CN113154882B - Pressureless rapid sintering device and sintering method for 3D printing - Google Patents
Pressureless rapid sintering device and sintering method for 3D printing Download PDFInfo
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- CN113154882B CN113154882B CN202110460023.0A CN202110460023A CN113154882B CN 113154882 B CN113154882 B CN 113154882B CN 202110460023 A CN202110460023 A CN 202110460023A CN 113154882 B CN113154882 B CN 113154882B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B21/00—Open or uncovered sintering apparatus; Other heat-treatment apparatus of like construction
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D9/00—Cooling of furnaces or of charges therein
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
- F27D2019/0003—Monitoring the temperature or a characteristic of the charge and using it as a controlling value
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
- F27D2019/0028—Regulation
- F27D2019/0056—Regulation involving cooling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to the technical field of 3D printing, in particular to a pressureless rapid sintering device and a sintering method for 3D printing. The pressureless rapid sintering device comprises a furnace body, a base, an upper electrode, a lower electrode, an upper graphite electrode, a lower graphite electrode, a sintering mold, a current control system and a sintering control system; the upper graphite electrode and the lower graphite electrode are respectively positioned at two ends of the sintering mold, the upper graphite electrode and the lower graphite electrode are respectively connected with the upper electrode and the lower electrode, and the lower electrode is separated from the furnace body through a base; the current control system is connected with the upper electrode and the lower electrode and is used for controlling the voltage and the current of the upper electrode and the lower electrode; the sintering control system is connected with the current control system and is used for controlling the starting of equipment and sintering process parameters. The invention effectively solves the problem that the existing rapid sintering equipment cannot be used for sintering 3D printing complex structural members, greatly improves the production and research efficiency, and can obtain 3D printing products with special properties of nanocrystalline ceramics.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to a pressureless rapid sintering device and a sintering method for 3D printing.
Background
The 3D printing is an additive manufacturing technology based on a discrete/stacked forming principle, a die is not needed in the forming process, the rapid manufacturing of hollow, thin-wall and other complex structural parts can be realized, and the method has wide application prospects in the fields of microfluidic chips, micromechanics, aerospace, automobiles and the like and is one of the current research hotspots. After the ceramic material is processed by 3D printing technologies such as photo-curing molding, adhesive injection molding, extrusion molding and the like, a sintering treatment process is also needed. Sintering is one of the most critical steps in the preparation of advanced structural and functional materials such as high-performance ceramics.
The rapid sintering can not only improve the production efficiency and reduce the energy consumption, but also obtain the materials with special properties such as nanocrystalline ceramics and the like, and is the research direction focused at home and abroad at present. The rapid sintering can inhibit neck growth and low efficiency loss of sintering activation energy caused by surface diffusion in the initial sintering stage in the heating process through extremely rapid heating rate, so that the green body retains stronger sintering activity and material diffusion rate in the middle sintering stage, and the sintering densification rate is improved. The sintering temperature can be reduced to a certain extent and the sintering time can be greatly shortened by rapid temperature rise, and the whole process can be completed within a few seconds. Because of the short sintering time, the grain growth is inhibited in the sintering process, so that a sintered product with finer grains can be obtained.
Current rapid sintering techniques mainly include microwave sintering (MW), spark Plasma Sintering (SPS), and flash Firing (FS). Microwave sintering depends on the microwave absorption characteristics of materials, and has a narrow application range. The SPS technique requires a mold to restrain the sintered material during sintering, and only products with simple structures such as sheets, bars and the like can be obtained. The flash firing needs to coat conductive electrodes on two sides of the sample, which causes certain pollution to the sample, and the shape is mainly dog-bone-shaped and wafer-shaped, so that the rapid sintering of complex structural members is difficult to realize.
