CN114101593A - A highly collapsible, recyclable silicon oxide-based ceramic core and its preparation method and application - Google Patents
A highly collapsible, recyclable silicon oxide-based ceramic core and its preparation method and application Download PDFInfo
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- CN114101593A CN114101593A CN202111426025.4A CN202111426025A CN114101593A CN 114101593 A CN114101593 A CN 114101593A CN 202111426025 A CN202111426025 A CN 202111426025A CN 114101593 A CN114101593 A CN 114101593A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 195
- 239000000919 ceramic Substances 0.000 title claims abstract description 124
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 86
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 45
- 239000000654 additive Substances 0.000 claims abstract description 31
- 230000000996 additive effect Effects 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004064 recycling Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 238000000280 densification Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 41
- 238000001035 drying Methods 0.000 claims description 31
- 238000005266 casting Methods 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 25
- 238000002425 crystallisation Methods 0.000 claims description 24
- 230000008025 crystallization Effects 0.000 claims description 24
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 20
- 235000015895 biscuits Nutrition 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 13
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 235000010216 calcium carbonate Nutrition 0.000 claims description 3
- 230000002401 inhibitory effect Effects 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000011667 zinc carbonate Substances 0.000 claims description 3
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 3
- 235000004416 zinc carbonate Nutrition 0.000 claims description 3
- 125000005587 carbonate group Chemical group 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 4
- 239000002585 base Substances 0.000 description 36
- 238000002156 mixing Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- 239000011230 binding agent Substances 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 239000010703 silicon Substances 0.000 description 12
- 238000001746 injection moulding Methods 0.000 description 9
- 238000000498 ball milling Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000011858 nanopowder Substances 0.000 description 6
- 239000005350 fused silica glass Substances 0.000 description 4
- 229910021426 porous silicon Inorganic materials 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005495 investment casting Methods 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 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 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052806 inorganic carbonate Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/10—Cores; Manufacture or installation of cores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
- B22C1/02—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by additives for special purposes, e.g. indicators, breakdown additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C1/00—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds
- B22C1/16—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents
- B22C1/18—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of inorganic agents
- B22C1/186—Compositions of refractory mould or core materials; Grain structures thereof; Chemical or physical features in the formation or manufacture of moulds characterised by the use of binding agents; Mixtures of binding agents of inorganic agents contaming ammonium or metal silicates, silica sols
- B22C1/188—Alkali metal silicates
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mold Materials And Core Materials (AREA)
- Molds, Cores, And Manufacturing Methods Thereof (AREA)
Abstract
本发明提供一种高溃散、可回收氧化硅基陶瓷型芯及其制备方法和应用，其制备原料包括：石英玻璃基础粉料、水玻璃、造孔剂、添加剂和水；所述石英玻璃基础粉料为纳米级二氧化硅及微米级二氧化硅经颗粒级配后的粉料，其中，按照质量百分比计，纳米级二氧化硅占10％～75％，微米级二氧化硅占25％～90％；所述添加剂为抑制石英玻璃基础粉料烧结致密化的陶瓷粉料；水玻璃、造孔剂、添加剂和水的加入量分别为石英玻璃基础粉料质量的1％～8％、0～15％、0～40％、5％～15％。所述陶瓷型芯无需脱脂或脱蜡而直接进行预热、浇注，溃散性高，可通过物理振动方式直接脱除；且剥落的陶瓷型芯可实现100％循环再利用。The present invention provides a highly collapsible, recyclable silicon oxide-based ceramic core and a preparation method and application thereof. The preparation raw materials include: quartz glass base powder, water glass, pore-forming agent, additives and water; The powder is the powder of nano-scale silica and micro-scale silica after particle grading, wherein, in terms of mass percentage, nano-scale silica accounts for 10% to 75%, and micro-scale silica accounts for 25%. ～90%; the additive is a ceramic powder that inhibits the sintering and densification of the quartz glass base powder; the addition amounts of water glass, pore-forming agent, additives and water are respectively 1% to 8% of the mass of the quartz glass base powder, 0～15%, 0～40%, 5%～15%. The ceramic core can be directly preheated and poured without degreasing or dewaxing, has high collapsibility, and can be directly removed by physical vibration; and the peeled ceramic core can realize 100% recycling.
