CN113582517A - Sintering process of glass injection molding blank, processing method of glass product and glass product - Google Patents
Sintering process of glass injection molding blank, processing method of glass product and glass product Download PDFInfo
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- CN113582517A CN113582517A CN202111022614.6A CN202111022614A CN113582517A CN 113582517 A CN113582517 A CN 113582517A CN 202111022614 A CN202111022614 A CN 202111022614A CN 113582517 A CN113582517 A CN 113582517A
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- sintering
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- 239000011521 glass Substances 0.000 title claims abstract description 264
- 238000001746 injection moulding Methods 0.000 title claims abstract description 159
- 238000005245 sintering Methods 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 74
- 230000008569 process Effects 0.000 title claims abstract description 61
- 238000003672 processing method Methods 0.000 title abstract description 14
- 238000002347 injection Methods 0.000 claims description 32
- 239000007924 injection Substances 0.000 claims description 32
- 238000005238 degreasing Methods 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 23
- 238000012545 processing Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 8
- 230000009477 glass transition Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 2
- 238000000280 densification Methods 0.000 abstract description 19
- 239000000463 material Substances 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 14
- 238000001035 drying Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000004031 devitrification Methods 0.000 description 7
- 238000013461 design Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000005354 aluminosilicate glass Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
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- 239000002002 slurry Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
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- 230000001737 promoting effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001778 solid-state sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000006018 Li-aluminosilicate Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000003247 decreasing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- 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
Abstract
The embodiment of the application provides a sintering process of a glass injection molding blank, a processing method of a glass product and the glass product. The sintering process of the glass injection molding blank provided by the embodiment of the application adopts two high-temperature pressurizing densification processes to realize, wherein the temperature and the pressure adopted by the second high-temperature pressurizing densification process are higher than those adopted by the first high-temperature pressurizing densification process, namely, the temperature of the glass injection molding blank is gradually improved by adopting the two processes, so that the softening degree of the glass injection molding blank is gradually improved, the pressure applied to the glass injection molding blank is gradually increased, the porosity of the glass injection molding blank is gradually reduced, and the densification degree is gradually improved.
Description
Technical Field
The application relates to the technical field of glass processing, in particular to a sintering process of a glass injection molding blank, a processing method of a glass product and the glass product.
Background
The glass injection molding process is a brand new glass molding method, and the glass injection molding raw material is prepared by mixing, drying and granulating organic adhesive and glass inorganic powder at a certain temperature. In the injection molding process, glass injection molding raw materials need to be converted into a molten state in a heating mode and have certain fluidity, and a molded glass injection molding blank is obtained through the setting of the injection molding process and the matching of an injection molding machine and a mold. And then the formed glass injection molding blank is degreased at low temperature in a tunnel kiln by normal pressure heating or vacuum heating, and after being taken out of the kiln, the degreased glass injection molding blank is densified again by high temperature sintering, and finally the glass finished piece required by design is obtained. However, there is no clear method or process route in the industry for sintering glass injection molding blanks.
Disclosure of Invention
The embodiment of the application provides a sintering process of a glass injection molding blank, a processing method of a glass product and the glass product.
In a first aspect, an embodiment of the present application provides a sintering process for a glass injection molding blank, including:
placing the glass injection molding blank body in a profiling mold, and sintering in sintering equipment, wherein an accommodating space is arranged in the profiling mold, and the shape of the accommodating space is matched with that of the profiling mold; wherein, the process of sintering in the sintering equipment comprises the following steps:
after the sintering temperature of the sintering equipment is raised to T1, applying pressure to the profiling mold, after the pressure is increased from 0 to P1, maintaining T1 and P1 unchanged, and keeping for 0.5-1.5 min, wherein T1 is 450-640 ℃, T1 is higher than the glass transition temperature of the glass injection molding blank body, and P1 is 0.1-0.5 MPa;
and after the sintering temperature of the sintering equipment is increased from T1 to T2, the pressure applied to the profiling mold is increased, after the pressure is increased from P1 to P2, the T2 and the P2 are maintained unchanged for 2-4 min, wherein T2 is 800-900 ℃, the T2 is less than or equal to the softening point temperature of the glass injection molding blank, and P2 is 1-5 MPa.
