CN113277715B - Method for manufacturing quartz glass device with complex structure - Google Patents
Method for manufacturing quartz glass device with complex structure Download PDFInfo
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- CN113277715B CN113277715B CN202110442058.1A CN202110442058A CN113277715B CN 113277715 B CN113277715 B CN 113277715B CN 202110442058 A CN202110442058 A CN 202110442058A CN 113277715 B CN113277715 B CN 113277715B
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- sintering
- silicon dioxide
- quartz glass
- temperature
- graphite electrode
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 156
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 88
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 45
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 238000010146 3D printing Methods 0.000 claims abstract description 20
- 238000005516 engineering process Methods 0.000 claims abstract description 16
- 238000004321 preservation Methods 0.000 claims abstract description 7
- 230000000630 rising effect Effects 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910002804 graphite Inorganic materials 0.000 claims description 25
- 239000010439 graphite Substances 0.000 claims description 25
- 238000000016 photochemical curing Methods 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 10
- 239000011268 mixed slurry Substances 0.000 claims description 9
- 230000005684 electric field Effects 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 abstract description 13
- 238000002360 preparation method Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 3
- 238000012827 research and development Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000009740 moulding (composite fabrication) Methods 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 5
- 238000001723 curing Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y80/00—Products made by additive manufacturing
-
- 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
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention relates to the technical field of material preparation, in particular to a preparation method of a quartz glass device with a complex structure. The preparation method comprises the following steps: step S1: preparing a silicon dioxide blank by adopting a 3D printing technology; step S2: placing the silicon dioxide blank body in a sintering mold for rapid sintering; the sintering temperature is 1150-1450 ℃, the sintering temperature rising rate is 50-1000 ℃/min, and the sintering heat preservation time is less than 20min. The invention adopts a rapid sintering process on the sintering process, thereby realizing rapid preparation of quartz glass devices with complex structures. The rapid heating of the sample is realized by the concentrated heat release of the sintering mold to the narrow space inside, the temperature rising rate of sintering is improved, the sintering time and the cooling time are greatly shortened, the whole sintering process can be completed within half an hour, and the research and development and production cost of quartz glass can be effectively reduced.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a preparation method of a quartz glass device with a complex structure.
Background
Quartz glass has become an indispensable important material in modern science and industry due to its superior properties, but it is difficult to obtain a quartz glass functional device of a complex structure by conventional techniques such as thermoforming and machining due to its high melting point and hard brittleness, thus limiting further applications of quartz glass. With the rise of 3D printing technology, the preparation of quartz glass using a photo-curing 3D printing technology has received a great deal of attention. Silica powder is used as a raw material, and a quartz glass device with a complex structure and special functions can be prepared by preparing slurry, photo-curing 3D printing and forming, degreasing and sintering.
In the method for preparing quartz glass by using the photocuring 3D printing technology, sintering is one of the most critical steps and is also the most important link for determining the performance of the quartz glass. The sintering temperature is too high and the sintering time is too long, so that the quartz glass can be crystallized, the transmittance of the quartz glass is reduced, the thermal stability is poor, and cracks can be caused to discard the sample. In addition, the quartz glass is usually required to be sintered in a vacuum environment, the cooling speed of the sample is low, the cooling process is as long as 12 hours, and the production efficiency is greatly reduced. The realization of rapid sintering of quartz glass has important significance for improving the quality and the production efficiency of photo-curing 3D printing quartz glass.
Disclosure of Invention
In view of the above, it is necessary to provide a method for manufacturing a quartz glass device having a complicated structure, in view of the above-described problems. The sintered blank prepared by the rapid sintering technology sintering 3D printing technology realizes rapid preparation of quartz glass devices with complex structures.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for manufacturing a quartz glass device having a complex structure, comprising the steps of:
step S1: preparing a silicon dioxide blank by adopting a 3D printing technology;
step S2: placing the silicon dioxide blank body in a sintering mold for rapid sintering; the sintering temperature is 1150-1450 ℃, the sintering temperature rising rate is 50-1000 ℃/min, and the sintering heat preservation time is less than 20min.
Further, in the method for manufacturing a quartz glass device having a complex structure, the silica blank is a blank having a certain shape after the 3D printing forming, degreasing and presintering processes are performed on the silica mixed slurry.
Further, in the above-described method for producing a quartz glass device having a complex structure, the silica mixed slurry raw material includes a photosensitive resin and a silica powder.
Further, in the above-mentioned method for producing a quartz glass device having a complex structure, the particle diameter of the silica is less than 500nm.
