CN108277375A - The preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of alkali corrosion resistance - Google Patents
The preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of alkali corrosion resistance Download PDFInfo
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- CN108277375A CN108277375A CN201810211038.1A CN201810211038A CN108277375A CN 108277375 A CN108277375 A CN 108277375A CN 201810211038 A CN201810211038 A CN 201810211038A CN 108277375 A CN108277375 A CN 108277375A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
Abstract
The present invention relates to a kind of preparation methods of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature, using the micro addition zirconium oxide by a certain percentage in nickel-base alloy, the technique of vanadium oxide and carbon, it realizes carbon in high temperature molten bath under vacuum and reacts to form part zirconium carbon compound and vanadium carbon compound is evenly dispersed in the alloy with zirconium oxide and vanadium oxide, there is excellent alkali corrosion resistance performance while so that nickel-base alloy obtained is kept preferable intensity at high temperature, technological process is simple, process costs are low, obtained alloy can for a long time use under 1000 DEG C of high temperature in corrosive environment, with high temperature resistant, the features such as alkali corrosion resistance, various high-temperature anticorrosion industry device accessories be can be widely applied to improve its performance and service life.
Description
This case is with the applying date on 08 19th, 2016, application No. is 201610689234.0, a kind of entitled " zirconium
The divisional application that the patent of invention of the preparation method of the corrosion-resistant nickel-base alloy of object doped high temperature " carries out for female case.
Technical field
The present invention relates to technical field of alloy, specifically a kind of preparation of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature
Method.
Background technology
It is especially resistant to alkali corrosion equipment and materials performance under high temperature environment to corrosion-resistant in chemical industry
It is required that being increasingly stringenter, corrosion resisting alloy fabricating technology is always the hot spot of alloy field research.Existing corrosion-resistant conjunction
Although gold can keep certain corrosion resistance in low temperature environment, when temperature is increased to 500 DEG C or more, especially exist
In strong basicity environment, grain boundary corrosion phenomenon will occur, cause alloy physics performance and corrosion resistance to reduce rapidly, use again
When high-temperature alkaline environment, alloy body will be accelerated to corrode, can not be further continued for using.Common nickel-base alloy preparation method also has
Document refers to doping zirconium technique, entitled " high strength anti-corrosion nickel alloy and its manufacturing method " such as Patent No. CN102628127A
Chinese invention patent, but it is using metal zirconium as raw material, and cost of material is high, and simple substance zirconium also is difficult to fuse, causes to close with Ni substrate
Golden product is also easy to produce crack and is even broken, while zirconium is scattered in nickel-base alloy in the form of metal zirconium in alloy, to being added
Nickel-bass alloy material performance such as quenching degree, fracture toughness etc. be affected, the corrosion resistance in high temperature strong alkali environment is not yet
Enough ideals.As how cheap cost prepare can alkali corrosion resistance under high temperature environment nickel-bass alloy material, while protecting again
The physical properties such as quenching degree, the fracture toughness of nickel-bass alloy material are demonstrate,proved, become those skilled in the art's urgent need to resolve one is big
Technical barrier.
Invention content
Technical problem to be solved by the invention is to provide it is a kind of it is simple for process, of low cost, can be in high temperature strong alkali environment
Under the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of good physical performances such as corrosion-resistant and quenching degree, fracture toughness preparation side
Method.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature, by nickel, chromium, zirconium oxide, vanadium oxide and carbon
According to melting in following weight ratio input vaccum sensitive stove：
Nickel: chromium: zirconium oxide: vanadium oxide: carbon=63.5-68.5: 27.5-33.5: 0.85-1.35: 0.55-0.85: 1.15-
1.75；
Smelting temperature is 1550-1700 DEG C, smelting time 90-180min, after the completion of melting under inert atmosphere protection
Casting obtains alloy pig.