Disclosure of Invention
In view of the foregoing, there is a need to provide a pressureless rapid sintering device and sintering method for 3D printing, which are used for sintering complex structural members printed by 3D printing technology, and which can increase the sintering rate of pressureless sintering, thereby improving the production and research efficiency.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the present invention provides a pressureless rapid sintering device for 3D printing, the pressureless rapid sintering device comprising a furnace body, a base, an upper electrode, a lower electrode, an upper graphite electrode, a lower graphite electrode, a sintering mold, a current control system and a sintering control system;
the upper graphite electrode and the lower graphite electrode are respectively positioned at two ends of the sintering die, the upper graphite electrode and the lower graphite electrode are respectively connected with the upper electrode and the lower electrode, and the lower electrode is separated from the furnace body through a base;
the current control system is connected with the upper electrode and the lower electrode and is used for controlling the voltage and the current of the upper electrode and the lower electrode;
the sintering control system is connected with the current control system and is used for controlling the starting of equipment and sintering process parameters.
Further, in the pressureless rapid sintering device for 3D printing, the sintering mold comprises an upper graphite cushion block, a hollow cylindrical graphite mold, a burning plate, a heat insulation block and a lower graphite cushion block; the upper graphite cushion block and the lower graphite cushion block are respectively connected with the upper graphite electrode and the lower graphite electrode; the upper graphite cushion block, the hollow cylindrical graphite mold and the lower graphite cushion block form a sealed sintering chamber; the heat insulation block is positioned in the sintering chamber and is arranged above the lower graphite cushion block; the burning plate is positioned above the heat insulation block and is used for placing a blank to be sintered; the heat insulation block separates the sintering bearing plate from the bottom of the sintering die, so that the blank to be sintered on the sintering bearing plate is heated more uniformly.
Further, in the pressureless rapid sintering device for 3D printing, the sintering mold further comprises a temperature measuring element arranged on the outer surface of the hollow cylindrical graphite mold. The temperature of the sintering mold can be measured and controlled by the temperature measuring element.
Further, in the pressureless rapid sintering device for 3D printing, the sintering device further comprises an atmosphere control system, and the furnace body is provided with an air inlet and an air outlet; the atmosphere control system is communicated with the inside of the furnace body through an air inlet and an air outlet on the furnace body; the atmosphere control system can control the inside of the furnace body to be vacuum or atmosphere.
Further, in the pressureless rapid sintering device for 3D printing, the sintering device further comprises a cooling control system; the cooling control system is connected with the furnace body, the base, the upper electrode, the lower electrode, the current control system, the atmosphere control system and the sintering control system through cooling water channels, and can help to dissipate heat and accelerate cooling speed.
Further, in the pressureless rapid sintering device for 3D printing, the current control system is a direct current power supply, a direct current pulse power supply or an alternating current power supply.
In a second aspect, the present invention provides a sintering method of the pressureless rapid sintering device for 3D printing, comprising the steps of:
(1) Preparing a blank to be sintered by a 3D printing technology;
(2) Placing the prepared blank to be sintered on a setter plate of a sintering mold;
(3) Starting the equipment through a sintering control system; then starting a cooling control system; vacuumizing the furnace body or introducing inert gas through an atmosphere control system;
(4) Inputting sintering process parameters through a sintering control system, and running a sintering program;
(5) After the sintering is finished, stopping the atmosphere control system after the temperature of the sintering mold is reduced to room temperature, and taking out the sintered product after the furnace body is restored to the atmosphere.
Further, in the above sintering method, the sintering process parameters include sintering temperature, heating rate, heat preservation time and cooling mode.
Further, in the above sintering method, the inert gas is nitrogen, argon or helium.
Further, in the above sintering method, the cooling mode may be natural cooling or temperature-controlled cooling.
The beneficial effects of the invention are as follows:
1. the invention provides a pressureless rapid sintering device and a sintering method for 3D printing, which can effectively solve the problem that the conventional rapid sintering equipment cannot be used for sintering 3D printing complex structural members, greatly improve the production and research and development efficiency, and can obtain 3D printing products with special properties such as nanocrystalline ceramics through rapid sintering.
2. The traditional spark plasma sintering equipment or hot pressing equipment needs to apply load force at two ends of a sample, so that the rapid sintering of the sample with simple structures such as a sheet shape, a rod shape and the like can be realized, and a complex pressure control system is needed, so that the equipment has a complex structure, is difficult to operate and is high in price. Compared with the traditional discharge plasma equipment or hot pressing equipment, the pressureless rapid sintering device provided by the invention has the advantages of simple structure and cost saving.
