CN116239385A - 3D printing silicon carbide slurry suitable for ink direct writing technology and preparation thereof - Google Patents
3D printing silicon carbide slurry suitable for ink direct writing technology and preparation thereof Download PDFInfo
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- CN116239385A CN116239385A CN202310092675.2A CN202310092675A CN116239385A CN 116239385 A CN116239385 A CN 116239385A CN 202310092675 A CN202310092675 A CN 202310092675A CN 116239385 A CN116239385 A CN 116239385A
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- silicon carbide
- cellulose
- loofah sponge
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 58
- 239000002002 slurry Substances 0.000 title claims abstract description 34
- 238000010146 3D printing Methods 0.000 title claims abstract description 21
- 238000005516 engineering process Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000001913 cellulose Substances 0.000 claims abstract description 53
- 229920002678 cellulose Polymers 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 50
- 244000280244 Luffa acutangula Species 0.000 claims abstract description 49
- 235000009814 Luffa aegyptiaca Nutrition 0.000 claims abstract description 49
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- 235000003956 Luffa Nutrition 0.000 claims abstract description 22
- 241000219138 Luffa Species 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000005406 washing Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 23
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- 239000000679 carrageenan Substances 0.000 claims description 13
- 235000010418 carrageenan Nutrition 0.000 claims description 13
- 229920001525 carrageenan Polymers 0.000 claims description 13
- 229940113118 carrageenan Drugs 0.000 claims description 13
- 235000011187 glycerol Nutrition 0.000 claims description 13
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000003921 oil Substances 0.000 claims description 12
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000004061 bleaching Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000000944 Soxhlet extraction Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000007639 printing Methods 0.000 abstract description 8
- 239000002270 dispersing agent Substances 0.000 abstract description 7
- 229910021426 porous silicon Inorganic materials 0.000 abstract description 7
- 238000005245 sintering Methods 0.000 abstract description 7
- 241000196324 Embryophyta Species 0.000 abstract description 4
- 229920001046 Nanocellulose Polymers 0.000 abstract description 4
- 238000003763 carbonization Methods 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000010297 mechanical methods and process Methods 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004513 sizing Methods 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 21
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 230000007935 neutral effect Effects 0.000 description 9
- 238000004321 preservation Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000011534 incubation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229940093932 potassium hydroxide Drugs 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 3
- 229960002218 sodium chlorite Drugs 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- 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
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Abstract
The invention relates to 3D printing silicon carbide slurry suitable for an ink direct writing technology and a preparation method thereof, wherein the slurry comprises 0.3-1% of luffa cellulose and 40-60% of silicon carbide ceramic powder by mass. The loofah sponge serving as a plant with high cellulose content can be treated by a chemical-mechanical method to prepare nano cellulose with excellent performance, and the nano cellulose serving as a dispersing agent is added into ceramic slurry, so that the plant has the advantages of easily available raw materials, low cost, environmental protection, no toxicity and the like. The sizing agent prepared by mixing cellulose and silicon carbide has the characteristics of stable extrusion speed, uniform density, difficult filament breakage, stable structure, difficult collapse and the like in the printing process. The luffa cellulose serving as a dispersing agent is uniformly dispersed in the silicon carbide particles, and the cellulose can play a role in connecting the silicon carbide particles to improve the strength and improve the overall conductivity through carbonization in the sintering process. The printed porous silicon carbide has good electromagnetic shielding performance and controllable heat conduction performance.
Description
Technical Field
The invention discloses a preparation method of 3D printing silicon carbide slurry suitable for an ink direct writing technology, and belongs to the technical field of 3D printing forming.
Background
The silicon carbide ceramic is mainly covalent bond and has high bonding strength, so that the silicon carbide ceramic has the advantages of high melting point, high hardness, high elastic modulus, good thermal conductivity, lower thermal expansion coefficient and the like, is a good high-temperature-resistant structural material, and is applied to various engineering fields. However, the high hardness and strength of silicon carbide make machining difficult, and lightweight preparation is difficult to achieve, so that the development of silicon carbide as a structural material is limited.
