CN117303893B - High-stability ceramic shell back layer slurry and preparation method thereof - Google Patents
High-stability ceramic shell back layer slurry and preparation method thereof Download PDFInfo
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- 239000002002 slurry Substances 0.000 title claims abstract description 147
- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000007613 slurry method Methods 0.000 title description 2
- 238000003756 stirring Methods 0.000 claims abstract description 122
- 239000002121 nanofiber Substances 0.000 claims abstract description 94
- 239000000843 powder Substances 0.000 claims abstract description 67
- 239000011230 binding agent Substances 0.000 claims abstract description 64
- 239000000080 wetting agent Substances 0.000 claims abstract description 55
- 239000013530 defoamer Substances 0.000 claims abstract description 44
- 239000011819 refractory material Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 36
- 230000008569 process Effects 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 27
- 238000007598 dipping method Methods 0.000 claims abstract description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 63
- 239000002904 solvent Substances 0.000 claims description 21
- 239000002518 antifoaming agent Substances 0.000 claims description 20
- 229920001709 polysilazane Polymers 0.000 claims description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 18
- 229920000642 polymer Polymers 0.000 claims description 13
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 239000000839 emulsion Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000013461 design Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 239000010431 corundum Substances 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 239000005350 fused silica glass Substances 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 27
- 239000011248 coating agent Substances 0.000 abstract description 15
- 238000000576 coating method Methods 0.000 abstract description 15
- 230000002776 aggregation Effects 0.000 abstract description 8
- 238000004220 aggregation Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 53
- 230000000694 effects Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000005495 investment casting Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000005266 casting Methods 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 239000006255 coating slurry Substances 0.000 description 3
- 125000000373 fatty alcohol group Chemical group 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241001078983 Tetradium ruticarpum Species 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- KBDSLGBFQAGHBE-MSGMIQHVSA-N limonin Chemical compound C=1([C@H]2[C@]3(C)CC[C@H]4[C@@]([C@@]53O[C@@H]5C(=O)O2)(C)C(=O)C[C@@H]2[C@]34COC(=O)C[C@@H]3OC2(C)C)C=COC=1 KBDSLGBFQAGHBE-MSGMIQHVSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
Classifications
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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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- 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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
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- C04B2235/5212—Organic
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/526—Fibers characterised by the length of the fibers
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5264—Fibers characterised by the diameter of the fibers
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
Abstract
The invention discloses a high-stability ceramic shell back layer slurry and a preparation method thereof, wherein the ceramic shell back layer slurry comprises 60-75wt% of refractory powder, 25-30wt% of binder, 0.3-0.5wt% of defoamer, 0.3-0.5wt% of wetting agent and 4-10wt% of nano fiber. The method comprises the following steps: preparing nanofiber by adopting an electrostatic spinning process; sequentially adding the binder, the defoamer and the wetting agent into a slurry mixing barrel for stirring, and respectively adding part of nano fibers and part of refractory material powder into the slurry mixing barrel for stirring for a certain time under the condition of keeping continuous stirring and not changing the stirring speed; adding the rest nanometer fiber and the rest refractory powder into a slurry mixing barrel respectively under the conditions of keeping continuous stirring and improving the stirring speed, and stirring for a certain time respectively; transferring the slurry in the slurry preparation barrel into a slurry dipping barrel, stirring to keep the slurry not to be settled, and obtaining the ceramic shell back layer slurry. The invention solves the problems of the ceramic shell that the weight and the thickness are increased and the coating uniformity is poor due to the aggregation of fibers into a bundle.
Description
Technical Field
The invention belongs to the technical field of precision investment casting, and particularly relates to high-stability ceramic shell back layer slurry and a preparation method thereof.
Background
Because of the advantages of the investment precision casting technology in the aspect of producing castings with high precision and complex structures, the investment precision casting technology is widely applied in the fields of aerospace, chemical industry and the like, and particularly in the manufacture of key hot end components such as turbine blades of aeroengines, blades of gas turbines and the like. The preparation of the ceramic shell is an extremely important link in precision investment casting, and the performance and quality of the ceramic shell directly influence the quality of castings. Some domestic and foreign scholars utilize the characteristics of high strength, high rigidity, light weight, fatigue resistance, high temperature resistance and the like of the fiber reinforced composite material, and adopt a fiber reinforced fine casting mold shell method to prepare a high-quality ceramic mold shell.
