CN106965291A - A kind of gel injection-moulding 3D printing preparation method of gradient ceramic - Google Patents

A kind of gel injection-moulding 3D printing preparation method of gradient ceramic Download PDF

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Publication number
CN106965291A
CN106965291A CN201710223073.0A CN201710223073A CN106965291A CN 106965291 A CN106965291 A CN 106965291A CN 201710223073 A CN201710223073 A CN 201710223073A CN 106965291 A CN106965291 A CN 106965291A
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Prior art keywords
printing
ceramic
gradient
print
moulding
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CN201710223073.0A
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Inventor
吴操
朱平平
鲍文辕
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Nanjing First Three Dimensional Technology Co Ltd
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Nanjing First Three Dimensional Technology Co Ltd
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Priority to CN201710223073.0A priority Critical patent/CN106965291A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/001Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing

Abstract

The invention discloses a kind of gel injection-moulding 3D printing preparation method of gradient ceramic, specific method comprises the following steps:The foundation of threedimensional model, first passes through microcomputer modelling software modeling, then the threedimensional model built up " subregion " is cut into slices, so as to instruct printer successively to print into the section that thickness is 50~120 μm;The raw material proportioning of gradient ceramic, is required according to the composition design of gradient ceramic, calculates the component proportion of ceramic gradient structural member diverse location, and computer is inputted as variable, the powder feeding ratio of diverse location during control printing;The setting of print parameters, setting print speed is 0.2~0.5m/s, and 60~100 μm of print resolution is that powder sending quantity is 0.1~5mm3/s.The present invention uses 3D printing technique to increase material preparation method, compared with traditional handicraft, saves raw material, it is to avoid waste.