In a second aspect, embodiments of the present application provide a method for processing a glass article, including:
providing a glass injection molding blank body;
degreasing the glass injection molding blank;
sintering the degreased glass injection molding blank according to the sintering process of the glass injection molding blank;
and cooling the sintered glass injection molding blank to obtain the glass product.
In a third aspect, embodiments of the present application provide a glass article, which is manufactured by the processing method of the glass article as described above.
The sintering process of the glass injection molding blank provided by the embodiment of the application adopts two high-temperature pressurizing densification processes to realize, wherein the temperature and the pressure adopted by the second high-temperature pressurizing densification process are higher than those adopted by the first high-temperature pressurizing densification process, namely, the temperature of the glass injection molding blank is gradually improved by adopting the two processes, so that the softening degree of the glass injection molding blank is gradually improved, the pressure applied to the glass injection molding blank is gradually increased, the porosity of the glass injection molding blank is gradually reduced, and the densification degree is gradually improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings used in the description of the embodiments will be briefly introduced below. It is obvious that the drawings in the following description are only some embodiments of the application, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
Fig. 1 is a flowchart of a sintering process of a glass injection molding blank according to an embodiment of the present disclosure.
Fig. 2 is a flow chart of a method for processing a glass article according to an embodiment of the present disclosure.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application 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 application.
Referring to fig. 1, fig. 1 is a flowchart illustrating a sintering process of a glass injection molding blank according to an embodiment of the present disclosure. The embodiment of the application provides a sintering process of a glass injection molding blank, which comprises the following steps: and placing the glass injection molding blank into a profiling mold, sintering in sintering equipment, wherein an accommodating space is arranged in the profiling mold, and the shape of the accommodating space is matched with that of the profiling mold.
It is understood that the processing method of the glass product may include the steps of preparing a glass injection molding blank, degreasing the glass injection molding blank, and sintering the glass injection molding blank, that is, the sintering process is applied after the degreasing process, in other words, the glass injection molding blank mentioned in the glass injection molding blank provided in the embodiments of the present application refers to the glass injection molding blank after the degreasing process.
It should be noted that, the glass injection molding blank is placed in the profiling mold, so that the profiling mold transmits the pressure to the glass injection molding blank by applying the pressure to the profiling mold in the sintering process, thereby implementing the pressure application to the glass injection molding blank, further accelerating the densification of the glass injection molding blank, and the profiling mold can limit the shape of the glass injection molding blank, thereby avoiding the shape change of the glass injection molding blank in the pressure application process.
By adopting the SPS Sintering furnace as the Sintering device, the embodiment of the application can utilize the advantage that the Plasma heat transfer speed is high, so that the Sintering device can rapidly heat up, the time for grain growth is greatly shortened, and the problem that the injection molding glass blank body is devitrified and devitrified after high-temperature Sintering due to grain growth to a larger size is avoided.
The inventor of the application compares an SPS sintering furnace with traditional solid state sintering (CCS) equipment in the research process, and finds that the problems of devitrification, cavitation, strength attenuation and the like of a glass injection molding blank easily occur after the glass injection molding blank is sintered by adopting the traditional solid state sintering equipment, and the SPS sintering furnace can greatly relieve the problems of devitrification and devitrification easiness and low densification degree of the glass injection molding blank during high-temperature sintering.