Researchers such as lib.b. found that the presence of fibers can effectively inhibit cracking of the shell by uniformly mixing the fibers into the refractory sand for the shell sanding, and that the fracture toughness of the shell increased with the increase in the fiber content. Researchers such as Yuan add a high molecular binder and nylon organic fibers into the slurry so as to reduce the shell making period on the premise of ensuring the wet strength of the shell, and when the shell is roasted, the nylon organic fibers are burnt out, so that a plurality of micropores are left in the shell, and the air permeability of the shell is greatly improved. However, the introduction of the fibers has a significant effect on the properties of the silica sol slurry, and as the content of the fibers and the length of the fibers increase, the flow viscosity of the silica sol slurry also increases, so that the fibers are agglomerated into bundles, which leads to an increase in the coating thickness and weight of the shell, and the uniformity of the coating is reduced, thereby limiting the exertion of the overall performance improvement effect of the fibers on the shell.
How to balance the fiber reinforcement effect and the impact of the fibers on the properties of the silica sol slurry to increase the overall properties of the ceramic shell is a direction of need for further research and improvement. The optimization and improvement of the ceramic shell can be better realized by exploring more suitable fiber types, optimizing the adding mode and adding amount of the fibers, improving the formula of the silica sol slurry and the like, and the method has positive promotion effect on the development and application of the investment precision casting technology.
The invention patent with application publication number of CN114833305A discloses a fiber reinforced ceramic shell back layer slurry of evodia rutaecarpa and a preparation method thereof, wherein the slurry comprises the following components in parts by mass: 55-80 parts of ceramic shell back powder, 0.5-2 parts of common evodia fruit fiber, 18.3-37 parts of binder, 0.1-0.5 part of defoamer, 0.1-0.5 part of preservative and 1-5 parts of deionized water. The method comprises the following steps: adding the binder into a pulp mixing barrel, keeping continuous stirring, adding the herba evodiae fiber into the binder, and stirring to uniformly disperse the herba evodiae fiber in the binder; and (3) continuously stirring, adding ceramic shell back powder into the binder, sequentially adding the defoaming agent, the preservative and the deionized water into a stirring barrel, continuously stirring, transferring the slurry into a slurry dipping barrel, continuously stirring, and keeping the slurry from settling until the viscosity is not changed. According to the technical scheme, although the air permeability of the shell can be improved, the shell is reinforced, the used fibers are natural fibers, the length and the diameter of the natural fibers are not controllable, the phenomenon of agglomeration and bundling can occur, and the shell slurry is unevenly coated.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides high-stability ceramic shell back layer slurry, wherein the ceramic shell back layer slurry comprises, by mass, 60-75wt% of refractory material powder, 25-30wt% of binder, 0.3-0.5wt% of defoaming agent, 0.3-0.5wt% of wetting agent and 4-10wt% of nanofiber.
Preferably, the refractory material powder is any one or more of zirconite, alumina, fused quartz powder, mullite powder, fused corundum powder, coal gangue powder and kaolin powder, and the granularity of the refractory material powder is 200-325 meshes; the binder is any one or more of silica sol, water glass and ethyl silicate hydrolysate; the defoaming agent is an organosilicon emulsion defoaming agent; the wetting agent is fatty phosphate and/or fatty alcohol polyoxyethylene ether; the viscosity of the ceramic shell back layer slurry is 25-42s, and the pH value of the ceramic shell back layer slurry is 3-9.
According to the invention, proper refractory material powder is selected according to the quality requirements of different castings and different pouring parameters, and particularly in the aspect of directional solidification or single-crystal superalloy investment precision casting, alumina or zircon is mainly used as ceramic shell refractory material powder. The defoaming agent is added into the ceramic shell back layer slurry, and the structure of the foam film can be destroyed by changing the surface tension, so that the defoaming and foam inhibiting effects are achieved. Viscosity directly reflects the flow properties of the slurry system and directly determines the coating quality of the slurry, the pH of which affects its viscosity.
In any of the above schemes, it is preferable that the nanofiber is a polymer filament with a nano-scale diameter prepared by an electrostatic spinning process, and the polymer solution used in the electrostatic spinning process is a precursor solution obtained by mixing polysilazane and polyvinylpyrrolidone with dimethylformamide as a solvent.
