CN102601307B - Preparation method of shell mold for investment casting of TiAl based alloy - Google Patents
Preparation method of shell mold for investment casting of TiAl based alloy Download PDFInfo
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Abstract
The invention relates to a preparation method of a shell mold for investment casting of a TiAl based alloy, and belongs to the technical field of precision casting. The preparation method comprises the following steps that: firstly, ZrO2 and zirconia sol are prepared into a slurry; after the slurry is coated with a wax pattern, ZrO2 sand with a particle degree of 120 to 180 meshes is spread; Al2O3 and ethyl silicate hydrolyzate are prepared into a slurry, and then after the slurry is coated with a mold shell, Al2O3 sand with a particle degree of 60 to 90 meshes is spread, the slurry coating and the sand spreading are repeated for several times, the sand is Al2O3 sand with the particle degree of 40 to 50, 20 to 30, and 6 to 10 meshes sequentially, and drying is carried out; and dewaxing and roasting are carried out. The preparation method has the advantages that: the strength of the mold shell is sufficient, the production cycle is short, the quality of the inner surface of the mold shell is good, the reaction between TiAl based alloy castings and the mold shell is small after casting, and the castings have high surface quality.
Description
Technical field
The invention belongs to the precision casting technology field, be specifically related to a kind of preparation method of model casting TiAl base alloy shell mould.
Background technology
TiAl base alloy has high strength, low-density, high elastic modulus, the advantages such as non-oxidizability and croop property are good, being a kind of very potential lightweight high-temperature structural material, is the class alloy [E.A.Loria.Quo vadis gamma titanium aluminide.Intermetallics.2001.9:997-1001] developed rapidly in the titanium casting field in the last few years.TiAl base alloy is expected to for the wing of the high temperature resistant component of the Aero-Space such as jet engine and turbine, auto industry and super speed vehicle, housing etc., be considered to have most the lightening fire resistant structural material [Li Jinshan of new generation of application potential, Zhang Tiebang, progress and the development trend of the .TiAl base intermetallic compounds such as Chang Hui. Chinese material progress .201029 (3): 1～2; Xinhua Wu.Review of alloy and process development of TiAl alloys.Intermetallics 14 (2006): 1114-1122].
Because TiAl base Alloy At Room Temperature plasticity is poor, obvious brittleness at room temperature is arranged, percentage elongation less than 1% in its drawing process, and in hot procedure, crystal grain can sharply be grown up, and causes further embrittlement, so machinability is very poor, and its application is met difficulty.
In view of the characteristic of TiAl base alloy, forging molding had obviously not only been required great effort but also waste material, particularly when making some complex-shaped parts, seemed especially unable to do what one wishes.So casting just naturally becomes the processing method that is suitable for TiAl base alloy, particularly nearly clean formation type technology---precision-investment casting.In the last few years, the type shell material of TiAl alloy precision commonly used casting had: 1. Delanium; 2. refractory metal (powder such as tungsten, molybdenum, niobium); 3. special type fire oxide (ZrO
2With some rare-earth oxides and calcium oxide thereof etc.), using more is the special type fire oxide widely.ZrO
2The ceramic shell thermal conductivity is low, and intensity is high, the titanium alloy casting of pourable high-quality.Its advantage is, for the molten titanium alloy, better chemical stability arranged, and particularly, by after appropriate grain size distribution, surface quality of continuous castings significantly improved.Due to ZrO
2What have has a superior function, and now also maximum to its research, much research has all concentrated on raising ZrO
2On surface layer shell mould performance.
Summary of the invention
The purpose of this invention is to provide a kind of easy to make, sufficient intensity is arranged and has than the preparation method of the formwork of high chemical stability for molten condition TiAl base alloy, adopt the method can meet the requirement of preparation TiAl base alloy component.
Technical scheme of the present invention is:
The preparation method of the formwork that a kind of model casting TiAl base alloy is used, is characterized in that, comprises that step is as follows:
1) by granularity be 300～400 purpose ZrO
2Powder and zirconium colloidal sol are within 2.5: 1～3.5: 1, to be configured to the slurry that room temperature flow cup viscosity is 40～55 seconds by powder liquor ratio g/ml;
2) above-mentioned slurry is coated on wax-pattern, spreading granularity is 120～180 purpose ZrO
2Sand, drying; Adopt 800～1100 purpose Al
2O
3Sand and silicate hydrolyzate liquid, by weight within 2.2: 1～2.4: 1, being configured to the slurry that room temperature flow cup viscosity is 35～55 seconds, apply the 2nd layer, and the stucco granularity is 60～90 purpose Al
2O
3Sand, ammonia is dry, drying;
3) slurry coating step 2 then), then to spread granularity be 30～50 purpose Al
2O
3Sand, repetitive coatings slurry and stucco successively, prepare 3rd～4 layers, and ammonia is dry, drying; Then coating step 2 again) slurry, spreading granularity is 16～25 purpose Al
2O
3Be coated with, and repetitive coatings slurry and stucco prepare 5th～7 layers successively, ammonia is dry, drying; Last coating step 2) slurry, and spread 6～10 purpose Al
2O
3Sand prepares last one deck, immerses hardening agent, drying;
4) dewaxing, sintering.