The beneficial effects of the present invention are：It is different from the prior art, the present invention uses in nickel-base alloy by a certain percentage
The technique of micro addition zirconium oxide, vanadium oxide and carbon realizes carbon and zirconium oxide and oxidation in high temperature molten bath under vacuum
Vanadium, which reacts, to form part zirconium carbon compound and vanadium carbon compound is evenly dispersed in the alloy, makes nickel-base alloy obtained at high temperature
Keep that there is excellent alkali corrosion resistance performance while preferable intensity, technological process is simple, and process costs are low, and obtained alloy can
It is used for a long time in corrosive environment under 1000 DEG C of high temperature, has the characteristics that high temperature resistant, alkali corrosion resistance, can be widely applied to various
High-temperature anticorrosion industry device accessory is to improve its performance and service life.
Specific implementation mode
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is:The addition of micro zirconium oxide, vanadium oxide and carbon is applied in nickel-base alloy,
Zirconium carbon, the vanadium carbon compound of even dispersion are formed when homogenizing cast ingot, small zirconium carbon, vanadium carbon compound even dispersion exist
In nickel-base alloy, while ensureing the physical properties such as nickel-base alloy quenching degree, fracture toughness, the high temperature for improving nickel-base alloy is anti-
Corrosive nature.
Specifically, the preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature provided by the invention, by nickel, chromium, oxygen
Change zirconium, vanadium oxide and carbon according to melting in following weight ratio input vaccum sensitive stove：
Nickel: chromium: zirconium oxide: vanadium oxide: carbon=63.5-68.5: 27.5-33.5: 0.85-1.35: 0.55-0.85: 1.15-
1.75；
Smelting temperature is 1550-1700 DEG C, smelting time 90-180min, after the completion of melting under inert atmosphere protection
Casting obtains alloy pig.
The reaction mechanism of the present invention is：Using metallic nickel as matrix, while with crome metal, micro-oxidation zirconium, micro-oxidation
Vanadium adds a certain amount of carbon to be that molten bath is added in raw material by a certain percentage, under vacuum carbon and zirconium oxide and vanadium oxide in high temperature molten bath
Reaction forms part zirconium carbon compound and vanadium carbon compound is evenly dispersed in the alloy, such zirconium, vanadium carbide dispersion-strengthened
Nickel-base alloy under the high temperature conditions can it is resistance to live highly basic etch, can in the high-temperature alkaline environment at up to 1000 DEG C
It is used for a long time, there is fabulous protective effect to the component of various high-temperature alkali environment and other perishable environmental works.
As can be seen from the above description, the beneficial effects of the present invention are：It is different from the prior art, the present invention is used in Ni-based conjunction
The technique for adding zirconium oxide, vanadium oxide and carbon micro by a certain percentage, realizes carbon in high temperature molten bath under vacuum in gold
It is reacted with zirconium oxide and vanadium oxide and to form part zirconium carbon compound and vanadium carbon compound is evenly dispersed in the alloy, make nickel obtained
Based alloy keeps having excellent alkali corrosion resistance performance while preferable intensity at high temperature, and technological process is simple, and process costs are low,
Obtained alloy can for a long time use under 1000 DEG C of high temperature in corrosive environment, have the characteristics that high temperature resistant, alkali corrosion resistance, can
It is widely used in various high-temperature anticorrosion industry device accessories to improve its performance and service life.
Further, first by nickel and chromium input vaccum sensitive stove in melting, after nickel and chromium fusing after, then will by zirconium oxide,
(carbon thermal reduction zirconium oxide and vanadium oxide prepare gold for melting in bead input vaccum sensitive stove made of vanadium oxide and carbon mixing compacting
Belong to zirconium and vanadium, so that reduction obtains metal zirconium and vanadium and nickel and chromium fusion reaction).
Further, the smelting time after bead input vaccum sensitive stove is controlled in 45min or more (so that fusion reaction
Fully).
Further, melting requires content of iron and manganese in control alloy to be respectively less than 0.1%, and aluminium, Ti content are respectively less than
0.07%.