In any of the above schemes, preferably, the addition amount of the polysilazane is 2-5% of the mass of the dimethylformamide solvent, and the addition amount of the polyvinylpyrrolidone is 20-23% of the mass of the dimethylformamide solvent; the length of the nanofiber is 1×10 7 -1.5×10 7 nm, and the diameter is 100-170nm. In the present invention, nanofibers are present in a ceramic shell backing slurry in the form of filaments having a length of 1X 10 7 -1.5×10 7 The diameter of the nano-fiber is 100-170nm, and the nano-fiber with the length and the diameter can realize the effects of uniform dispersion and no agglomeration into a bundle.
The invention also provides a preparation method of the high-stability ceramic shell back layer slurry, which is used for preparing the high-stability ceramic shell back layer slurry, and comprises the following steps in sequence:
step one: weighing dimethylformamide, polysilazane and polyvinylpyrrolidone according to design requirements for standby, taking the dimethylformamide as a solvent, adding polysilazane and polyvinylpyrrolidone into the solvent, uniformly mixing the mixture to obtain a polymer solution for an electrostatic spinning process, and preparing nanofibers for standby by adopting the electrostatic spinning process;
step two: sequentially adding the binder, the defoaming agent and the wetting agent into a slurry mixing barrel, and simultaneously starting a stirrer to stir; after the stirring of the binder, the defoamer and the wetting agent is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding part of nano fibers into a slurry mixing barrel to continue stirring;
step three: after the stirring of the binder, the defoamer, the wetting agent and part of the nano fibers is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding part of refractory material powder into the slurry mixing barrel for continuous stirring;
step four: after the stirring of the binder, the defoamer, the wetting agent, part of the nanofibers and part of the refractory material powder is finished, keeping the stirrer in a starting state, improving the stirring speed, and simultaneously adding the rest of the nanofibers into the slurry mixing barrel to continue stirring;
step five: after the stirring of the binder, the defoamer, the wetting agent, the nano fibers and part of the refractory material powder is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding the rest part of the refractory material powder into the slurry mixing barrel for continuous stirring;
step six: after the stirring of the binder, the defoamer, the wetting agent, the nano fibers and the refractory material powder is finished, transferring the slurry in the slurry preparation barrel to the slurry dipping barrel, and simultaneously starting the stirrer to stir, so as to keep the slurry from settling, thereby obtaining the high-stability ceramic shell back layer slurry.
Preferably, in the first step, the nanofiber is prepared by adopting an electrostatic spinning process, and the process parameters are as follows: the temperature is room temperature, the humidity is 40-45%, the voltage is 25-28kV, the distance between needle plates is 20-23cm, and the flow rate of feed liquid is 1-1.2ml/h.
In any of the above schemes, preferably, in the second step, the stirring speed of the binder, the defoamer and the wetting agent is 400-500r/min, and the stirring time is 2-3min; the mass percentage of the part of nano fibers is 50-70wt%, the stirring speed of the binder, the defoamer, the wetting agent and the part of nano fibers is 400-500r/min, and the stirring time is 3-5min.
In any of the above schemes, preferably, in the third step, the mass percentage of the part of refractory powder is 50-60wt%, the stirring speed of the binder, the defoamer, the wetting agent, the part of nano fibers and the part of refractory powder is 400-500r/min, and the stirring time is 20-30min.
In any of the above schemes, preferably, in the fourth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and part of the refractory powder is 800-900r/min, and the stirring time is 3-5min.
In any of the above-mentioned embodiments, it is preferable that in the fifth step, the stirring speed of the binder, the antifoaming agent, the wetting agent, the nanofibers and the refractory powder is 800 to 900r/min and the stirring time is 6 to 8 hours.
In any of the above schemes, preferably, in the step six, the stirring speed of the slurry in the slurry dipping barrel is 800-900r/min, and the slurry is not settled, namely vortex appears on the surface of the slurry.
