CN103255330B - Nickel-niobium intermediate alloy and preparation method thereof - Google Patents
Nickel-niobium intermediate alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nickel-niobium intermediate alloy material which comprises the following components in percentage by mass: 60-70% of niobium, 26.5-36.5% of nickel, less than or equal to 1.5% of aluminum, less than or equal to 0.1% of oxygen, less than or equal to 0.05% of nitrogen, less than or equal to 0.3% of silicon, less than or equal to 0.01% of phosphorus, less than or equal to 1% of iron, less than or equal to 0.2% of tantalum, less than or equal to 0.1% of titanium, less than or equal to 0.005% of lead, less than or equal to 0.005% of tin, less than or equal to 0.05% of carbon, less than or equal to 0.01% of sulfur and the balance being impurities. The invention further discloses a preparation method of the nickel-niobium intermediate alloy material. By utilizing the nickel-niobium intermediate alloy, the temperature of smelting of a niobium-nickel base containing alloy is greatly decreased; as strict raw material control is adopted during the preparation of the nickel-niobium intermediate alloy, the prepared product has high purity, low impurity content, good controllability; the prepared alloy using the nickel-niobium intermediate alloy has low alloy nitrogen oxygen content and is purer; and the production efficiency is high.
Description
Technical field
The present invention relates to metal material field, be specifically related to a kind of nickel niobium master alloy and preparation method thereof.
Background technology
The fusing point of pure niobium bar of the prior art is 2467 DEG C, fusing point is too high, be unfavorable for industrial production, in addition, the not strict control starting material of alloy material of current production and reaction environment cause the purity of product not high, and the residue produced in reaction process and alloy pig are not easily separated, make the nitrogen oxygen level in alloy higher, thus cause purity not high.
Along with development in science and technology, add the performance that niobium element is more and more used for improving specific alloy material, such as nickel base superalloy is most widely used in superalloy, that hot strength the is the highest class alloy.It not only have good high-temperature oxidation resistant system can and corrosion resistance, and have higher hot strength, creep strength and enduring quality and good anti-fatigue performance.It is modern aeroengine, and the crucial hot-end component material of space flight equipment and rocket engine and naval vessels and industrial combustion gas wheel is also reactor, the important high-temperature structural material that the aspects such as chemical industry equipment, coal transformation technology need.And nickel niobium master alloy is the indispensable niobium element additive of Ni-based production nickel base superalloy, in nickel base superalloy preparation process, add nickel niobium master alloy more to one's profit than directly adding niobium bar cost, smelting temperature is lower, the nickel base high temperature alloy composition of formation evenly, performance is more superior, therefore the product confrontation aviation of ickel-niobium alloy, navigation, chemical industry, the key part of automobile and other industries has important impact.
Summary of the invention
Goal of the invention: the object of the invention is to disclose a kind of nickel niobium intermediate alloy material, high purity nickel niobium master alloy and preparation method thereof.The nickel niobium master alloy cost using the method to prepare is low, and alloy quality is high, to aviation, and navigation, the field important in inhibitings such as chemical industry.
Technical scheme: technical scheme of the present invention is as follows: a kind of nickel niobium intermediate alloy material, it is characterized in that: the mass percent of each component of described alloy material is: niobium 60%-70%, nickel 26.5%-36.5%, aluminium≤1.5%, oxygen≤0.1%, nitrogen≤0.05%, silicon≤0.3%, phosphorus≤0.01%, iron≤1%, tantalum≤0.2%, titanium≤0.1%, plumbous≤0.005%, tin≤0.005%, carbon≤0.05%, sulphur≤0.01%, surplus are impurity, and the content sum of above-mentioned each composition is 100%.
The mass percent of each component of described alloy material is: niobium 60%-70%, nickel 30%-36.5%, aluminium≤1.5%, oxygen≤0.1%, nitrogen≤0.05%, silicon≤0.2%, phosphorus≤0.01%, iron≤1%, tantalum≤0.1%, titanium≤0.1%, plumbous≤0.005%, tin≤0.005%, carbon≤0.01%, sulphur≤0.01%, surplus are impurity, and the content sum of above-mentioned each composition is 100%.
The fusing point of described nickel niobium intermediate alloy material is less than 1500 DEG C.