Further, purity >=99.9wt% of nickel, purity >=99.9wt% of chromium, the purity of zirconium oxide >=
99.8wt%, purity >=99.8wt% of vanadium oxide, purity >=99wt% of carbon.
Embodiment one
1, prepared by raw material：It is nickel: chromium: zirconium oxide: vanadium oxide: carbon=64.5: 33.5: 1.2: 0.59: 1.6 according to weight ratio
Weigh raw material, wherein metallic nickel purity >=99.9%, crome metal purity >=99.9%, zirconium oxide purity >=99.8%, vanadium oxide
>=99.8%, carbon purity >=99%, zirconium oxide, vanadium oxide and carbon are preferably graininess or powdered, by zirconium oxide, vanadium oxide and
Carbon mixing is pressed into bead (spherolite diameter 0-30mm, pressure ball so that contact is abundant, so that thermal reduction reaction is more efficient).
2, melting：First by melting in nickel and chromium input vaccum sensitive stove, the smelting temperature for controlling vaccum sensitive stove is 1650
DEG C, after nickel and chromium fusing, then it will be mixed by zirconium oxide, vanadium oxide and carbon and be melted in bead input vaccum sensitive stove made of compacting
Refining, the smelting time controlled after bead input vaccum sensitive stove is 45min, and it is 180min to control total smelting time.
3, it casts：Melted alloy melt is cast into alloy pig under inert atmosphere protection to mix to get to zirconium compound
Miscellaneous high temperature corrosion-resisting nickel-base alloy.
Testing result：
(1) nickel-base alloy obtained is subjected to Metallographic Analysis and composition detection it is found that in alloy containing zirconium carbon compound and
Vanadium carbon compound, and zirconium carbon compound and vanadium carbon compound are evenly dispersed in the alloy, content of iron and manganese are respectively less than 0.1%, aluminium,
Ti content is respectively less than 0.07%.
(2) nickel-base alloy obtained is placed in sodium carbonate strong basicity material, it is small that 48 is placed in 980 DEG C of Muffle furnaces
When, it so recycles 10 times and does not find that its surface is corroded, high temperature corrosion resistance is good.
Embodiment two
1, prepared by raw material：It is nickel: chromium: zirconium oxide: vanadium oxide: carbon=66.75: 30.3: 0.993: 0.845 according to weight ratio
: 1.55 weigh raw material, wherein metallic nickel purity >=99.9%, crome metal purity >=99.9%, zirconium oxide purity >=99.8%,
Vanadium oxide >=99.8%, carbon purity >=99%, zirconium oxide, vanadium oxide and carbon are preferably graininess or powdered, by zirconium oxide, oxygen
Change vanadium and carbon mixing is pressed into bead.
2, melting：First by melting in nickel and chromium input vaccum sensitive stove, the smelting temperature for controlling vaccum sensitive stove is 1600
DEG C, after nickel and chromium fusing, then it will be mixed by zirconium oxide, vanadium oxide and carbon and be melted in bead input vaccum sensitive stove made of compacting
Refining, the smelting time controlled after bead input vaccum sensitive stove is 50min, and it is 150min to control total smelting time.
3, it casts：Melted alloy melt is cast into alloy pig under inert atmosphere protection to mix to get to zirconium compound
Miscellaneous high temperature corrosion-resisting nickel-base alloy.
Testing result：
(1) nickel-base alloy obtained is subjected to Metallographic Analysis and composition detection it is found that in alloy containing zirconium carbon compound and
Vanadium carbon compound, and zirconium carbon compound and vanadium carbon compound are evenly dispersed in the alloy, content of iron and manganese are respectively less than 0.1%, aluminium,
Ti content is respectively less than 0.07%.
(2) nickel-base alloy obtained is placed in sodium carbonate strong basicity material, it is small that 48 is placed in 1000 DEG C of Muffle furnaces
When, it so recycles 10 times and does not find that its surface is corroded, high temperature corrosion resistance is good.