In the invention, the inner walls of the slurry preparation barrel and the slurry dipping barrel are provided with the circulating cooling system, and the structure and the model of the circulating cooling system are not particularly required, so long as the circulating cooling system can keep the temperature of each substance of the ceramic shell back layer slurry in the whole stirring process at 22 ℃ or below. In addition, in the preparation process of the ceramic shell back layer slurry, the addition sequence, the addition amount, the stirring speed, the stirring time and other technological parameters of each material are very important, and the process directly influences the performance and the quality of the prepared ceramic shell back layer slurry, and whether the back layer slurry with good stability can be obtained. Meanwhile, in the preparation process of the ceramic shell back layer slurry, the stirrer is always kept in a starting state, and the slurry can be effectively prevented from sedimentation and coagulation by keeping continuous stirring.
According to the invention, the nanofiber prepared by adopting the electrostatic spinning process not only can effectively play a role in reinforcing the ceramic shell, but also can be uniformly dispersed in the ceramic shell back layer slurry, so that the viscosity of the ceramic shell back layer slurry is stabilized for a long time and the plate weight is increased under the condition of field use, the effect of improving the uniformity of coating slurry is achieved, and particularly, the coating amount can be effectively increased for the places which are not easy to coat slurry, such as part of R angle (generally referred to as a transitional circular arc area), and the like, and the problem of the prior art that the weight and the thickness of the ceramic shell are increased and the coating uniformity is poor due to fiber aggregation is solved.
The high-stability ceramic shell back layer slurry and the preparation method thereof have the following beneficial effects:
(1) The nanofiber is prepared from precursor solutions of polysilazane and polyvinylpyrrolidone by adopting an electrostatic spinning process, the prepared bundle-shaped nanofiber has higher porosity and larger specific surface area, the bundle-shaped nanofiber is added into other substances and is dispersed into a monofilament shape after being fully stirred, and the monofilament-shaped nanofiber is interwoven into a reticular structure in a gap between a binder and refractory material powder and does not have the phenomenon of agglomeration and bundling, so that the bundle-shaped nanofiber is uniformly dispersed in ceramic shell back layer slurry. In addition, the ablation effect of the fibers in the roasting stage can increase the porosity degree inside the ceramic shell and improve the air permeability of the ceramic shell.
(2) The added nano fiber can effectively prevent the movement of refractory material powder and binder in the ceramic shell back layer slurry, is beneficial to stabilizing the viscosity of the ceramic shell back layer slurry for a long time and increasing the plate weight under the condition of field use, plays a role in improving the uniformity of coating slurry, increases the plane thickness by 15 percent, increases the thickness of places which are difficult to coat slurry, such as part of R angle, by 45 percent, and greatly improves the coating quantity. Therefore, the nanofiber is added, and the reduction of the coating layer number and the coating amount are realized on the premise of ensuring the thickness of the ceramic shell, so that the production period and the production cost are reduced.
Drawings
FIG. 1 is a flow chart of a preferred embodiment of a high stability ceramic shell backing slurry and method of making the same in accordance with the present invention;
FIG. 2 is a photograph of the microscopic morphology of nanofibers produced using the electrospinning process in the embodiment of FIG. 1;
FIG. 3 is a photograph of a test panel coated with a high stability ceramic shell backing slurry prepared in accordance with the embodiment of FIG. 1;
fig. 4 is a cross-sectional photograph of a test panel coated with a high stability ceramic shell backing slurry in the embodiment shown in fig. 1.
Detailed Description
For a further understanding of the present invention, the present invention will be described in detail with reference to the following examples.
Embodiment one:
according to a preferred embodiment of the high-stability ceramic shell back layer slurry, the ceramic shell back layer slurry comprises 65wt% of refractory powder, 27wt% of binder, 0.4wt% of defoaming agent, 0.4wt% of wetting agent and 7.2wt% of nano fibers.
The refractory material powder is zirconite, and the granularity of the zirconite is 250 meshes; the binder is silica sol; the defoaming agent is an organosilicon emulsion defoaming agent; the wetting agent is fatty alcohol polyoxyethylene ether; the viscosity of the ceramic shell back layer slurry was 35s, and the pH of the ceramic shell back layer slurry was 6. In the embodiment, the defoaming agent is added into the ceramic shell back layer slurry, and the structure of the foam film can be damaged by changing the surface tension, so that the defoaming and foam inhibiting effects are achieved; viscosity directly reflects the flow properties of the slurry system and directly determines the coating quality of the slurry, the pH of which affects its viscosity.