The 3D printing technique (additive manufacturing) is a rapid prototyping technique. The technology is based on a digital model file, and near net shaping is realized by using a powder or polymer and other bondable materials in a layer-by-layer printing mode. The development of 3D printed ceramic materials has made ceramic weight reduction possible. The silicon carbide powder is one of the most common ceramic powder, and the slurry prepared by the silicon carbide powder has the characteristics of easy sedimentation, easy agglomeration, poor fluidity and the like, and is easy to separate from the water in the process of extruding the nozzle. It is therefore necessary to add a large amount of dispersant to the slurry.
Cellulose has the characteristic of hydrophilic crosslinking in solution, and is a widely used dispersing agent. The loofah sponge serving as a plant with high cellulose content can be treated by a chemical-mechanical method to prepare nano cellulose with excellent performance, and the nano cellulose serving as a dispersing agent is added into ceramic slurry, so that the plant has the advantages of easily available raw materials, low cost, environmental protection, no toxicity and the like.
Disclosure of Invention
The invention aims to provide 3D printing silicon carbide slurry suitable for an ink direct writing technology and a preparation method thereof, so as to solve the problem that water-based slurry of silicon carbide ceramic powder is easy to separate from water in the process of extruding a nozzle due to self-dispersion, and further solve the problem that the silicon carbide ceramic slurry cannot be applied to the 3D printing field of the ink direct writing technology.
The technical scheme of the invention is as follows:
the utility model provides a 3D prints carborundum thick liquids suitable for ink write-through technique which characterized in that: the slurry comprises 40-60% of silicon carbide ceramic powder and 0.3-1% of luffa cellulose by mass percent.
The slurry of the invention can be composed of: 40 to 60wt percent of silicon carbide ceramic powder, 0.3 to 1wt percent of luffa cellulose, 10 to 15wt percent of glycerol, 0.05 to 0.1wt percent of carrageenan and the balance of deionized water.
Wherein the silicon carbide ceramic powder is silicon carbide whisker and/or silicon carbide particle, the particle size is 50 nm-50 mu m, and the purity is 99% -99.99%.
Wherein the luffa cellulose is in a thread shape or a sheet shape, and the size range is 10 nm-1 mu m.
The invention also provides a preparation method of the 3D printing silicon carbide slurry suitable for the ink direct writing technology, which is characterized by comprising the following steps:
(1) Mixing deionized water and glycerin according to a volume ratio of 2:1-1:1 to obtain a water-oil mixed solution;
(2) Respectively putting the luffa cellulose and carrageenan into the water-oil mixed solution according to the feed-liquid ratio of 10-50 g:1L and 2-5 g:1L, stirring for 30min at 80 ℃, and cooling to room temperature;
(3) Mixing silicon carbide ceramic powder with the solution obtained in the step (2) according to the mass ratio of 3:1-2:1, and filtering the obtained slurry by using a 2000-mesh screen.
In the step (3), the mixing process of the silicon carbide ceramic powder and the solution is stirring and/or ball milling; wherein:
the stirring speed is 10-500 rpm, and the stirring time is more than 0.5h;
the ball milling speed is 30-300 rpm, the ball milling time is 4-10 h, and the mass ratio of the grinding balls to the slurry is more than 0.1.