Description
Technical Field
The invention relates to the field of precision casting, in particular to a high-collapsibility recyclable silicon oxide-based ceramic core and a preparation method and application thereof.
Background
The ceramic core is widely applied to the precision casting fields of turbine engine hollow blades in the aviation industry, high-thrust engine hollow blades for ships, golf club heads, large thin-wall aluminum alloy castings, impellers for chemical engineering and the like. The ceramic cores commonly used at home and abroad are mainly divided into silicon-based ceramic cores and aluminum-based ceramic cores according to matrix materials. The base material of the silicon-based ceramic core is quartz glass powder, meanwhile, zircon, mullite or rare earth oxide is added as a mineralizer, and the content of cristobalite generated in the sintering process is controlled, so that the core has good physical and mechanical properties, small thermal expansion coefficient, good fire resistance, easy dissolution in molten alkali and hydrofluoric acid, and convenient core removal, and therefore, the silicon-based ceramic core is most researched at present, is most widely applied and has the most mature technology.
At present, the precision silicon-based ceramic core has many defects and needs to be solved urgently. Firstly, the molding mode usually adopts injection molding or slip casting, so that wax base or organic lipid is added in the formula as a binder, a long-time degreasing or dewaxing process is required in the sintering process, the production period is long, the shrinkage rate in the dewaxing process is large, and the size of a core is difficult to control accurately; in recent years, water-based adhesives have been widely used, but they have a high water content in their base stock, require evaporation of a large amount of water, have a large heat loss during drying, have many defects such as deformation and cracking, and also require addition of an organic polymer. Secondly, after casting, the mold core needs to be removed by chemical methods such as alkaline boiling and the like, VOCs and solid waste discharge are enlarged, the environmental protection performance is poor, and the automation degree is not high; in addition, the collapsed core is difficult to recycle due to the residue of wax base or organic lipid, which results in high production cost.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the high-collapsibility recyclable silicon oxide-based ceramic core and the preparation method and application thereof, wherein the ceramic core has the advantages of high drying and hardening speed, small shrinkage deformation and higher dimensional precision; the preheating and the pouring are directly carried out without degreasing or dewaxing, so that the production period is greatly shortened; the ceramic core has high collapsibility and can be directly removed through a physical vibration mode; and the spalled ceramic core can be recycled to 100%.
The invention is realized by the following technical scheme:
a high-collapsibility recyclable silica-based ceramic core is prepared from the following raw materials: quartz glass base powder, water glass, a pore-forming agent, an additive and water;
the quartz glass base powder is prepared by grading nano-scale silicon dioxide and micron-scale silicon dioxide, wherein the nano-scale silicon dioxide accounts for 10-75% and the micron-scale silicon dioxide accounts for 25-90% by mass percent;
the additive is ceramic powder for inhibiting sintering densification of quartz glass base powder;
the adding amount of the water glass is 1-8% of the mass of the quartz glass base powder, the adding amount of the pore-forming agent is 0-15% of the mass of the quartz glass base powder, the adding amount of the additive is 0-40% of the mass of the quartz glass base powder, and the adding amount of the water is 5-15% of the mass of the quartz glass base powder.
Preferably, the pore-forming agent is carbonate.
Preferably, the carbonate is at least one of calcium carbonate, ammonium carbonate and zinc carbonate.
Preferably, the additive is cristobalite crystals.
The preparation method of the high-collapsibility recyclable silica-based ceramic core comprises the following steps:
(1) fully and uniformly stirring the quartz glass base powder, the water glass, the pore-forming agent, the additive and the water to obtain a paste;
(2) injecting or injecting the mud paste into a cavity of a ceramic core mould, and demoulding to obtain a ceramic core blank;
(3) drying the ceramic core blank body to obtain a biscuit;
(4) and checking and modifying the biscuit to obtain the silicon oxide-based ceramic core.