Description

A kind of gel injection-moulding 3D printing preparation method of gradient ceramic
Technical field
The present invention relates to gradient ceramic field shaping technique, more particularly to a kind of gel injection-moulding of gradient ceramic 3D printing preparation method.
Background technology
Ceramic FGM combines the characteristics such as the corrosion-and high-temp-resistant of ceramic material and the group of FGM The characteristics of dividing consecutive variations and controllable performance, there is important application valency in fields such as national defense and military, biologic medical, machinings Value.Especially with the rise of superelevation velocity of sound aircraft, many performance ceramic material demands of high intensity are urgent again simultaneously for high temperature resistant, And require that the different parts of some parts possess different performances, but general homogeneous material is extremely difficult to this requirement, because This disclosure satisfy that the FGM of this condition turns into the focus of research.
The main preparation method of ceramic FGM is gel casting, and gel casting is by U.S. Oak Tree The wet-forming technique of ridge National Laboratory invention, the technology is set up on the basis of conventional forming techniques and producing high-molecular theory On, its core is to use organic monomer solution, and the solution can aggregate into high intensity, the polymer gel of lateral connection, make slurry Expect in-situ solidifying formation base substrate, densification product is obtained through drying, sintering.Compared with conventional wet forming technology, with easy shaping The advantages of complicated shape large-scale part, body composition are uniform, intensity is high, defect is few, but gel casting is preparing ceramics It is difficult to ensure that the uniformity of gel, can exist when uniformity is poor on the quality of finished-product material influences, institute during FGM To be left to be desired on ceramic slurry homogeneity question is prepared, while sizing material molding rate is slower, production efficiency is low.
The content of the invention
It is contemplated that at least solving one of technical problem in correlation technique to a certain extent.Therefore, the present invention One purpose is the gel injection-moulding 3D printing preparation method for proposing a kind of gradient ceramic, and 3D printing technique is prepared to increase material Method, compared with traditional handicraft, saves raw material, it is to avoid waste.
A kind of gel injection-moulding 3D printing preparation method of gradient ceramic proposed by the present invention, specific method includes following Step:
A. the foundation of threedimensional model
First pass through microcomputer modelling software modeling, then by the threedimensional model built up " subregion " into thickness be 50~120 μm Section, that is, cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, calculate the component proportion of ceramic gradient structural member diverse location, Computer is inputted as variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.2~0.5m/s, and 60~100 μm of print resolution is that powder sending quantity is 0.1~5mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 0.05~10 μm of ceramic powder component; Organic monomer and crosslinking agent are pressed 10~20:1 weight ratio is dissolved in deionized water, be made into organic matter mass fraction for 10~ 20% premixed liquid;Premixed liquid is loaded into the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device and carry out 3D printing, feed appliance enters 3D printheads, the first transfusion according to the proportioning feeding of setting Rifle and the second transfusion rifle send into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, Printed according to the track of setting, speed;According to trajectory, printing line by line forms face, then successively printing forms three-dimensional ceramic ladder Spend material;In print procedure, control work room temperature is at 50~70 DEG C, in favor of gel process;
F. sinter
Take out green compact be put into sintering furnace, be filled with argon gas or nitrogen protected, sintering temperature 600~1000 DEG C it Between, sintering time 3~5 hours closes heating power supply after the completion of sintering, taken out after being cooled down 8~10 hours with sintering furnace.
Preferably, the crosslinking agent is methylene-bisacrylamide, hydroxy propyl methacrylate, divinylbenzene, N- hydroxyls One or more in Methacrylamide, DAAM.
Preferably, the organic monomer is one kind in acrylamide, Methacrylamide or vinyl pyrrole ketone.
Preferably, the premixed liquid addition and the volume ratio of solid phase ceramic powders are 6~10:1.
Preferably, the catalyst is tetramethylethylenediamine.
Compared with prior art, the beneficial effect in the present invention is:
(1) strictly control the raw material components at diverse location to match by computer, then pass through the first transfusion rifle, second defeated Liquid rifle carries out Mechanical course to slurry, makes slurry more uniform, so as to truly realize the gradient distribution of composition;
(2) feeding, mixing, printing and gel are completed simultaneously using 3D printing, improves operating efficiency;
(3) 3D printing technique compared with traditional handicraft, saves raw material to increase material preparation method, it is to avoid waste.
Embodiment
Embodiment 1
A. the foundation of threedimensional model
Microcomputer modelling software modeling is first passed through, then by the threedimensional model built up " subregion " into the section that thickness is 50 μm, Cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, calculate the component proportion of ceramic gradient structural member diverse location, Computer is inputted as variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.2m/s, and 60 μm of print resolution is that powder sending quantity is 0.1mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 0.05 μm of ceramic powder component;To have Machine monomer presses 10 with crosslinking agent:1 weight ratio is dissolved in deionized water, is made into the premixed liquid that organic matter mass fraction is 10%; Premixed liquid is loaded into the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device and carry out 3D printing, feed appliance enters 3D printing head, the first transfusion according to the proportioning feeding of setting Rifle and the second transfusion rifle send into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, Printed according to the track of setting, speed;According to trajectory, printing line by line forms face, then successively printing forms three-dimensional ceramic ladder Spend material;In print procedure, control work room temperature is at 50 DEG C, in favor of gel process;
F. sinter
Take out green compact to be put into sintering furnace, be filled with argon gas or nitrogen is protected, sintering temperature is between 600 DEG C, sintering 3 hours time, heating power supply is closed after the completion of sintering, taken out after being cooled down 8 hours with sintering furnace.
Crosslinking agent is methylene-bisacrylamide;
Organic monomer is acrylamide;
Premixed liquid addition and the volume ratio of solid phase ceramic powders are 6:1.
Embodiment 2
A. the foundation of threedimensional model
