339489A (en) * 1993-02-26 1994-12-13 Asahi Optical Co Ltd Artificial auditory ossicle
JPH07329097A (en) * 1994-06-06 1995-12-19 Olympus Optical Co Ltd Injection molding method of metallic powder
US20110266724A1 (en) * 2009-05-08 2011-11-03 Hoowaki, Llc Method for manufacturing microstructured metal or ceramic parts from feedstock
CN106563808A (en) * 2016-10-14 2017-04-19 安泰科技股份有限公司 Passive middle ear implantation device and preparation method for same
CN108852569A (en) * 2018-05-21 2018-11-23 柏为(武汉)医疗科技股份有限公司 A kind of degradable support diaphragm apparatus for preventing and treating Asherman's syndrom
WO2020130426A1 (en) * 2018-12-17 2020-06-25 (주) 엘지화학 Injection mold, injection molding machine comprising same, and method for manufacturing injection product by using same
US10828816B1 (en) * 2017-02-14 2020-11-10 University Of North Florida Board Of Trustees 3D printed injection mold coating to extend lifetime and performance
CN112402055A (en) * 2020-12-04 2021-02-26 柏为(武汉)医疗科技股份有限公司 Similar ring-shaped ossicle prosthesis

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06339489A (en) * 1993-02-26 1994-12-13 Asahi Optical Co Ltd Artificial auditory ossicle
JPH07329097A (en) * 1994-06-06 1995-12-19 Olympus Optical Co Ltd Injection molding method of metallic powder
US20110266724A1 (en) * 2009-05-08 2011-11-03 Hoowaki, Llc Method for manufacturing microstructured metal or ceramic parts from feedstock
CN106563808A (en) * 2016-10-14 2017-04-19 安泰科技股份有限公司 Passive middle ear implantation device and preparation method for same
US10828816B1 (en) * 2017-02-14 2020-11-10 University Of North Florida Board Of Trustees 3D printed injection mold coating to extend lifetime and performance
CN108852569A (en) * 2018-05-21 2018-11-23 柏为(武汉)医疗科技股份有限公司 A kind of degradable support diaphragm apparatus for preventing and treating Asherman's syndrom
WO2020130426A1 (en) * 2018-12-17 2020-06-25 (주) 엘지화학 Injection mold, injection molding machine comprising same, and method for manufacturing injection product by using same
CN112402055A (en) * 2020-12-04 2021-02-26 柏为(武汉)医疗科技股份有限公司 Similar ring-shaped ossicle prosthesis

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘建华等: "《材料成型工艺基础(第三版)》", 29 February 2016, 西安电子科技大学出版社 *
罗铁钢等: "粉末微注射成形的现状与展望", 《粉末冶金工业》 *
范景莲, 中国标准出版社 *

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