For example, the profiling mold may include a first mold and a second mold, and the "placing the glass injection molding blank in the profiling mold" may specifically include: the glass injection molding blank is placed between a first mold and a second mold, and a gap of 0.03mm to 0.08mm (e.g., 0.03mm, 0.04mm, 0.05mm, 0.06mm, 0.07mm, 0.08mm, etc.) is maintained between the first mold and the second mold. By controlling the gap between the first mold and the second mold to be 0.03-0.08 mm, the deformation amount of the glass injection molding blank in the subsequent pressurizing process can be controlled within a reasonable range, and the glass injection molding blank is prevented from being seriously deformed after being pressurized.
For example, the first mold may be a male mold, and the second mold may be a female mold; alternatively, the first mold may be a female mold and the second mold may be a male mold. The surface of the female die can be subjected to profiling design according to the appearance of the glass injection molding blank, and when the glass injection molding blank is used, the glass injection molding blank is placed in the female die and then covered with the male die.
The material of the first mold and the material of the second mold may be selected from graphite, silicon carbide, tungsten steel or other composite materials, and it is understood that the mold material is required to be non-wetting and non-sticking with glass below 1050 ℃ so as to avoid the product of the sintered glass product from being affected. Illustratively, the material of the first mold and the material of the second mold are the same.
The process of "sintering in a sintering apparatus" may specifically include:
and 310, after the sintering temperature of the sintering equipment is raised to T1, applying pressure to the profiling mold, and after the pressure is increased from 0 to P1, keeping T1 and P1 unchanged for 0.5-1.5 min (such as 0.5min, 0.7min, 0.9min, 1.0min, 1.2min, 1.5min and the like), wherein T1 is greater than the glass transition temperature of the glass injection molding blank, and P1 is 0.1-0.5 MPa (such as 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, 0.5MPa and the like).
For T1 and P1, it should be noted that T1 must exceed the glass transition temperature Tg of the glass material selected, otherwise the glass injection molded blank is easily broken after pressing; if the pressure P1 is too high (exceeding 0.5 MPa), the glass preform is easily broken, and if it is too low (less than 0.1 MPa), it does not contribute to the compression densification.
Illustratively, the sintering temperature of the sintering device may be raised from room temperature to T1 over a period of 2min to 5min (e.g., 2min, 2.5min, 3min, 3.5min, 4min, 4.5min, 5min, etc.).
It is understood that the profiling mold must be pressed after the temperature of the glass preform has risen to T1(450 ℃ C. to 640 ℃ C.) (i.e., after the initial softening), otherwise the glass preform may be broken.
320, after the sintering temperature of the sintering equipment is increased from T1 to T2, the pressure applied to the profiling mold is increased, and after the pressure is increased from P1 to P2, the pressure is kept unchanged from T2 to P2 for 2min to 4min (such as 2min, 2.5min, 3min, 3.5min, 4min, 4.5min, 5min and the like), wherein T2 is more than T1, T2 is less than or equal to the softening point temperature of the glass injection molding blank, and P2 is 1MPa to 5MPa (such as 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa, 4MPa, 4.5MPa, 5MPa and the like).
With respect to T2, it is noted that T2 must be less than or equal to the softening point of the glass material selected, otherwise the glass preform would be severely deformed after pressurization.
Because the glass transition temperature of the existing glass material is about 420 ℃, and the softening point temperature is about 900 ℃, the inventor screens out the temperature range of T1 between 450 ℃ and 640 ℃ and the temperature range of T2 between 800 ℃ and 900 ℃ after a plurality of experimental trials, when T1 and T2 are respectively selected from the temperature values of the two intervals, the glass injection molding blank can not generate the situation that the blank is broken due to overlarge hardness in the hot pressing process, and can not generate the situation that the blank is deformed after being pressed due to overlarge softening degree, after two times of hot pressing, the compactness degree of the glass injection molding blank is greatly improved, and the deformation or damage can not occur, so that the hot pressing effect is better.
Illustratively, T1 can be any temperature value in the range of 450 ℃ to 640 ℃, such as 450 ℃, 480 ℃, 500 ℃, 530 ℃, 550 ℃, 570 ℃, 600 ℃, 620 ℃, 640 ℃, and T2 can be any temperature value in the range of 800 ℃ to 900 ℃, such as 800 ℃, 820 ℃, 840 ℃, 860 ℃, 880 ℃, 900 ℃.