Embodiment three
1, prepared by raw material：It is nickel: chromium: zirconium oxide: vanadium oxide: carbon=63.5 according to weight ratio: 27.5: 0.85: 0.55:
1.15 weigh raw material, wherein metallic nickel purity >=99.9%, crome metal purity >=99.9%, zirconium oxide purity >=99.8%, oxygen
Change vanadium >=99.8%, carbon purity >=99%, zirconium oxide, vanadium oxide and carbon are preferably graininess or powdered, by zirconium oxide, oxidation
Vanadium and carbon mixing are pressed into bead.
2, melting：First by melting in nickel and chromium input vaccum sensitive stove, the smelting temperature for controlling vaccum sensitive stove is 1550
DEG C, after nickel and chromium fusing, then it will be mixed by zirconium oxide, vanadium oxide and carbon and be melted in bead input vaccum sensitive stove made of compacting
Refining, the smelting time controlled after bead input vaccum sensitive stove is 45min, and it is 90min to control total smelting time.
3, it casts：Melted alloy melt is cast into alloy pig under inert atmosphere protection to mix to get to zirconium compound
Miscellaneous high temperature corrosion-resisting nickel-base alloy.
Testing result：
(1) nickel-base alloy obtained is subjected to Metallographic Analysis and composition detection it is found that in alloy containing zirconium carbon compound and
Vanadium carbon compound, and zirconium carbon compound and vanadium carbon compound are evenly dispersed in the alloy, content of iron and manganese are respectively less than 0.1%, aluminium,
Ti content is respectively less than 0.07%.
(2) nickel-base alloy obtained is placed in sodium carbonate strong basicity material, it is small that 48 is placed in 1000 DEG C of Muffle furnaces
When, it so recycles 10 times and does not find that its surface is corroded, high temperature corrosion resistance is good.
Example IV
1, prepared by raw material：It is nickel: chromium: zirconium oxide: vanadium oxide: carbon=68.5 according to weight ratio: 33.5: 1.35: 0.85:
1.75 weigh raw material, wherein metallic nickel purity >=99.9%, crome metal purity >=99.9%, zirconium oxide purity >=99.8%, oxygen
Change vanadium >=99.8%, carbon purity >=99%, zirconium oxide, vanadium oxide and carbon are preferably graininess or powdered, by zirconium oxide, oxidation
Vanadium and carbon mixing are pressed into bead.
2, melting：First by melting in nickel and chromium input vaccum sensitive stove, the smelting temperature for controlling vaccum sensitive stove is 1700
DEG C, after nickel and chromium fusing, then it will be mixed by zirconium oxide, vanadium oxide and carbon and be melted in bead input vaccum sensitive stove made of compacting
Refining, the smelting time controlled after bead input vaccum sensitive stove is 55min, and it is 180min to control total smelting time.
3, it casts：Melted alloy melt is cast into alloy pig under inert atmosphere protection to mix to get to zirconium compound
Miscellaneous high temperature corrosion-resisting nickel-base alloy.
Testing result：
(1) nickel-base alloy obtained is subjected to Metallographic Analysis and composition detection it is found that in alloy containing zirconium carbon compound and
Vanadium carbon compound, and zirconium carbon compound and vanadium carbon compound are evenly dispersed in the alloy, content of iron and manganese are respectively less than 0.1%, aluminium,
Ti content is respectively less than 0.07%.
(2) nickel-base alloy obtained is placed in sodium carbonate strong basicity material, it is small that 48 is placed in 1000 DEG C of Muffle furnaces
When, it so recycles 10 times and does not find that its surface is corroded, high temperature corrosion resistance is good.
Comparative example one
What is different from the first embodiment is that not including zirconium oxide in raw material, bead is suppressed by vanadium oxide and carbon mixing,
His all same.
Nickel-base alloy obtained is placed in sodium carbonate strong basicity material, is placed 48 hours in 1000 DEG C of Muffle furnaces,
Find that its surface is gradually corroded after so recycling 3 times, surface has ferrous metal compound to fall off, and high temperature corrosion resistance is inadequate
It is good.
