CN103043668B - Preparation method of core additive - Google Patents
Preparation method of core additive Download PDFInfo
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- CN103043668B CN103043668B CN201110309780.4A CN201110309780A CN103043668B CN 103043668 B CN103043668 B CN 103043668B CN 201110309780 A CN201110309780 A CN 201110309780A CN 103043668 B CN103043668 B CN 103043668B
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Abstract
The invention relates to a preparation method of a core additive, which sequentially comprises the following steps: heating liquid silicasol to 500+/-100 DEG C, keeping the temperature for 2-6 hours, and carrying out furnace cooling on the material to room temperature; weighing the obtained solid, adding the solid into a ball grinder, adding a grinding body according to the weight ratio of 1:(0.7-1.5), carrying out ball grinding for 8-10 hours, and passing through a 150-250-mesh screen to obtain powder; carrying out high-temperature calcination on the powder at 1100-1250 DEG C for 3-10 hours, and carrying out furnace cooling on the material; and weighing the material, adding into a ball grinder, adding a grinding body according to the weight ratio of 1:(0.7-1.5), and carrying out ball grinding for 4-15 hours to obtain amorphous silica core additive powder of which the grain diameter is 7-60 mu m. The silyl core prepared from the amorphous silica additive has the advantages of large specific area and high core pressure molding rate, and enhances the suspensibility and flowability of the core slurry; the sintering characteristic is good; the room-temperature strength and high-temperature strength of the core are high; and the core is easy to strip, and the casting qualification rate is up to 70%.
Description
Technical field
The present invention relates to a kind of preparation technology of ceramic core additive, it has improved especially a kind ofly can improve ceramic core room temperature strength and hot strength, reduces the preparation method of the additive of high temperature deformation.
Background technology
Along with improving constantly of inlet temperature before engine turbine, blade to hold warm Capability Requirement more and more higher.The hollow blade that adopts the precision casting technology of ceramic core to prepare, inner chamber road shape complexity, can make the warm ability of holding of blade improve, uniformity of temperature profile, the work-ing life of prolongation blade.The working conditions of ceramic core is very severe, needs higher room temperature strength and hot strength.The silica-based core adopting at present, in pressing process, easily break in thinner and small place, and when teeming temperature improves, flexural strength is low, and qualified cast rate is low.Meanwhile, along with engine manufacturing technology improves constantly, the manufacturing technology to core and performance index require higher, and existing silica-based core can not meet founding requirement, and the new technological method of active demand improves the performance index of core.
Summary of the invention
This object is to provide the preparation method of the better core additive of a kind of technique effect.Key is to improve room temperature strength and the hot strength of core, controls better separating out of cristobalite content in the plasticity of core pressing process and roasting process, reduces crackle and the distortion of core.By adding the soft silica of development voluntarily, improve the reactivity on core powder surface, the distortion of core hygrometric state reduces, and room temperature strength, hot strength and sintering character improve.
The preparation method who the invention provides a kind of core additive, is characterized in that: the preparation method of described core additive requires as follows successively:
1. step, is first heated to 500 ± 100 DEG C by liquid-state silicon colloidal sol, insulation 2-6 hour, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, by weight 1:(0.7-1.5) add grinding element, Ball-milling Time 8 ~ 10h, crosses 150-250 mesh sieve, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained carries out high-temperature calcination to step under 1100 DEG C of-1250 DEG C of conditions, and soaking time is 3-10 hour, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, by weight 1:(0.7-1.5) add grinding element ball milling, Ball-milling Time 4-15h, the soft silica core additive powder of acquisition, particle size diameter is 7-60 μ m.
The preparation method of core additive of the present invention, preferably meets following requirement:
1. step, is heated to 500 ± 20 DEG C by liquid-state silicon colloidal sol, insulation 3.5-5 hour, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, by weight 1:(0.9-1.1) add grinding element, Ball-milling Time 8 ~ 10h, crosses 200 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained carries out high-temperature calcination to step under 1160 DEG C of-1200 DEG C of conditions, and soaking time is 3.5-5 hour, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, by weight 1:(0.9-1.1) add grinding element ball milling, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4 ~ 6h, particle size diameter is 50 ~ 60 μ m; Its two, Ball-milling Time 7 ~ 10h, particle size diameter is 30 ~ 20 μ m; Its three, Ball-milling Time 11 ~ 15h, particle size diameter is 20 ~ 10 μ m.