Illustratively, the sintering temperature of the sintering equipment can be increased from T1 to T2 for 1min to 2min (e.g., 1min, 1.2min, 1.4min, 1.6min, 1.8min, 2min, etc.) to ensure a faster temperature increase rate, and it is understood that the temperature increase time from T1 to T2 is controlled to be 1min to 2min to ensure a faster temperature increase rate, so that the time for the glass injection molding blank to stay in the nucleation point temperature and the grain growth temperature interval of the crystal grains is shortened as much as possible, the crystal grains are prevented from growing to a larger size, and the phenomenon of devitrification and devitrification (i.e., reduction in transparency) of the glass injection molding blank after sintering is avoided.
It can be understood that 310 and 320 are two high-temperature pressing densification processes, respectively, and the densification process of the glass injection molded blank can be accelerated and the porosity can be reduced by pressing the glass injection molded blank in the high-temperature sintering process, and the temperature and pressure adopted in the second high-temperature pressing densification process (320) are higher than those adopted in the first high-temperature pressing densification process (310), that is, the temperature of the glass injection molded blank is gradually increased by adopting the two processes, so that the softening degree of the glass injection molded blank is gradually increased, and the pressure applied to the glass injection molded blank is gradually increased, so that the porosity of the glass injection molded blank is gradually reduced and the densification degree is gradually increased.
Experiments prove that after the sintering process of the glass injection molding blank provided by the embodiment of the application is adopted for sintering, the density of the glass injection molding blank can reach 2.0g/cm3～2.2g/cm3It is known that the glass powder used in the production of the glass injection molded bodies of the examples of the present application is derived from waste (i.e., scrap) of Corning glass, which has a density of 2.3g/cm, and is obtained by crushing and grinding3Therefore, it can be seen that the sintering process of the glass injection molding blank body in the embodiment of the application has a strong advantage in improving the compactness.
In addition, the inventor of the present application found in research that, after degreasing the glass injection molding blank, a large number of pores may appear in the glass injection molding blank due to volatilization of organic matters in the glass injection molding blank, so that the porosity of the glass injection molding blank after degreasing is usually greater than 20%, and the compactness is poor, and thus how to reduce the porosity of the glass injection molding blank and further improve the compactness becomes an urgent technical problem to be solved Deformation, insufficient glue discharge and large shrinkage deformation.
To sum up, the sintering process of the glass injection molding blank provided by the embodiment of the application is realized by adopting two high-temperature pressurizing and densifying processes, wherein the temperature and the pressure adopted by the second high-temperature pressurizing and densifying process are higher than those adopted by the first high-temperature pressurizing and densifying process, and the compactness of the glass injection molding blank is greatly improved after sintering.
Referring to fig. 2, fig. 2 is a flowchart of a method for processing a glass product according to an embodiment of the present disclosure. The embodiment of the application also provides a processing method of the glass product, which comprises the following steps:
100, providing a glass injection molding blank.
The "providing a glass injection molding preform" may specifically include:
and 110, providing glass raw materials, and grinding the glass raw materials to obtain glass powder, wherein the particle size of the glass powder is controlled within the range of 200-250 nm.
It can be understood that the smaller the size of the glass powder, the larger the surface energy, the more unstable the system is, according to the thermodynamic principle, the surface energy of the system has a significant effect on the melting temperature of the solid powder, the surface energy is increased, the melting temperature of the powder is decreased, but at the same time, the larger the surface energy means that the system is more prone to devitrification.
Illustratively, the glass frit may be crystal, quartz, soda lime glass, aluminosilicate glass, lithium aluminosilicate glass, or other chemically structured glass.
And 120, drying and sieving the dried glass powder.