Further, in the above method for manufacturing a quartz glass device having a complex structure, the 3D printing technique is photo-curing 3D printing.
Further, in the above-described method for manufacturing a quartz glass device having a complex structure, the sintering atmosphere is a vacuum or inert atmosphere; the inert atmosphere is argon, helium or nitrogen.
Further, in the above method for manufacturing a quartz glass device having a complex structure, the sintering mold comprises an upper graphite electrode, a hollow cylindrical graphite mold, a lower graphite electrode, a heat insulating block, and a setter plate; the upper graphite electrode and the lower graphite electrode are respectively positioned at two ends of the hollow cylindrical graphite die and form a closed sintering chamber with the hollow cylindrical graphite die; the heat insulation block is positioned above the lower graphite electrode; the burning bearing plate is positioned above the heat insulation block.
Further, in the above method for manufacturing a quartz glass device having a complex structure, the sintering mold further includes a temperature measuring element located on an outer surface of the hollow cylindrical graphite mold. The temperature of the sintering mold is measured and controlled by a temperature measuring element.
Further, in the above-mentioned method for manufacturing a quartz glass device having a complex structure, in step S2, the sintering mold is heated by the upper graphite electrode and the lower graphite electrode by means of electric field heating, so as to rapidly sinter the silica blank in the sintering mold.
Further, in the above-mentioned method for manufacturing a quartz glass device having a complex structure, the method further comprises an S3 cooling step; the cooling step may be natural cooling or temperature controlled cooling.
The quartz glass device is prepared by adopting the preparation method of the quartz glass device with the complex structure.
The beneficial effects of the invention are as follows:
1. compared with the photo-curing 3D printing technology of quartz glass in the prior art, the rapid sintering process is adopted in the sintering process, so that the rapid preparation of the quartz glass device with the complex structure can be realized. The prepared quartz glass device has high transparency, no crystallization and good quality in the sintering temperature and sintering time of the preparation method.
2. Compared with the traditional pressureless sintering process, the invention realizes rapid heating of the sample by intensively releasing heat in a narrow space inside the sintering mold, improves the temperature rising rate of sintering, greatly shortens the sintering time and the cooling time, can complete the whole sintering process within half an hour, and can effectively reduce the research, development and production cost of quartz glass.
3. The invention utilizes an electric field heating mode to heat the sintering mould, thereby rapidly sintering the silicon dioxide blank. The sintering sample is not directly subjected to the action of pressure, so that quartz glass with a complex structure can be manufactured, and the traditional electric field heating sintering equipment such as a spark plasma sintering technology and a hot press sintering technology can only obtain quartz glass with simple structures such as a sheet shape, a rod shape and the like under the action of pressure.
Drawings
FIG. 1 is a schematic view of the structure of a sintering mold according to the present invention;
FIG. 2 is a diagram showing a quartz glass having a complicated structure obtained by sintering in example 1 of the present invention;
FIG. 3 is an XRD pattern of a quartz glass obtained by sintering in example 1 of the present invention;
FIG. 4 is a graph showing the temperature profile of the sintering process in example 2 of the present invention;
FIG. 5 is a physical view of sintered samples in example 2, comparative example 1 and comparative example 2 of the present invention;
FIG. 6 is an XRD pattern of a quartz glass obtained by sintering in comparative example 1 of the present invention;
FIG. 7 is an XRD pattern of a quartz glass obtained by sintering in comparative example 2 of the present invention;
FIG. 8 is a temperature profile of the sintering process in comparative example 3 of the present invention;
the figures are marked as follows:
1-upper graphite electrode, 2-hollow cylindrical graphite mould, 3-silicon dioxide blank, 4-setter plate, 5-heat insulation block, 6-lower graphite electrode and 7-temperature measuring element.
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.
Example 1
A method for manufacturing a quartz glass device having a complex structure, comprising the steps of:
step S1: preparing a silicon dioxide blank by adopting a photocuring 3D printing technology:
(1) Dispersing silicon dioxide powder into photosensitive resin to prepare silicon dioxide slurry with the solid content of 55wt%, wherein the particle size of the silicon dioxide powder is 40nm; after uniform mixing, removing bubbles by ultrasonic waves to obtain silicon dioxide mixed slurry;
(2) Curing and forming the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405nm; carrying out thermal degreasing and presintering on the obtained molded part in air, heating to 600 ℃ at 1 ℃/min and preserving heat for 2 hours, heating to 1000 ℃ at 5 ℃/min and preserving heat for 2 hours, and cooling along with a furnace after the heat preservation is finished to obtain a silicon dioxide blank;
step S2: the prepared silica green body was put into a sintering mold of an electric field heating sintering apparatus, which is shown in fig. 1. Setting the sintering temperature to 1350 ℃, keeping the temperature for 5min, heating the mixture at a speed of 150 ℃/min, and operating the sintering program under a vacuum degree of 5Pa.