The nanofiber is a polymer filament with a nanoscale diameter prepared by adopting an electrostatic spinning process, and a polymer solution used by the electrostatic spinning process is a precursor solution obtained by mixing polysilazane and polyvinylpyrrolidone by taking dimethylformamide as a solvent. The addition amount of the polysilazane is 4% of the mass of the dimethylformamide solvent, and the addition amount of the polyvinylpyrrolidone is 21% of the mass of the dimethylformamide solvent; the length of the nanofiber is 1.2×10 7 nm, 130nm in diameter. In this example, the nanofibers were present in the ceramic shell backing slurry in the form of filaments having a length of 1.2X10 7 The diameter of the nano-fiber is 130nm, and the nano-fiber with the length and the diameter can realize the effects of uniform dispersion and no aggregation into a bundle.
As shown in fig. 1, this embodiment also provides a method for preparing the high-stability ceramic shell back layer slurry, which is used for preparing the high-stability ceramic shell back layer slurry, and includes the following steps in sequence:
step one: weighing dimethylformamide, polysilazane and polyvinylpyrrolidone according to design requirements for standby, taking the dimethylformamide as a solvent, adding polysilazane and polyvinylpyrrolidone into the solvent, uniformly mixing the mixture to obtain a polymer solution for an electrostatic spinning process, and preparing nanofibers for standby by adopting the electrostatic spinning process;
step two: sequentially adding the binder, the defoaming agent and the wetting agent into a slurry mixing barrel, and simultaneously starting a stirrer to stir; after the stirring of the binder, the defoamer and the wetting agent is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding part of nano fibers into a slurry mixing barrel to continue stirring;
step three: after the stirring of the binder, the defoamer, the wetting agent and part of the nano fibers is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding part of refractory material powder into the slurry mixing barrel for continuous stirring;
step four: after the stirring of the binder, the defoamer, the wetting agent, part of the nanofibers and part of the refractory material powder is finished, keeping the stirrer in a starting state, improving the stirring speed, and simultaneously adding the rest of the nanofibers into the slurry mixing barrel to continue stirring;
step five: after the stirring of the binder, the defoamer, the wetting agent, the nano fibers and part of the refractory material powder is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding the rest part of the refractory material powder into the slurry mixing barrel for continuous stirring;
step six: after the stirring of the binder, the defoamer, the wetting agent, the nano fibers and the refractory material powder is finished, transferring the slurry in the slurry preparation barrel to the slurry dipping barrel, and simultaneously starting the stirrer to stir, so as to keep the slurry from settling, thereby obtaining the high-stability ceramic shell back layer slurry.
In the first step, the electrostatic spinning technology is adopted to prepare the nanofiber, and the technological parameters are as follows: the temperature is room temperature, the humidity is 42%, the voltage is 26kV, the distance between needle plates is 22cm, and the flow rate of feed liquid is 1.1ml/h.
In the second step, the stirring speed of the binder, the defoamer and the wetting agent is 450r/min, and the stirring time is 2.5min; the mass percentage of the part of nano fibers to the nano fibers is 60 percent, the stirring speed of the binder, the defoamer, the wetting agent and the part of nano fibers is 450r/min, and the stirring time is 4min.
In the third step, the mass percentage of part of refractory material powder is 55wt%, the stirring speed of the binder, the defoamer, the wetting agent, the part of nano fibers and the part of refractory material powder is 450r/min, and the stirring time is 25min.
In the fourth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and part of the refractory powder is 850r/min, and the stirring time is 4min.
In the fifth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and the refractory powder is 850r/min, and the stirring time is 7h.
In the sixth step, the stirring speed of the slurry in the slurry dipping barrel is 850r/min, and the slurry is not settled, so that vortex appears on the surface of the slurry.
In the embodiment, the inner walls of the slurry preparation barrel and the slurry dipping barrel are provided with the circulating cooling system, and the structure and the model of the circulating cooling system are not particularly required, so long as the circulating cooling system can keep the temperature of each substance of the ceramic shell back layer slurry in the whole stirring process at 22 ℃ or below. In addition, in the preparation process of the ceramic shell back layer slurry, the addition sequence, the addition amount, the stirring speed, the stirring time and other technological parameters of each material are very important, and the process directly influences the performance and the quality of the prepared ceramic shell back layer slurry, and whether the back layer slurry with good stability can be obtained. Meanwhile, in the preparation process of the ceramic shell back layer slurry, the stirrer is always kept in a starting state, and the slurry can be effectively prevented from sedimentation and coagulation by keeping continuous stirring.