The preparation method of core additive of the present invention, further preferably meets following requirement:
In the preparation method of described core additive, meet following requirement:
1. step, packs liquid-state silicon colloidal sol in clean stainless steel cask into, puts into electrically heated drying cabinet and is heated to 500 DEG C, is incubated 4 hours, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, adds grinding element by weight 1:1, and Ball-milling Time 9h crosses 200 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained is put into ceramic disc to step, packs in chamber type electric resistance furnace, under 1160 DEG C of-1200 DEG C of conditions, carries out high-temperature calcination, and soaking time is 4 hours, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, add grinding element ball milling by weight 1:1, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4 ~ 6h, particle size diameter is 50 ~ 60 μ m; Its two, Ball-milling Time 7 ~ 10h, particle size diameter is 30 ~ 20 μ m; Its three, Ball-milling Time 11 ~ 15h, particle size diameter is 20 ~ 10 μ m.
Add the silica-based core of soft silica additive prepared by the present invention, through evidence:
1, soft silica powder contains many micropores, specific surface area is large, has improved suspension and the mobility of core slurry, and core compression moulding rate improves.
2, soft silica micro mist material, can fully be filled in core substrate material particle gap, promotes core sintering character, has reduced crackle and the distortion of core, and the room temperature strength of core and hot strength improve.
3, soft silica powder can promote cristobalite.In silica glass, add a certain amount of additive, in the core after roasting, cristobalite content increases, and core warp resistance deformability improves.
Step 3. in, adopt different calcining temperatures, can detect the inversion quantity of cristobalite under differing temps.Test-results shows, when high-temperature calcination temperature is 1200 DEG C, have a small amount of cristobalite to separate out.When calcining temperature is 1180 DEG C and 1190 DEG C, gained material has good surfactivity, and separates out without cristobalite, and material is soft silica.Amorphous silica particles contains many micropores, and good surface activity adds certain soft silica additive at quartz glass substrate material, can improve the reactivity on powder surface.In compacting core, improve suspension and the mobility of core slurry, be easy to press forming.In roasting process, easy-sintering.In casting process, soft silica powder can promote cristobaliteization growth, improves core hot strength and high temperature anti-crawl agentdefiection and deformability.
Material after high-temperature calcination is that 50 ~ 40 μ m, 30 ~ 20 μ m and 20 ~ 10 μ m grinding are sieved by size-grade distribution.Soft silica micro mist material, can fully be filled in core substrate material particle gap, promotes core sintering character, improves room temperature strength and the hot strength of core.Test-results shows, size-grade distribution is the performance that the additive of 20 ~ 10 μ m significantly improves silica-based core, makes it have good room temperature strength, hot strength and sintering character.
The soft silica additive that uses the present invention to prepare, room temperature strength and the hot strength of silica-based core significantly improve, and core has good coking property, is easy to depoling, and cast qualification rate brings up to 70% by 30 ~ 50%.
Brief description of the drawings
Below in conjunction with drawings and the embodiments, the present invention is further detailed explanation:
Fig. 1 is that the II of restriking of adding soft silica is led core; Due to core structure complexity, in pressing process, easily break in thinner and small place; Soft silica additive can improve the reactivity on powder surface; In compacting core, improve suspension and the mobility of core slurry, be easy to press forming;
Fig. 2 is directional vane core; Because directional vane requires to have higher high temperature bend strength in crystal pulling process with core, soft silica additive powder, can fully be filled in core substrate material particle gap, promotes core sintering character, improved the high-temperature behavior of core, blade casting qualification rate significantly improves;
Fig. 3 is single crystal blade core; Single crystal blade requires to have high hot strength and good depoling performance with core; Soft silica additive powder, can fully be filled in core substrate material particle gap, promotes core sintering character, makes core have good hot strength, and is easy to depoling.
Embodiment
Embodiment 1
In the preparation method of described core additive, meet following requirement:
1. step, packs liquid-state silicon colloidal sol in clean stainless steel cask into, puts into electrically heated drying cabinet and is heated to 500 DEG C, is incubated 4 hours, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, adds grinding element by weight 1:1, and Ball-milling Time 9h crosses 200 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained is put into ceramic disc to step, packs in chamber type electric resistance furnace, under 1160 DEG C of-1200 DEG C of conditions, carries out high-temperature calcination, and soaking time is 4 hours, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, add grinding element ball milling by weight 1:1, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4 ~ 6h, particle size diameter is 50 ~ 60 μ m; Its two, Ball-milling Time 7 ~ 10h, particle size diameter is 30 ~ 20 μ m; Its three, Ball-milling Time 11 ~ 15h, particle size diameter is 20 ~ 10 μ m.