After the sintering, the quartz glass device with a complex structure shown in fig. 2 can be obtained by cooling, and the XRD pattern of the quartz glass obtained by sintering in example 1 is shown in fig. 3.
Example 2
A method for manufacturing a quartz glass device having a complex structure, comprising the steps of:
step S1: preparing a silicon dioxide blank by adopting a photocuring 3D printing technology:
(1) Dispersing silicon dioxide powder into photosensitive resin to prepare silicon dioxide slurry with the solid content of 55wt%, wherein the particle size of the silicon dioxide powder is 40nm; after uniform mixing, removing bubbles by ultrasonic waves to obtain silicon dioxide mixed slurry;
(2) Curing and forming the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405nm; carrying out thermal degreasing and presintering on the obtained molded part in air, heating to 600 ℃ at 1 ℃/min and preserving heat for 2 hours, heating to 1000 ℃ at 5 ℃/min and preserving heat for 2 hours, and cooling along with a furnace after the heat preservation is finished to obtain a silicon dioxide blank;
step S2: the prepared silica green body was put into a sintering mold of an electric field heating sintering apparatus, which is shown in fig. 1. Setting the sintering temperature to 1350 ℃, keeping the temperature for 5min, heating the mixture at a rate of 450 ℃/min, and operating the sintering program under the vacuum degree of 5Pa. The temperature profile of the sintering process is shown in fig. 4.
And cooling after sintering to obtain quartz glass. The quartz glass produced is shown in fig. 5 a.
Example 3
A method for manufacturing a quartz glass device having a complex structure, comprising the steps of:
step S1: preparing a silicon dioxide blank by adopting a photocuring 3D printing technology:
(1) Dispersing silicon dioxide powder into photosensitive resin to prepare silicon dioxide slurry with the solid content of 55wt%, wherein the particle size of the silicon dioxide powder is 40nm; after uniform mixing, removing bubbles by ultrasonic waves to obtain silicon dioxide mixed slurry;
(2) Curing and forming the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405nm; carrying out thermal degreasing and presintering on the obtained molded part in air, heating to 600 ℃ at 1 ℃/min and preserving heat for 2 hours, heating to 1000 ℃ at 5 ℃/min and preserving heat for 2 hours, and cooling along with a furnace after the heat preservation is finished to obtain a silicon dioxide blank;
step S2: the prepared silica green body was put into a sintering mold of an electric field heating sintering apparatus, which is shown in fig. 1. Setting the sintering temperature at 1300 ℃, keeping the temperature for 10min, heating up at 100 ℃/min, and operating the sintering program under the vacuum degree of 5Pa.
And cooling after sintering to obtain quartz glass.
Example 4
A method for manufacturing a quartz glass device having a complex structure, comprising the steps of:
step S1: preparing a silicon dioxide blank by adopting a photocuring 3D printing technology:
(1) Dispersing silicon dioxide powder into photosensitive resin to prepare silicon dioxide slurry with the solid content of 55wt%, wherein the particle size of the silicon dioxide powder is 40nm; after uniform mixing, removing bubbles by ultrasonic waves to obtain silicon dioxide mixed slurry;
(2) Curing and forming the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405nm; carrying out thermal degreasing and presintering on the obtained molded part in air, heating to 600 ℃ at 1 ℃/min and preserving heat for 2 hours, heating to 1000 ℃ at 5 ℃/min and preserving heat for 2 hours, and cooling along with a furnace after the heat preservation is finished to obtain a silicon dioxide blank;
step S2: the prepared silica green body was put into a sintering mold of an electric field heating sintering apparatus, which is shown in fig. 1. Setting sintering temperature at 1400 ℃, preserving heat for 5min, heating up at 300 ℃/min, vacuum degree at 5Pa, and running sintering program.
And cooling after sintering to obtain quartz glass.
Comparative example 1
The difference between this comparative example and example 2 is that the sintering temperature was set at 1500℃in step S2, the holding time was 5min, the heating rate was 150℃per min, and the vacuum degree was 5Pa.
