CN104788106A - Manufacturing method of crucible for vacuum induction melting of high-temperature alloy - Google Patents
Manufacturing method of crucible for vacuum induction melting of high-temperature alloy Download PDFInfo
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Abstract
The invention provides a manufacturing method of a crucible for vacuum induction melting of a high-temperature alloy; the manufacturing method comprises the steps: 1) preparing a raw material by mixing fused alumina zirconia having the particle size of 1-4 mm, fused alumina zirconia having the particle size of 0.1-1 mm, fused alumina zirconia having the particle size of less than 0.1 mm, bimodal activated alpha-alumina and nanocrystalline alpha-alumina with the mass percentage of (15-40):(15-40):(15-40):(3-8):(3-8), and then mixing the raw material with ammonium polyacrylate and a binder to obtain a slurry, wherein the addition amounts of ammonium polyacrylate and the binder are respectively 0.5-2% and 5-15% of the total mass of the raw material; 2) adding a water-soluble azo or piperidine initiator with the amount of 0.1-0.3% of the total mass of the slurry into the slurry, and mixing for 3-10 min at the temperature of 2-30 DEG C; 3) carrying out vacuum degassing on the slurry obtained in the step 2) for 5 min at the temperature of 2-30 DEG C, and then immediately pouring into a crucible forming mold; 4) heating together with the mold to 45-55 DEG C, keeping for 5-35 min, then demolding, and drying a crucible blank at room temperature; and 5) placing the crucible blank at the temperature of 1500-1650 DEG C, keeping for more than 3 h, then cooling to room temperature, and thus obtaining the target object. The crucible prepared by the method has low content of impurity elements during melting of the high-temperature alloy.
Description
Technical field
The present invention relates to a kind of manufacture method of vacuum induction melting superalloy crucible, belong to metallurgical technology field.
Background technology
Key part when crucible is vacuum induction melting superalloy.Under high temperature and vacuum condition, between crucible and superalloy melt, various physics chemical action can occur, result will cause that crucible material is etched, melt is contaminated.Therefore, require that crucible material should have good chemical stability.Meanwhile, crucible in use periodically stands the effect of heating and cooling, produces and expands and string stress, thus crack, cause melt leakage, therefore, require that crucible material has good thermal shock resistance in crucible inside.
The mechanical properties of impurity element on superalloy such as oxygen, nitrogen, sulphur, phosphorus have to be affected significantly.Nitrogen usually exists with the form of nitride or carbonitride in superalloy, these compounds are highly stable, can not melt in melt under common smelting temperature, for reducing the nitrogen content in superalloy, higher smelting temperature must be adopted, exacerbate so again the physics chemical action between crucible and melt further, cause and melt is polluted greatly.
At present, the crucible material mainly magnesia crucible that vacuum induction melting superalloy uses, but due to magnesium oxide under high temperature and high vacuum effect can by superalloy in carbon, aluminium, titanium, niobium, chromium isoreactivity element reduce and pollute alloy, be difficult to the purity reducing superalloy further.For overcoming the shortcoming of magnesia crucible, testing and adopting the higher calcareous crucible for smelting superalloy of oxidation of stability at elevated temperature, but there is easy aquation, not easy-formation and high in cost of production shortcoming due to calcium oxide, do not obtain industrial applications.Pure corundum (aluminum oxide) matter crucible chemical stability is good, at high temperature chemical reaction can not occur with superalloy melt, can be used for the high-purity superalloy of melting.But due to existing pure corundum crucible, its thermal shock resistance is poor, easy to crack, can't as vacuum induction melting superalloy crucible.For overcoming the deficiency of pure corundum crucible, Chinese patent (ZL 201210440801.0) discloses a kind of corundum spinel crucible and preparation method thereof, because the high volume stability of magnesium-aluminium spinel and thermal shock resistance are all better than magnesia material, heat-shock resistance is better than corundum, resistance to fouling and oxidation-reduction resistance are better than mullite, with the crucible that it is prepared, there is excellent applied at elevated temperature performance, but the composition still containing purer corundum stability at elevated temperature difference in its composition exists.