Wherein, Al
2O
3For the electric smelting Al through calcining
2O
3The mixed liquor that the composition of silicate hydrolyzate liquid is ethyl orthosilicate, water, absolute ethyl alcohol, hydrochloric acid and boric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g: boric acid g is (800-1200): (150-180): (600-650): (8-10): (3-4); The mixed liquor that the composition of hardening agent is ethyl orthosilicate, water, absolute ethyl alcohol and hydrochloric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g is (800-1200): (150-180): (600-650): (4-6).
Step 1) also add wetting agent, defoamer in described slurry preparation process, wherein to account for the weight percentage of slurry be 1～3 ‰ to wetting agent, and the percentage by weight that defoamer accounts for slurry is 3～5 ‰, and wherein wetting agent is n-octyl alcohol; Zirconium colloidal sol limit is stirred by ZrO in limit
2Powder adds, and then add wetting agent successively, defoamer, stir more than 2 hours, but place coating after 12 hours.
Step 2) concrete steps and 3) are preferably: wax-pattern is immersed in above-mentioned slurry, soaks 5～10 seconds, during rotate wax-pattern in case coating to cover type even, take out the wax-pattern rear overhang and put 3～5 seconds, the unnecessary coating that pours off, spread the ZrO that granularity is 120～180 order numbers
2Sand, be 25～27 ℃ in temperature, dry more than 12 hours under the environment that humidity is 50～70%, forms surface layer; Al with 800～1100 order numbers
2O
3Sand and silicate hydrolyzate liquid by weight within 2.2: 1～2.4: 1, being configured to the slurry that room temperature flow cup viscosity is 35～55 seconds, are coated with the 2nd layer, and mode is to be coated with ground floor similar, and spreading granularity is 60～90 purpose Al
2O
3Sand, be 25～27 ℃ in temperature, under the environment that humidity is 50～70% air-dry 15～30 minutes, then the shell mould is put into to enclosed environment, and place ammoniacal liquor, ammonia concn is 40%, preferred every 1m
3Corresponding 10ml ammoniacal liquor, carry out ammonia dry 15～45 minutes, and purpose is to make the shell quick-hardening; After ammonia is dry, then to be placed on temperature be 25～27 ℃, under the ventilated environment that humidity is 50～70% dry 15～20 minutes; Then adopt identical method, apply 800～1100 purpose Al
2O
3The slurry that sand and silicate hydrolyzate liquid form, spreading granularity is 35～45 purpose Al
2O
3Sand is coated with 3rd～4 layers, drying, and ammonia is dry, drying; Spreading granularity is 20～30 purpose Al
2O
3Be coated with 5th～7 layers, drying, ammonia is dry, drier; Finally spreading granularity is the electric smelting Al after 6～10 purpose calcinings
2O
3Sand, drying, ammonia is dry, then the shell mould is soaked 2～3 minutes in hardening agent, in ventilation, puts 7～12 hours.
Step 3), shell mould after steam dewaxing or warm water dewaxing is placed after 1～2 hour and is carried out sintering, sintering process is for being heated to 400～500 ℃ of insulations 1～1.5 hour, be heated to again 700～800 ℃ of insulations 1～1.5 hour, finally be heated to 900～1100 ℃ of insulations 1～2 hour, can take out after being cooled to room temperature.
Advantage of the present invention:
1, the ZrO that the present invention adopts
2As surface material, ZrO
2Have heat endurance and chemical stability preferably with respect to molten state TiAl base alloy, the foundry goods cast out has high surface quality and surface smoothness.
2, the backing layer type shell material that the present invention adopts is Al
2O
3Sand, the emergy low price, fusing point is high, good heat conductivity, thermal coefficient of expansion is little.