The microscopic morphology photo of the nanofiber prepared by adopting the electrostatic spinning process in this embodiment is shown in fig. 2, and the length and the diameter of the nanofiber are both nano-scale. The photographs of the test plate coated with the high-stability ceramic shell back layer slurry and the photographs of the cross sections thereof prepared by the embodiment are respectively shown in fig. 3 and 4, and the overall coating uniformity of the slurry is good, and particularly the coating amount can be effectively increased for the R angle part and the coating uniformity is good.
In the embodiment, the nanofiber prepared by adopting the electrostatic spinning process not only can effectively play a role in reinforcing the ceramic shell, but also can be uniformly dispersed in the ceramic shell back layer slurry, so that the viscosity of the ceramic shell back layer slurry is stabilized for a long time and the weight of a plate is increased under the condition of field use, the effect of improving the uniformity of coating slurry is achieved, the coating quantity can be effectively increased especially for the places, such as part of R angles, where the slurry is difficult to coat and hang, and the problem of the prior art that the weight and the thickness of the ceramic shell are increased and the coating uniformity is poor due to aggregation of fibers is solved.
The high-stability ceramic shell back layer slurry and the preparation method thereof have the following beneficial effects: (1) The nanofiber is prepared from precursor solutions of polysilazane and polyvinylpyrrolidone by adopting an electrostatic spinning process, the prepared bundle-shaped nanofiber has higher porosity and larger specific surface area, the bundle-shaped nanofiber is added into other substances and is dispersed into a single filament shape after being fully stirred, and the single filament-shaped nanofiber is interwoven into a reticular structure in a gap between a binder and refractory material powder and does not have the phenomenon of aggregation and bundling, so that the bundle-shaped nanofiber is uniformly dispersed in ceramic shell back layer slurry; (2) The addition of the nano fiber realizes the reduction of the coating layer number and the reduction of the coating amount on the premise of ensuring the thickness of the ceramic shell, thereby reducing the production period and the production cost.
Embodiment two:
according to another preferred embodiment of the high stability ceramic shell back layer slurry and the preparation method thereof of the present invention, the composition of each substance, the preparation method, the technical principle, the beneficial effects and the like are basically the same as those of the first embodiment, except that:
(1) For high-stability ceramic shell back layer slurry
The ceramic shell back layer slurry comprises, by mass, 60% of refractory powder, 29% of binder, 0.5% of defoaming agent, 0.5% of wetting agent and 10% of nanofiber.
The refractory material powder is alumina, and the granularity of the alumina is 200 meshes; the binder is silica sol; the defoaming agent is an organosilicon emulsion defoaming agent; the wetting agent is fatty alcohol polyoxyethylene ether; the viscosity of the ceramic shell back layer slurry was 42s, and the pH of the ceramic shell back layer slurry was 9.
The nanofiber is a polymer filament with a nanoscale diameter prepared by adopting an electrostatic spinning process, and a polymer solution used by the electrostatic spinning process is a precursor solution obtained by mixing polysilazane and polyvinylpyrrolidone by taking dimethylformamide as a solvent. The addition amount of the polysilazane is 5% of the mass of the dimethylformamide solvent, and the addition amount of the polyvinylpyrrolidone is 23% of the mass of the dimethylformamide solvent; the length of the nanofiber is 1.5X10 7 nm, diameter 170nm.
Preparation method for high-stability ceramic shell back layer slurry
In the first step, the electrostatic spinning technology is adopted to prepare the nanofiber, and the technological parameters are as follows: the temperature is room temperature, the humidity is 45%, the voltage is 28kV, the distance between needle plates is 23cm, and the flow rate of feed liquid is 1.2ml/h.
In the second step, the stirring speed of the binder, the defoamer and the wetting agent is 500r/min, and the stirring time is 2min; the mass percentage of the part of nano fibers is 70 percent, the stirring speed of the binder, the defoamer, the wetting agent and the part of nano fibers is 500r/min, and the stirring time is 3min.
