CN113277715A - 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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- CN113277715A CN113277715A CN202110442058.1A CN202110442058A CN113277715A CN 113277715 A CN113277715 A CN 113277715A CN 202110442058 A CN202110442058 A CN 202110442058A CN 113277715 A CN113277715 A CN 113277715A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 94
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 42
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 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 11
- 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
- 238000010438 heat treatment Methods 0.000 claims description 23
- 238000000016 photochemical curing Methods 0.000 claims description 19
- 230000005684 electric field Effects 0.000 claims description 8
- 238000005238 degreasing Methods 0.000 claims description 7
- 239000011268 mixed slurry Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 3
- 230000000630 rising effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002002 slurry Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 238000001723 curing Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000001272 pressureless sintering Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007731 hot pressing Methods 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
- 238000012827 research and development Methods 0.000 description 1
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Classifications
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- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Civil Engineering (AREA)
- Composite Materials (AREA)
- Structural Engineering (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
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 in a sintering mold for rapid sintering; the sintering temperature is 1150-1450 ℃, the sintering temperature rise rate is 50-1000 ℃/min, and the sintering heat preservation time is less than 20 min. The invention adopts a rapid sintering process on the sintering process, and realizes the rapid preparation of the quartz glass device with a complex structure. The sample is heated rapidly by the concentrated heat release of the sintering mold to the internal narrow space, 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, 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 because of its superior properties, but because of its high melting point and hard brittleness, it is difficult to obtain a quartz glass functional device with a complex structure by traditional techniques such as thermal forming and machining, thus limiting further applications of quartz glass. With the rise of 3D printing technology, the preparation of quartz glass by using the photo-curing 3D printing technology has received much 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, photocuring 3D printing and molding, 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 the most important link for determining the performance of the quartz glass. The quartz glass can be devitrified due to the excessively high sintering temperature and the excessively long sintering time, so that the transmittance of the quartz glass is reduced, the thermal stability is poor, and a sample can be scrapped due to cracks. In addition, the quartz glass is generally required to be sintered in a vacuum environment, the cooling speed of the sample is slow, the cooling process is as long as 12 hours, and the production efficiency is greatly reduced. The realization of the rapid sintering of the quartz glass has important significance for improving the quality and the production efficiency of the photocuring 3D printing quartz glass.
Disclosure of Invention
In view of the above, it is desirable to provide a method for manufacturing a silica glass device having a complicated structure. According to the invention, the sintered body prepared by the 3D printing technology is sintered by a rapid sintering process, so that the rapid preparation of the quartz glass device with a complex structure is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for manufacturing a silica glass device having a complicated 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 in a sintering mold for rapid sintering; the sintering temperature is 1150-1450 ℃, the sintering temperature rise rate is 50-1000 ℃/min, and the sintering heat preservation time is less than 20 min.
Further, in the above method for manufacturing a silica glass device having a complex structure, the silica body is a body having a certain shape after the silica mixed slurry is subjected to 3D printing molding, degreasing and pre-sintering processes.
Further, in the above-described method for manufacturing a silica glass device having a complicated structure, the silica mixed slurry raw material includes a photosensitive resin and silica powder.
Further, in the above method for producing a silica glass device having a complicated structure, the silica has a particle size of less than 500 nm.
Further, in the above method for manufacturing a silica glass device having a complex structure, the 3D printing technique is photocuring 3D printing.
Further, in the above-described method for producing a quartz glass device having a complicated 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 silica glass device having a complicated structure, the sintering mold includes 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 mould and form a closed sintering chamber with the hollow cylindrical graphite mould; 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 silica glass device having a complicated 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 method for manufacturing a quartz glass device with a complex structure, in step S2, the sintering mold is heated by the upper graphite electrode and the lower graphite electrode in an electric field heating manner, so as to rapidly sinter the silica blank in the sintering mold.
Further, in the above-mentioned method for producing a silica glass device having a complicated structure, a cooling step of S3 is further included; the cooling step can be natural cooling or temperature-controlled cooling.
The quartz glass device prepared by the preparation method of the quartz glass device with the complex structure is adopted.
The invention has the beneficial effects that:
1. compared with the quartz glass photocuring 3D printing technology in the prior art, the method for preparing the quartz glass device with the complex structure adopts the rapid sintering technology on the sintering technology, so that the rapid preparation of the quartz glass device with the complex structure can be realized. In the sintering temperature and the sintering time of the preparation method, the prepared quartz glass device has high transparency, no crystallization and good quality.