Preferably, in the step (2), the pressure of injection or injection is 10-40 MPa.
Preferably, in the step (3), the drying temperature is 50-200 ℃, and the drying time is 60-120 min.
The application of the silicon oxide-based ceramic core with high collapsibility and recoverability comprises preheating and casting the silicon oxide-based ceramic core; and removing the silica-based ceramic core from the casting precursor obtained by pouring in a physical vibration mode to obtain a casting finished product.
Preferably, when the additive is a cristobalite crystal, the silicon oxide-based ceramic core is removed from the cast precursor obtained by casting in a physical vibration mode to obtain a peeled silicon oxide-based ceramic core, and the peeled silicon oxide-based ceramic core is crushed, ball-milled and crystallized to form the cristobalite crystal which is used as the additive for recycling.
Preferably, the crystallization temperature is 1200-1400 ℃, and the crystallization time is 2-24 h.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts powder material of nano-scale and micron-scale silicon dioxide after grain grading as basic powder material, and adds inorganic water glass as binder, wherein the nano-scale silicon dioxide powder can play a role of plasticizer, which is convenient for shaping the mold core. Particularly, when ceramic powder for inhibiting the sintering densification of quartz glass base powder is added, the viscosity of fused quartz at high temperature (in the preheating and pouring processes) is increased, the sintering densification is hindered, the effective action of a pore-forming agent is combined, a porous silicon-based ceramic core is formed, and the collapsibility of the porous silicon-based ceramic core is further greatly improved while the high-temperature strength in the pouring process is ensured. The ceramic core after finishing the process has high collapsibility and can be directly removed by a physical vibration mode; and the peeled ceramic core is crushed, ball-milled and crystallized to be used as an additive to realize 100 percent recycling.
According to the preparation method, the green body is directly demoulded after being formed, so that the turnover time of a forming process can be reduced, and the green body has the advantages of low water content, high drying and hardening speed, small shrinkage deformation and high dimensional precision; the preheating and the pouring can be directly carried out without degreasing or dewaxing, thereby greatly shortening the production period; the preparation method is simple, degreasing and other processes are not needed, the production period is greatly shortened, the operation is simple and convenient, the automation degree is high, the production cost is low, the pollution is less, and the green and efficient production of the ceramic core can be realized.
Drawings
FIG. 1 shows the three-point bending strength of the highly collapsible, recyclable silica-based ceramic cores prepared in examples 1-5.
FIG. 2 is an XRD pattern of the high collapsible, recyclable silica-based ceramic core prepared in example 1 after casting.
FIG. 3 is an SEM photograph of the high collapse, recyclable silica-based ceramic core prepared in example 1 after casting.
FIG. 4 is a photograph of the high collapsibility, recyclable silica-based ceramic core prepared in example 2 after casting.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The preparation method of the high-collapsibility recyclable silicon oxide-based ceramic core comprises the following steps of:
(1) sequentially adding quartz glass base powder, a binder, a pore-forming agent, an additive and water into special pug mill equipment, fully stirring and uniformly mixing, and mixing pug into a semi-solid paste shape;
(2) injecting (or injecting) the mud paste prepared in the step (1) into a cavity of a ceramic core mould, drawing the mould under a wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with a shape;
(3) putting the ceramic core blank prepared in the step (2) and the special forming die into a drying furnace together for drying to obtain a biscuit;
(4) inspecting and modifying the biscuit prepared in the step (3) to obtain a silicon oxide-based ceramic core for pouring, and then assembling, preheating and pouring according to actual production requirements;
(5) and (4) removing the silica-based ceramic core from the casting cast in the step (4) in a physical vibration mode, wherein the collapsibility is high, and the peeled silica-based ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal which is used as an additive to realize 100% recycling.
In the method, the quartz glass base powder in the step (1) is powder prepared by grading nano-scale and micron-scale silicon dioxide particles, wherein the nano-scale silicon dioxide accounts for 10-75% by mass and plays the role of a plasticizer, and the micron-scale silicon dioxide accounts for 25-90%.