Summary of the invention
The object of this invention is to provide a kind of manufacture method of vacuum induction melting superalloy crucible that can overcome above-mentioned defect, excellent working performance, its technical scheme is:
A manufacture method for vacuum induction melting superalloy crucible, is characterized in that comprising the following steps:
1) feed composition is by mass percentage: the zircon corundum 15-40% that the zircon corundum 15-40% that particle size is 1-4mm, particle size are 0.1-1mm, particle size are zircon corundum 15-40%, the bimodal activity Alpha-alumina 3-8% of below 0.1mm and nanocrystalline Alpha-alumina 3-8%; Dispersion agent is ammonium polyacrylate; Bonding agent is the mixed aqueous solution of acrylamide and N, N '-methylene-bisacrylamide, and the mass ratio of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%; Raw material, dispersion agent, bonding agent are mixed with the mass ratio of 100:0.5-2:5-15 and obtains slurry;
2) by step 1) add initiator in the slurry that obtains, at 2-30 DEG C of mixing 3-10min, initiator is water-soluble azo class or piperidines initiator, and add-on is the 0.1-0.3% of slurry total mass;
3) by step 2) slurry that obtains is after 2-30 DEG C of vacuum outgas 5min, and pour into crucible forming mould immediately, wherein devolatilization vacuum degree is less than 10Pa;
4) be heated to 45-55 DEG C together with mould and keep the demoulding after 5-35min, by crucible base substrate drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1500-1650 DEG C, hold-time more than 3h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
The present invention compared with prior art, its advantage is: vacuum induction melting superalloy crucible disclosed by the invention selects zircon corundum to be raw material, adopt special technique casting, the composition of finished product crucible is the monoclinic phase m-ZrO2 of the α-Al2O3 of corundum structure, the Tetragonal t-ZrO2 of square structure and monocline mutually, stability at elevated temperature and thermal shock resistance good; The adjuvant used not sulfur-bearing of shaping crucible and phosphorus, can not increase sulphur and phosphorus to melt during melting superalloy; Add bimodal activity Alpha-alumina and nanocrystalline Alpha-alumina, and burn till through 1500-1650 DEG C of high temperature, bonding strength is high, and anti-melt scouring capability is strong.Adopt crucible for smelting superalloy of the present invention, can carry out more than 1700 DEG C melt pyroprocessing, the impurity content such as ALLOY O, N, S, P of melting is low.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
The quality proportioning of each embodiment Raw is in table 1.
Execute example 1
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 0.5% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 5% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 30 DEG C of mixing 3min, initiator is water-soluble 2,2'-diazo salt hydrochlorates, and add-on is 0.3% of slurry total mass;
3) by step 2) slurry that obtains at 30 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 9Pa;
4) be heated to 45 DEG C together with mould and keep the demoulding after 30min, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1650 DEG C, hold-time 3.5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 2
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 1.5% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 10% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 25 DEG C of mixing 6min, initiator is piperidine hydrochlorate, and add-on is 0.2% of slurry total mass;
3) by step 2) slurry that obtains at 25 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 8Pa;
4) be heated to 50 DEG C together with mould and keep the 35min demoulding, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1600 DEG C, hold-time 4h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 3
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 2% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 15% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 20 DEG C of mixing 8min, initiator is 2,2'-diazo salt hydrochlorate, and add-on is 0.15% of slurry total mass;
3) by step 2) slurry that obtains at 20 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 7Pa;
4) be heated to 55 DEG C together with mould and keep the 35min demoulding, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1500 DEG C, hold-time 5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 4
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 1% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 8% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 15 DEG C of mixing 10min, initiator is piperidine hydrochlorate, and add-on is 0.1% of slurry total mass;
3) by step 2) slurry that obtains at 15 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 6Pa;
4) be heated to 55 DEG C together with mould and keep the 35min demoulding, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1550 DEG C, hold-time 5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 5
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 1.5% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 12% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 15 DEG C of mixing 10min, initiator is 2,2'-diazo salt hydrochlorate, and add-on is 0.2% of slurry total mass;
3) by step 2) slurry that obtains at 15 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 6Pa;
4) be heated to 50 DEG C together with mould and keep the 20min demoulding, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1580 DEG C, hold-time 5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 6
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 2% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 10% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 25 DEG C of mixing 5min, initiator is piperidine hydrochlorate, and add-on is 0.25% of slurry total mass;
3) by step 2) slurry that obtains at 25 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 9Pa;
4) be heated to 45 DEG C together with mould and keep the 30min demoulding, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1650 DEG C, hold-time 5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 7
