CN113385666A - Preparation method of artificial ossicle made of titanium - Google Patents
Preparation method of artificial ossicle made of titanium Download PDFInfo
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- 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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- titanium
- ossicle
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000010936 titanium Substances 0.000 title claims abstract description 33
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000005238 degreasing Methods 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 230000003197 catalytic effect Effects 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 18
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 15
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000002347 injection Methods 0.000 claims abstract description 5
- 239000007924 injection Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 239000004809 Teflon Substances 0.000 claims description 4
- 229920006362 Teflon® Polymers 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 210000003094 ear ossicle Anatomy 0.000 abstract description 11
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 210000001050 stape Anatomy 0.000 description 3
- 241000878128 Malleus Species 0.000 description 2
- 210000001785 incus Anatomy 0.000 description 2
- 210000003041 ligament Anatomy 0.000 description 2
- 210000002331 malleus Anatomy 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 210000000959 ear middle Anatomy 0.000 description 1
- 210000005069 ears Anatomy 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 210000003454 tympanic membrane Anatomy 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture 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
- B22F3/225—Manufacture 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal 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
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 ℃.
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Citations (8)
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---|---|---|---|---|
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 |
-
2021
- 2021-05-19 CN CN202110546138.1A patent/CN113385666A/en active Pending
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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 |
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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 * |
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