The addition amount of the binder in the step (1) is 1-8% of the mass of the quartz glass base powder, the addition amount of the pore-forming agent is 0-15% of the mass of the quartz glass base powder, the addition amount of the additive is 0-40% of the mass of the quartz glass base powder, and the addition amount of the water is 5-15% of the mass of the quartz glass base powder. The binder is water glass, the pore-forming agent is inorganic carbonate, the carbonate is at least one of calcium carbonate, ammonium carbonate and zinc carbonate, and the additive is cristobalite crystal powder.
Step (2), the injection molding pressure is 10-40 MPa; the drying temperature in the step (3) is 50-200 ℃, and the drying time is 60-120 min; the preheating temperature in the step (4) is 1100-1300 ℃, the preheating time is 20-60 min, and the pouring temperature is 1400-1600 ℃; and (5) crystallizing at 1200-1400 ℃ for 2-24 h.
Example 1:
(1) taking quartz glass base powder (wherein the proportion of nano powder (D50 is 50-100 nm) is 10%, the proportion of micron powder (D50 is 20-60 mu m) is 90%), water glass binder, calcium carbonate, cristobalite crystal powder and water, ensuring the mass ratio of the quartz glass base powder to the micron powder to be 1:0.01:0:0:0.05, adding the quartz glass base powder to special pug mill equipment in sequence, fully stirring and uniformly mixing, and mixing pug to be semisolid mud paste;
(2) injecting the paste into a cavity of a ceramic core mould, wherein the injection molding pressure is 10MPa, drawing the mould under the wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with the shape;
(3) putting the ceramic core blank body and the special forming die into a drying furnace for drying at the drying temperature of 50 ℃ for 120min to obtain a biscuit;
(4) and (3) checking and modifying the prepared biscuit to obtain the silicon-based ceramic core for pouring, and then assembling, preheating and pouring according to actual production requirements, wherein the preheating temperature is 1100 ℃, the preheating time is 60min, and the pouring temperature is 1400 ℃.
(5) And (3) removing the ceramic core from the cast casting in a physical vibration mode, wherein the collapsibility is high, and the peeled ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal, wherein the crystallization temperature is 1200 ℃, and the crystallization time is 24 hours, so that cristobalite powder with the crystallinity of more than 80% can be obtained, and the cristobalite powder can be used as an additive to realize 100% recycling.
Example 2:
(1) taking quartz glass base powder (wherein 75 percent of nano powder (D50 is 50-100 nm), 25 percent of micron powder (D50 is 20-60 mu m), water glass binder, calcium carbonate, cristobalite crystal powder and water, ensuring the mass ratio to be 1:0.01: 0.4:0.05, adding the materials into special pug mill equipment in sequence, fully stirring and uniformly mixing, and mixing the pug into a semisolid pug paste;
(2) injecting the paste into a cavity of a ceramic core mould, wherein the injection molding pressure is 10MPa, drawing the mould under the wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with the shape;
(3) putting the ceramic core blank body and the special forming die into a drying furnace for drying at the drying temperature of 50 ℃ for 120min to obtain a biscuit;
(4) and (3) checking and modifying the prepared biscuit to obtain the silicon-based ceramic core for pouring, and then assembling, preheating and pouring according to actual production requirements, wherein the preheating temperature is 1100 ℃, the preheating time is 60min, and the pouring temperature is 1400 ℃.
(5) And (3) removing the ceramic core from the cast casting in a physical vibration mode, wherein the collapsibility is high, and the peeled ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal, wherein the crystallization temperature is 1200 ℃, and the crystallization time is 24 hours, so that cristobalite powder with the crystallinity of more than 80% can be obtained, and the cristobalite powder can be used as an additive to realize 100% recycling.