Experimental results: as shown in fig. 5 b. Compared to fig. 5a, the sintered sample of example 2 has good transmittance and the sintered sample of comparative example 1 has lower transmittance in the same background. The XRD pattern of the silica glass prepared in comparative example 1 is shown in FIG. 6, and it can be seen from FIG. 6 that the silica glass sample is devitrified.
Comparative example 2
The difference between this comparative example and example 2 is that the sintering temperature was set at 1350℃in step S2, the holding time was 20min, the heating rate was 150℃per minute, and the vacuum degree was 5Pa.
Experimental results: as shown in fig. 5 c. Compared to fig. 5a, the sintered sample of example 2 has good transmittance and the sintered sample of comparative example 2 has lower transmittance under the same background. The XRD pattern of the silica glass prepared in comparative example 2 is shown in FIG. 7, and it can be seen from FIG. 7 that the silica glass sample is devitrified.
Comparative example 3
Comparative example 3 differs from example 2 in that the conventional pressureless sintering is used instead of rapid sintering in step S2, the sintering curve being first heated to 1000 c at 5 c/min, then heated to 1250 c at 3 c/min and incubated for 3h. And cooling along with the furnace after sintering.
Experimental results: the sintered sample was transparent and the sintering curve is shown in fig. 8. In the case of transparent sintered samples, as can be seen from fig. 3 and 8, the sintering time of the rapid sintering of example 1 and the ordinary pressureless sintering of comparative example 3 were 23.6667min and 23.5333h, respectively (both cooled to 100 ℃ and the oven door opened), and the preparation method of the present invention reduced the time required for the sintering process by 98.32% by rapid sintering.
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 (2)
1. A method for manufacturing a quartz glass device having a complex structure, comprising the steps of:
step S1: preparing a silicon dioxide blank by adopting a 3D printing technology; the silicon dioxide blank is formed by 3D printing of silicon dioxide mixed slurry, the obtained formed piece is subjected to thermal degreasing and presintering in air, the temperature is raised to 600 ℃ at 1 ℃/min and kept at 2h, and then the temperature is raised to 1000 ℃ at 5 ℃/min and kept at 2h, so that the blank with a certain shape is obtained; the particle size of the silicon dioxide in the silicon dioxide mixed slurry is less than 500nm; the 3D printing technology is photo-curing 3D printing;
step S2: placing the silicon dioxide blank body in a sintering mold for rapid sintering; the sintering temperature is 1350-1450 ℃, the sintering temperature rising rate is 100-450 ℃/min, and the sintering heat preservation time is less than 10min; the sintering environment is vacuum, and the vacuum degree is 5 Pa; the sintering mold comprises an upper graphite electrode, a hollow cylindrical graphite mold, a lower graphite electrode, a heat insulation block and a burning bearing plate; the sintering die further comprises a temperature measuring element, wherein the temperature measuring element is positioned on the outer surface of the hollow cylindrical graphite die; the upper graphite electrode and the lower graphite electrode are respectively positioned at two ends of the hollow cylindrical graphite die and form a closed sintering chamber with the hollow cylindrical graphite die; the heat insulation block is positioned above the lower graphite electrode; the burning bearing plate is positioned above the heat insulation block;
the silicon dioxide mixed slurry is prepared by dispersing silicon dioxide powder into photosensitive resin to prepare silicon dioxide slurry with the solid content of 55 wt%;
in the step S2, the sintering mold is heated by the upper graphite electrode and the lower graphite electrode by means of electric field heating.
2. The method for manufacturing a quartz glass device having a complex structure according to claim 1, further comprising an S3 cooling step; the cooling step may be natural cooling or temperature controlled cooling.
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DE102016012003A1 (en) * | 2016-10-06 | 2018-04-12 | Karlsruher Institut für Technologie | Composition and method for producing a shaped body from high-purity, transparent quartz glass by means of additive manufacturing |
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TW565536B (en) * | 2002-10-03 | 2003-12-11 | Yuan-Jie Ding | Manufacturing method of quartz glass component |
JP2006321691A (en) * | 2005-05-20 | 2006-11-30 | Shinetsu Quartz Prod Co Ltd | Method for manufacturing silica molded product and method for manufacturing silica glass article by sintering the silica molded product |
CN103159407A (en) * | 2013-03-19 | 2013-06-19 | 东华大学 | Fluorescent powder/silicon-based mesoporous material composite fluorescent glass and preparation method thereof |
CN106312067A (en) * | 2016-10-11 | 2017-01-11 | 河海大学 | Graphite die for pressureless spark plasma sintering |
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