CN116135818A - Ceramic blank glue discharging method and ceramic workpiece preparation method - Google Patents
Ceramic blank glue discharging method and ceramic workpiece preparation method Download PDFInfo
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- CN116135818A CN116135818A CN202310198426.1A CN202310198426A CN116135818A CN 116135818 A CN116135818 A CN 116135818A CN 202310198426 A CN202310198426 A CN 202310198426A CN 116135818 A CN116135818 A CN 116135818A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 174
- 239000003292 glue Substances 0.000 title claims abstract description 81
- 238000007599 discharging Methods 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 102
- 239000012298 atmosphere Substances 0.000 claims abstract description 71
- 238000004321 preservation Methods 0.000 claims abstract description 54
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000011282 treatment Methods 0.000 claims description 39
- 238000001816 cooling Methods 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000000016 photochemical curing Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010146 3D printing Methods 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 abstract description 21
- 238000005336 cracking Methods 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 27
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 12
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 description 11
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 description 11
- 238000010586 diagram Methods 0.000 description 8
- 239000005416 organic matter Substances 0.000 description 8
- ZDHCZVWCTKTBRY-UHFFFAOYSA-N omega-Hydroxydodecanoic acid Natural products OCCCCCCCCCCCC(O)=O ZDHCZVWCTKTBRY-UHFFFAOYSA-N 0.000 description 6
- 238000007639 printing Methods 0.000 description 6
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000003776 cleavage reaction Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000007017 scission Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000002245 particle 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
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to the technical field of additive manufacturing, in particular to a glue discharging method of a ceramic blank and a preparation method of a ceramic workpiece. The glue discharging method comprises the following steps: 1) Preheating the ceramic blank in inert atmosphere at 150-250 ℃; 2) And (2) carrying out heat preservation and heat treatment on the ceramic blank obtained in the step (1) in an atmosphere containing oxygen, wherein the initial temperature of the heat preservation and heat treatment is 100-300 ℃ and the final temperature of the heat preservation and heat treatment is 450-800 ℃. The preparation method of the ceramic workpiece comprises the following steps: 1) The ceramic blank is subjected to glue discharging by adopting the glue discharging method; 2) And sintering the ceramic blank after the glue discharge to obtain the ceramic workpiece. The invention can effectively reduce the decomposition rate of organic matters in the ceramic blank body, reduce the cracking tendency of the ceramic blank body and improve the success rate of glue discharge.
Description
Technical Field
The invention relates to the technical field of additive manufacturing, in particular to a glue discharging method of a ceramic blank and a preparation method of a ceramic workpiece.
Background
Ceramic stereolithography (Cer-SLA) is a common ceramic indirect forming additive manufacturing technology, which is used for obtaining an initial blank by solidifying photosensitive slurry containing ceramic particles, and obtaining a final ceramic part through pyrolysis, glue discharging and sintering processes. The organic components in the initial green body account for about 50vol% and this portion needs to be removed by the pyrolysis de-glue process. The process can generate a large amount of gas, and the blank is often cracked by an improper heat treatment process, so that cracks generated by glue discharge are difficult to heal in the sintering process, and the performance of the final part is affected. At present, the design idea of the general glue discharging process is that a heat preservation section is arranged at a decomposition peak value under the condition of single atmosphere. However, the peak corresponds to the maximum decomposition rate point, after which the decomposition rate of the organic matters in the blank body is continuously reduced, which means that the decomposition rate cannot be effectively reduced by the general glue discharging process design curve. In addition, as the organic matters are decomposed and escape for a long time, the continuous temperature rise can lead the decomposition of the organic matters to shift to a high-temperature area, which can strengthen the impact of decomposed gas on a green body and easily lead to the cracking of parts.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a method for removing glue from a ceramic blank and a method for preparing a ceramic workpiece, which can effectively reduce the decomposition rate of organic matters in the ceramic blank, reduce the cracking tendency of the ceramic blank, and improve the success rate of removing glue.
To achieve the above and other related objects, a first aspect of the present invention provides a method for discharging glue from a ceramic body, including the steps of:
1) Preheating the ceramic blank in inert atmosphere at 150-250 deg.c, such as 150-200 deg.c or 200-250 deg.c;
the inert atmosphere is an atmosphere which does not contain oxygen and does not participate in the cracking reaction of the organic matters;
2) And (2) carrying out heat preservation and heat treatment on the ceramic blank obtained in the step (1) in an atmosphere containing oxygen, wherein the initial temperature of the heat preservation and heat treatment is 100-300 ℃, such as 100-200 ℃, 200-250 ℃ or 250-300 ℃, and the final temperature is 450-800 ℃, such as 450-500 ℃, 500-600 ℃ or 600-800 ℃.
