CN103451458B - Preparing method of nickel-silicon alloy cast ingot - Google Patents

Preparing method of nickel-silicon alloy cast ingot Download PDF

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CN103451458B
CN103451458B CN201310467928.6A CN201310467928A CN103451458B CN 103451458 B CN103451458 B CN 103451458B CN 201310467928 A CN201310467928 A CN 201310467928A CN 103451458 B CN103451458 B CN 103451458B
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silicon
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刘洋
侯军涛
郭磊
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Xi'an Refra Tungsten & Molybdenum Co Ltd
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Abstract

The invention provides a preparing method of a nickel-silicon alloy cast ingot. The preparing method includes the following steps that (1) a nickel bar and silicon powder are wrapped by a nickel foil and made into an alloy package after being mixed evenly, and then a smelted electrode is manufactured in a pressing mode; (2) first vacuum self-consuming electric arc melting is carried out to obtain a first ingot blank; (3) mass content of silicon in the first ingot blank is calculated; (4) the theoretical mass mSi of silicon needing to be added is calculated; (5) a blind hole is drilled in the first ingot blank, silicon powder with the mass ranging from 1.5mSi to 1.6mSi is added into the blind hole, and then secondary vacuum self-consuming electric arc melting is carried out to obtain a second ingot blank; (6) third vacuum self-consuming electric arc melting is carried out to obtain the nickel-silicon alloy cast ingot. The preparing method is low in production cost, simple in production process, strong in repeatability, high in yield, and suitable for large-scale industrial production. The nickel-silicon alloy cast ingot prepared through the method is accurate and controllable in silicon content, good in distribution uniformity and high in density.

Description

A kind of preparation method of nickel silicon alloy ingot casting
Technical field
The invention belongs to nickel silicon alloy technical field, be specifically related to a kind of preparation method of nickel silicon alloy ingot casting.
Background technology
Nickel silicon alloy is developed in the later stage thirties 20th century the earliest, and the mid-50 China starts to carry out correlative study and production.The mechanical property of nickel silicon alloy is high, hot and cold pressure good processability, excellent corrosion resistance, has chemical stability in air, fresh water and seawater, the corrosion of various neutral solution, slightly acidic solution and organic solvent can be tolerated, especially the excellent materials of alkali corrosion resistant.Nickel silicon alloy is widely used in the corrosion-resistant structure of machinery, chemical industry equipment in recent years, main as precision instrument structural part, electron tube and wireless apparatus part, medicine equipment and foodstuffs industry dinnerware.Modal nickel silicon alloy goods have Nickel-Silicom thermocouple and NSI3 type nickel silicon alloy pipe, bar etc.Along with China's national defense military project and aerospace demand, the component proportions of nickel silicon alloy and physicochemical property are had higher requirement.Therefore, and realistic meaning necessary to the research of nickel silicon alloy preparation technology is carried out.