Example 3:
(1) taking quartz glass base powder (wherein the proportion of nano powder (D50 is 50-100 nm) is 25%, the proportion of micron powder (D50 is 20-60 mu m) is 75%), water glass binder, calcium carbonate, cristobalite crystal powder and water, ensuring the mass ratio of the quartz glass base powder to the micron powder to be 1:0.03:0.05:0.3:0.08, adding the quartz glass base powder to special pug mill equipment in sequence, fully stirring and uniformly mixing, and mixing pug to be semisolid paste;
(2) injecting the paste into a cavity of a ceramic core mould, wherein the injection molding pressure is 20MPa, drawing the mould under the wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with the shape;
(3) putting the ceramic core blank body and the special forming die into a drying furnace for drying at 100 ℃ for 90min to obtain a biscuit;
(4) and (3) checking and modifying the prepared biscuit to obtain a silicon-based ceramic core for casting, and then assembling, preheating and casting according to actual production requirements, wherein the preheating temperature is 1150 ℃, the preheating time is 50min, and the casting temperature is 1450 ℃.
(5) And (3) removing the ceramic core from the cast casting in a physical vibration mode, wherein the collapsibility is high, and the peeled ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal, wherein the crystallization temperature is 1250 ℃, and the crystallization time is 20 hours, so that cristobalite powder with the crystallinity of more than 80% can be obtained, and the cristobalite powder can be used as an additive to realize 100% recycling.
Example 4:
(1) taking quartz glass base powder (wherein the proportion of nano powder (D50 is 50-100 nm) is 35%, the proportion of micron powder (D50 is 20-60 mu m) is 65%), water glass binder, calcium carbonate, cristobalite crystal powder and water, ensuring the mass ratio of the quartz glass base powder to the micron powder to be 1:0.05:0.08:0.25:0.1, adding the quartz glass base powder to a special pug mill in sequence, fully stirring and uniformly mixing, and mixing pug to be semisolid paste;
(2) injecting the paste into a cavity of a ceramic core mould, wherein the injection molding pressure is 25MPa, drawing the mould under the wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with the shape;
(3) putting the ceramic core blank body and the special forming die into a drying furnace for drying at the drying temperature of 150 ℃ for 80min to obtain a biscuit;
(4) and (3) checking and modifying the prepared biscuit to obtain the silicon-based ceramic core for pouring, and then assembling, preheating and pouring according to actual production requirements, wherein the preheating temperature is 1200 ℃, the preheating time is 40min, and the pouring temperature is 1500 ℃.
(5) And (3) removing the ceramic core from the cast casting in a physical vibration mode, wherein the collapsibility is high, and the peeled ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal, wherein the crystallization temperature is 1300 ℃, and the crystallization time is 15 hours, so that cristobalite powder with the crystallinity of more than 80% can be obtained, and the cristobalite powder can be used as an additive to realize 100% recycling.
Example 5:
(1) taking quartz glass base powder (wherein 50% of nano powder (D50 is 50-100 nm), 50% of micron powder (D50 is 20-60 mu m), water glass binder, calcium carbonate, cristobalite crystal powder and water, ensuring the mass ratio of the quartz glass base powder to the micron powder to be 1:0.07:0.12:0.35:0.12, sequentially adding the quartz glass base powder to a special pug mill device, fully stirring and uniformly mixing, and mixing pug to be semisolid paste;
(2) injecting the paste into a cavity of a ceramic core mould, wherein the injection molding pressure is 30MPa, drawing the mould under the wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with the shape;
(3) putting the ceramic core blank body and the special forming die into a drying furnace for drying at 180 ℃ for 70min to obtain a biscuit;
(4) and (3) checking and modifying the prepared biscuit to obtain the silicon-based ceramic core for pouring, and then assembling, preheating and pouring according to actual production requirements, wherein the preheating temperature is 1250 ℃, the preheating time is 30min, and the pouring temperature is 1550 ℃.
(5) And (3) removing the ceramic core from the cast casting in a physical vibration mode, wherein the collapsibility is high, and the peeled ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal, wherein the crystallization temperature is 1350 ℃, and the crystallization time is 8 hours, so that cristobalite powder with the crystallinity of more than 80% can be obtained, and the cristobalite powder can be used as an additive to realize 100% recycling.