Preferably, in step 1), at least one of the following technical features is further included:
11 Heating to the temperature of the preheating treatment at a heating rate of 0.1-5 ℃/min, such as 0.1-1 ℃/min or 1-5 ℃/min;
12 The preheating treatment time is 1-3 hr, such as 1-2 hr or 2-3 hr;
13 The preheating treatment is carried out under the condition of heat preservation;
14 The inert atmosphere is at least one selected from nitrogen, argon and vacuum atmosphere;
15 Cooling the ceramic body obtained by the preheating treatment to room temperature.
More preferably, in feature 15), the temperature is naturally reduced to room temperature, or alternatively, the rate of reduction is 1-5 ℃/min, such as 1-2.5 ℃/min or 2.5-5 ℃/min.
Preferably, in step 2), at least one of the following technical features is further included:
21 The atmosphere containing oxygen is air atmosphere or gas atmosphere with the volume content of 5-100 percent;
22 The ceramic blank obtained by the preheating treatment is cooled to room temperature and then is sequentially subjected to heating and heat treatment, and the temperature is raised to the initial temperature of the heat treatment;
23 The heat preservation heat treatment is multi-section heat preservation heat treatment, namely, a plurality of sections of heat preservation sections are arranged at intervals of a certain temperature gradient, and the peak decomposition rate point of the organic matters is not used as a process reference.
More preferably, at least one of the following technical features is further included:
221 In feature 22), the rate of temperature increase is 0.1 to 5 ℃/min, such as 0.1 to 1 ℃/min or 1 to 5 ℃/min;
231 In feature 23), the temperature gradient between the stages in the multi-stage insulation heat treatment is 5 to 50 ℃, such as 5 to 25 ℃ or 25 to 50 ℃;
232 In 23), the temperature rise rate between each stage in the multi-stage heat preservation heat treatment is 0.1 to 5 ℃/min, such as 0.1 to 1 ℃/min or 1 to 5 ℃/min;
233 In feature 23), the heat-retaining heat treatment time of each stage in the multi-stage heat-retaining heat treatment is 0.5 to 3hr, such as 0.5 to 45min or 45min to 3hr;
234 23) the initial temperature in the multi-stage heat preservation heat treatment is 100 to 300 ℃, such as 100 to 200 ℃,200 to 250 ℃ or 250 to 300 ℃;
235 In feature 23), the final temperature in the multi-stage soaking heat treatment is 450 to 800 ℃, such as 450 to 500 ℃, 500 to 600 ℃ or 600 to 800 ℃.
Preferably, in step 2), the heat-insulating heat treatment is followed by cooling. Naturally cooling to room temperature or cooling rate of 1-5 deg.c/min, such as 1-2.5 deg.c/min or 2.5-5 deg.c/min.
Preferably, the ceramic body has a volume fraction of organics ranging from 40 to 60%, such as 40 to 50% or 50 to 60%.
Preferably, the ceramic body is obtained by a stereolithography preparation method.
More preferably, the stereolithography preparation method specifically comprises the following steps: and carrying out photo-curing three-dimensional printing on the photosensitive slurry, wherein the photosensitive slurry comprises ceramic powder, photosensitive resin, a photoinitiator and an optional dispersing agent. The ceramic powder can be one or more of alumina, silicon oxide, zirconia, magnesia, silicon nitride, silicon carbide and the like, and the volume percentage can be 40-60%. The photosensitive resin can be one or more of HDDA, TMPTA, di-TMPTA, NPG2PODA and the like, and the volume percentage can be 30-50%. The photoinitiator can be one or more of 184, 651, TPO and the like, and the volume percentage can be 3-6%. The dispersing agent can be KH560, KH550, SA, BYK110, etc., and the volume percentage is 0-4% or 4-7%. The ceramic body obtained by printing can be subjected to glue discharging after being cleaned.
The second aspect of the present invention provides a method for producing a ceramic workpiece, comprising the steps of:
1) The ceramic blank is subjected to glue discharging by adopting the glue discharging method of the ceramic blank;
2) And sintering the ceramic blank after the glue discharge to obtain the ceramic workpiece.
The technical scheme has at least one of the following beneficial effects:
1) The invention provides a glue discharging method of a ceramic blank, which can be used for ceramic blanks manufactured by a stereo lithography technology, and can effectively reduce the decomposition rate of organic matters in the ceramic blank, reduce the cracking tendency of the ceramic blank, improve the glue discharging success rate, and especially improve the glue discharging success rate in the aspect of ceramic blanks with large wall thickness (more than or equal to 1 cm) and improve the glue discharging efficiency.