The preparation method of the loofah sponge cellulose comprises the following steps:
1) Pretreatment of raw materials: cleaning the loofah sponge, drying the loofah sponge at 80-90 ℃ for 4-6 hours, crushing the loofah sponge, and sieving the crushed loofah sponge with a 40-mesh sieve to obtain loofah sponge powder;
2) Preparing benzene-ethanol solution according to a volume ratio of 2:1, wrapping loofah sponge powder with filter paper, and placing the loofah sponge powder into a Soxhlet extractor according to a feed liquid ratio of 1g:20 mL-1 g:50mL, and carrying out Soxhlet extraction for 6-12 h at 80-100 ℃; naturally cooling to room temperature, washing with deionized water for 4-6 times, and suction filtering;
3) Putting the loofah sponge powder obtained in the step 2) into 20 g/L-30 g/L NaClO according to the ratio of 1g to 20g to 50g of the solution to the solution 2 In the aqueous solution, glacial acetic acid is used for regulating the pH value to 2-3, bleaching is carried out for 2-4 hours at 80 ℃, natural cooling is carried out to room temperature, deionized water is used for washing and suction filtration is carried out, and the whole step is repeated for three times;
4) Putting the loofah sponge powder obtained in the step 3) into a KOH aqueous solution with the mass fraction of 10% according to the feed-liquid ratio of 1g to 20mL to 1g to 50mL, performing alkaline washing at 80 ℃ for 4 to 6 hours, cooling, washing to neutrality, and performing suction filtration;
5) Putting the loofah sponge powder obtained in the step 4) into H with the mass fraction of 50% -60% according to the ratio of 1g to 20 mL-1 g to 50mL of feed liquid 2 SO 4 Washing with acid for 6-8 h at 50 ℃ in aqueous solution, cooling, washing with water to neutrality, and centrifugally washing to neutrality;
6) Ultrasonic treatment is carried out on the cellulose aqueous solution obtained in the step 5) for 1 to 3 hours in a cell crusher under the power of 60 to 200W;
7) And (3) placing the aqueous solution of cellulose obtained in the step (6) into a freeze dryer, and drying for 20-40 h at a temperature lower than-40 ℃ to obtain the loofah sponge cellulose.
Compared with the prior art, the invention has the following advantages:
the 3D printing silicon carbide slurry provided by the invention can be suitable for an ink direct-writing type 3D printer, and the printing height can exceed one centimeter. In the printing process, the paste has the characteristics of stable extrusion speed, uniform density, difficult filament breakage, stable structure, difficult collapse and the like. The luffa cellulose serving as a dispersing agent is uniformly dispersed in the silicon carbide particles, and the cellulose can play a role in connecting the silicon carbide particles to improve the strength and improve the overall conductivity through carbonization in the sintering process. The printed porous silicon carbide has good electromagnetic shielding performance and controllable heat conduction performance.
Drawings
Fig. 1 is a physical image of the luffa cellulose of example 1 after a freeze-drying step.
FIG. 2 is a graph showing the tyndall effect of an aqueous dispersion of low concentration luffa cellulose in example 1.
FIG. 3 is a photograph of Zeta potential of an aqueous dispersion of low concentration retinervus Luffae cellulose of example 1.
FIG. 4 is a scanning electron micrograph of retinervus Luffae cellulose of example 1.
Fig. 5 is a transmission electron micrograph of retinervus luffae cellulose of example 1.
Fig. 6 is a graphical representation of the silicon carbide dispersing ability of luffa cellulose at various concentrations in example 1.
FIG. 7 is a photograph of Zeta potential of 10g/L luffa cellulose dispersion of example 1.
FIG. 8 is a photograph of Zeta potential of 20g/L luffa cellulose dispersion of example 1.
Fig. 9 is a 3D printed physical image of the silicon carbide slurry prepared in example 1 through the ink direct writing technique.
Fig. 10 is a physical picture of the 3D printing samples prepared in examples 1 (a), 2 (b) and comparative example 1 (c).
FIG. 11 is a macroscopic scanning electron micrograph of the 3D printed coupon prepared in example 1 after incubation for 2h at 1600 ℃.
FIG. 12 is a microscopic scanning electron micrograph of the 3D printed coupon prepared in example 1 after incubation at 1600℃for 2h.
FIG. 13 is a graph showing the resistivity of the 3D printed sample prepared in example 1 after heat preservation at 1600℃for 2 hours.
Fig. 14 is a graph showing electromagnetic shielding performance of the 3D printing sample prepared in example 1 after heat preservation at 1600 ℃ for 2 hours, wherein (a) electromagnetic shielding performance value and (b) shielding coefficient.
Fig. 15 is a graph showing the density and thermal conductivity of the 3D printed sample prepared in example 3 after 2 hours of incubation at 1600 ℃.
Detailed Description
Example 1:
the 3D printing silicon carbide slurry suitable for the ink direct writing technology comprises the following components in percentage by mass: 40 to 60wt percent of silicon carbide ceramic powder, 0.3 to 1wt percent of luffa cellulose, 10 to 15wt percent of glycerol, 0.05 to 0.1wt percent of carrageenan and the balance of deionized water.