In the third step, the mass percentage of part of refractory material powder is 60wt%, the stirring speed of the binder, the defoamer, the wetting agent, the part of nano fibers and the part of refractory material powder is 500r/min, and the stirring time is 20min.
In the fourth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and part of the refractory powder is 900r/min, and the stirring time is 3min.
In the fifth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and the refractory powder is 900r/min, and the stirring time is 6h.
In the sixth step, the stirring speed of the slurry in the slurry dipping barrel is 900r/min, and the slurry is not settled, so that vortex appears on the surface of the slurry.
Embodiment III:
according to another preferred embodiment of the high stability ceramic shell back layer slurry and the preparation method thereof of the present invention, the composition of each substance, the preparation method, the technical principle, the beneficial effects and the like are basically the same as those of the first embodiment, except that:
(1) For high-stability ceramic shell back layer slurry
The ceramic shell back layer slurry comprises, by mass, 70.4% of refractory powder, 25% of binder, 0.3% of defoamer, 0.3% of wetting agent and 4% of nanofiber.
The refractory material powder is alumina, and the granularity of the alumina is 325 meshes; the binder is silica sol; the defoaming agent is an organosilicon emulsion defoaming agent; the wetting agent is fatty alcohol polyoxyethylene ether; the viscosity of the ceramic shell back layer slurry was 25s, and the pH of the ceramic shell back layer slurry was 3.
The nanofiber is a polymer filament with a nanoscale diameter prepared by adopting an electrostatic spinning process, and a polymer solution used by the electrostatic spinning process is a precursor solution obtained by mixing polysilazane and polyvinylpyrrolidone by taking dimethylformamide as a solvent. The addition amount of polysilazane is 2% of the mass of the dimethylformamide solvent, and the addition amount of polyvinylpyrrolidone is 20% of the mass of the dimethylformamide solvent; the length of the nanofiber is 1×10 7 nm, diameter 100nm.
(2) Preparation method for high-stability ceramic shell back layer slurry
In the first step, the electrostatic spinning technology is adopted to prepare the nanofiber, and the technological parameters are as follows: the temperature is room temperature, the humidity is 40%, the voltage is 25kV, the distance between needle plates is 20cm, and the flow rate of feed liquid is 1ml/h.
In the second step, the stirring speed of the binder, the defoamer and the wetting agent is 400r/min, and the stirring time is 3min; the mass percentage of the part of nano fibers is 50 percent, the stirring speed of the binder, the defoamer, the wetting agent and the part of nano fibers is 400r/min, and the stirring time is 5min.
In the third step, the mass percentage of part of refractory material powder is 50wt%, the stirring speed of the binder, the defoamer, the wetting agent, the part of nano fibers and the part of refractory material powder is 400r/min, and the stirring time is 30min.
In the fourth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and part of the refractory powder is 800r/min, and the stirring time is 5min.
In the fifth step, the stirring speed of the binder, the defoamer, the wetting agent, the nanofibers and the refractory powder is 800r/min, and the stirring time is 8h.
In the sixth step, the stirring speed of the slurry in the slurry dipping barrel is 800r/min, and the slurry is not settled, so that vortex appears on the surface of the slurry.
The specific description is as follows: the technical scheme of the invention relates to a plurality of parameters, and the beneficial effects and remarkable progress of the invention can be obtained by comprehensively considering the synergistic effect among the parameters. In addition, the value ranges of all the parameters in the technical scheme are obtained through a large number of tests, and aiming at each parameter and the mutual combination of all the parameters, the inventor records a large number of test data, and the specific test data are not disclosed herein for a long period of time.