For example, the dried glass frit may be dried in an oven.
And 130, providing an injection mold, injecting an injection material into a mold cavity of the injection mold, and heating and pressurizing to obtain the glass injection molding blank.
The injection material can comprise glass powder and an organic binder, and it can be understood that the organic binder mainly plays a role in promoting the bonding of the glass powder, and is beneficial to promoting the molding of the glass injection molding blank and improving the quality of the blank.
For example, the injection mold may include a male mold half and a female mold half, which enclose a mold cavity when the male mold half and the female mold half are closed.
Illustratively, the conditions of heating and pressurizing include: the temperature is 90-110 ℃, the pressure is 35-45 bar, and the heat preservation and pressure maintaining time is 2-6 seconds.
200, degreasing the glass injection molding blank.
The "degreasing the glass injection molded body" may include: and (3) placing the glass injection molding blank in a profiling mold for degreasing treatment.
When the profiling mold comprises a first mold and a second mold, the glass injection molding blank is placed between the first mold and the second mold, and a gap of 0.03-0.08 mm is kept between the first mold and the second mold. By controlling the gap between the first mold and the second mold to be 0.03 mm-0.08 mm, organic matters volatilized from the glass injection molding blank in the degreasing process can be ensured to smoothly overflow from the molds.
It is understood that after the glass injection molding blank is placed in the profiling mold for degreasing treatment, the glass injection molding blank can be transferred to a sintering device (i.e. SPS sintering furnace) together with the profiling mold for sintering while maintaining the state of the glass injection molding blank in the profiling mold.
Illustratively, the degreasing treatment may include:
pre-degreasing the glass injection-molded body by keeping the temperature of the glass injection-molded body at 100 to 180 ℃ (e.g., 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃ and the like) for 0.5 to 1.5 hours (e.g., 0.5 hour, 0.7 hour, 1 hour, 1.3 hours, 1.5 hours and the like);
after the pre-degreasing treatment, the glass injection molded blank is gradually heated to 420 to 480 ℃ (for example, 420 ℃, 430 ℃, 440 ℃, 450 ℃, 460 ℃, 470 ℃, 480 ℃ and the like) for 24 to 48 hours (for example, 24 hours, 28 hours, 32 hours, 36 hours, 40 hours, 44 hours, 48 hours and the like) to be degreased.
300, sintering the degreased glass injection molding blank according to the sintering process of the glass injection molding blank in any embodiment.
And 400, cooling the sintered glass injection molding blank to obtain the glass product.
Exemplarily, "cooling the sintered glass injection molded blank" may specifically include: and taking the sintered glass injection molding blank out of the sintering equipment, and naturally cooling the glass injection molding blank in the air.
The method of processing a glass article may further comprise:
and 500, annealing the cooled glass product.
It can be understood that by annealing the glass product, the stress generated during the cooling process of the glass product can be eliminated, and the self-explosion of the glass product can be avoided.
Illustratively, the conditions of the annealing treatment may include: the annealing temperature is 500 ℃ to 680 ℃ (e.g., 500 ℃, 530 ℃, 550 ℃, 580 ℃, 600 ℃, 620 ℃, 650 ℃, 680 ℃, etc.), and the holding time is 0.2 hours to 1 hour (e.g., 0.2 hour, 0.4 hour, 0.6 hour, 0.8 hour, 1 hour, etc.).
Illustratively, the annealing process may be performed in a nitrogen atmosphere sintering furnace, which helps prevent devitrification.