2. Compared with the traditional pressureless sintering process, the invention realizes the rapid heating of the sample by the concentrated heat release of the sintering mould to the internal narrow space, improves the temperature rise 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 and development and production cost of quartz glass.
3. The invention utilizes an electric field heating mode to heat the sintering mold, thereby rapidly sintering the silicon dioxide blank. The sintered sample in the invention is not directly acted by pressure, so that the quartz glass with a complex structure can be manufactured, and the traditional electric field heating sintering equipment such as a discharge plasma sintering technology and a hot pressing sintering technology can only obtain the quartz glass with simple structures such as a sheet shape, a rod shape and the like due to the pressure.
Drawings
FIG. 1 is a schematic structural view 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 temperature profile of the sintering process in example 2 of the present invention;
FIG. 5 is a physical representation of sintered samples in example 2, comparative example 1 and comparative example 2 of the present invention;
FIG. 6 is an XRD pattern of quartz glass obtained by sintering in comparative example 1 of the present invention;
FIG. 7 is an XRD pattern of 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 respective symbols in the figure are 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 clearer, the technical solutions of the present invention will be further clearly and completely described below with reference to the embodiments of the present invention. It should be noted that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for manufacturing a silica glass device having a complicated 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 55 wt%, wherein the particle size of the silicon dioxide powder is 40 nm; uniformly mixing, and ultrasonically removing bubbles to obtain silicon dioxide mixed slurry;
(2) curing and molding the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405 nm; carrying out thermal degreasing and presintering on the obtained formed part in the air, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, then heating to 1000 ℃ at the speed of 5 ℃/min, 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 body is put into a sintering mold of an electric field heating sintering device, and the sintering mold is shown as figure 1. Setting the sintering temperature to 1350 ℃, the heat preservation time to 5min, the heating rate to 150 ℃/min and the vacuum degree to 5Pa, and operating the sintering program.
After the sintering, the quartz glass device with a complex structure as 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 silica glass device having a complicated 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 55 wt%, wherein the particle size of the silicon dioxide powder is 40 nm; uniformly mixing, and ultrasonically removing bubbles to obtain silicon dioxide mixed slurry;
(2) curing and molding the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405 nm; carrying out thermal degreasing and presintering on the obtained formed part in the air, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, then heating to 1000 ℃ at the speed of 5 ℃/min, 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 body is put into a sintering mold of an electric field heating sintering device, and the sintering mold is shown as figure 1. Setting the sintering temperature to 1350 ℃, the heat preservation time to 5min, the heating rate to 450 ℃/min and the vacuum degree to 5Pa, and operating the sintering program. The temperature profile of the sintering process is shown in fig. 4.
And cooling after sintering to obtain the quartz glass. The quartz glass prepared is shown in fig. 5 a.
Example 3
A method for manufacturing a silica glass device having a complicated 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 55 wt%, wherein the particle size of the silicon dioxide powder is 40 nm; uniformly mixing, and ultrasonically removing bubbles to obtain silicon dioxide mixed slurry;
(2) curing and molding the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405 nm; carrying out thermal degreasing and presintering on the obtained formed part in the air, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, then heating to 1000 ℃ at the speed of 5 ℃/min, 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 body is put into a sintering mold of an electric field heating sintering device, and the sintering mold is shown as figure 1. Setting the sintering temperature at 1300 ℃, the heat preservation time at 10min, the heating rate at 100 ℃/min and the vacuum degree at 5Pa, and operating the sintering program.
And cooling after sintering to obtain the quartz glass.
Example 4
A method for manufacturing a silica glass device having a complicated 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 55 wt%, wherein the particle size of the silicon dioxide powder is 40 nm; uniformly mixing, and ultrasonically removing bubbles to obtain silicon dioxide mixed slurry;
(2) curing and molding the obtained silicon dioxide slurry on a DLP photocuring 3D printer platform, wherein the light source wavelength of the photocuring 3D printer is 405 nm; carrying out thermal degreasing and presintering on the obtained formed part in the air, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 2 hours, then heating to 1000 ℃ at the speed of 5 ℃/min, 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 body is put into a sintering mold of an electric field heating sintering device, and the sintering mold is shown as figure 1. Setting the sintering temperature to 1400 ℃, the heat preservation time to 5min, the heating rate to 300 ℃/min and the vacuum degree to 5Pa, and operating the sintering program.