2) The glue discharging method carries out the preheating treatment under the inert atmosphere, the temperature of the preheating treatment is 150-250 ℃, the step can prevent oxygen from intervening low-temperature section small molecular organic matters from decomposing, and simultaneously, the organic matters in the blank body are secondarily solidified, so that the ceramic blank body can be prevented from cracking.
3) In the glue discharging method, the heat-preserving heat treatment is carried out in the atmosphere containing oxygen, and the ceramic blank is subjected to secondary heat treatment, preferably, the heat-preserving heat treatment is multistage heat-preserving heat treatment: and setting a plurality of sections of heat preservation sections with a certain temperature gradient as intervals, transferring the organic matter decomposition from the temperature rising section to the plurality of sections of heat preservation sections, and slowing down the accumulation of the organic matter so that the decomposition temperature is lower.
4) The glue discharging method can effectively control cracking of the ceramic blank in the glue discharging process, and ensure reliable performance of the ceramic workpiece.
Drawings
FIG. 1 is a physical image (200 ℃ C.) of the ceramic body of the glue discharging in the air atmosphere and the inert atmosphere in the step 1) in the example 1.
FIG. 2 is a physical image (150 ℃ C.) of the ceramic body of the glue discharging in the air atmosphere and the inert atmosphere in the step 1) in the example 1.
FIG. 3 is a physical image (250 ℃ C.) of the ceramic body of step 1) of example 1, which was discharged under an air atmosphere and an inert atmosphere, respectively.
Fig. 4 is a physical image of the ceramic body after the multi-stage heat-insulating treatment in example 1 and a physical image of the ceramic body after the treatments of step 1) and step 2) in example 2.
FIG. 5 is the weight loss data of the adhesive-removing ceramic body under different conditions.
FIG. 6 is a graph showing the decomposition rate statistics of the multi-stage thermal insulation paste ejection and the conventional paste ejection in example 3.
Fig. 7 is a physical diagram of a ceramic body obtained after the first and second ceramic body discharging treatments in example 4.
FIG. 8 is a graph showing the temperature profile of the adhesive discharge in the different processes of example 5.
FIG. 9 is a graph showing statistics of cleavage rates in the cleavage zone of the organic main body in example 6 under different processes.
Fig. 10 is a physical view of ceramic bodies of example 1, example 6 and example 7 after the glue is discharged.
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present invention, which is described by the following specific examples.
It should be understood that the structures, proportions, sizes, etc. shown in the drawings are for illustration purposes only and should not be construed as limiting the invention to the extent that it can be practiced, since modifications, changes in the proportions, or otherwise, used in the practice of the invention, are not intended to be critical to the essential characteristics of the invention, but are intended to fall within the spirit and scope of the invention. Also, the terms such as "upper," "lower," "left," "right," "middle," and "a" and the like recited in the present specification are merely for descriptive purposes and are not intended to limit the scope of the invention, but are intended to provide relative positional changes or modifications without materially altering the technical context in which the invention may be practiced.
The glue discharging method provided by the invention comprises two parts: 1) Preheating in inert atmosphere at the upper limit of 250 ℃, wherein the aim is to dry the blank body and remove uncured micromolecular substances; 2) And (3) performing heat-insulating treatment in an air atmosphere at the temperature of 800 ℃, wherein the aim is to crack organic matters in the blank body at high temperature, and the organic matters are decomposed into gaseous molecules to escape from the ceramic blank body in the process of glue discharging.
In fig. 5, the cracking behavior of organic matters in the ceramic body under the inert atmosphere and the air atmosphere is shown, and the results indicate that: under the air condition, the organic matters begin to decompose at about 100 ℃ and end at about 450 ℃, and the organic matters decompose in a four-stage decomposition mode; under an inert atmosphere, the organic matter starts to decompose at about 250 ℃ and ends at about 500 ℃, and the organic matter decomposition behavior is represented as a single-stage decomposition mode. It should be noted that, under an inert atmosphere, organic matters in the ceramic body may generate cracked carbon residues in the body due to lack of oxygen.
FIG. 5 shows that the temperature of the first stage of the invention does not reach the organic matter cracking temperature, the main purpose is drying, and the temperature of the second stage is raised to the organic matter cracking temperature, and the second stage is a glue discharging stage.
Example 1
Preparing a ceramic blank:
a) Mixing ceramic powder with photosensitive resin, photoinitiator and dispersing agent to prepare photosensitive slurry, wherein the ceramic powder is zirconia, and the volume percentage is 50%; the photosensitive resin is 1, 6-hexanediol diacrylate HDDA with the volume percentage of 40%; the photoinitiator is (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide TPO, and the volume percentage is 3%; the dispersing agent is silane coupling agent KH560, and the volume percentage is 7%.
b) Printing the photosensitive slurry obtained in the step 1) by using a photocuring 3D printer to obtain a ceramic blank, wherein the size of the ceramic blank is 10mm x 4mm cuboid, and the volume ratio of organic matters in the ceramic blank is 50%.