Microcomputer modelling software modeling is first passed through, then by the threedimensional model built up " subregion " into the section that thickness is 70 μm, Cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, calculate the component proportion of ceramic gradient structural member diverse location, Computer is inputted as variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.3m/s, and 70 μm of print resolution is that powder sending quantity is 1mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 0.5 μm of ceramic powder component;To have Machine monomer presses 15 with crosslinking agent:1 weight ratio is dissolved in deionized water, is made into the premixed liquid that organic matter mass fraction is 12%; Premixed liquid is loaded into the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device and carry out 3D printing, feed appliance enters 3D printing head, the first transfusion according to the proportioning feeding of setting Rifle and the second transfusion rifle send into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, Printed according to the track of setting, speed;According to trajectory, printing line by line forms face, then successively printing forms three-dimensional ceramic ladder Spend material;In print procedure, control work room temperature is at 60 DEG C, in favor of gel process;
F. sinter
Take out green compact to be put into sintering furnace, be filled with argon gas or nitrogen is protected, sintering temperature is between 700 DEG C, sintering 4 hours time, heating power supply is closed after the completion of sintering, taken out after being cooled down 9 hours with sintering furnace.
Crosslinking agent is hydroxy propyl methacrylate;
Organic monomer is Methacrylamide;
Premixed liquid addition and the volume ratio of solid phase ceramic powders are 7:1.
Embodiment 3
A. the foundation of threedimensional model
Microcomputer modelling software modeling is first passed through, then by the threedimensional model built up " subregion " into the section that thickness is 80 μm, Cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, calculate the component proportion of ceramic gradient structural member diverse location, Computer is inputted as variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.4m/s, and 80 μm of print resolution is that powder sending quantity is 2.5mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 2 μm of ceramic powder component;Will be organic Monomer presses 15 with crosslinking agent:1 weight ratio is dissolved in deionized water, is made into the premixed liquid that organic matter mass fraction is 14%;Will Premixed liquid loads the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device and carry out 3D printing, feed appliance enters 3D printing head, the first transfusion according to the proportioning feeding of setting Rifle and the second transfusion rifle send into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, Printed according to the track of setting, speed;According to trajectory, printing line by line forms face, then successively printing forms three-dimensional ceramic ladder Spend material;In print procedure, control work room temperature is at 65 DEG C, in favor of gel process;
F. sinter
Take out green compact to be put into sintering furnace, be filled with argon gas or nitrogen is protected, sintering temperature is between 700 DEG C, sintering 3 hours time, heating power supply is closed after the completion of sintering, taken out after being cooled down 9 hours with sintering furnace.
Crosslinking agent is hydroxy propyl methacrylate, N hydroxymethyl acrylamide, and mixed proportion is 2:1;
Organic monomer is vinyl pyrrole ketone;
Premixed liquid addition and the volume ratio of solid phase ceramic powders are 8:1.
Embodiment 4
A. the foundation of threedimensional model
Microcomputer modelling software modeling is first passed through, then by the threedimensional model built up " subregion " into the section that thickness is 100 μm, Cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, calculate the component proportion of ceramic gradient structural member diverse location, Computer is inputted as variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.5m/s, and 100 μm of print resolution is that powder sending quantity is 3.5mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 8 μm of ceramic powder component;Will be organic Monomer presses 20 with crosslinking agent:1 weight ratio is dissolved in deionized water, is made into the premixed liquid that organic matter mass fraction is 18%;Will Premixed liquid loads the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device and carry out 3D printing, feed appliance enters 3D printing head, the first transfusion according to the proportioning feeding of setting Rifle and the second transfusion rifle send into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, Printed according to the track of setting, speed;According to trajectory, printing line by line forms face, then successively printing forms three-dimensional ceramic ladder Spend material;In print procedure, control work room temperature is at 70 DEG C, in favor of gel process;
F. sinter
Take out green compact to be put into sintering furnace, be filled with argon gas or nitrogen is protected, sintering temperature is between 900 DEG C, sintering 5 hours time, heating power supply is closed after the completion of sintering, taken out after being cooled down 10 hours with sintering furnace.
Crosslinking agent is hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, and mixed proportion is 2:1:1;
Organic monomer is Methacrylamide;
Premixed liquid addition and the volume ratio of solid phase ceramic powders are 9:1.
Embodiment 5
A. the foundation of threedimensional model
Microcomputer modelling software modeling is first passed through, then by the threedimensional model built up " subregion " into the section that thickness is 120 μm, Cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, calculate the component proportion of ceramic gradient structural member diverse location, Computer is inputted as variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.45m/s, and 100 μm of print resolution is that powder sending quantity is 5mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 10 μm of ceramic powder component;Will be organic Monomer presses 19 with crosslinking agent:1 weight ratio is dissolved in deionized water, is made into the premixed liquid that organic matter mass fraction is 20%;Will Premixed liquid loads the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device and carry out 3D printing, feed appliance enters 3D printing head, the first transfusion according to the proportioning feeding of setting Rifle and the second transfusion rifle send into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, Printed according to the track of setting, speed;According to trajectory, printing line by line forms face, then successively printing forms three-dimensional ceramic ladder Spend material;In print procedure, control work room temperature is at 70 DEG C, in favor of gel process;
F. sinter
Take out green compact to be put into sintering furnace, be filled with argon gas or nitrogen is protected, sintering temperature is between 1000 DEG C, sintering 5 hours time, heating power supply is closed after the completion of sintering, taken out after being cooled down 10 hours with sintering furnace.
Crosslinking agent is methylene-bisacrylamide, hydroxy propyl methacrylate, divinylbenzene, N- methylol acryloyls Amine, DAAM, mixed proportion are 1:1:1:1:1;
Organic monomer is acrylamide;
Premixed liquid addition and the volume ratio of solid phase ceramic powders are 10:1.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.