3. Compared with the conventional pressureless sintering device which performs sintering in a furnace body, the pressureless rapid sintering device for 3D printing provided by the invention has the advantages that the rapid heating of a sample is realized through concentrated heat release of the sintering die to a narrow space inside, the heating rate can reach more than 500 ℃/min, and the heating rate of the conventional pressureless sintering device is generally not more than 20 ℃/min.
Drawings
FIG. 1 is a schematic diagram of the pressureless rapid sintering apparatus of the present invention;
FIG. 2 is a physical view of a green body to be sintered and a sintered product in example 1 of the present invention;
FIG. 3 is a physical view of the green body to be sintered in example 2 and example 3 of the present invention;
FIG. 4 is a physical view of the sintered product of example 2 and example 3 of the present invention;
the labels in fig. 1 are as follows:
the device comprises a 1-upper electrode, a 2-upper graphite electrode, a 3-upper graphite cushion block, a 4-hollow cylindrical graphite mold, a 5-blank to be sintered, a 6-setter plate, a 7-heat insulation block, an 8-lower graphite cushion block, a 9-lower graphite electrode, a 10-lower electrode, a 11-base, a 12-temperature measuring element, a 13-furnace body, a 14-current control system, a 15-cooling control system, a 16-sintering control system, a 17-atmosphere control system and an 18-sintering mold.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be further clearly and completely described in the following in conjunction with the embodiments of the present invention. It should be noted that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be understood that the terms "upper," "lower," "inner," "outer," and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the scope of the present invention.
Example 1
As shown in fig. 1, the present embodiment provides a pressureless rapid sintering device for 3D printing, which includes a furnace body 13, a base 11, an upper electrode 1, a lower electrode 10, an upper graphite electrode 2, a lower graphite electrode 9, a sintering mold 18, a current control system 14, and a sintering control system 16;
the upper graphite electrode 2 and the lower graphite electrode 9 are respectively positioned at two ends of the sintering mold 18, the upper graphite electrode 2 and the lower graphite electrode 9 are respectively connected with the upper electrode 1 and the lower electrode 10, and the lower electrode 10 is separated from the furnace body 13 through the base 11;
the current control system 14 is connected with the upper electrode 1 and the lower electrode 10 and is used for controlling the voltage and the current of the upper electrode 1 and the lower electrode 10;
the sintering control system 16 is connected to the current control system 14 for controlling the start-up of the apparatus and the sintering process parameters.
The sintering mold 18 comprises an upper graphite cushion block 3, a hollow cylindrical graphite mold 4, a burning plate 6, a heat insulation block 7 and a lower graphite cushion block 8; the upper graphite cushion block 3 and the lower graphite cushion block 8 are respectively connected with the upper graphite electrode 2 and the lower graphite electrode 9; the upper graphite cushion block 3, the hollow cylindrical graphite mold 4 and the lower graphite cushion block 3 form a sealed sintering chamber; the heat insulation block 7 is positioned in the sintering chamber and is arranged above the lower graphite cushion block 8; the setter plate 6 is positioned above the heat insulation block 7.
Wherein, the sintering mould 18 also comprises a temperature measuring element 12 arranged on the outer surface of the hollow cylindrical graphite mould 4.
Wherein the pressureless rapid sintering device further comprises an atmosphere control system 17 and a cooling control system 15; the atmosphere control system 17 is communicated with the inside of the furnace body 13 through an air inlet and an air outlet on the furnace body 13; for controlling the vacuum or atmosphere environment inside the furnace body 13. The cooling control system 15 is connected with the furnace body 13, the base 11, the upper electrode 1, the lower electrode 10, the current control system 14, the atmosphere control system 17 and the sintering control system 16 through cooling water channels, so that the cooling can be assisted and the cooling speed can be increased; the pressureless rapid sintering device for 3D printing of this embodiment adopts the following sintering method: the method comprises the following steps:
(1) Preparing a blank 5 to be sintered by a photocuring 3D printing technology;
(2) Placing the prepared blank 5 to be sintered on a setter plate 6 of a sintering mold 18;
(3) Starting the device by the sinter control system 16; then the cooling control system 15 is turned on; vacuumizing the furnace body 13 through an atmosphere control system 17;
(4) Inputting sintering process parameters through a sintering control system 16, setting sintering temperature to 1250 ℃, keeping the temperature for 20min, heating the temperature at 312.5 ℃/min, and running a sintering program;
(5) After the sintering is finished, the atmosphere control system 17 is stopped after the temperature of the sintering mold 18 is reduced to room temperature, and the sintered product is taken out after the inside of the furnace body 13 is restored to the atmosphere. The sintering material of this example is silicon oxide, and the green body to be sintered and the sintered product are shown in fig. 2a and 2 b.