The preparation method of described nickel niobium intermediate alloy material, comprises the following steps:
1) following raw material is put into stoving oven and dry 12-24 hour at 300-370 DEG C, described raw material is made up of following mass fraction: Niobium Pentxoxide 140-151.5 part, nickel protoxide 74.5-63.9 part, aluminium powder 70-75 part, sodium chlorate 3-4 part.
2) raw material after oven dry is taken according to the mass fraction in step 1), put into mixer to mix, the above-mentioned raw material mixed is put into aluminum oxide stove bucket and carries out reaction 1min-2min, reaction terminates rear cooling and obtains alloy pig in more than 40 hours, alloy pig is separated with residue, takes out alloy pig and carry out finishing, magnetic separation, inspection, packaging.
Raw material in described step 1) is made up of following mass fraction: Niobium Pentxoxide 151.5, nickel protoxide 63.9, aluminium powder 72, sodium chlorate 3.
Niobium Pentxoxide purity in described step 1) reaches more than 99.5%, and nickel protoxide purity reaches more than 99.5%, and aluminium powder purity reaches more than 99.7%.
Described step 2) in oxidation Aluminum Drum be the oxidation Aluminum Drum be made up of aluminum oxide and binding agent.
Al in described oxidation Aluminum Drum
2o
3massfraction>=99.2%.
Described step 2) in mixing time material temperature control below 180 DEG C, mixing time is more than 15 minutes.
Beneficial effect: compared with prior art, advantage of the present invention is as follows:
The fusing point of nickel niobium master alloy is less than 1500 DEG C, and the fusing point of pure niobium bar is 2467 DEG C, therefore adopts nickel niobium master alloy greatly can reduce the temperature of melting containing niobium nickel-base alloy; Nickel niobium master alloy prepared by present method have employed strict control with raw material, pure aluminum oxide Reaktionsofen bucket and strict controlling of production process, and product product degree is high, and product foreign matter content is low, and controllability is good; The method produces ickel-niobium alloy, and in continuous prodution, every stove can produce the alloy pig of hundreds of kilogram, and production efficiency is high; Alumina crucible heat-insulating property is better, and alloy is long in the liquid time, is conducive to being separated of slag and alloy, from but alloy do not exist and be mingled with, raw material and reactive aluminum more fully, make alloy nitrogen oxygen level low, purer simultaneously.
Embodiment
Below according to specific embodiment, set forth the present invention further.
Embodiment 1: a kind of percent mass such as table 1 of nickel niobium intermediate alloy material: table 1
A preparation method for nickel niobium intermediate alloy material, comprises the following steps:
1) material choice and analysis: raw material adopts Niobium Pentxoxide, nickel protoxide, aluminium powder, and the control of purity of sodium chlorate and foundry returns is as table 2:
Table 2
2) raw materials pretreatment: raw material is put into stoving oven, dries 24 hours at 350 DEG C of (± 20 DEG C) temperature.
3) aluminum oxide stove bucket preparation: the aluminum oxide of certain particle size proportioning and binding agent are mixed, tie a knot shaping, and be placed in stoving oven and toast and sinter, the aluminum oxide stove bucket after baking be cooled to less than 300 DEG C stand-by, aluminum oxide stove bucket in atmosphere the shelf-time no more than 24 hours.
4) batch mixing: taken according to formula by the raw material after baking, and put into v-shaped mixer and mix, during batch mixing, temperature of charge controls below 180 DEG C, must ensure that material fully mixes, material batch mixing ensures that the time is 15 minutes.
5) react: the raw material mixed is put into aluminum oxide stove bucket, an electrical ignition element, react spontaneous and carry out.
6) cool: be placed in air cooling 40 hours.
7) be separated: taken apart by stove bucket, be separated by alloy pig with slag, alloy pig takes out.
8) finishing: beat removal surface hole defect by hand, band slag part; Alloy pig is put into shot-blasting machine ball blast, remove slag inclusion, then by alloy breaks down to requiring granularity.
9) magnetic separation: alloy carries out magnetic separation, removes the impurity iron filings brought into by disintegrating apparatus.
10) check: laboratory samples, and each principal element content of alloy and impurity component carry out assay.
11) pack: if composition is completely qualified, just can packs and dispatch from the factory.