Claims (5)

1. the gel injection-moulding 3D printing preparation method of a kind of gradient ceramic, it is characterised in that specific method includes following step Suddenly:
A. the foundation of threedimensional model
Microcomputer modelling software modeling is first passed through, then by the threedimensional model built up " subregion " into the section that thickness is 50~120 μm, Cut into slices, so as to instruct printer successively to print;
B. the raw material proportioning of gradient ceramic
Required according to the composition design of gradient ceramic, the component proportion of ceramic gradient structural member diverse location is calculated, with this Computer is inputted for variable, the powder feeding ratio of diverse location during control printing;
C. the setting of print parameters
Setting print speed is 0.2~0.5m/s, and 60~100 μm of print resolution is that powder sending quantity is 0.1~5mm3/s;
D. the preparation of raw material
Particle diameter is respectively put into the feed cylinder in feed appliance after pretreatment for 0.05~10 μm of ceramic powder component;To have Machine monomer presses 10~20 with crosslinking agent:1 weight ratio is dissolved in deionized water, and it is 10~20% to be made into organic matter mass fraction Premixed liquid;Premixed liquid is loaded into the first transfusion rifle;Initiator and catalyst are loaded into the second transfusion rifle;
E. gel injection-moulding 3D printing
Start printing device carry out 3D printing, feed appliance according to setting proportioning feeding enter 3D printing head, first transfusion rifle and Second transfusion rifle sends into premixed liquid, initiator and catalyst to 3D printing head;Above-mentioned raw materials in printhead after mixing, according to The track of setting, speed are printed;According to trajectory, printing forms face line by line, then successively printing forms three-dimensional ceramic gradient material Material;In print procedure, control work room temperature is at 50~70 DEG C, in favor of gel process;
F. sinter
Take out green compact to be put into sintering furnace, be filled with argon gas or nitrogen is protected, sintering temperature is burnt between 600~1000 DEG C 3~5 hours knot time, heating power supply is closed after the completion of sintering, taken out after being cooled down 8~10 hours with sintering furnace.
2. a kind of gel injection-moulding 3D printing preparation method of gradient ceramic according to claim 1, it is characterised in that: The crosslinking agent is methylene-bisacrylamide, hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, double One or more in acetone acrylamide.
3. a kind of gel injection-moulding 3D printing preparation method of gradient ceramic according to claim 1, it is characterised in that: The organic monomer is one kind in acrylamide, Methacrylamide or vinyl pyrrole ketone.
4. a kind of gel injection-moulding 3D printing preparation method of gradient ceramic according to claim 1, it is characterised in that: The premixed liquid addition and the volume ratio of solid phase ceramic powders are 6~10:1.
5. a kind of gel injection-moulding 3D printing preparation method of gradient ceramic according to claim 1, it is characterised in that: The catalyst is tetramethylethylenediamine.
CN201710223073.0A 2017-04-07 2017-04-07 A kind of gel injection-moulding 3D printing preparation method of gradient ceramic Pending CN106965291A (en)