And (3) discharging glue from the ceramic blank and sintering to obtain a ceramic workpiece:
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was subjected to a preheating treatment using an atmosphere furnace under an inert atmosphere of nitrogen at a temperature of 200 ℃ (a temperature rising rate of 1 ℃/min from room temperature to 200 ℃) and was kept at 200 ℃ for 2 hours. And after the preheating treatment is finished, naturally cooling the ceramic body to room temperature. The physical image of the ceramic body cooled to room temperature is shown in a photograph of the inert atmosphere in fig. 1.
The inert atmosphere in the step is changed into air atmosphere, other conditions are not changed, and the physical image of the ceramic blank cooled to room temperature is shown in a photo of air in fig. 1 (crack generation exists).
In addition, the temperature of the preheating treatment under the nitrogen in the inert atmosphere in the step 1) is changed to 150 ℃, other conditions are the same, and a physical diagram of the ceramic blank cooled to room temperature is shown in a photo of the inert atmosphere in the figure 2; the inert atmosphere is changed into air atmosphere, the treatment temperature is changed into 150 ℃, other conditions are the same, and the physical image of the ceramic blank cooled to room temperature is shown in the photo of air (crack generation) in fig. 2.
Changing the temperature of the preheating treatment under the nitrogen in the inert atmosphere in the step 1) to 250 ℃, wherein other conditions are the same, and the physical diagram of the ceramic blank cooled to the room temperature is shown in a photo of the inert atmosphere in the figure 3; the inert atmosphere is changed into air atmosphere, the treatment temperature is changed into 250 ℃, other conditions are the same, and the physical image of the ceramic blank cooled to room temperature is shown in a photo of air in fig. 3 (cracks are generated and blackening occurs).
2) Carrying out multistage heat-preserving heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 100 ℃ at a heating rate of 1 ℃/min, and carrying out sectional heat preservation heat treatment at a temperature gradient of 25 ℃ between the sections, wherein the heat preservation time of each section is 45min, and the heating rate of each section is 1 ℃/min; then cooling to room temperature at a cooling rate of 2.5 ℃/min. The physical diagram of the ceramic body after the multi-section heat-preservation heat treatment is shown in the middle photo in fig. 10.
3) And after the glue discharging is completed, sintering treatment is carried out to obtain the ceramic workpiece.
Example 2
Ceramic body glue discharging:
1) The same ceramic body as in example 1 (rectangular parallelepiped with dimensions of 10mm x 4 mm) was heated to 200 ℃ at a rate of 1 ℃/min in an argon atmosphere and incubated for 2 hours, then naturally cooled to room temperature;
2) Carrying out multistage heat-insulating heat treatment on the ceramic blank obtained in the step 2) in an air atmosphere: heating from room temperature to 100 ℃ at a heating rate of 1 ℃/min, and carrying out sectional heat preservation heat treatment at a temperature gradient of 25 ℃ between the sections, wherein the heat preservation time of each section is 45min, and the heating rate of each section is 1 ℃/min; and then naturally cooling to room temperature to obtain a ceramic body physical image, wherein the right photo (no crack is generated) in the figure 4.
And (2) ceramic green body glue discharging:
the same ceramic body as in example 1 (rectangular parallelepiped with dimensions of 10mm x 4 mm) was heated to 330 ℃ at 1 ℃/min in an air atmosphere, incubated for 180 minutes, heated to 390 ℃ at 1 ℃/min in an air atmosphere, incubated for 180 minutes, heated to 600 ℃ at 1 ℃/min in an air atmosphere, and then naturally cooled to room temperature, to give a photograph of the left side of the ceramic body (with cracks generated) as seen in the physical diagram of fig. 4.
Example 3
Multistage heat preservation and glue discharge: performing heat preservation heat treatment on the ceramic blank (same as in the embodiment 1) in an air atmosphere, wherein the heat preservation heat treatment is multi-stage heat preservation heat treatment, the initial temperature in the multi-stage heat preservation treatment is 300 ℃, the final temperature is 450 ℃, the temperature is increased from room temperature to the initial temperature of the heat preservation heat treatment at a heating rate of 1 ℃/min, the heating rate of 1 ℃/min between the stages in the multi-stage heat preservation heat treatment is 25 ℃, and the heat preservation heat treatment time of the stages is 30 minutes; the decomposition rate was counted every 15 seconds during the above process, see the statistical chart on the left side of fig. 6.