The raw materials mainly comprise silicon carbide powder (average particle size 600 nm), retinervus Luffae fructus, benzene, absolute ethyl alcohol, sodium chlorite, glacial acetic acid, potassium hydroxide, concentrated sulfuric acid, glycerol and carrageenan, and the preparation process comprises the following steps:
(1) And mixing deionized water and glycerol according to a volume ratio of 2:1 to obtain a water-oil mixed solution.
(2) And (3) respectively putting the luffa cellulose and the carrageenan into the water-oil mixed solution according to the feed-liquid ratio of 10g to 1L and 2g to 1L, stirring at 80 ℃ for 30min, and cooling to room temperature.
(3) Mixing and stirring the silicon carbide ceramic powder and the solution obtained in the step (2) according to the mass ratio of 2:1, wherein the stirring speed is 100rpm, the stirring time is 1.0h, and the obtained slurry is filtered by a 2000-mesh screen. The physical pictures printed by the direct writing type 3d are shown in fig. 9 and 10 (a).
(4) And (3) carrying out heat preservation on the obtained porous silicon carbide sample at 1600 ℃ for 2 hours, sintering under the protection of atmosphere, and the microcosmic appearance of the sintered sample is shown in figures 11-12.
The preparation method of the loofah sponge cellulose comprises the following steps:
1) Pretreatment of raw materials: cleaning retinervus Luffae fructus, drying at 80-90deg.C for 4 hr, pulverizing, and sieving with 40 mesh sieve to obtain retinervus Luffae fructus powder.
2) Preparing benzene-ethanol solution according to a volume ratio of 2:1, wrapping the loofah sponge powder with filter paper, and placing the loofah sponge powder into a Soxhlet extractor according to a feed liquid ratio of 1g to 20mL, and Soxhlet extracting for 12h at 100 ℃. Naturally cooling to room temperature, washing with deionized water for 5 times, and suction filtering.
3) Putting the loofah sponge powder obtained in the step 2) into 25g/L NaClO according to the feed-to-liquid ratio of 1g to 20mL 2 In the aqueous solution, glacial acetic acid is used for regulating the pH value to 3, bleaching is carried out for 3 hours at 80 ℃, and deionized water is used for washing after natural cooling to room temperatureAnd (5) carrying out suction filtration, and repeating the whole step three times.
4) And (3) putting the loofah sponge powder obtained in the step (3) into a KOH aqueous solution with the mass fraction of 10% according to the feed-liquid ratio of 1g to 20mL, performing alkaline washing at 80 ℃ for 5 hours, cooling, washing with water to be neutral, and performing suction filtration.
5) Putting the loofah sponge powder obtained in the step 4) into H with the mass fraction of 60% according to the feed-liquid ratio of 1g to 20mL 2 SO 4 In the aqueous solution, the mixture is washed with acid for 7 hours at 50 ℃, cooled, washed with water to be neutral, and centrifugally washed to be neutral.
6) The aqueous cellulose solution obtained in step 5) was sonicated in a cell breaker for 3h at 150W power.
7) And (3) placing the aqueous solution of cellulose obtained in the step (6) into a freeze dryer, and drying for 48 hours at a temperature lower than-40 ℃ to obtain the loofah sponge cellulose, as shown in figures 1-5.
The prepared silicon carbide slurry is suitable for an ink direct-writing type 3D printer, and the printing height can exceed one centimeter. In the printing process, the paste has the characteristics of stable extrusion speed, uniform density, difficult filament breakage, stable structure, difficult collapse and the like. The luffa cellulose can well disperse silicon carbide (figures 6-8) and be uniformly dispersed in the silicon carbide particles as a dispersing agent, and the cellulose can play a role in connecting the silicon carbide particles to improve the strength and improve the overall conductivity in the sintering process through carbonization, as shown in figure 13. The printed porous silicon carbide has good electromagnetic shielding properties (fig. 14) and controllable thermal conductivity (fig. 15).