Nickel silicon alloy generally adopts hot pressing sintering method, conbustion synthesis method of fusion or vacuum melting method to be prepared from.Wherein, hot pressing sintering method is loaded in mould nickel powder and silica flour, and then put into hot-pressed sintering furnace pressure sintering, products made thereby compactness is better, but high for the requirement of mould and equipment, and production cost is high.Conbustion synthesis method of fusion required equipment is simple, but products made thereby compactness is poor, and qualification rate is low.Vacuum melting method is lower to the requirement of equipment due to it, and products made thereby compactness is good, obtains increasingly extensive application.But traditional vacuum melting technique is fed intake by design mix at nickel and silicon, then form through secondary or three meltings, because the fusing point of silicon is lower than nickel, and there is very big-difference in the density of the density of silicon and nickel, make the volatilization of silicon in Vacuum Melting and loss larger, cause in nickel silicon alloy ingot casting that silicone content is too low, distributing homogeneity is poor, compactness is low, can not technical requirements be met.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of nickel silicon alloy ingot casting.The method preparation cost is low, and production technique is simple, and repeatable strong, yield rate is high, is suitable for industrialization scale operation; In the nickel silicon alloy ingot casting adopting the method to prepare, silicone content is accurately controlled, and distributing homogeneity is good, and compactness extent is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of nickel silicon alloy ingot casting, and it is characterized in that, the method comprises the following steps:
Step one, take nickel bar, silica flour and nickel foil according to the design mix of the nickel silicon alloy ingot casting of required preparation, nickel bar and silica flour are mixed rear nickel foil and carries out coated, make alloy bag, then utilize oil press alloy bag to suppress, obtain smelting electrode;
Step 2, smelting electrode described in step one is placed in vacuum consumable electrode arc furnace, is not more than 8.0 × 10 in vacuum tightness -2carry out first time vacuum consumable arc-melting under the condition of Pa, after water-cooled, take surface scale off, obtain the first ingot blank; Described first time, the smelting parameter of vacuum consumable arc-melting was: fusion current 800A ~ 950A, melting voltage 27V ~ 28V, stabilising arc electric current 5A ~ 6A;
Step 3, employing drainage record the density p of the first ingot blank described in step 2 niSi-1, then according to formula calculate the mass percentage x of silicon in the first ingot blank, wherein, ρ nifor the density of nickel, ρ sifor the density of silicon, ρ ni, ρ siand ρ niSi-1unit be g/cm 3;
Step 4, according to formula calculate the Theoretical Mass m that need add silicon si, wherein, y is the mass percentage of silicon in the nickel silicon alloy ingot casting that need prepare, m niSi-1be the quality of the first ingot blank, m siand m niSi-1unit be g;
Step 5, on the first ingot blank, being drilled with blind hole, is 1.5m by quality si~ 1.6m sisilica flour add in blind hole, then the first ingot blank being added with silica flour is placed in vacuum consumable electrode arc furnace, is not more than 8.0 × 10 in vacuum tightness -2carry out second time vacuum consumable arc-melting under the condition of Pa, after water-cooled, take surface scale off, obtain the second ingot blank; The smelting parameter of described second time vacuum consumable arc-melting is: fusion current 800A ~ 950A, melting voltage 27V ~ 28V, stabilising arc electric current 5A ~ 6A;
Step 6, the second ingot blank described in step 5 is placed in vacuum consumable electrode arc furnace, is not more than 8.0 × 10 in vacuum tightness -2carry out third time vacuum consumable arc-melting under the condition of Pa, after water-cooled, take surface scale off, obtain nickel silicon alloy ingot casting; In described nickel silicon alloy ingot casting, the mass percentage y of silicon is 4% ~ 15%, and surplus is nickel; Described third time, the smelting parameter of vacuum consumable arc-melting was: fusion current 800A ~ 950A, melting voltage 27V ~ 28V, stabilising arc electric current 5A ~ 6A.
The preparation method of above-mentioned a kind of nickel silicon alloy ingot casting, is characterized in that, described in step 2, the smelting parameter of vacuum consumable arc-melting is for the first time: fusion current 800A, melting voltage 28V, stabilising arc electric current 5.5A.
The preparation method of above-mentioned a kind of nickel silicon alloy ingot casting, is characterized in that, the smelting parameter of the vacuum consumable arc-melting of second time described in step 5 is: fusion current 850A, melting voltage 28V, stabilising arc electric current 5.8A.
The preparation method of above-mentioned a kind of nickel silicon alloy ingot casting, is characterized in that, described in step 6, the smelting parameter of vacuum consumable arc-melting is for the third time: fusion current 900A, melting voltage 28V, stabilising arc electric current 6.0A.