Comparative example two
What is different from the first embodiment is that nickel: chromium: zirconium oxide: vanadium oxide: carbon=64.5: 33.5: 2.5: 2.5: 1.6, other
All same.
Nickel-base alloy obtained is placed in sodium carbonate strong basicity material, is placed 48 hours in 1000 DEG C of Muffle furnaces,
It so recycles 10 times and does not find that its surface is corroded, high temperature corrosion resistance is good.But quenching degree, fracture toughness are substantially reduced, object
Rationality can be poor.
Comparative example three
What is different from the first embodiment is that nickel: chromium: zirconium oxide: vanadium oxide: carbon=64.5: 33.5: 0.1: 0.3: 1.6, other
All same.
Nickel-base alloy obtained is placed in sodium carbonate strong basicity material, is placed 48 hours in 1000 DEG C of Muffle furnaces,
Find that its surface is gradually corroded after so recycling 6 times, surface has ferrous metal compound to fall off, and high temperature corrosion resistance is inadequate
It is good.
In conclusion the preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature provided by the invention, technological process
Simply, process costs are low, and nickel-base alloy obtained keeps having excellent alkali corrosion resistance performance while preferable intensity at high temperature,
It can for a long time be used in corrosive environment under 1000 DEG C of high temperature, have the characteristics that high temperature resistant, alkali corrosion resistance, can be widely applied to each
Kind high-temperature anticorrosion industry device accessory is to improve its performance and service life.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (2)
1. a kind of preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of alkali corrosion resistance, it is characterised in that：By nickel,
Chromium, zirconium oxide, vanadium oxide and carbon carry out melting according to following weight ratio：
Nickel: chromium: zirconium oxide: vanadium oxide: carbon=63.5-68.5: 27.5-33.5: 0.85-1.35: 0.55-0.85: 1.15-
1.75；
Smelting temperature is 1550-1700 DEG C, smelting time 90-180min, is cast under inert atmosphere protection after the completion of melting
Obtain alloy pig；
Nickel and chromium are first subjected to melting, after nickel and chromium fusing, then will be mixed by zirconium oxide, vanadium oxide and carbon small made of compacting
Ball carries out melting；
Melting requires content of iron and manganese in control alloy to be respectively less than 0.1%, and aluminium, Ti content are respectively less than 0.07%.
2. the preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of alkali corrosion resistance according to claim 1,
It is characterized in that：Smelting time after bead input vaccum sensitive stove is controlled in 45min or more.
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| CN201810211038.1A CN108277375B (en) | 2016-08-19 | 2016-08-19 | The preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of alkali corrosion resistance |
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| CN201810211038.1A CN108277375B (en) | 2016-08-19 | 2016-08-19 | The preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature of alkali corrosion resistance |
| CN201610689234.0A CN106282636B (en) | 2016-08-19 | 2016-08-19 | A kind of preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature |
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| CN201610689234.0A Active CN106282636B (en) | 2016-08-19 | 2016-08-19 | A kind of preparation method of the corrosion-resistant nickel-base alloy of zirconium compound doped high temperature |
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| EP0648850A1 (en) * | 1993-09-20 | 1995-04-19 | Mitsubishi Materials Corporation | Nickel-based alloy |
| CN101466857A (en) * | 2006-06-16 | 2009-06-24 | 科卢斯博材料有限公司 | Ni-base wear and corrosion resistant alloy |
| CN102808111A (en) * | 2012-08-24 | 2012-12-05 | 杨学焦 | Preparation method for nickel-based superalloy for exhaust valve |
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|---|---|
| CN106282636A (en) | 2017-01-04 |
| CN106282636B (en) | 2018-05-18 |
| CN108559863B (en) | 2020-03-10 |
| CN108277375B (en) | 2019-11-01 |
| CN108559863A (en) | 2018-09-21 |
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