Example 2:
the 3D printing silicon carbide slurry suitable for the ink direct writing technology mainly comprises silicon carbide powder (average particle size of 600 nm), loofah sponge, benzene, absolute ethyl alcohol, sodium chlorite, glacial acetic acid, potassium hydroxide, concentrated sulfuric acid, glycerol and carrageenan as raw materials, and the preparation process comprises the following steps:
(1) And mixing deionized water and glycerol according to a volume ratio of 2:1 to obtain a water-oil mixed solution.
(2) And (3) respectively adding the luffa cellulose and the carrageenan into the water-oil mixed solution according to the ratio of 20g to 1L and 2g to 1L, stirring at 80 ℃ for 30min, and cooling to room temperature.
(3) Mixing and stirring the silicon carbide ceramic powder and the solution obtained in the step (2) according to the mass ratio of 2:1, wherein the stirring speed is 100rpm, the stirring time is 1.0h, and the obtained slurry is filtered by a 2000-mesh screen. The physical picture after direct-write 3d printing is shown in fig. 10 (b).
(4) And (3) carrying out heat preservation on the obtained porous silicon carbide sample at 1600 ℃ for 2 hours, and sintering under the protection of atmosphere.
The preparation method of the loofah sponge cellulose comprises the following steps:
1) Pretreatment of raw materials: cleaning retinervus Luffae fructus, drying at 80-90deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain retinervus Luffae fructus powder.
2) Preparing benzene-ethanol solution according to a volume ratio of 2:1, wrapping the loofah sponge powder with filter paper, and placing the loofah sponge powder into a Soxhlet extractor according to a feed liquid ratio of 1g to 20mL, and Soxhlet extracting for 12h at 100 ℃. Naturally cooling to room temperature, washing with deionized water for 5 times, and suction filtering.
3) Putting the loofah sponge powder obtained in the step 2) into 25g/L NaClO according to the feed-to-liquid ratio of 1g to 20mL 2 In the aqueous solution, the pH value is regulated to 3 by glacial acetic acid, bleaching is carried out for 3 hours at 80 ℃, natural cooling is carried out to room temperature, washing is carried out by deionized water, suction filtration is carried out, and the whole step is repeated for three times.
4) And (3) putting the loofah sponge powder obtained in the step (3) into a KOH aqueous solution with the mass fraction of 10% according to the feed-liquid ratio of 1g to 20mL, performing alkaline washing at 80 ℃ for 5 hours, cooling, washing with water to be neutral, and performing suction filtration.
5) Putting the loofah sponge powder obtained in the step 4) into H with the mass fraction of 60% according to the feed-liquid ratio of 1g to 20mL 2 SO 4 In the aqueous solution, the mixture is washed with acid for 7 hours at 50 ℃, cooled, washed with water to be neutral, and centrifugally washed to be neutral.
6) The aqueous cellulose solution obtained in step 5) was sonicated in a cell breaker at 200W power for 2h.
7) And (3) placing the aqueous solution of cellulose obtained in the step (6) into a freeze dryer, and drying for 48 hours at a temperature lower than-40 ℃ to obtain the loofah sponge cellulose.
Example 3:
the 3D printing silicon carbide slurry suitable for the ink direct writing technology mainly comprises silicon carbide powder (average particle size of 600 nm), loofah sponge, benzene, absolute ethyl alcohol, sodium chlorite, glacial acetic acid, potassium hydroxide, concentrated sulfuric acid, glycerol and carrageenan as raw materials, and the preparation process comprises the following steps:
(1) And mixing deionized water and glycerol according to a volume ratio of 3:1 to obtain a water-oil mixed solution.
(2) And (3) respectively adding the luffa cellulose and the carrageenan into the water-oil mixed solution according to the feed-liquid ratio of 50g to 1L and 2g to 1L, stirring at 80 ℃ for 30min, and cooling to room temperature.
(3) Mixing and stirring the silicon carbide ceramic powder and the solution obtained in the step (2) according to the mass ratio of 2:1, wherein the stirring speed is 100rpm, the stirring time is 1.0h, and the obtained slurry is filtered by a 2000-mesh screen.
(4) And (3) carrying out heat preservation on the obtained porous silicon carbide sample at 1600 ℃ for 2 hours, and sintering under the protection of atmosphere.