3, backing layer binding agent of the present invention is homemade silicate hydrolyzate liquid, and this hydrolyzate is easy to make, and the holding time is long, nontoxic, and the formwork after making has enough intensity.
4, the present invention's surface layer refractory material used granularity that sands is 120～180 purpose ZrO
2Fine sand, form the highly polished surface layer of compact surfaces, can play to reinforce surface layer and can prevent that again larger sand grains from penetrating surface layer slurry and causing mo(U)ld face coarse.
5, the present invention adds ammonia to do dry run between the shell dry period, and greatly shortened drying time, has improved shell efficiency processed.
The specific embodiment
In following examples, ethyl orthosilicate is (with SiO
2Meter) the 28% zirconium colloidal sol place of production: this promise New Chemical Material science and technology Co., Ltd of Dalian, room temperature is 25 ℃.
Embodiment 1
1) under room temperature by granularity, be 325 purpose ZrO
2With zirconium colloidal sol 3: 1 (g/ml) proportional arrangement form slurry of pressing the powder liquor ratio, then add n-octyl alcohol and defoamer, the percentage by weight of two kinds of additives is respectively 3 ‰, 5 ‰, in zirconium colloidal sol whipping process, adds ZrO
2Powder, n-octyl alcohol, defoamer (commercialization), then stir 1.5 hours, and standing 24 hours, at this moment the viscosity of slurry was flow cup viscosity 49 seconds.
2) wax-pattern is immersed in coating to 8 seconds also fine rotation, make slurry cover wax-pattern fully, wax-pattern is taken out, vacant 5 seconds, unnecessary slurry is flowed away, and guarantee last slurry uniform fold wax-pattern on wax-pattern, spreading granularity is 120 purpose ZrO
2Sand, as surface layer, is then 25 ℃ in temperature, under the non-negotiable environment that humidity is 65%, places 12 hours.By granularity, be the electric smelting Al after 800 purposes are calcined
2O
3By with silicate hydrolyzate liquid weight ratio, pouring silicate hydrolyzate liquid in stirring and continuous stirring at 2.2: 1 1.5 hours, after stirring, flow cup viscosity is 43 seconds; Shell is immersed in slurry, place 8 seconds, and slight rotation, take out shell, vacant 2 seconds, spreading granularity was the electric smelting Al after 70 purpose calcinings
2O
3Sand, then being placed on temperature is 25 ℃, 20 minutes, micro-ventilation that humidity is 65%; Put into that to contain ammonia concn be 40% closed cabinet 15 minutes; Be placed into the place 10 minutes of ventilation, this is the 2nd layer; Then spreading granularity is the electric smelting Al after 40 purpose calcinings
2O
3Sand, and, under above same steps as, be coated with 3～4 layers; Spreading granularity is the electric smelting Al after 20 purpose calcinings
2O
3Sand, repeat identical coating step, is coated with 5～7 layers, and finally spreading granularity is the electric smelting Al after 5 purpose calcinings
2O
3Sand after repeating same steps as, finally soaks 3 minutes in hardening agent again, then dry 12 hours
Model is put in heating furnace and is heated to 150 ℃, after dewaxing, place 2 hours, then carry out sintering, sintering method is 450 ℃ of insulations 1.5 hours, and 780 ℃ are incubated 1.5 hours, finally 980 ℃ of insulations 2 hours.When being as cold as room temperature, takes out by stove shell.The shell inner surface is smooth, and intensity is enough.After cast, TiAl base alloy-steel casting reacts little with formwork, has high surface quality.
The mixed liquor that the composition of above-mentioned silicate hydrolyzate liquid is ethyl orthosilicate, water, absolute ethyl alcohol, hydrochloric acid and boric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g: boric acid g is 800: 160: 600: 8: 4; The mixed liquor that the composition of hardening agent is ethyl orthosilicate, water, absolute ethyl alcohol and hydrochloric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g is 900: 180: 650: 4.
The formwork prepared with said method is carried out to the casting experiment of TiAl alloy, gained casting pouring surface quality is high, and without scab phenomenon, the shell collapsibility is good, intensity 3.5MPa.
Embodiment 2
3) by granularity be 400 purpose ZrO
2With zirconium colloidal sol 2.8: 1 (g/ml) proportional arrangement form slurry of pressing the powder liquor ratio, then add n-octyl alcohol and defoamer, the percentage by weight of two kinds of additives is respectively 1 ‰, 3 ‰, in zirconium colloidal sol whipping process, adds ZrO
2Powder, n-octyl alcohol, defoamer, then stir 1 hour, and standing 24 hours, at this moment the viscosity of slurry was flow cup viscosity 58 seconds.