Example 2
A pressureless rapid sintering device for 3D printing has the same structure as in example 1.
The following sintering method is adopted in this example:
(1) Preparing a blank 5 to be sintered by a photocuring 3D printing technology;
(2) Placing the prepared blank 5 to be sintered on a setter plate 6 of a sintering mold 18;
(3) Starting the device by the sinter control system 16; then the cooling control system 15 is turned on; vacuumizing the furnace body 13 through an atmosphere control system 17;
(4) Inputting sintering process parameters through a sintering control system 16, setting the sintering temperature to 1500 ℃, keeping the temperature for 5min, heating the temperature at a rate of 150 ℃/min, and running a sintering program;
(5) After the sintering is finished, the atmosphere control system 17 is stopped after the temperature of the sintering mold 18 is reduced to room temperature, and the sintered product is taken out after the inside of the furnace body 13 is restored to the atmosphere. The sintered material of this example is alumina, and the green body to be sintered and the sintered product are shown in fig. 3a and 4 a.
Example 3
A pressureless rapid sintering device for 3D printing has the same structure as in example 1.
The following sintering method is adopted in this example:
(1) Preparing a blank 5 to be sintered by a photocuring 3D printing technology;
(2) Placing the prepared blank 5 to be sintered on a setter plate 6 of a sintering mold 18;
(3) Starting the device by the sinter control system 16; then the cooling control system 15 is turned on; vacuumizing the furnace body 13 through an atmosphere control system 17;
(4) Inputting sintering process parameters through a sintering control system 16, setting the sintering temperature to 1450 ℃, keeping the temperature for 5min, heating the temperature at 145 ℃/min, and running a sintering program;
(5) After the sintering is finished, the atmosphere control system 17 is stopped after the temperature of the sintering mold 18 is reduced to room temperature, and the sintered product is taken out after the inside of the furnace body 13 is restored to the atmosphere. The sintered material of this example is zirconia, and the green body to be sintered and the sintered product are shown in fig. 3b and 4 b.
Comparative example 1
And sintering the 3D printed silicon oxide blank to be sintered, which is the same as that in the embodiment 1, by adopting a spark plasma sintering device, wherein the load pressure of the blank to be sintered is increased due to spark plasma sintering, so that the complex structure of the blank to be sintered is damaged.
Comparative example 2
The 3D printed silica green body identical to example 1 was sintered using a conventional pressureless sintering apparatus (GF 16Q, nanjing bo on instrument technology limited) with a sintering curve of first heating to 1000 ℃ at 5 ℃/min, then heating to 1250 ℃ at 3 ℃/min and maintaining the temperature for 1.5 hours. And cooling along with the furnace after sintering.
Experimental results: the sintered sample shape remained intact, but the sintering time for comparative example 2 was approximately 24 hours, while the rapid sintering time for example 1 was approximately 30 minutes.
Comparative example 3
The 3D printed alumina green body identical to example 2 was sintered using a conventional pressureless sintering apparatus (GF 16Q, nanjing bo on instruments science, ltd.) with a sintering curve of raising the temperature to 1500 ℃ at 5 ℃/min and maintaining the temperature for 3 hours. And cooling along with the furnace after sintering.
Experimental results: the sintered sample shape remained intact, but the sintering time for comparative example 3 was approximately 24 hours, while the rapid sintering time for example 2 was approximately 30 minutes.
Comparative example 4
The 3D printed zirconia green body as in example 3 was sintered using a conventional pressureless sintering apparatus (GF 16Q, nanjing bo on instrument technology co.) with a sintering curve of 5 ℃/min to 1450 ℃ and incubated for 3 hours. And cooling along with the furnace after sintering.