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 2% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 8% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 30 DEG C of mixing 8min, initiator is 2,2'-diazo salt hydrochlorate, and add-on is 0.2% of slurry total mass;
3) by step 2) slurry that obtains at 30 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 9Pa;
4) be heated to 50 DEG C together with mould and keep the demoulding after 15min, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1600 DEG C, hold-time 3.5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 8
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 1.5% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 10% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 2 DEG C of mixing 3min, initiator is piperidine hydrochlorate, and add-on is 0.2% of slurry total mass;
3) by step 2) slurry that obtains at 2 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 5Pa;
4) be heated to 50 DEG C together with mould and keep the demoulding after 20min, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1620 DEG C, hold-time 4h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 9
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 2% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 10% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 10 DEG C of mixing 5min, initiator is 2,2'-diazo salt hydrochlorate, and add-on is 0.2% of slurry total mass;
3) by step 2) slurry that obtains at 10 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 9Pa;
4) be heated to 50 DEG C together with mould and keep the demoulding after 15min, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1500 DEG C, hold-time 5h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Embodiment 10
The manufacture of vacuum induction melting superalloy crucible comprises the following steps:
1) after weighing by the proportioning of table 1 and dispersion agent and bonding agent be mixed to get uniform slurry, dispersion agent used is ammonium polyacrylate, add-on is 1.5% of raw material total mass, bonding agent is acrylamide and N, the mixed aqueous solution of N '-methylene-bisacrylamide, the quality proportioning of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%, and the add-on of bonding agent is 12% of raw material total mass;
2) by step 1) add initiator in the slurry that obtains, at 15 DEG C of mixing 7min, initiator is piperidine hydrochlorate, and add-on is 0.2% of slurry total mass;
3) by step 2) slurry that obtains at 15 DEG C of vacuum outgas 5min, pour into crucible forming mould immediately, wherein devolatilization vacuum degree 8Pa;
4) be heated to 50 DEG C together with mould and keep the demoulding after 5min, then in drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1650 DEG C, hold-time 4h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
Adopt embodiment make crucible carries out vacuum induction melting, vacuum pouring nickel-base cast superalloy K417 test, in fusion process employing 1750 DEG C of melt pyroprocessing.Sample from the alloy pig of cast, adopt TC-436 oxygen-nitrogen analyzer to analyze oxygen and nitrogen content, the results are shown in Table 2.Visible, adopt the gas content in the nickel-base cast superalloy of crucible for smelting of the present invention very low.
The proportioning (mass percent) of each embodiment Raw of table 1
Table 2 adopts the oxygen and nitrogen content (× 0.0001%, mass percent) in the nickel-base cast superalloy K417 of crucible vacuum induction melting of the present invention
| Embodiment | Oxygen | Nitrogen |
| Embodiment 1 | 4 | 3 |
| Embodiment 2 | 6 | 5 |
| Embodiment 3 | 5 | 4 |
| Embodiment 4 | 6 | 5 |
| Embodiment 5 | 5 | 4 |
| Embodiment 6 | 4 | 3 |
| Embodiment 7 | 6 | 5 |
| Embodiment 8 | 5 | 4 |
| Embodiment 9 | 6 | 5 |
| Embodiment 10 | 6 | 3 |
Claims (1)
1. a manufacture method for vacuum induction melting superalloy crucible, is characterized in that comprising the following steps:
1) feed composition is by mass percentage: the zircon corundum 15-40% that the zircon corundum 15-40% that particle size is 1-4mm, particle size are 0.1-1mm, particle size are zircon corundum 15-40%, the bimodal activity Alpha-alumina 3-8% of below 0.1mm and nanocrystalline Alpha-alumina 3-8%; Dispersion agent is ammonium polyacrylate; Bonding agent is the mixed aqueous solution of acrylamide and N, N '-methylene-bisacrylamide, and the mass ratio of the two is 10:1, and the total mass percent concentration of mixed aqueous solution is 14%; Raw material, dispersion agent, bonding agent are mixed with the mass ratio of 100:0.5-2:5-15 and obtains slurry;
2) by step 1) add initiator in the slurry that obtains, at 2-30 DEG C of mixing 3-10min, initiator is water-soluble azo class or piperidines initiator, and add-on is the 0.1-0.3% of slurry total mass;
3) by step 2) slurry that obtains is after 2-30 DEG C of vacuum outgas 5min, and pour into crucible forming mould immediately, wherein devolatilization vacuum degree is less than 10Pa;
4) be heated to 45-55 DEG C together with mould and keep the demoulding after 5-35min, by crucible base substrate drying at room temperature;
5) dried crucible base substrate is placed in kiln to sinter, sintering temperature is 1500-1650 DEG C, hold-time more than 3h, is then cooled to room temperature and obtains vacuum induction melting superalloy crucible.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112809010A (en) * | 2020-12-29 | 2021-05-18 | 辽宁冠达新材料科技有限公司 | Preparation method of GH5188 cobalt-based high-temperature alloy powder for 3D printing |
| CN113480295A (en) * | 2021-08-04 | 2021-10-08 | 中钢集团洛阳耐火材料研究院有限公司 | Ceramic crucible for nickel-based high-temperature alloy and preparation method |
| CN116177999A (en) * | 2022-12-16 | 2023-05-30 | 中航装甲科技有限公司 | Alumina crucible for high-temperature alloy smelting and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112809010A (en) * | 2020-12-29 | 2021-05-18 | 辽宁冠达新材料科技有限公司 | Preparation method of GH5188 cobalt-based high-temperature alloy powder for 3D printing |
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| CN116177999A (en) * | 2022-12-16 | 2023-05-30 | 中航装甲科技有限公司 | Alumina crucible for high-temperature alloy smelting and preparation method thereof |
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