4) wax-pattern is immersed in coating to 8 seconds also fine rotation, make slurry cover wax-pattern fully, wax-pattern is taken out, vacant 5 seconds, unnecessary slurry is flowed away, and guarantee last slurry uniform fold wax-pattern on wax-pattern, spreading granularity is 100 purpose ZrO
2Sand, as surface layer, is then 28 ℃ in temperature, under the non-negotiable environment that humidity is 70%, places 12 hours.By granularity, be the electric smelting Al after 1100 purposes are calcined
2O
3By with silicate hydrolyzate liquid weight ratio, pouring silicate hydrolyzate liquid in stirring and continuous stirring at 2.4: 11 hour, after stirring, flow cup viscosity is 38 seconds; Shell is immersed in slurry, place 5 seconds, and slight rotation, take out shell, vacant 2 seconds, spreading granularity was the electric smelting Al after 80 purpose calcinings
2O
3Sand, then being placed on temperature is 28 ℃, 15 minutes, micro-ventilation that humidity is 70%; Put into that to contain ammonia concn be 40% closed cabinet 15 minutes; Be placed into the place 15 minutes of ventilation, this is the 2nd layer; Then spreading granularity is the electric smelting Al after 50 purpose calcinings
2O
3Sand, and, under above same steps as, be coated with 3～4 layers; Spreading granularity is the electric smelting Al after 30 purpose calcinings
2O
3Sand, repeat same steps as, is coated with 5～7 layers, and finally spreading granularity is the electric smelting Al after 4 purpose calcinings
2O
3Sand after repeating same steps as, finally soaks 2 minutes in hardening agent again, then dry 12 hours
5) model is put in heating furnace and is heated to 150 ℃, after dewaxing, place 2 hours, then carry out sintering, sintering method is 400 ℃ of insulations 2 hours, and 800 ℃ are incubated 2 hours, finally 900 ℃ of insulations 2 hours.When being as cold as room temperature, takes out by stove shell.The shell inner surface is smooth, and intensity is enough 4.0MPa.
The mixed liquor that the composition of silicate hydrolyzate liquid is ethyl orthosilicate, water, absolute ethyl alcohol, hydrochloric acid and boric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g: boric acid g is 1000: 170: 630: 10: 3.5; The mixed liquor that the composition of hardening agent is ethyl orthosilicate, water, absolute ethyl alcohol and hydrochloric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g is 1100: 165: 645: 5.The formwork inner surface quality is good, and after cast, TiAl base alloy-steel casting reacts little with formwork, has high surface quality.
Claims (2)
1. the preparation method of a model casting TiAl base alloy shell mould, is characterized in that, comprises the following steps:
1) under room temperature by granularity, be 325 purpose ZrO
2Press powder liquor ratio 3:1 (g/ml) proportional arrangement form slurry with zirconium colloidal sol, then add n-octyl alcohol and defoamer, the percentage by weight of two kinds of additives is respectively 3 ‰, 5 ‰, in zirconium colloidal sol whipping process, adds ZrO
2Powder, n-octyl alcohol, defoamer, then stir 1.5 hours, and standing 24 hours, at this moment the viscosity of slurry was flow cup viscosity 49 seconds;
2) wax-pattern is immersed in coating to 8 seconds also fine rotation, make slurry cover wax-pattern fully, wax-pattern is taken out, vacant 5 seconds, unnecessary slurry is flowed away, and guarantee last slurry uniform fold wax-pattern on wax-pattern, spreading granularity is 120 purpose ZrO
2Sand, as surface layer, is then 25 ℃ in temperature, under the non-negotiable environment that humidity is 65%, places 12 hours, and by granularity, be the electric smelting Al after 800 purposes are calcined
2O
3By with silicate hydrolyzate liquid weight ratio 2.2:1, pouring silicate hydrolyzate liquid in stirring and continuous stirring into 1.5 hours, after stirring, flow cup viscosity is 43 seconds; Shell is immersed in slurry, place 8 seconds, and slight rotation, take out shell, vacant 2 seconds, spreading granularity was the electric smelting Al after 70 purpose calcinings
2O
3Sand, then being placed on temperature is 25 ℃, 20 minutes, micro-ventilation that humidity is 65%; Put into that to contain ammonia concn be 40% closed cabinet 15 minutes; Be placed into the place 10 minutes of ventilation, this is the 2nd layer; Then spreading granularity is the electric smelting Al after 40 purpose calcinings
2O
3Sand, and, under above same steps as, be coated with 3～4 layers; Spreading granularity is the electric smelting Al after 20 purpose calcinings
2O
3Sand, repeat identical coating step, is coated with 5～7 layers, and finally spreading granularity is the electric smelting Al after 5 purpose calcinings
2O
3Sand after repeating same steps as, finally soaks 3 minutes in hardening agent again, then dry 12 hours;
Model is put in heating furnace and is heated to 150 ℃, after dewaxing, place 2 hours, then carry out sintering, sintering method is 450 ℃ of insulations 1.5 hours, and 780 ℃ are incubated 1.5 hours, finally 980 ℃ of insulations 2 hours, takes out shell when stove is as cold as room temperature;
The mixed liquor that the composition of above-mentioned silicate hydrolyzate liquid is ethyl orthosilicate, water, absolute ethyl alcohol, hydrochloric acid and boric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g: boric acid g is 800:160:600:8:4; The mixed liquor that the composition of hardening agent is ethyl orthosilicate, water, absolute ethyl alcohol and hydrochloric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g is 900:180:650:4, and ethyl orthosilicate is with SiO
2Count 28%.