Soft silica after the high-temperature calcination that employing obtains through above-mentioned preparation process, as additive, obtains the silica-based core of equiax crystal blade by following formula compacting.
Silica-based core formula for equiax crystal blade: silica additive: weight percent 10-20%; Fused silica powder+mineralizer: weight percent is surplus.
Equiax crystal blade selects the II of restriking to lead as carrier with silica-based core, and adopting the soft silica after high-temperature calcination is additive, by above-mentioned formula compacting core.The II of restriking is led core structure complexity (as shown in Figure 1), and in pressing process, easily break in thinner and small place, and soft silica additive has improved suspension and the mobility of slurry, makes core have good wet strength, and plasticity improves.
Embodiment 2
In the preparation method of described core additive, meet following requirement:
1. step, packs liquid-state silicon colloidal sol in clean stainless steel cask into, puts into electrically heated drying cabinet and is heated to 520 DEG C, is incubated 4 hours, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, adds grinding element by weight 1:1.1, and Ball-milling Time 10h crosses 150 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained is put into ceramic disc to step, packs in chamber type electric resistance furnace, under 1160 DEG C of-1200 DEG C of conditions, carries out high-temperature calcination, and soaking time is 5 hours, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, add grinding element ball milling by weight 1:1.1, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4 ~ 6h, particle size diameter is 50 ~ 60 μ m; Its two, Ball-milling Time 7 ~ 10h, particle size diameter is 30 ~ 20 μ m; Its three, Ball-milling Time 11 ~ 15h, particle size diameter is 20 ~ 10 μ m.
Soft silica after the high-temperature calcination that employing obtains through above-mentioned preparation process, as additive, obtains the silica-based core of directional vane by following formula compacting.
Silica-based core formula for directional vane: silica additive: weight percent 5-15%; Fused silica powder+mineralizer: weight percent is surplus.
Directional vane is prepared core powder, compacting core with silica-based core by above-mentioned formula.Because directional vane requires to have more high bending strength in crystal pulling process with core, soft silica additive powder, can fully be filled in core substrate material particle gap, promotes core sintering character, the high-temperature behavior that improves core, has improved blade casting qualification rate.
Embodiment 3
In the preparation method of described core additive, meet following requirement:
1. step, packs liquid-state silicon colloidal sol in clean stainless steel cask into, puts into electrically heated drying cabinet and is heated to 480 DEG C, is incubated 3.5 hours, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, adds grinding element by weight 1:0.9, and Ball-milling Time 8h crosses 250 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained is put into ceramic disc to step, packs in chamber type electric resistance furnace, under 1160 DEG C of-1200 DEG C of conditions, carries out high-temperature calcination, and soaking time is 3.5 hours, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, add grinding element ball milling by weight 1:0.9, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4 ~ 6h, particle size diameter is 50 ~ 60 μ m; Its two, Ball-milling Time 7 ~ 10h, particle size diameter is 30 ~ 20 μ m; Its three, Ball-milling Time 11 ~ 15h, particle size diameter is 20 ~ 10 μ m.
Soft silica after the high-temperature calcination that employing obtains through above-mentioned preparation process, as additive, obtains the silica-based core of single crystal blade by following formula compacting.
Silica-based core formula for single crystal blade: silica additive: weight percent 1-10%; Fused silica powder+mineralizer: weight percent is surplus.
Single crystal blade is prepared core powder, compacting core with silica-based core by above-mentioned formula.Single crystal blade requires to have high hot strength and good depoling performance with core.Soft silica additive powder, can fully be filled in core substrate material particle gap, promotes core sintering character, makes core have good hot strength, and is easy to depoling.
Claims (3)
1. a preparation method for core additive, is characterized in that: the preparation method of described core additive requires as follows successively:
1. step, is first heated to 500 ± 100 DEG C by liquid-state silicon colloidal sol, insulation 2-6 hour, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, by weight 1:(0.7-1.5) add grinding element, Ball-milling Time 8-10h, crosses 150-250 mesh sieve, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained carries out high-temperature calcination to step under 1100 DEG C of-1250 DEG C of conditions, and soaking time is 3-10 hour, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, by weight 1:(0.7-1.5) add grinding element ball milling, Ball-milling Time 4-15h, the soft silica core additive powder of acquisition, particle size diameter is 7-60 μ m.