The present invention compared with prior art has the following advantages:
1, the present invention is by furtheing investigate in a large number the change of nisiloy content in each stage fusion process, and repeatedly regulates melting technology, and final optimization pass goes out the technical scheme of employing three vacuum consumable arc-meltings.Wherein, the present invention feeds intake according to design mix when first time melting, by controlling smelting parameter, can avoid, because nisiloy density difference occurs apart from excessive or the excessive problem causing ingot blank homogeneity to decline of melting whipping force, significantly reducing silicon loss simultaneously; During second time melting, the present invention fully takes into account the loss of silicon in fusion process, by adding suitably excessive silicon, and controls smelting parameter, and the hardness of the second ingot blank and compactness are greatly improved; During third time melting, the present invention, by controlling smelting parameter, makes the homogeneity of ingot blank, compactness and hardness be further enhanced, and finally obtains the nickel silicon alloy ingot casting that nisiloy content is accurate, good uniformity, compactness extent are high.
2, the present invention adopts conventional vacuum smelting equipment can prepare superior in quality nickel silicon alloy ingot casting, and production cost is low, and production technique is simple, repeatable strong, is suitable for industrialization scale operation.
3, the nickel silicon alloy ingot casting prepared of the present invention is without defects such as obvious segregation, shrinkage cavity, crackles, and superior in quality, homogeneous microstructure, yield rate is high.
4, generate without the pollutent such as spent acid, waste gas in preparation process of the present invention, clean environment firendly.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the present invention.
Embodiment
Embodiment 1
The preparation of composition graphs 1, Ni-11.15Si nickel silicon alloy ingot casting:
Step one, according to design mix (the i.e. mass ratio 88.85: 11.15 of nickel and silicon need preparing Ni-11.15Si nickel silicon alloy ingot casting, the mass percentage y=11.15% of silicon) take nickel bar, silica flour and nickel foil, again nickel bar and silica flour being mixed rear nickel foil carries out coated, make alloy bag, then utilize oil press alloy bag to suppress, obtain smelting electrode;
Step 2, smelting electrode described in step one is placed in vacuum consumable electrode arc furnace carries out first time vacuum consumable arc-melting, take surface scale off after water-cooled, obtaining diameter of section is Ф 50mm, quality m niSi-1first ingot blank of=3000g; Described first time vacuum consumable arc-melting smelting parameter in table 1;
Step 3, Archimedes' principle is utilized to record the density p of the first ingot blank described in step 2 niSi-1=7.36g/cm 3, then according to formula calculate the mass percentage x=7.43% of silicon in the first ingot blank, ρ in formula ni=8.902g/cm 3, ρ si=2.330g/cm 3;
Step 4, according to formula calculate the Theoretical Mass m that need add silicon si=125g;
Step 5, on the first ingot blank, be drilled with blind hole, then 195g silica flour is added in blind hole, then the first ingot blank being added with silica flour is placed in vacuum consumable electrode arc furnace and carries out second time vacuum consumable arc-melting, after water-cooled, take surface scale off, obtain the second ingot blank; The smelting parameter of described second time vacuum consumable arc-melting is in table 1;
Step 6, the second ingot blank described in step 5 is placed in vacuum consumable electrode arc furnace carries out third time vacuum consumable arc-melting, take surface scale off after water-cooled, obtain Ni-11.15Si nickel silicon alloy ingot casting; Described third time vacuum consumable arc-melting smelting parameter in table 1.
Table 1 embodiment of the present invention 1 vacuum consumable arc-melting parameter
The density adopting drainage to record the present embodiment Ni-11.15Si nickel silicon alloy ingot casting is 6.75g/cm 3, with the calculated theoretical density 6.77g/cm of Ni-11.15Si nickel silicon alloy 3closely, the mass percentage extrapolating silicon in ingot casting is thus 11.30%, and surplus is nickel.The present embodiment Ni-11.15Si nickel silicon alloy ingot casting is without defects such as obvious segregation, shrinkage cavity, crackles, and superior in quality, homogeneous microstructure, yield rate is high, and nisiloy content is accurately controlled, and analysis deviation is little, meets associated specifications.