Traditional glue discharging: the ceramic body (same as in example 1) was subjected to paste ejection under an air atmosphere: heating from room temperature to 330 ℃ at a heating rate of 1 ℃/min, and preserving heat for 3 hours; heating to 390 ℃ at a heating rate of 1 ℃/min, and preserving heat for 3 hours; heating to 600 ℃ at a heating rate of 1 ℃/min, and immediately cooling to room temperature at the speed of 1 ℃/min; the decomposition rate was counted every 15 seconds during the above process, see the statistical chart on the left side of fig. 6.
FIG. 6 is a graph showing statistics of cleavage rate in the organic main cleavage zone at the same temperature increase rate (1 ℃ C./min). The results show that: the multi-section heat preservation and glue discharge can reduce the cracking rate from 8.7681 per mill/min to 5.5570 per mill/min by 36.62 percent. This is mainly because, in multistage heat preservation row glue, organic matter mainly breaks down in continuous heat preservation section, reduces organic matter accumulation utility. The traditional adhesive discharging lacks a continuous heat preservation section, and organic matters can be accumulated continuously due to incomplete decomposition, so that the peak decomposition temperature is increased. Therefore, the invention can more surely complete the glue discharging process and reduce the possibility of cracking the ceramic body under the same heating rate.
Example 4
Preparing a ceramic blank:
a) Mixing ceramic powder with photosensitive resin, photoinitiator and dispersing agent to prepare photosensitive slurry, wherein the ceramic powder is zirconia, and the volume percentage is 50%; the photosensitive resin is 1, 6-hexanediol diacrylate HDDA with the volume percentage of 40%; the photoinitiator is (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide TPO, and the volume percentage is 3%; the dispersing agent is silane coupling agent KH560, and the volume percentage is 7%.
b) Printing the photosensitive paste obtained in the step 1) by using a photocuring 3D printer to obtain a ceramic blank, wherein the size is as follows: a cylinder with the diameter of 10mm and the height of 10mm, and the volume ratio of organic matters in the ceramic body is 50%.
Ceramic body glue discharging:
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was subjected to a preheating treatment using an atmosphere furnace under an inert atmosphere of nitrogen at a temperature of 200 ℃ (a temperature rising rate of 1 ℃/min from room temperature to 200 ℃) and was kept at 200 ℃ for 2 hours. And after the preheating treatment is finished, naturally cooling the ceramic body to room temperature.
2) Carrying out multistage heat-preserving heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 100 ℃ at a heating rate of 1 ℃/min, and carrying out sectional heat preservation heat treatment at a temperature gradient of 25 ℃ between the sections, wherein the heat preservation time of each section is 45min, and the heating rate of each section is 1 ℃/min; then cooling to room temperature at a cooling rate of 2.5 ℃/min. The physical diagram of the ceramic body after the multi-section heat-preservation heat treatment is shown in the left photo in fig. 7.
And (2) ceramic green body glue discharging:
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was heat treated using an atmosphere furnace under an inert atmosphere of nitrogen at 200 ℃ (temperature was raised from room temperature to 200 ℃ at a temperature-raising rate of 1 ℃/min) and was kept at 200 ℃ for 2 hours. And after the heat treatment is finished, naturally cooling the ceramic body to room temperature.
2) Carrying out heat preservation and heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 330 ℃ at a heating rate of 1 ℃/min, and preserving heat for 3 hours; heating to 390 ℃ at a heating rate of 1 ℃/min, and preserving heat for 3 hours; heating to 600 ℃ at a heating rate of 1 ℃/min, and naturally cooling the ceramic blank to room temperature at a cooling rate of 2.5 ℃/min. The physical image of the treated ceramic body is shown in the right photo (with cracks) in fig. 7.
The results show that: the ceramic body glue discharging second has higher cracking tendency on the ceramic body with large wall thickness than the ceramic body glue discharging first (namely the glue discharging method of the invention). The glue discharging method is more stable, and the success rate of glue discharging of ceramic parts with large wall thickness (more than or equal to 1 cm) is higher.
Example 5
Preparing a ceramic blank:
a) Mixing ceramic powder with photosensitive resin, photoinitiator and dispersing agent to prepare photosensitive slurry, wherein the ceramic powder is zirconia, and the volume percentage is 50%; the photosensitive resin is 1, 6-hexanediol diacrylate HDDA with the volume percentage of 40%; the photoinitiator is (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide TPO, and the volume percentage is 3%; the dispersing agent is silane coupling agent KH560, and the volume percentage is 7%.
b) Printing the photosensitive paste obtained in the step 1) by using a photocuring 3D printer to obtain a ceramic blank, wherein the size is as follows: a cylinder with the diameter of 10mm and the height of 10mm, and the volume ratio of organic matters in the ceramic body is 50%.