The embodiment of the application also provides a glass product which is prepared by adopting the processing method of the glass product in any embodiment. Illustratively, the density of the glass article is 2.0g/cm3～2.2g/cm3。
It can be understood that the processing method of the glass product (i.e. glass injection molding process) provided in the embodiment of the present application can be used for preparing various glass products, and is particularly suitable for preparing products that cannot be prepared by the conventional glass processing process (i.e. glass products with complex structures and small volumes), but the processing method of the glass product (glass injection molding process) provided in the embodiment of the present application has higher production cost compared with the conventional glass processing process, so theoretically, the glass product provided in the embodiment of the present application can be any glass product, but from the viewpoints of applicability of the manufacturing process and production cost, the glass product can be a glass product with complex structures and small volumes, such as a housing of an in-ear earphone or a front cover plate of a smart watch, and parts, such as a back cover and a front cover glass plate, in a mobile phone can also be prepared by the processing method of the glass product, but the production costs are relatively high compared to conventional glass processing techniques.
The sintering process of the glass injection molding blank and the processing method of the glass product provided by the embodiment of the present application are exemplified by the following specific embodiments.
Example 1
1. Grinding: strictly controlling the particle size of the aluminosilicate glass powder to be 200-220 nm through ball milling and sand milling processes; wherein the alumina-silica glass powder has a density of 2.3g/cm3The glass leftover material is prepared by crushing;
2. drying and granulating: putting the ball-milled slurry into an oven for drying, and sieving the dried powder;
3. injection molding: closing the male die and the female die, injecting an injection material into a die cavity enclosed by the male die and the female die, and maintaining the pressure for one time to obtain a glass injection molding blank;
4. placing the glass injection molding blank into a profiling mold, wherein the mold is divided into a convex mold and a concave mold corresponding to the convex mold, the surface of the concave mold is subjected to profiling design according to the appearance of the glass injection molding blank, then placing the glass injection molding blank into the concave mold, covering the convex mold, controlling the mold closing gap between the convex mold and the concave mold to be 0.05mm, and then performing degreasing treatment, wherein the porosity of the degreased glass injection molding blank is 22.5%;
SPS sintering: placing the glass injection molding blank body and the profiling mold into an SPS sintering furnace for sintering densification, wherein the SPS sintering process comprises the following steps: (1) heating to 620 deg.C for 2min, maintaining the sintering pressure at P1, and maintaining the sintering pressure at P1 of 0.1MPa for 1 min; (2) heating to 880 deg.C for 1min, and sintering at P1 to P2 under P2 MPa for 2 min; wherein, after SPS sintering, the porosity of the glass injection molding blank is measured to be 1.8%, and the density of the glass injection molding blank is measured to be 2.20g/cm3；
6. And (3) cooling: placing the sintered glass injection molding blank body in air for natural cooling;
7. annealing: and (3) placing the cooled glass injection molding blank body in a nitrogen atmosphere sintering furnace, heating to 630 ℃, and preserving heat for 0.2 hour.
As can be seen from example 1, a large amount of pores are generated on the glass injection molded blank after the degreasing treatment in step 4, and the porosity of the glass injection molded blank is 22.5%, but the porosity of the glass injection molded blank after the sintering treatment in step 5 is greatly reduced to 1.8%, that is, the compactness of the glass injection molded blank after sintering is greatly improved.
In addition, step 1 describes that the alumina-silica glass powder adopted by the glass injection molding process has a density of 2.3g/cm3It can be seen that after the sintering in step 5, the density of the glass injection-molded green body reached 2.20g/cm3The density of the sintered glass injection molding blank is close to that of a glass raw material, so that the sintered glass injection molding blank has higher compactness.