Embodiment 2
The preparation of composition graphs 1, Ni-10Si nickel silicon alloy ingot casting:
Step one, according to design mix (the i.e. mass ratio 90: 10 of nickel and silicon need preparing Ni-10Si nickel silicon alloy ingot casting, the mass percentage y=10% of silicon) take nickel bar, silica flour and nickel foil, again nickel bar and silica flour being mixed rear nickel foil carries out coated, make alloy bag, then utilize oil press alloy bag to suppress, obtain smelting electrode;
Step 2, smelting electrode described in step one is placed in vacuum consumable electrode arc furnace carries out first time vacuum consumable arc-melting, take surface scale off after water-cooled, obtaining diameter of section is Ф 60mm, quality m niSi-1first ingot blank of=4000g; Described first time vacuum consumable arc-melting smelting parameter in table 2;
Step 3, Archimedes' principle is utilized to record the density p of the first ingot blank described in step 2 niSi-1=7.55g/cm 3, then according to formula calculate the mass percentage x=6.35% of silicon in the first ingot blank, ρ in formula ni=8.902g/cm 3, ρ si=2.330g/cm 3;
Step 4, according to formula calculate the Theoretical Mass m that need add silicon si=162g;
Step 5, on the first ingot blank, be drilled with blind hole, then 243g silica flour is added in blind hole, then the first ingot blank being added with silica flour is placed in vacuum consumable electrode arc furnace and carries out second time vacuum consumable arc-melting, after water-cooled, take surface scale off, obtain the second ingot blank; The smelting parameter of described second time vacuum consumable arc-melting is in table 2;
Step 6, the second ingot blank described in step 5 is placed in vacuum consumable electrode arc furnace carries out third time vacuum consumable arc-melting, take surface scale off after water-cooled, obtain Ni-10Si nickel silicon alloy ingot casting; Described third time vacuum consumable arc-melting smelting parameter in table 2.
Table 2 embodiment of the present invention 2 vacuum consumable arc-melting parameter
The density adopting drainage to record the present embodiment Ni-10Si nickel silicon alloy ingot casting is 6.91g/cm 3, with the calculated theoretical density 6.94g/cm of Ni-10Si nickel silicon alloy 3closely, the mass percentage extrapolating silicon in ingot casting is thus 10.22%, and surplus is nickel.The present embodiment Ni-10Si nickel silicon alloy ingot casting is without defects such as obvious segregation, shrinkage cavity, crackles, and superior in quality, homogeneous microstructure, yield rate is high, and nisiloy content is accurately controlled, and analysis deviation is little, meets associated specifications.
Embodiment 3
The preparation of composition graphs 1, Ni-15Si nickel silicon alloy ingot casting:
Step one, according to design mix (the i.e. mass ratio 85: 15 of nickel and silicon need preparing Ni-15Si nickel silicon alloy ingot casting, the mass percentage y=15% of silicon) take nickel bar, silica flour and nickel foil, again nickel bar and silica flour being mixed rear nickel foil carries out coated, make alloy bag, then utilize oil press alloy bag to suppress, obtain smelting electrode;
Step 2, smelting electrode described in step one is placed in vacuum consumable electrode arc furnace carries out first time vacuum consumable arc-melting, take surface scale off after water-cooled, obtaining diameter of section is Ф 30mm, quality m niSi-1first ingot blank of=2000g; Described first time vacuum consumable arc-melting smelting parameter in table 3;
Step 3, Archimedes' principle is utilized to record the density p of the first ingot blank described in step 2 niSi-1=6.93g/cm 3, then according to formula calculate the mass percentage x=10.09% of silicon in the first ingot blank, ρ in formula ni=8.902g/cm 3, ρ si=2.330g/cm 3;
Step 4, according to formula calculate the Theoretical Mass m that need add silicon si=115g;
Step 5, on the first ingot blank, be drilled with blind hole, then 184g silica flour is added in blind hole, then the first ingot blank being added with silica flour is placed in vacuum consumable electrode arc furnace and carries out second time vacuum consumable arc-melting, after water-cooled, take surface scale off, obtain the second ingot blank; The smelting parameter of described second time vacuum consumable arc-melting is in table 3;
Step 6, the second ingot blank described in step 5 is placed in vacuum consumable electrode arc furnace carries out third time vacuum consumable arc-melting, take surface scale off after water-cooled, obtain Ni-15Si nickel silicon alloy ingot casting; Described third time vacuum consumable arc-melting smelting parameter in table 3.