2. according to the preparation method of core additive described in claim 1, it is characterized in that: in the preparation method of described core additive, meet following requirement:
1. step, is heated to 500 ± 20 DEG C by liquid-state silicon colloidal sol, insulation 3.5-5 hour, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, by weight 1:(0.9-1.1) add grinding element, Ball-milling Time 8-10h, crosses 200 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained carries out high-temperature calcination to step under 1160 DEG C of-1200 DEG C of conditions, and soaking time is 3.5-5 hour, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, by weight 1:(0.9-1.1) add grinding element ball milling, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4-6h, particle size diameter is 50-60 μ m; Its two, Ball-milling Time 7-10h, particle size diameter is 30-20 μ m; Its three, Ball-milling Time 11-15h, particle size diameter is 20-10 μ m.
3. according to the preparation method of core additive described in claim 1, it is characterized in that: in the preparation method of described core additive, meet following requirement:
1. step, packs liquid-state silicon colloidal sol in clean stainless steel cask into, puts into electrically heated drying cabinet and is heated to 500 DEG C, is incubated 4 hours, and then material cools to room temperature with the furnace;
2. step, weighs a upper process gained solid, puts into ball mill, adds grinding element by weight 1:1, and Ball-milling Time 9h crosses 200 mesh sieves, crosses grinding element and obtains powder;
3., the powder that a upper process is obtained is put into ceramic disc to step, packs in chamber type electric resistance furnace, under 1160 DEG C of-1200 DEG C of conditions, carries out high-temperature calcination, and soaking time is 4 hours, material furnace cooling;
4. step, by the material metage after high-temperature calcination, puts into ball mill, add grinding element ball milling by weight 1:1, the core additive powder particles diameter of Ball-milling Time and acquisition meets one of following requirement: one, and Ball-milling Time 4-6h, particle size diameter is 50-60 μ m; Its two, Ball-milling Time 7-10h, particle size diameter is 30-20 μ m; Its three, Ball-milling Time 11-15h, particle size diameter is 20-10 μ m.
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| US4093017A (en) * | 1975-12-29 | 1978-06-06 | Sherwood Refractories, Inc. | Cores for investment casting process |
| US4989664A (en) * | 1988-07-07 | 1991-02-05 | United Technologies Corporation | Core molding composition |
| CN1793011A (en) * | 2005-11-29 | 2006-06-28 | 辽宁省轻工科学研究院 | Composite ceramic core material adopting nano silicon dioxide |
| CN1830774A (en) * | 2005-09-15 | 2006-09-13 | 成都理工大学 | Method of preparing high purity spherical nanometer noncrystalline silicon micropowder using natural powder quartz |
| CN101033068A (en) * | 2007-02-13 | 2007-09-12 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN102079653A (en) * | 2010-12-06 | 2011-06-01 | 北京航空航天大学 | Method for producing silicon-based ceramic core for aircraft engine blade |
-
2011
- 2011-10-13 CN CN201110309780.4A patent/CN103043668B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4093017A (en) * | 1975-12-29 | 1978-06-06 | Sherwood Refractories, Inc. | Cores for investment casting process |
| US4989664A (en) * | 1988-07-07 | 1991-02-05 | United Technologies Corporation | Core molding composition |
| CN1830774A (en) * | 2005-09-15 | 2006-09-13 | 成都理工大学 | Method of preparing high purity spherical nanometer noncrystalline silicon micropowder using natural powder quartz |
| CN1793011A (en) * | 2005-11-29 | 2006-06-28 | 辽宁省轻工科学研究院 | Composite ceramic core material adopting nano silicon dioxide |
| CN101033068A (en) * | 2007-02-13 | 2007-09-12 | 袁茂豪 | Method of preparing high-purity ultra-fine sphere silicon micro-powder |
| CN102079653A (en) * | 2010-12-06 | 2011-06-01 | 北京航空航天大学 | Method for producing silicon-based ceramic core for aircraft engine blade |
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Address after: 110043 Dong TA street, Dadong District, Shenyang, Liaoning Province, No. 6 Patentee after: Chinese Hangfa Shenyang Liming Aero engine limited liability company Address before: 110043 Dong TA street, Dadong District, Shenyang, Liaoning Province, No. 6 Patentee before: Liming Aeroplane Engine (Group) Co., Ltd., Shenyang City |