Example 2
1. Grinding: strictly controlling the particle size of the aluminosilicate glass powder to be 230-250 nm through ball milling and sand milling processes; wherein the alumina-silica glass powder has a density of 2.3g/cm3The glass leftover material is prepared by crushing;
2. drying and granulating: putting the ball-milled slurry into an oven for drying, and sieving the dried powder;
3. injection molding: closing the male die and the female die, injecting an injection material into a die cavity enclosed by the male die and the female die, and maintaining the pressure for one time to obtain a glass injection molding blank;
4. placing the glass injection molding blank into a profiling mold, wherein the mold is divided into a convex mold and a concave mold corresponding to the convex mold, the surface of the concave mold is subjected to profiling design according to the appearance of the glass injection molding blank, then placing the glass injection molding blank into the concave mold, covering the convex mold, controlling the mold closing gap between the convex mold and the concave mold to be 0.04mm, and then performing degreasing treatment, wherein the porosity of the degreased glass injection molding blank is 23.6%;
SPS sintering: placing the glass injection molding blank body and the profiling mold into an SPS sintering furnace for sintering densification, wherein the SPS sintering process comprises the following steps: (1) heating to 550 deg.C for 3min, maintaining the sintering pressure at P1, the sintering pressure P1 is 0.3MPa, and maintaining the constant temperature and pressure for 1.2 min; (2)1.5min heating to 850 deg.C, sintering at P1 to P2 under P2 MPa for 4 min; wherein, after SPS sintering, the porosity of the glass injection molding blank is measured to be 2.1%, and the density of the glass injection molding blank is 2.16g/cm3；
6. And (3) cooling: placing the sintered glass injection molding blank body in air for natural cooling;
7. annealing: and (3) placing the cooled glass injection molding blank body in a nitrogen atmosphere sintering furnace, heating to 580 ℃, and preserving heat for 0.5 hour.
As can be seen from example 2, a large amount of pores are generated on the glass injection molded blank after the degreasing treatment in step 4, and the porosity of the glass injection molded blank is 23.6%, but the porosity of the glass injection molded blank after the sintering treatment in step 5 is greatly reduced to 2.1%, that is, the compactness of the glass injection molded blank after sintering is greatly improved.
In addition, step 1 describes that the alumina-silica glass powder adopted by the glass injection molding process has a density of 2.3g/cm3Can see the glass raw material after the stepsAfter the sintering in step 5, the density of the glass injection molding blank reaches 2.16g/cm3The density of the sintered glass injection molding blank is close to that of a glass raw material, so that the sintered glass injection molding blank has higher compactness.
Example 3
1. Grinding: strictly controlling the particle size of the aluminosilicate glass powder to be 220-240 nm through ball milling and sand milling processes; wherein the alumina-silica glass powder has a density of 2.3g/cm3The glass leftover material is prepared by crushing;
2. drying and granulating: putting the ball-milled slurry into an oven for drying, and sieving the dried powder;
3. injection molding: closing the male die and the female die, injecting an injection material into a die cavity enclosed by the male die and the female die, and maintaining the pressure for one time to obtain a glass injection molding blank;
4. placing the glass injection molding blank into a profiling mold, wherein the mold is divided into a convex mold and a concave mold corresponding to the convex mold, the surface of the concave mold is subjected to profiling design according to the appearance of the glass injection molding blank, then placing the glass injection molding blank into the concave mold, covering the convex mold, controlling the mold closing gap between the convex mold and the concave mold to be 0.07mm, and then performing degreasing treatment, wherein the porosity of the degreased glass injection molding blank is 24.1%;
SPS sintering: placing the glass injection molding blank body and the profiling mold into an SPS sintering furnace for sintering densification, wherein the SPS sintering process comprises the following steps: (1) heating to 600 deg.C for 4min, maintaining the sintering pressure at P1, and maintaining the sintering pressure at P1 of 0.4MPa for 1.5 min; (2)1.7min heating to 830 deg.C, sintering at P1 to P2 under P2 MPa for 3 min; wherein, after SPS sintering, the porosity of the glass injection molding blank is measured to be 2.6%, and the density of the glass injection molding blank is measured to be 2.09g/cm3；
6. And (3) cooling: placing the sintered glass injection molding blank body in air for natural cooling;
7. annealing: and (3) placing the cooled glass injection molding blank body in a nitrogen atmosphere sintering furnace, heating to 550 ℃, and preserving heat for 0.8 hour.