Table 3 embodiment of the present invention 3 vacuum consumable arc-melting parameter
The density adopting drainage to record the present embodiment Ni-15Si nickel silicon alloy ingot casting is 6.26g/cm 3, with the calculated theoretical density 6.25g/cm of Ni-15Si nickel silicon alloy 3closely, the mass percentage extrapolating silicon in ingot casting is thus 14.97%, and surplus is nickel.The present embodiment Ni-15Si nickel silicon alloy ingot casting is without defects such as obvious segregation, shrinkage cavity, crackles, and superior in quality, homogeneous microstructure, yield rate is high, and nisiloy content is accurately controlled, and analysis deviation is little, meets associated specifications.
Embodiment 4
The preparation of composition graphs 1, Ni-4Si nickel silicon alloy ingot casting:
Step one, according to design mix (the i.e. mass ratio 96: 4 of nickel and silicon need preparing Ni-4Si nickel silicon alloy ingot casting, the mass percentage y=4% of silicon) take nickel bar, silica flour and nickel foil, again nickel bar and silica flour being mixed rear nickel foil carries out coated, make alloy bag, then utilize oil press alloy bag to suppress, obtain smelting electrode;
Step 2, smelting electrode described in step one is placed in vacuum consumable electrode arc furnace carries out first time vacuum consumable arc-melting, take surface scale off after water-cooled, obtaining diameter of section is Ф 60mm, quality m niSi-1first ingot blank of=5000g; Described first time vacuum consumable arc-melting smelting parameter in table 4;
Step 3, Archimedes' principle is utilized to record the density p of the first ingot blank described in step 2 niSi-1=8.24g/cm 3, then according to formula calculate the mass percentage x=2.85% of silicon in the first ingot blank, ρ in formula ni=8.902g/cm 3, ρ si=2.330g/cm 3;
Step 4, according to formula calculate the Theoretical Mass m that need add silicon si=60g;
Step 5, on the first ingot blank, be drilled with blind hole, then 95g silica flour added in blind hole, then the first ingot blank being added with silica flour is placed in vacuum consumable electrode arc furnace and carries out second time vacuum consumable arc-melting, after water-cooled, take surface scale off, obtain the second ingot blank; The smelting parameter of described second time vacuum consumable arc-melting is in table 4;
Step 6, the second ingot blank described in step 5 is placed in vacuum consumable electrode arc furnace carries out third time vacuum consumable arc-melting, take surface scale off after water-cooled, obtain Ni-4Si nickel silicon alloy ingot casting; Described third time vacuum consumable arc-melting smelting parameter in table 4.
Table 4 embodiment of the present invention 4 vacuum consumable arc-melting parameter
The density adopting drainage to record the present embodiment Ni-4Si nickel silicon alloy ingot casting is 8.01g/cm 3, with the calculated theoretical density 7.98g/cm of Ni-4Si nickel silicon alloy 3closely, the mass percentage extrapolating silicon in ingot casting is thus 3.95%, and surplus is nickel.The present embodiment Ni-4Si nickel silicon alloy ingot casting is without defects such as obvious segregation, shrinkage cavity, crackles, and superior in quality, homogeneous microstructure, yield rate is high, and nisiloy content is accurately controlled, and analysis deviation is little, meets associated specifications.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.