Experimental results: the sintered sample shape remained intact, but the sintering time for comparative example 4 was approximately 24 hours, while the rapid sintering time for example 3 was approximately 30 minutes.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (9)
1. The pressureless rapid sintering device for 3D printing is characterized by comprising a furnace body, a base, an upper electrode, a lower electrode, an upper graphite electrode, a lower graphite electrode, a sintering mold, a current control system and a sintering control system;
the upper graphite electrode and the lower graphite electrode are respectively positioned at two ends of the sintering die, the upper graphite electrode and the lower graphite electrode are respectively connected with the upper electrode and the lower electrode, and the lower electrode is separated from the furnace body through a base;
the current control system is connected with the upper electrode and the lower electrode and is used for controlling the voltage and the current of the upper electrode and the lower electrode;
the sintering control system is connected with the current control system and is used for controlling the starting of equipment and sintering process parameters;
the sintering die comprises an upper graphite cushion block, a hollow cylindrical graphite die, a burning plate, a heat insulation block and a lower graphite cushion block; the upper graphite cushion block and the lower graphite cushion block are respectively connected with the upper graphite electrode and the lower graphite electrode; the upper graphite cushion block, the hollow cylindrical graphite mold and the lower graphite cushion block form a sealed sintering chamber; the heat insulation block is positioned in the sintering chamber and is arranged above the lower graphite cushion block; the burning bearing plate is positioned above the heat insulation block.
2. The pressureless rapid sintering apparatus for 3D printing of claim 1, wherein the sintering mold further comprises a temperature measuring element disposed on an outer surface of the hollow cylindrical graphite mold.
3. The pressureless rapid sintering device for 3D printing of claim 1, further comprising an atmosphere control system, wherein the furnace body is provided with an air inlet and an air outlet; the atmosphere control system is communicated with the inside of the furnace body through an air inlet and an air outlet on the furnace body; the atmosphere control system can control the inside of the furnace body to be vacuum or atmosphere.
4. The pressureless rapid sintering apparatus for 3D printing of claim 3, further comprising a cooling control system; the cooling control system is connected with the furnace body, the base, the upper electrode, the lower electrode, the current control system, the atmosphere control system and the sintering control system through cooling water channels.
5. The pressureless rapid sintering apparatus for 3D printing of claim 1, wherein the current control system is a dc power supply, a dc pulse power supply, or an alternating current power supply.
6. The sintering method of the pressureless rapid sintering apparatus for 3D printing according to any one of claims 1 to 5, comprising the steps of:
(1) Preparing a blank to be sintered by a 3D printing technology;
(2) Placing the prepared blank to be sintered on a setter plate of a sintering mold;
(3) Starting the equipment through a sintering control system; then starting a cooling control system; vacuumizing the furnace body or introducing inert gas through an atmosphere control system;
(4) Inputting sintering process parameters through a sintering control system, and running a sintering program;
(5) After the sintering is finished, stopping the atmosphere control system after the temperature of the sintering mold is reduced to room temperature, and taking out the sintered product after the furnace body is restored to the atmosphere.
7. The sintering method according to claim 6, wherein the sintering process parameters include sintering temperature, heating rate, holding time and cooling mode.
8. The sintering method according to claim 6, wherein the inert gas is nitrogen, argon or helium.
9. The sintering method according to claim 6, wherein the cooling mode is natural cooling or temperature-controlled cooling.
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| CN111981847A (en) * | 2020-07-24 | 2020-11-24 | 北京科技大学 | Pressure-assisted induction heating vacuum atmosphere flash sintering device |
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2021
- 2021-04-27 CN CN202110460023.0A patent/CN113154882B/en active Active
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| CN102632238A (en) * | 2012-04-05 | 2012-08-15 | 华南师范大学 | Sintering mould |
| CN103819202A (en) * | 2014-01-14 | 2014-05-28 | 苏州永佳超硬耐磨材料有限公司 | Ceramic material sintering furnace and isostatic pressing field-controlled spark pulse sintering method |
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| CN106312067A (en) * | 2016-10-11 | 2017-01-11 | 河海大学 | Graphite die for pressureless spark plasma sintering |
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