2. the preparation method of a model casting TiAl base alloy shell mould, is characterized in that, comprises the following steps:
1) by granularity be 400 purpose ZrO
2Press powder liquor ratio 2.8:1 (g/ml) proportional arrangement form slurry with zirconium colloidal sol, then add n-octyl alcohol and defoamer, the percentage by weight of two kinds of additives is respectively 1 ‰, 3 ‰, in zirconium colloidal sol whipping process, adds ZrO
2Powder, n-octyl alcohol, defoamer, then stir 1 hour, and standing 24 hours, at this moment the viscosity of slurry was flow cup viscosity 58 seconds;
2) wax-pattern is immersed in coating to 8 seconds also fine rotation, make slurry cover wax-pattern fully, wax-pattern is taken out, vacant 5 seconds, unnecessary slurry is flowed away, and guarantee last slurry uniform fold wax-pattern on wax-pattern, spreading granularity is 100 purpose ZrO
2Sand, as surface layer, is then 28 ℃ in temperature, under the non-negotiable environment that humidity is 70%, places 12 hours, and by granularity, be the electric smelting Al after 1100 purposes are calcined
2O
3By with silicate hydrolyzate liquid weight ratio 2.4:1, pouring silicate hydrolyzate liquid in stirring and continuous stirring into 1 hour, after stirring, flow cup viscosity is 38 seconds; Shell is immersed in slurry, place 5 seconds, and slight rotation, take out shell, vacant 2 seconds, spreading granularity was the electric smelting Al after 80 purpose calcinings
2O
3Sand, then being placed on temperature is 28 ℃, 15 minutes, micro-ventilation that humidity is 70%; Put into that to contain ammonia concn be 40% closed cabinet 15 minutes; Be placed into the place 15 minutes of ventilation, this is the 2nd layer; Then spreading granularity is the electric smelting Al after 50 purpose calcinings
2O
3Sand, and, under above same steps as, be coated with 3～4 layers; Spreading granularity is the electric smelting Al after 30 purpose calcinings
2O
3Sand, repeat same steps as, is coated with 5～7 layers, and finally spreading granularity is the electric smelting Al after 4 purpose calcinings
2O
3Sand after repeating same steps as, finally soaks 2 minutes in hardening agent again, then dry 12 hours;
3) model is put in heating furnace and is heated to 150 ℃, after dewaxing, place 2 hours, then carry out sintering, sintering method is 400 ℃ of insulations 2 hours, and 800 ℃ are incubated 2 hours, finally 900 ℃ of insulations 2 hours, takes out shell when stove is as cold as room temperature;
The mixed liquor that the composition of silicate hydrolyzate liquid is ethyl orthosilicate, water, absolute ethyl alcohol, hydrochloric acid and boric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g: boric acid g is 1000:170:630:10:3.5; The mixed liquor that the composition of hardening agent is ethyl orthosilicate, water, absolute ethyl alcohol and hydrochloric acid, it is ethyl orthosilicate ml with magnitude relation: water ml: absolute ethyl alcohol ml: concentrated hydrochloric acid g is 1100:165:645:5, and ethyl orthosilicate is with SiO
2Count 28%.
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| CN105642831B (en) * | 2016-01-27 | 2017-12-08 | 北京工业大学 | A kind of formwork for being used for TiAl-base alloy hot investment casting or directional solidification and the method for preparing the formwork |
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