The preparation method of the loofah sponge cellulose comprises the following steps:
1) Pretreatment of raw materials: cleaning retinervus Luffae fructus, drying at 80-90deg.C for 6 hr, pulverizing, and sieving with 40 mesh sieve to obtain retinervus Luffae fructus powder.
2) Preparing benzene-ethanol solution according to a volume ratio of 2:1, wrapping the loofah sponge powder with filter paper, and placing the loofah sponge powder into a Soxhlet extractor according to a feed liquid ratio of 1g to 20mL, and Soxhlet extracting for 12h at 100 ℃. Naturally cooling to room temperature, washing with deionized water for 5 times, and suction filtering.
3) Putting the loofah sponge powder obtained in the step 2) into 25g/L NaClO according to the feed-to-liquid ratio of 1g to 20mL 2 In the aqueous solution, the pH value is regulated to 3 by glacial acetic acid, bleaching is carried out for 3 hours at 80 ℃, natural cooling is carried out to room temperature, washing is carried out by deionized water, suction filtration is carried out, and the whole step is repeated for three times.
4) And (3) putting the loofah sponge powder obtained in the step (3) into a KOH aqueous solution with the mass fraction of 10% according to the feed-liquid ratio of 1g to 20mL, performing alkaline washing at 80 ℃ for 5 hours, cooling, washing with water to be neutral, and performing suction filtration.
5) Putting the loofah sponge powder obtained in the step 4) into H with the mass fraction of 60% according to the feed-liquid ratio of 1g to 20mL 2 SO 4 In the aqueous solution, the mixture is washed with acid for 7 hours at 50 ℃, cooled, washed with water to be neutral, and centrifugally washed to be neutral.
6) The aqueous cellulose solution obtained in step 5) was sonicated in a cell breaker at 200W power for 2h.
7) And (3) placing the aqueous solution of cellulose obtained in the step (6) into a freeze dryer, and drying for 48 hours at a temperature lower than-40 ℃ to obtain the loofah sponge cellulose.
Comparative example 1:
comparative example 1 differs from examples 1, 2, 3 mainly in that: the prepared slurry is not added with luffa cellulose, and the preparation method is as follows:
the 3D printing silicon carbide slurry comprises the following components in percentage by mass: 40 to 60wt.% of silicon carbide ceramic powder, 10 to 15wt.% of glycerol, 0.05 to 0.1wt.% of carrageenan and the balance of deionized water.
(1) And mixing deionized water and glycerol according to a volume ratio of 2:1 to obtain a water-oil mixed solution.
(2) And (3) putting carrageenan into the water-oil mixed solution according to the feed-liquid ratio of 2g to 1L, stirring for 30min at 80 ℃, and cooling to room temperature.
(3) Mixing and stirring the silicon carbide ceramic powder and the solution obtained in the step (2) according to the mass ratio of 2:1, wherein the stirring speed is 100rpm, the stirring time is 1.0h, and the obtained slurry is filtered by a 2000-mesh screen. The physical picture after direct-writing 3d printing is shown in fig. 10 (c).
(4) And (3) carrying out heat preservation on the obtained porous silicon carbide sample at 1600 ℃ for 2 hours, and sintering under the protection of atmosphere.
The cellulose content in the solutions was 0g/L (comparative example 1), 10g/L (example 1), 20g/L (example 2), 50g/L (example 3) and the resistivities of the samples were 658.61kΩ·cm, 495.26kΩ·cm, 360.55kΩ·cm, 8.82kΩ·cm, respectively.
The invention is not a matter of the known technology.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (8)
1. The utility model provides a 3D prints carborundum thick liquids suitable for ink write-through technique which characterized in that: the slurry comprises 40-60% of silicon carbide ceramic powder and 0.3-1% of luffa cellulose by mass percent.
2. The 3D printing silicon carbide paste suitable for use in ink direct write technology according to claim 1, wherein the paste has a composition of: 40 to 60wt percent of silicon carbide ceramic powder, 0.3 to 1wt percent of luffa cellulose, 10 to 15wt percent of glycerol, 0.05 to 0.1wt percent of carrageenan and the balance of deionized water.