It will be appreciated by those skilled in the art that the high stability ceramic shell back layer slurry and method of making the same of the present invention includes any combination of the above summary of the invention and detailed description of the invention and the various parts shown in the drawings, is limited in scope and does not constitute a complete description of the various aspects of these combinations for brevity. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A high stability ceramic shell backing slurry characterized by: the ceramic shell back layer slurry comprises, by mass, 60-75wt% of refractory powder, 25-30wt% of binder, 0.3-0.5wt% of defoamer, 0.3-0.5wt% of wetting agent, 4-10wt% of nanofiber, and the total mass percentage of the above substances is 100%;
the refractory material powder is any one or more of zirconite, alumina, fused quartz powder, mullite powder, fused corundum powder, gangue powder and kaolin powder, and the granularity of the refractory material powder is 200-325 meshes; the binder is any one or more of silica sol, water glass and ethyl silicate hydrolysate; the defoaming agent is an organosilicon emulsion defoaming agent; the wetting agent is fatty phosphate and/or fatty alcohol polyoxyethylene ether; the viscosity of the ceramic shell back layer slurry is 25-42s, and the pH value of the ceramic shell back layer slurry is 3-9;
the nanofiber is a polymer filament with a nanoscale diameter prepared by adopting an electrostatic spinning process, and a polymer solution used by the electrostatic spinning process is a precursor solution obtained by mixing polysilazane and polyvinylpyrrolidone with dimethylformamide as a solvent; the addition amount of polysilazane is 2-5% of the mass of the dimethylformamide solvent, and the addition amount of polyvinylpyrrolidone is 20-23% of the mass of the dimethylformamide solvent; the length of the nanofiber is 1×10 7 -1.5×10 7 nm, diameter 100-170nm;
the preparation method of the high-stability ceramic shell back layer slurry comprises the following steps in sequence:
step one: weighing dimethylformamide, polysilazane and polyvinylpyrrolidone according to design requirements for standby, taking the dimethylformamide as a solvent, adding polysilazane and polyvinylpyrrolidone into the solvent, uniformly mixing the mixture to obtain a polymer solution for an electrostatic spinning process, and preparing nanofibers for standby by adopting the electrostatic spinning process;
step two: sequentially adding the binder, the defoaming agent and the wetting agent into a slurry mixing barrel, and simultaneously starting a stirrer to stir; after the stirring of the binder, the defoamer and the wetting agent is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding part of nano fibers into a slurry mixing barrel to continue stirring;
step three: after the stirring of the binder, the defoamer, the wetting agent and part of the nano fibers is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding part of refractory material powder into the slurry mixing barrel for continuous stirring;
step four: after the stirring of the binder, the defoamer, the wetting agent, part of the nanofibers and part of the refractory material powder is finished, keeping the stirrer in a starting state, improving the stirring speed, and simultaneously adding the rest of the nanofibers into the slurry mixing barrel to continue stirring;
step five: after the stirring of the binder, the defoamer, the wetting agent, the nano fibers and part of the refractory material powder is finished, keeping the stirrer in a starting state without changing the stirring speed, and simultaneously adding the rest part of the refractory material powder into the slurry mixing barrel for continuous stirring;
step six: after the stirring of the binder, the defoamer, the wetting agent, the nano fibers and the refractory material powder is finished, transferring the slurry in the slurry preparation barrel into a slurry dipping barrel, and simultaneously starting a stirrer to stir, so as to keep the slurry from settling, thus obtaining the high-stability ceramic shell back layer slurry;
step one, preparing nanofibers by adopting an electrostatic spinning process, wherein the process parameters are that the temperature is room temperature, the humidity is 40-45%, the voltage is 25-28kV, the distance between needle plates is 20-23cm, and the flow rate of feed liquid is 1-1.2mL/h;
in the second step, the stirring speed of the binder, the defoamer and the wetting agent is 400-500r/min, and the stirring time is 2-3min; the mass percentage of the part of nano fibers is 50-70wt%, the stirring speed of the binder, the defoamer, the wetting agent and the part of nano fibers is 400-500r/min, and the stirring time is 3-5min;
in the third step, the mass percentage of part of refractory material powder is 50-60wt%, the stirring speed of the binder, the defoamer, the wetting agent, the part of nano fiber and the part of refractory material powder is 400-500r/min, and the stirring time is 20-30min;
in the fourth step, the stirring speed of the binder, the defoamer, the wetting agent, the nano fiber and part of refractory material powder is 800-900r/min, and the stirring time is 3-5min;
in the fifth step, the stirring speed of the binder, the defoamer, the wetting agent, the nano fiber and the refractory powder is 800-900r/min, and the stirring time is 6-8h.
2. The high stability ceramic shell back layer slurry of claim 1, wherein: in the sixth step, the stirring speed of the slurry in the slurry dipping barrel is 800-900r/min, and the slurry is not settled, so that vortex appears on the surface of the slurry.
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