And cooling after sintering to obtain the quartz glass.
Comparative example 1
The difference between the comparative example and example 2 is that in step S2, the sintering temperature is set to 1500 ℃, the holding time is 5min, the heating rate is 150 ℃/min, and the vacuum degree is 5 Pa.
The experimental results are as follows: as shown in fig. 5 b. In comparison with fig. 5a, the sintered sample of example 2 has a good transmittance and the sintered sample of comparative example 1 has a lower transmittance under 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 crystallized.
Comparative example 2
The difference between this comparative example and example 2 is that in step S2, the sintering temperature is set to 1350 ℃, the holding time is 20min, the heating rate is 150 ℃/min, and the vacuum degree is 5 Pa.
The experimental results are as follows: as shown in fig. 5 c. In comparison with fig. 5a, the sintered sample of example 2 has a good transmittance and the sintered sample of comparative example 2 has a lower transmittance under the same background. The XRD pattern of the quartz glass prepared in comparative example 2 is shown in fig. 7, and it can be seen from fig. 7 that the quartz glass sample is devitrified.
Comparative example 3
The difference between the comparative example 3 and the example 2 is that the ordinary pressureless sintering is adopted to replace the rapid sintering in the step S2, and the sintering curve is that the temperature is raised to 1000 ℃ at the speed of 5 ℃/min, then raised to 1250 ℃ at the speed of 3 ℃/min and kept for 3 h. And cooling along with the furnace after sintering.
The experimental results are as follows: the sintered sample was transparent and the sintering curve is shown in FIG. 8. In the case that the sintered sample is transparent, as can be seen from fig. 3 and 8, the sintering time of the rapid sintering of example 1 and the sintering time of the conventional pressureless sintering of comparative example 3 are 23.6667min and 23.5333h, respectively (both are cooled to 100 ℃ C. and the oven door is opened), and the preparation method of the present invention reduces the time required for the sintering process by 98.32% using the rapid sintering.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for manufacturing a silica glass device having a complicated 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 in a sintering mold for rapid sintering; the sintering temperature is 1150-1450 ℃, the sintering temperature rise rate is 50-1000 ℃/min, and the sintering heat preservation time is less than 20 min.
2. The method for manufacturing a quartz glass device with a complex structure according to claim 1, wherein the silica body is a body with a certain shape after the silica mixed slurry is processed by 3D printing molding, degreasing and pre-sintering processes.
3. The method for producing a silica glass device having a complicated structure according to claim 2, wherein the particle size of the silica is less than 500 nm.
4. The method for producing a silica glass device having a complicated structure according to claim 1, wherein the 3D printing technique is photocuring 3D printing.
5. The method for producing a silica glass device having a complicated structure according to claim 1, wherein the sintering atmosphere is a vacuum or inert atmosphere; the inert atmosphere is argon, helium or nitrogen.
6. The method for producing a quartz glass device having a complicated structure according to claim 1, wherein the sintering mold comprises an upper graphite electrode, a hollow cylindrical graphite mold, a lower graphite electrode, a heat insulating block, a setter plate; the upper graphite electrode and the lower graphite electrode are respectively positioned at two ends of the hollow cylindrical graphite mould and form a closed sintering chamber with the hollow cylindrical graphite mould; the heat insulation block is positioned above the lower graphite electrode; the burning bearing plate is positioned above the heat insulation block.
7. The method for producing a silica glass device having a complicated structure according to claim 6, wherein the sintering mold further comprises a temperature measuring element which is located on an outer surface of the hollow cylindrical graphite mold.
8. The method of manufacturing a silica glass device having a complicated structure according to claim 6, wherein the sintering mold is heated by the upper graphite electrode and the lower graphite electrode in step S2 by means of electric field heating.
9. The method for producing a silica glass device having a complicated structure according to claim 1, further comprising a cooling step of S3; the cooling step can be natural cooling or temperature-controlled cooling.
10. The silica glass device produced by the method for producing a silica glass device having a complicated structure according to any one of claims 1 to 9.
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Cited By (1)
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| CN114573214A (en) * | 2022-03-16 | 2022-06-03 | 中国地质大学（武汉） | 3D printing glass slurry based on waste recovery and preparation and printing methods thereof |
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