As can be seen from example 3, a large amount of pores are generated on the glass injection molded blank after the degreasing treatment in step 4, and the porosity of the glass injection molded blank is 24.1%, but the porosity of the glass injection molded blank after the sintering treatment in step 5 is greatly reduced to 2.6%, that is, the compactness of the glass injection molded blank after sintering is greatly improved.
In addition, step 1 describes that the alumina-silica glass powder adopted by the glass injection molding process has a density of 2.3g/cm3It can be seen that the density of the glass injection-molded green body after the sintering in step 5 reached 2.09g/cm3The density of the sintered glass injection molding blank is close to that of a glass raw material, so that the sintered glass injection molding blank has higher compactness.
The sintering process of the glass injection molding blank, the processing method of the glass product and the glass product provided by the embodiment of the application are described in detail above. The principles and implementations of the present application are described herein using specific examples, which are presented only to aid in understanding the present application. Meanwhile, for those skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
Claims (11)
1. A sintering process of a glass injection molding blank is characterized by comprising the following steps:
placing the glass injection molding blank body in a profiling mold, and sintering in sintering equipment, wherein an accommodating space is arranged in the profiling mold, and the shape of the accommodating space is matched with that of the profiling mold; wherein, the process of sintering in the sintering equipment comprises the following steps:
after the sintering temperature of the sintering equipment is increased to T1, applying pressure to the profiling mold, after the pressure is increased from 0 to P1, maintaining T1 and P1 unchanged, and keeping for 0.5-1.5 min, wherein T1 is greater than the glass transition temperature of the glass injection molding blank body, and P1 is 0.1-0.5 MPa;
after the sintering temperature of the sintering equipment is increased from T1 to T2, the pressure applied to the profiling mold is increased, after the pressure is increased from P1 to P2, the T2 and the P2 are maintained unchanged and are kept for 2-4 min, wherein T2 is larger than T1, T2 is smaller than or equal to the softening point temperature of the glass injection molding blank, and P2 is 1-5 MPa.
2. The sintering process of a glass injection molding blank according to claim 1, wherein T1 is 450 ℃ to 640 ℃ and T2 is 800 ℃ to 900 ℃.
3. The sintering process of a glass injection molding blank according to claim 1, wherein the sintering temperature of the sintering equipment is increased from room temperature to T1 in 2-5 min, and from T1 to T2 in 1-2 min.
4. The sintering process of a glass injection molding blank according to claim 1, wherein the sintering equipment is an SPS sintering furnace.
5. A sintering process of a glass injection molding blank according to any one of claims 1-4, wherein the profiling mold comprises a first mold and a second mold, the placing the glass injection molding blank in the profiling mold comprises: and placing the glass injection molding blank between the first mold and the second mold, and keeping a gap of 0.03-0.08 mm between the first mold and the second mold.
6. A method of processing a glass article, comprising:
providing a glass injection molding blank body;
degreasing the glass injection molding blank;
sintering the degreased glass injection molding blank according to the sintering process of the glass injection molding blank according to any one of claims 1 to 5;
and cooling the sintered glass injection molding blank to obtain the glass product.
7. The method of claim 6, wherein the providing the glass injection molding blank comprises: and carrying out injection molding on the glass powder with the particle size of 200-250 nm to obtain the glass injection molding blank.
8. The method of processing a glass article according to claim 6, further comprising:
and annealing the cooled glass product.
9. The method of processing a glass article according to claim 8, wherein the conditions of the annealing treatment include: the annealing temperature is 500-680 ℃, and the heat preservation time is 0.2-1 hour.
10. The method for processing a glass product according to any of claims 6 to 9, wherein the degreasing treatment of the glass injection molded blank comprises: and placing the glass injection molding blank in the profiling mold for degreasing treatment.
11. A glass article produced by the method of processing a glass article according to any one of claims 6 to 10.
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| CN116922546A (en) * | 2023-09-18 | 2023-10-24 | 成都永益泵业股份有限公司 | Method for manufacturing molded part by using zirconia and pump flow passage component |
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