3. 3D printing silicon carbide paste suitable for use in ink direct writing technology according to claim 1 or 2, wherein: the silicon carbide ceramic powder is silicon carbide whisker and/or silicon carbide particle, the particle size is 50 nm-50 mu m, and the purity is 99% -99.99%.
4. 3D printing silicon carbide paste suitable for use in ink direct writing technology according to claim 1 or 2, wherein: the luffa cellulose is in a thread shape or a sheet shape, and the size range is 10 nm-1 mu m.
5. A method of preparing a 3D printed silicon carbide paste suitable for use in ink direct write technology as claimed in claim 1, comprising the steps of:
(1) Mixing deionized water and glycerin according to a volume ratio of 2:1-1:1 to obtain a water-oil mixed solution;
(2) Respectively putting the luffa cellulose and carrageenan into the water-oil mixed solution according to the feed-liquid ratio of 10-50 g:1L and 2-5 g:1L, stirring for 30min at 80 ℃, and cooling to room temperature;
(3) Mixing silicon carbide ceramic powder with the solution obtained in the step (2) according to the mass ratio of 3:1-2:1, and filtering the obtained slurry by using a 2000-mesh screen.
6. The method for preparing 3D printing silicon carbide slurry suitable for ink direct writing technology according to claim 5, wherein in the step (3), the mixing process of silicon carbide ceramic powder and solution is stirring and/or ball milling; wherein:
the stirring speed is 10-500 rpm, and the stirring time is more than 0.5h;
the ball milling speed is 30-300 rpm, the ball milling time is 4-10 h, and the mass ratio of the grinding balls to the slurry is more than 0.1.
7. The method for preparing the 3D printing silicon carbide slurry suitable for the ink direct writing technology according to claim 5, wherein the method for preparing the loofah sponge cellulose is as follows:
1) Pretreatment of raw materials: cleaning the loofah sponge, drying the loofah sponge at 80-90 ℃ for 4-6 hours, crushing the loofah sponge, and sieving the crushed loofah sponge with a 40-mesh sieve to obtain loofah sponge powder;
2) Preparing benzene-ethanol solution according to a volume ratio of 2:1, wrapping loofah sponge powder with filter paper, and placing the loofah sponge powder into a Soxhlet extractor according to a feed liquid ratio of 1g:20 mL-1 g:50mL, and carrying out Soxhlet extraction for 6-12 h at 80-100 ℃; naturally cooling to room temperature, washing with deionized water for 4-6 times, and suction filtering;
3) Putting the loofah sponge powder obtained in the step 2) into 20 g/L-30 g/L NaClO according to the ratio of 1g to 20g to 50g of the solution to the solution 2 In the aqueous solution, glacial acetic acid is used for regulating the pH value to 2-3, bleaching is carried out for 2-4 hours at 80 ℃, natural cooling is carried out to room temperature, deionized water is used for washing and suction filtration is carried out, and the whole step is repeated for three times;
4) Putting the loofah sponge powder obtained in the step 3) into a KOH aqueous solution with the mass fraction of 10% according to the feed-liquid ratio of 1g to 20mL to 1g to 50mL, performing alkaline washing at 80 ℃ for 4 to 6 hours, cooling, washing to neutrality, and performing suction filtration;
5) Putting the loofah sponge powder obtained in the step 4) into H with the mass fraction of 50% -60% according to the ratio of 1g to 20 mL-1 g to 50mL of feed liquid 2 SO 4 Washing with acid for 6-8 h at 50 ℃ in aqueous solution, cooling, washing with water to neutrality, and centrifugally washing to neutrality;
6) Ultrasonic treatment is carried out on the cellulose aqueous solution obtained in the step 5) for 1 to 3 hours in a cell crusher under the power of 60 to 200W;
7) And (3) putting the cellulose aqueous solution obtained in the step (6) into a freeze dryer for drying for 20-40 h to prepare the loofah sponge cellulose.
8. The method of preparing a 3D printed silicon carbide paste suitable for use in ink direct writing techniques according to claim 5, wherein the temperature in the freeze dryer in step 7) is less than-40 ℃.
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