Ceramic body glue discharging one (glue discharging temperature curve is shown in the multi-step heat preservation in figure 8):
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was subjected to a preheating treatment using an atmosphere furnace under an inert atmosphere of nitrogen at a temperature of 200 ℃ (a temperature rising rate of 1 ℃/min from room temperature to 200 ℃) and was kept at 200 ℃ for 120 minutes. And after the preheating treatment is finished, naturally cooling the ceramic body to room temperature.
2) Carrying out multistage heat-preserving heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 100 ℃ at a heating rate of 5 ℃/min, and carrying out sectional heat preservation heat treatment at a temperature gradient of 25 ℃ between the sections, wherein the heat preservation time of each section is 45min, and the heating rate of each section is 5 ℃/min; then cooling to room temperature at a cooling rate of 5 ℃/min.
The decomposition rate was counted every 15 seconds after the temperature was raised to 100℃in step 2), see the graph on the right side of FIG. 9.
Ceramic body glue discharging two (glue discharging temperature curve is shown in figure 8, two-step heat preservation is that two-step glue discharging):
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was heat treated using an atmosphere furnace under an inert atmosphere of nitrogen at 600 ℃ (temperature was raised from room temperature to 600 ℃ at a temperature-raising rate of 1 ℃/min) and incubated at 600 ℃ for 120 minutes. And after the heat treatment is finished, naturally cooling the ceramic body to room temperature.
2) Carrying out heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 600 ℃ at a heating rate of 1 ℃/min, and keeping the temperature for 120 minutes; then cooling to room temperature at a cooling rate of 1 ℃/min.
The decomposition rate was counted every 15 seconds during the above process, see the statistical chart on the left side of fig. 9.
FIG. 9 shows the organic cracking rate statistics for the two-step dispensing (two-step hold) process and the multi-step dispensing (multi-step hold) process at different ramp rates. The results show that: the multi-step glue discharging process can achieve the effect of the two-step glue discharging process at a faster glue discharging rate due to the existence of the continuous heat preservation section. At 5 ℃/min, the glue discharging speed of the multi-step glue discharging process can be equivalent to that of the two-step glue discharging process at 1 ℃/min. This shows that for small wall thickness parts, the multi-step dispensing process can more quickly complete the dispensing process.
FIG. 8 shows the two-step and multi-step dispensing process dispensing curves at different heating rates. The two-step glue discharging process takes about 42 hours, while the multi-step glue discharging process takes about 27 hours under the same effect, the time consumption is reduced by about 35.71%, and the glue discharging efficiency is improved.
Example 6
Preparing a ceramic blank:
a) Mixing ceramic powder with photosensitive resin, photoinitiator and dispersing agent to prepare photosensitive slurry, wherein the ceramic powder is zirconia, and the volume percentage is 50%; the photosensitive resin is 1, 6-hexanediol diacrylate HDDA with the volume percentage of 40%; the photoinitiator is (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide TPO, and the volume percentage is 3%; the dispersing agent is silane coupling agent KH560, and the volume percentage is 7%.
b) Printing the photosensitive slurry obtained in the step 1) by using a photocuring 3D printer to obtain a ceramic blank, wherein the size of the ceramic blank is 10mm x 4mm cuboid, and the volume ratio of organic matters in the ceramic blank is 50%.
And (3) ceramic green body glue discharging:
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was subjected to a preheating treatment using an atmosphere furnace under an inert atmosphere of nitrogen at a temperature of 150 ℃ (a temperature rising rate of 0.1 ℃/min from room temperature to 150 ℃) and was kept at 150 ℃ for 3 hours. And after the preheating treatment is finished, naturally cooling the ceramic body to room temperature. The ceramic body cooled to room temperature is crack-free.
2) Carrying out multistage heat-preserving heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 250 ℃ at a heating rate of 5 ℃/min, and carrying out sectional heat preservation heat treatment at a temperature gradient of between 250 and 800 ℃ at 5 ℃, wherein the heat preservation time of each section is 30 minutes, and the heating rate of each section is 5 ℃/min; and then cooling to room temperature, wherein the cooling rate is 5 ℃/min, and the obtained ceramic blank has no crack, and the physical diagram is shown in the right-most photograph in fig. 10.
Example 7
Preparing a ceramic blank:
a) Mixing ceramic powder with photosensitive resin, photoinitiator and dispersing agent to prepare photosensitive slurry, wherein the ceramic powder is zirconia, and the volume percentage is 50%; the photosensitive resin is 1, 6-hexanediol diacrylate HDDA with the volume percentage of 40%; the photoinitiator is (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide TPO, and the volume percentage is 3%; the dispersing agent is silane coupling agent KH560, and the volume percentage is 7%.
b) Printing the photosensitive slurry obtained in the step 1) by using a photocuring 3D printer to obtain a ceramic blank, wherein the size of the ceramic blank is 10mm x 4mm cuboid, and the volume ratio of organic matters in the ceramic blank is 50%.