1, processing condition are as table 3: table 3
| Raw material storing temperature | 350℃（±20℃） | Raw material baking time | 24 hours |
| Mixing time | 15 minutes | Loading temperature | 75℃ |
| Reaction times | 1 minute | Cooling time | 45 hours |
| Alloy pig weight | 149.8㎏ | Particle size after cracking | 10～30㎜ |
2, formula is in table 4: table 4
| Raw material | Weight (㎏) |
| Niobium Pentxoxide | 151.5 |
| Nickel protoxide | 63.9 |
| Aluminium powder | 72 |
| Sodium chlorate | 3 |
| Foundry returns | 0 |
3, response situation: reaction is fierce, and the niobium rate of recovery is 94.84%, and nickel recovery is 94.59%.
4, alloy analysis the results are shown in Table 5
Table 5
Embodiment 2
A kind of percent mass such as table 6 of nickel niobium intermediate alloy material:
Table 6
A kind of preparation method of nickel niobium intermediate alloy material is substantially the same manner as Example 1, distinguishes as follows:
1, processing condition: table 7
| Raw material storing temperature | 350℃（±20℃） | Raw material baking time | 24 hours |
| Mixing time | 15 minutes | Loading temperature | 65℃ |
| Reaction times | 2 minutes | Cooling time | 40 hours |
| Alloy pig weight | 150.5㎏ | Particle size after cracking | 10～30㎜ |
2, fill a prescription: table 8
| Raw material | Weight (㎏) |
| Niobium Pentxoxide | 140 |
| Nickel protoxide | 74.5 |
| Aluminium powder | 70 |
| Sodium chlorate | 4 |
| Foundry returns | 0 |
3, response situation: reaction is fierce, the niobium rate of recovery: 95.16%, nickel recovery: 94.13%.
4, alloy analysis result is as table 9:
Table 9
Embodiment 3
A kind of percent mass such as table 10 of nickel niobium intermediate alloy material:
Table 10
A kind of preparation method of nickel niobium intermediate alloy material is substantially the same manner as Example 1, distinguishes as follows:
1. processing condition are as table 11:
Table 11
| Raw material storing temperature | 350℃（±20℃） | Raw material baking time | 24 hours |
| Mixing time | 15 minutes | Loading temperature | 68℃ |
| Reaction times | 1 point 35 seconds | Cooling time | 40 hours |
| Alloy pig weight | 156.3㎏ | Particle size after cracking | 10～30㎜ |
2. formula is as table 12:
Table 12
| Raw material | Weight (㎏) |
| Niobium Pentxoxide | 145 |
| Nickel protoxide | 70.2 |
| Aluminium powder | 73.5 |
| Sodium chlorate | 3.3 |
| Foundry returns | 4 |
3. response situation: reaction is fierce, the niobium rate of recovery: 96.53%, nickel recovery: 95.85%.
4. alloy analysis result is as table 13:
Table 13
Embodiment 4:
A kind of percent mass such as table 14 of nickel niobium intermediate alloy material:
Table 14
A kind of preparation method of nickel niobium intermediate alloy material is substantially the same manner as Example 1, distinguishes as follows:
5. processing condition are as table 15: table 15
| Raw material storing temperature | 350℃（±20℃） | Raw material baking time | 24 hours |
| Mixing time | 15 minutes | Loading temperature | 70℃ |
| Reaction times | 1 point 35 seconds | Cooling time | 40 hours |
| Alloy pig weight | 156.3㎏ | Particle size after cracking | 10～30㎜ |
6. fill a prescription: table 16
| Raw material | Weight (㎏) |
| Niobium Pentxoxide | 151.2 |
| Nickel protoxide | 63.6 |
| Aluminium powder | 73.5 |
| Sodium chlorate | 3.3 |
| Foundry returns | 4 |
7. response situation: reaction is fierce, the niobium rate of recovery: 97.23%, nickel recovery: 95.25%.
4. alloy analysis result is as table 17:
Table 17
Embodiment 5:
A kind of percent mass such as table 18 of nickel niobium intermediate alloy material:
Table 18
A kind of preparation method of nickel niobium intermediate alloy material is substantially the same manner as Example 1, distinguishes as follows:
8. processing condition are as table 19:
Table 19
| Raw material storing temperature | 350℃ | Raw material baking time | 24 hours |
| Mixing time | 20 minutes | Loading temperature | 72℃ |
| Reaction times | 1 point 35 seconds | Cooling time | 40 hours |
| Alloy pig weight | 156.3㎏ | Particle size after cracking | 10～30㎜ |
9. formula is as table 20:
Table 20
| Raw material | Weight (㎏) |
| Niobium Pentxoxide | 151.2 |
| Nickel protoxide | 63.6 |
| Aluminium powder | 73.5 |
| Sodium chlorate | 3.3 |
| Foundry returns | 4 |
10. response situation: reaction is fierce, the niobium rate of recovery: 97.23%, nickel recovery: 96.25%.