Example 6:
(1) taking quartz glass base powder (wherein the proportion of nano powder (D50 is 50-100 nm) is 10%, the proportion of micron powder (D50 is 20-60 mu m) is 90%), water glass binder, calcium carbonate, cristobalite crystal powder and water, ensuring the mass ratio of the quartz glass base powder to the micron powder to be 1:0.08:0.15, adding the quartz glass base powder to special pug mill equipment in sequence, fully stirring and uniformly mixing, and mixing pug to be semisolid paste;
(2) injecting the paste into a cavity of a ceramic core mould, wherein the injection molding pressure is 40MPa, drawing the mould under the wet condition to obtain a ceramic core blank, and then placing the ceramic core blank into a special mould with the shape;
(3) putting the ceramic core blank body and the special forming die into a drying furnace for drying at the drying temperature of 200 ℃ for 60min to obtain a biscuit;
(4) and (3) checking and modifying the prepared biscuit to obtain the silicon-based ceramic core for pouring, and then assembling, preheating and pouring according to actual production requirements, wherein the preheating temperature is 1300 ℃, the preheating time is 20min, and the pouring temperature is 1600 ℃.
(5) And (3) removing the ceramic core from the cast casting in a physical vibration mode, wherein the collapsibility is high, and the peeled ceramic core is subjected to crushing, ball milling and crystallization to form a cristobalite crystal, wherein the crystallization temperature is 1400 ℃, and the crystallization time is 2 hours, so that cristobalite powder with the crystallinity of more than 80% can be obtained, and the cristobalite powder can be used as an additive to realize 100% recycling.
Table 1 shows the collapse of the specific examples:
TABLE 1 examples collapse
As can be seen from Table 1, the collapsibility of example 1 of the present invention was further improved by adding the pore-forming agent and the additive. The collapsibility of example 3 was the highest.
FIG. 1 shows the three-point bending strength of the highly collapsible, recyclable silica-based ceramic cores prepared in examples 1-6, which shows that the bending strength of the cores after pore-forming agent (calcium carbonate) and cristobalite crystal powder are added is generally low, wherein the bending strength of the core in example 3 is the lowest, which is reduced to about 6 MPa. FIG. 2 is an XRD pattern of the highly collapsible, recyclable silica-based ceramic core prepared in example 3 after casting, fully illustrating that the addition of cristobalite crystals promotes the transformation of the fused silica phase to the cristobalite phase, the rate of cristobalite precipitation is increased, and the amount of cristobalite is increased. FIG. 3 is an SEM photograph of the cast high-collapse, recyclable silica-based ceramic core prepared in example 3, showing that, in one aspect, the porosity of the core is increased due to the addition of a carbonate pore former; on the other hand, after the cristobalite crystal is added, the liquid phase flow is hindered, so that the liquid phase viscosity is increased, the specific surface area of the fused quartz after crystallization is increased, the contact area among particles is reduced, the combination is loose, the pores are obviously increased, and the liquid phase sintering degree is low. FIG. 4 is a photograph of the high collapsibility, recyclable silica-based ceramic core prepared in example 3 after casting, showing that (a) is a photograph of the high collapsibility, and (b) is a photograph of the high collapsibility, recyclable silica-based ceramic core after vibration, and the high collapsibility and good casting quality are obtained.