Claims (4)

1. a preparation method for nickel silicon alloy ingot casting, is characterized in that, the method comprises the following steps:
Step one, take nickel bar, silica flour and nickel foil according to the design mix of the nickel silicon alloy ingot casting of required preparation, nickel bar and silica flour are mixed rear nickel foil and carries out coated, make alloy bag, then utilize oil press alloy bag to suppress, obtain smelting electrode;
Step 2, smelting electrode described in step one is placed in vacuum consumable electrode arc furnace, is not more than 8.0 × 10 in vacuum tightness -2carry out first time vacuum consumable arc-melting under the condition of Pa, after water-cooled, take surface scale off, obtain the first ingot blank; Described first time, the smelting parameter of vacuum consumable arc-melting was: fusion current 800A ~ 950A, melting voltage 27V ~ 28V, stabilising arc electric current 5A ~ 6A;
Step 3, employing drainage record the density p of the first ingot blank described in step 2 niSi-1, then according to formula calculate the mass percentage x of silicon in the first ingot blank, wherein, ρ nifor the density of nickel, ρ sifor the density of silicon, ρ ni, ρ siand ρ niSi-1unit be g/cm 3;
Step 4, according to formula calculate the Theoretical Mass m that need add silicon si, wherein, y is the mass percentage of silicon in the nickel silicon alloy ingot casting that need prepare, m niSi-1be the quality of the first ingot blank, m siand m niSi-1unit be g;
Step 5, on the first ingot blank, being drilled with blind hole, is 1.5m by quality si~ 1.6m sisilica flour add in blind hole, then the first ingot blank being added with silica flour is placed in vacuum consumable electrode arc furnace, is not more than 8.0 × 10 in vacuum tightness -2carry out second time vacuum consumable arc-melting under the condition of Pa, after water-cooled, take surface scale off, obtain the second ingot blank; The smelting parameter of described second time vacuum consumable arc-melting is: fusion current 800A ~ 950A, melting voltage 27V ~ 28V, stabilising arc electric current 5A ~ 6A;
Step 6, the second ingot blank described in step 5 is placed in vacuum consumable electrode arc furnace, is not more than 8.0 × 10 in vacuum tightness -2carry out third time vacuum consumable arc-melting under the condition of Pa, after water-cooled, take surface scale off, obtain nickel silicon alloy ingot casting; In described nickel silicon alloy ingot casting, the mass percentage y of silicon is 4% ~ 15%, and surplus is nickel; Described third time, the smelting parameter of vacuum consumable arc-melting was: fusion current 800A ~ 950A, melting voltage 27V ~ 28V, stabilising arc electric current 5A ~ 6A.
2. the preparation method of a kind of nickel silicon alloy ingot casting according to claim 1, is characterized in that, described in step 2, the smelting parameter of vacuum consumable arc-melting is for the first time: fusion current 800A, melting voltage 28V, stabilising arc electric current 5.5A.
3. the preparation method of a kind of nickel silicon alloy ingot casting according to claim 1, is characterized in that, the smelting parameter of the vacuum consumable arc-melting of second time described in step 5 is: fusion current 850A, melting voltage 28V, stabilising arc electric current 5.8A.
4. the preparation method of a kind of nickel silicon alloy ingot casting according to claim 1, is characterized in that, described in step 6, the smelting parameter of vacuum consumable arc-melting is for the third time: fusion current 900A, melting voltage 28V, stabilising arc electric current 6.0A.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4118254A (en) * 1977-04-04 1978-10-03 Eutectic Corporation Wear and corrosion resistant nickel-base alloy
CN101476061A (en) * 2009-02-06 2009-07-08 洛阳双瑞精铸钛业有限公司 High temperature resistant titanium and aluminum based alloy and manufacturing method thereof
CN103243227A (en) * 2013-04-27 2013-08-14 西安赛特金属材料开发有限公司 Preparation method of equal-atomic-ratio titanium-nickel alloy ingots

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4118254A (en) * 1977-04-04 1978-10-03 Eutectic Corporation Wear and corrosion resistant nickel-base alloy
CN101476061A (en) * 2009-02-06 2009-07-08 洛阳双瑞精铸钛业有限公司 High temperature resistant titanium and aluminum based alloy and manufacturing method thereof
CN103243227A (en) * 2013-04-27 2013-08-14 西安赛特金属材料开发有限公司 Preparation method of equal-atomic-ratio titanium-nickel alloy ingots

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