4. alloy analysis result is as table 21:
Table 21
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a nickel niobium intermediate alloy material, it is characterized in that: the mass percent of each component of described alloy material is: niobium 66.83 %-66.92%, nickel 31.25%-31.3%, aluminium≤1.5%, oxygen≤0.015%, nitrogen≤0.013%, silicon≤0.3%, phosphorus≤0.01%, iron≤1%, tantalum≤0.2%, titanium≤0.1%, plumbous≤0.005%, tin≤0.005%, carbon≤0.05%, sulphur≤0.01%, surplus are impurity, and the content sum of above-mentioned each composition is 100%.
2. the preparation method of nickel niobium intermediate alloy material according to claim 1, is characterized in that comprising the following steps:
1) following raw material is put into stoving oven and dry 12-24 hour at 300-370 DEG C, described raw material is made up of following mass fraction: Niobium Pentxoxide 140-151.5 part, nickel protoxide 74.5-63.9 part, aluminium powder 70-75 part, sodium chlorate 3-4 part;
2) raw material after oven dry is taken according to the mass fraction in step 1), put into mixer to mix, the above-mentioned raw material mixed is put into aluminum oxide stove bucket and carries out reaction 1min-2min, reaction terminates rear cooling and obtains alloy pig in more than 40 hours, alloy pig is separated with residue, takes out alloy pig and carry out finishing, magnetic separation, inspection, packaging.
3. the preparation method of nickel niobium intermediate alloy material according to claim 2: it is characterized in that: the raw material in described step 1) is made up of following mass fraction: Niobium Pentxoxide 151.5, nickel protoxide 63.9, aluminium powder 72, sodium chlorate 3.
4. the preparation method of nickel niobium intermediate alloy material according to claim 2: it is characterized in that: the Niobium Pentxoxide purity in described step 1) reaches more than 99.5%, and nickel protoxide purity reaches more than 99.5%, and aluminium powder purity reaches more than 99.7%.
5. the preparation method of nickel niobium intermediate alloy material according to claim 2: it is characterized in that: described step 2) in oxidation Aluminum Drum be the oxidation Aluminum Drum be made up of aluminum oxide and binding agent.
6. the preparation method of nickel niobium intermediate alloy material according to claim 5: it is characterized in that: Al in described oxidation Aluminum Drum
2o
3massfraction>=99.2%.
7. the preparation method of nickel niobium intermediate alloy material according to claim 2: it is characterized in that: described step 2) in mixing time material temperature control below 180 DEG C, mixing time is more than 15 minutes.
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| CN103484675A (en) * | 2013-08-23 | 2014-01-01 | 大连融德特种材料有限公司 | Method for breaking residue caused by aluminothermic reduction reaction for intermediate alloy |
| CN104988341A (en) * | 2015-06-19 | 2015-10-21 | 承德天大钒业有限责任公司 | Preparation method of nickel niobium alloy |
| CN105018759A (en) * | 2015-07-16 | 2015-11-04 | 江苏圣亚有色金属材料有限公司 | Preparation technology of vacuum-grade niobium-nickel alloy |
| CN110358947B (en) * | 2019-07-31 | 2021-03-19 | 江苏美特林科特殊合金股份有限公司 | Nickel-tungsten intermediate alloy for smelting high-temperature alloy and preparation method and application thereof |
| CN110358957B (en) * | 2019-07-31 | 2021-05-14 | 江苏美特林科特殊合金股份有限公司 | Nickel-vanadium intermediate alloy and preparation method thereof |
| CN111663056A (en) * | 2020-06-17 | 2020-09-15 | 承德天大钒业有限责任公司 | Nickel-tantalum intermediate alloy and preparation method thereof |
| CN113528924B (en) * | 2021-07-23 | 2022-04-15 | 承德天大钒业有限责任公司 | Nickel-niobium-chromium intermediate alloy and preparation method thereof |
| CN114635049B (en) * | 2022-03-28 | 2022-09-30 | 江苏美特林科特殊合金股份有限公司 | Production method of high-purity nickel-niobium intermediate alloy |
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