And (3) ceramic green body glue discharging:
the ceramic blank is subjected to glue discharging treatment after being cleaned, and the specific steps are as follows:
1) The ceramic body was subjected to a preheating treatment using an atmosphere furnace under an inert atmosphere of nitrogen at a temperature of 250 ℃ (a temperature rising rate of 5 ℃/min from room temperature to 250 ℃) and was kept at 250 ℃ for 1 hour. And after the preheating treatment is finished, naturally cooling the ceramic body to room temperature. The ceramic body cooled to room temperature is crack-free.
2) Carrying out multistage heat-preserving heat treatment on the ceramic blank obtained in the step 1) in an air atmosphere: heating from room temperature to 200 ℃ at a heating rate of 0.1 ℃/min, and carrying out sectional heat preservation heat treatment at 200-500 ℃ with a temperature gradient of 50 ℃ between each two sections, wherein the heat preservation time of each section is 3hr, and the heating rate of each section is 0.1 ℃/min; and then cooling to room temperature, wherein the cooling rate is 1 ℃/min, and the obtained ceramic blank has no crack, and the physical diagram is shown in the leftmost photo in fig. 10.
In summary, the present invention effectively overcomes the disadvantages of the prior art and has high industrial utility value.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. The glue discharging method of the ceramic blank is characterized by comprising the following steps of:
1) Preheating the ceramic blank in inert atmosphere at 150-250 ℃;
2) And (2) carrying out heat preservation and heat treatment on the ceramic blank obtained in the step (1) in an atmosphere containing oxygen, wherein the initial temperature of the heat preservation and heat treatment is 100-300 ℃ and the final temperature of the heat preservation and heat treatment is 450-800 ℃.
2. The method for discharging glue from a ceramic body according to claim 1, wherein in step 1), at least one of the following technical features is further included:
11 Heating to the temperature of the preheating treatment at a heating rate of 0.1-5 ℃/min;
12 The preheating treatment time is 1-3 hr;
13 The preheating treatment is carried out under the condition of heat preservation;
14 The inert atmosphere is at least one selected from nitrogen, argon and vacuum atmosphere;
15 Cooling the ceramic body obtained by the preheating treatment to room temperature.
3. The method for discharging a paste on a ceramic body according to claim 2, wherein in the step 15), the temperature is naturally lowered to room temperature or the temperature lowering rate is 1 to 5 ℃/min.
4. The method for discharging glue from a ceramic body according to claim 1, wherein in step 2), at least one of the following technical features is further included:
21 The atmosphere containing oxygen is air atmosphere or gas atmosphere with the volume content of 5-100 percent;
22 The ceramic blank obtained by the preheating treatment is cooled to room temperature and then is sequentially subjected to heating and heat treatment, and the temperature is raised to the initial temperature of the heat treatment;
23 The heat preservation heat treatment is multi-stage heat preservation heat treatment.
5. The method of dispensing ceramic green body of claim 4, further comprising at least one of the following features:
221 In the feature 22), the heating rate is 0.1-5 ℃/min;
231 In the feature 23), the temperature gradient between each section in the multi-section heat preservation heat treatment is 5-50 ℃;
232 In the characteristic 23), the temperature rising rate between each two sections in the multi-section heat preservation and heat treatment is 0.1-5 ℃/min;
233 In the feature 23), the heat-retaining heat treatment time of each stage in the multi-stage heat-retaining heat treatment is 0.5 to 3hr;
234 In the step 23), the initial temperature in the multi-stage heat preservation heat treatment is 100-300 ℃;
235 In the feature 23), the final temperature in the multi-stage heat preservation heat treatment is 450-800 ℃.
6. The method for discharging paste from a ceramic body according to claim 1, wherein in the step 2), the cooling is performed after the heat-retaining heat treatment.
7. The method for discharging glue from a ceramic body according to any one of claims 1 to 6, wherein the volume ratio of organic matters in the ceramic body is 40-60%.
8. The method for discharging a ceramic body according to any one of claims 1 to 6, wherein the ceramic body is obtained by a stereolithography preparation method.
9. The method for discharging paste from a ceramic body according to claim 8, wherein said method for preparing by stereolithography comprises the steps of: and carrying out photo-curing three-dimensional printing on the photosensitive slurry, wherein the photosensitive slurry comprises ceramic powder, photosensitive resin, a photoinitiator and an optional dispersing agent.
10. The preparation method of the ceramic workpiece is characterized by comprising the following steps:
1) Performing glue discharging on the ceramic blank by adopting the glue discharging method of the ceramic blank according to any one of claims 1 to 9;
2) And sintering the ceramic blank after the glue discharge to obtain the ceramic workpiece.