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CN107417262A (en) * 2017-09-20 2017-12-01 吴江中瑞机电科技有限公司 3D printing technique prepares material of graded ceramicses and preparation method thereof
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CN107963886A (en) * 2017-12-24 2018-04-27 湖南工业大学 A kind of water-based titanium dioxide zirconium base 3D printing base substrate method and its forming method
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CN107986763A (en) * 2017-12-24 2018-05-04 湖南工业大学 A kind of water-based 3D printing base substrate method and its forming method
CN108017394A (en) * 2017-12-24 2018-05-11 湖南工业大学 A kind of water-based nitridation silicon substrate 3D printing base substrate method and its forming method
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CN108031835A (en) * 2017-12-24 2018-05-15 湖南工业大学 A kind of ink WC bases stainless steel powder 3D printing base substrate method and its forming method
CN108044110A (en) * 2017-12-24 2018-05-18 湖南工业大学 A kind of ink WC base cemented carbides 3D printing green body method and its forming method
CN111317589A (en) * 2019-11-29 2020-06-23 南昌市第一医院 Manufacturing method of gum expander
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CN113620717A (en) * 2021-09-03 2021-11-09 萍乡旭材科技有限公司 Preparation method of silicon nitride ceramic with gradient layered structure
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CN107417262A (en) * 2017-09-20 2017-12-01 吴江中瑞机电科技有限公司 3D printing technique prepares material of graded ceramicses and preparation method thereof
CN107877848A (en) * 2017-12-24 2018-04-06 湖南工业大学 A kind of copper-based powder 3D printing base substrate method of ink WC bases and its forming method
CN107876779A (en) * 2017-12-24 2018-04-06 湖南工业大学 A kind of water nano silver 3D printing base substrate method and its forming method
CN107963886A (en) * 2017-12-24 2018-04-27 湖南工业大学 A kind of water-based titanium dioxide zirconium base 3D printing base substrate method and its forming method
CN107963892A (en) * 2017-12-24 2018-04-27 湖南工业大学 A kind of ink silicon-nitride-based ceramic powder 3D printing base substrate method and its forming method
CN107973875A (en) * 2017-12-24 2018-05-01 湖南工业大学 A kind of ink 3D printing base substrate method and its forming method
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CN108017394A (en) * 2017-12-24 2018-05-11 湖南工业大学 A kind of water-based nitridation silicon substrate 3D printing base substrate method and its forming method
CN108017378A (en) * 2017-12-24 2018-05-11 湖南工业大学 A kind of water-based alumina base 3D printing base substrate method and its forming method
CN108031835A (en) * 2017-12-24 2018-05-15 湖南工业大学 A kind of ink WC bases stainless steel powder 3D printing base substrate method and its forming method
CN108044110A (en) * 2017-12-24 2018-05-18 湖南工业大学 A kind of ink WC base cemented carbides 3D printing green body method and its forming method
CN111317589A (en) * 2019-11-29 2020-06-23 南昌市第一医院 Manufacturing method of gum expander
CN111317589B (en) * 2019-11-29 2021-06-18 南昌市第一医院 Manufacturing method of gum expander
CN113292332A (en) * 2021-06-11 2021-08-24 四川大学 Calcium phosphate ceramic high-throughput screening model based on 3D printing, preparation method and application
CN113620717A (en) * 2021-09-03 2021-11-09 萍乡旭材科技有限公司 Preparation method of silicon nitride ceramic with gradient layered structure
CN115042428A (en) * 2022-06-07 2022-09-13 山东大学 Additive manufacturing method for constructing multiple continuous gradient functional bone scaffold

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Application publication date: 20170721