The invention adopts powder material of nanoscale and micron-sized silicon dioxide after particle grading as base powder material, wherein the nanoscale silicon dioxide powder can play a role of a plasticizer, inorganic water glass is added as a binder, pore-forming agent, additive and the like are added on the basis to jointly form original powder material, a certain proportion of water is added, the silicon-based ceramic core for pouring is obtained through pugging, injection molding and drying, then the silicon-based ceramic core for pouring is assembled, preheated and poured according to actual production requirements, and finally the ceramic core is removed from the poured casting in a physical vibration mode. Therefore, by adopting the preparation method, the blank is directly demoulded after being formed, the turnover time of the forming process can be reduced, and the blank has lower water content, high drying and hardening speed, small shrinkage deformation and higher dimensional precision; the preheating and the pouring are directly carried out without degreasing or dewaxing, so that the production period is greatly shortened; particularly, due to the addition of the cristobalite crystals, the viscosity of fused quartz at high temperature (in the preheating and pouring processes) is increased, sintering densification is hindered, and a porous silicon-based ceramic core is formed by combining the effective action of a pore-forming agent, so that the collapsibility of the porous silicon-based ceramic core is greatly improved while the high-temperature strength in the pouring process is ensured. The ceramic core after finishing the process has high collapsibility and can be directly removed by a physical vibration mode; and the peeled ceramic core is crushed, ball-milled and crystallized to form cristobalite crystals which are used as additives to realize 100 percent recycling. The preparation method is simple, degreasing and other processes are not needed, the production period is greatly shortened, the operation is simple and convenient, the automation degree is high, the production cost is low, the pollution is less, and the green and efficient production of the ceramic core can be realized.
Claims (10)
1. A high-collapsibility recyclable silica-based ceramic core is characterized in that the preparation raw materials comprise: quartz glass base powder, water glass, a pore-forming agent, an additive and water;
the quartz glass base powder is prepared by grading nano-scale silicon dioxide and micron-scale silicon dioxide, wherein the nano-scale silicon dioxide accounts for 10-75% and the micron-scale silicon dioxide accounts for 25-90% by mass percent;
the additive is ceramic powder for inhibiting sintering densification of quartz glass base powder;
the adding amount of the water glass is 1-8% of the mass of the quartz glass base powder, the adding amount of the pore-forming agent is 0-15% of the mass of the quartz glass base powder, the adding amount of the additive is 0-40% of the mass of the quartz glass base powder, and the adding amount of the water is 5-15% of the mass of the quartz glass base powder.
2. The high collapse, recyclable silica-based ceramic core of claim 1 wherein the pore former is a carbonate.
3. The high collapse, recyclable silica-based ceramic core according to claim 1, wherein the carbonate is at least one of calcium carbonate, ammonium carbonate and zinc carbonate.
4. The high collapse, recyclable silicon oxide based ceramic core as claimed in claim 1 wherein the additive is cristobalite crystals.
5. The method of making a high-collapse, recyclable silica-based ceramic core as described in any of claims 1 to 4 comprising the steps of:
(1) fully and uniformly stirring the quartz glass base powder, the water glass, the pore-forming agent, the additive and the water to obtain a paste;
(2) injecting or injecting the mud paste into a cavity of a ceramic core mould, and demoulding to obtain a ceramic core blank;
(3) drying the ceramic core blank body to obtain a biscuit;
(4) and checking and modifying the biscuit to obtain the silicon oxide-based ceramic core.
6. The method for preparing the high-collapsibility, recyclable silica-based ceramic core as claimed in claim 5, wherein the pressure of the injection or shot in the step (2) is 10 to 40 MPa.
7. The method for preparing the high-collapsibility and recyclable silica-based ceramic core as claimed in claim 5, wherein the drying temperature in step (3) is 50-200 ℃ and the drying time is 60-120 min.
8. Use of the high-collapse, recyclable silica-based ceramic core of any of claims 1-4 wherein the silica-based ceramic core is preheated and cast; and removing the silica-based ceramic core from the casting precursor obtained by pouring in a physical vibration mode to obtain a casting finished product.
9. The use of the highly collapsible, recyclable silica-based ceramic cores as defined in claim 8 wherein, when the additive is cristobalite crystals, the silica-based ceramic cores are removed from the cast precursors by physical vibration to obtain exfoliated silica-based ceramic cores, and the exfoliated silica-based ceramic cores are crushed, ball milled and crystallized to form cristobalite crystals for recycling as the additive.
10. The use of the high-collapse, recyclable silica-based ceramic core as claimed in claim 9, wherein the crystallization temperature is 1200-1400 ℃ and the crystallization time is 2-24 hours.
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