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| CN117550902A (en) * | 2023-11-24 | 2024-02-13 | 苏州众芯联电子材料有限公司 | Glue discharging method suitable for high-heat-conductivity aluminum nitride ceramic |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06345544A (en) * | 1993-06-14 | 1994-12-20 | Honda Motor Co Ltd | Method for dewaxing molded body |
| CN103664190A (en) * | 2013-11-26 | 2014-03-26 | 河海大学 | Method for preparing porous silicon nitride ceramic |
| CN105330268A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Manufacturing method of laminated ceramics |
| CN106631037A (en) * | 2016-12-14 | 2017-05-10 | 潮州三环（集团）股份有限公司 | Binder removal method of aluminum nitride green body and preparation method of aluminum nitride ceramic substrate |
| CN109650887A (en) * | 2019-01-23 | 2019-04-19 | 南京航空航天大学 | A kind of preparation method of the lead free piezoelectric ceramics of potassium sodium niobate of Stereolithography |
| CN110372398A (en) * | 2019-07-05 | 2019-10-25 | 武汉理工大学 | A kind of quick degreasing sintered method of Stereolithography ceramic body |
| CN111302771A (en) * | 2020-02-23 | 2020-06-19 | 西北工业大学 | Two-step degreasing method for 3D printing ceramic core biscuit |
| CN112898032A (en) * | 2021-02-04 | 2021-06-04 | 江西理工大学 | Method for controlling thermal degreasing rate of gel-casting ceramic green body |
| CN112939581A (en) * | 2021-02-02 | 2021-06-11 | 广东工业大学 | Zirconia toughened alumina cutter and preparation method thereof |
| CN113956023A (en) * | 2021-11-16 | 2022-01-21 | 中国人民解放军国防科技大学 | Method for preparing aluminum oxide ceramic based on sinking type DLP photocuring 3D printing |
| CN114685148A (en) * | 2022-03-31 | 2022-07-01 | 广东康荣高科新材料股份有限公司 | Preparation method of alumina ceramic suitable for double degreasing process |
| CN115010481A (en) * | 2022-02-22 | 2022-09-06 | 成都大学 | Method for 3D printing of transparent ceramic with complex shape without support |
-
2023
- 2023-03-03 CN CN202310198426.1A patent/CN116135818A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06345544A (en) * | 1993-06-14 | 1994-12-20 | Honda Motor Co Ltd | Method for dewaxing molded body |
| CN103664190A (en) * | 2013-11-26 | 2014-03-26 | 河海大学 | Method for preparing porous silicon nitride ceramic |
| CN105330268A (en) * | 2015-12-03 | 2016-02-17 | 广东工业大学 | Manufacturing method of laminated ceramics |
| CN106631037A (en) * | 2016-12-14 | 2017-05-10 | 潮州三环（集团）股份有限公司 | Binder removal method of aluminum nitride green body and preparation method of aluminum nitride ceramic substrate |
| CN109650887A (en) * | 2019-01-23 | 2019-04-19 | 南京航空航天大学 | A kind of preparation method of the lead free piezoelectric ceramics of potassium sodium niobate of Stereolithography |
| CN110372398A (en) * | 2019-07-05 | 2019-10-25 | 武汉理工大学 | A kind of quick degreasing sintered method of Stereolithography ceramic body |
| CN111302771A (en) * | 2020-02-23 | 2020-06-19 | 西北工业大学 | Two-step degreasing method for 3D printing ceramic core biscuit |
| CN112939581A (en) * | 2021-02-02 | 2021-06-11 | 广东工业大学 | Zirconia toughened alumina cutter and preparation method thereof |
| CN112898032A (en) * | 2021-02-04 | 2021-06-04 | 江西理工大学 | Method for controlling thermal degreasing rate of gel-casting ceramic green body |
| CN113956023A (en) * | 2021-11-16 | 2022-01-21 | 中国人民解放军国防科技大学 | Method for preparing aluminum oxide ceramic based on sinking type DLP photocuring 3D printing |
| CN115010481A (en) * | 2022-02-22 | 2022-09-06 | 成都大学 | Method for 3D printing of transparent ceramic with complex shape without support |
| CN114685148A (en) * | 2022-03-31 | 2022-07-01 | 广东康荣高科新材料股份有限公司 | Preparation method of alumina ceramic suitable for double degreasing process |
Non-Patent Citations (1)
| Title |
|---|
| 张旭东等: "无机非金属材料学", 30 November 2000, 山东大学出版社, pages: 71 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117550902A (en) * | 2023-11-24 | 2024-02-13 | 苏州众芯联电子材料有限公司 | Glue discharging method suitable for high-heat-conductivity aluminum nitride ceramic |
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