CN108893648A - A kind of preparation method of yttrium-base heavy rare earth corronil - Google Patents
A kind of preparation method of yttrium-base heavy rare earth corronil Download PDFInfo
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- CN108893648A CN108893648A CN201810801717.4A CN201810801717A CN108893648A CN 108893648 A CN108893648 A CN 108893648A CN 201810801717 A CN201810801717 A CN 201810801717A CN 108893648 A CN108893648 A CN 108893648A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
The present invention relates to one kind to improve cupro-nickel by rare earth modified and bounding engineering（CuNi）It is the field of alloy corrosion resistance energy, Chemical Composition Characteristics are（Mass fraction/%）:Ni:9~12%；Fe:1.0~2.0%；Mn:0.5~1.5%；S<0.01%；P<0.01%；C<0.01%；Y：50~300ppm, other impurity content summations are less than<0.1%, surplus is copper.Alloy is smelted into slab, then forged → hot rolling → once cold rolling → intermediate annealing → secondary cold-rolling → finished product annealing process through vacuum gas protection.High anti-corrosion CuNi system alloy structure is α-Cu matrix and Yttrium base rare earth complex inclusion, matrix grain size（Do not consider twin）It is 40-60 μm, and low energy coincidence lattice grain boundary ratio is greater than 75%, the ratio of maximum free crystal boundary length and free crystal boundary total length is less than 0.3.CuNi system alloy preparation cost disclosed in this invention is low, and simple process is easy to operate, is applicable to plate, band product, is provided simultaneously with excellent corrosion resistance, especially adapts in the corrosion-resistant more demanding Service Environment of seawater.
Description
Technical field
The present invention relates to a kind of high anti-corrosion CuNi system alloy fields, set particular by yttrium-base heavy rare earth addition and technique
Meter, improves its corrosion resistance using Grain Boundary Character optimization.
Background technique
Corronil（B10, B30 etc.）Be with nickel be main addition element acid bronze alloy, due to possess excellent electric conductivity,
Thermal conductivity, preferable processing performance and excellent corrosion resistance and be widely used in marine engineering equipment, power equipment with
And shipbuilding equipment.In recent years, for the corrosion resisting property for improving corronil, many researchers have carried out extensive work.1952
Year Bailey etc. proposes to add iron on the basis of corronil earliest（Fe）And manganese（Mn）The resistance to of White brass alloy can be significantly improved
Corrosion energy, due to the dvielement can promote alloy surface to form fine and close passivating film, to improve its corrosion resistance.[clear 58-
81944] and [clear 58-34154] is individually disclosed can greatly improve the corrosion resistance of White brass alloy in copper-based middle addition Fe, Mn
Energy.[flat 1-136945] proposes [BFe10-1-1]（Abbreviation B10）Alloy, wherein Fe, Mn are the main additions other than nickel
Element.It is worth noting that, corronil is under different Service Environments, however it remains due to being on active service the longevity caused by corrosion default
The problems such as life shortens, such as grain boundary corrosion, electrochemical corrosion, den-ickel corrosion and spot corrosion etc..
Studies have shown that Fe element is easily enriched in grain boundaries under certain conditions, so that the continuity of passivation film is destroyed,
To which the corrosion resistance of White brass alloy can be reduced.In addition to this, the fluctuation of processing technology also easily leads to grain uniformity and crystal boundary is special
The variation of sign, to influence its corrosive nature.Therefore, part researcher attempts to improve by adding a certain amount of microalloy element
The corrosion resisting property of corronil, such as addition Cr can effectively realize crystal boundary occupy-place, and the segregation of Fe element is inhibited to improve matrix
Corrosive nature.[special open 2001-131658] and [US4830825] two patent disclose a kind of high strength anti-corrosion for adding Al
Corronil forms Ni3Al precipitated phase by the addition of two element of Ni and Al to improve intensity and corrosion resisting property.In addition to this,
The pertinent literature report addition elements such as Co, Ti, B also will affect the corrosion potential of White brass alloy, surface passivated membrane compactness etc., from
And its corrosive nature can be improved.Therefore, its corrosion resistance can be effectively improved by White brass alloy optimization of Chemical Composition.
Application of the RE element in copper has relevant report, and effect can be embodied in the following aspects：（1）Can with O,
S, H-shaped purifies matrix at RE field trash, reduces primary battery number；（2）Ingot structure tissue signature can be improved, especially pressed down
Make unfavorable element（P,S,Pb,Bi）Crystal boundary distribution, to improve resistance to grain boundary corrosion performance；（3）Heterogeneous nucleation is promoted to realize
Refined crystalline strengthening and controlled micro crystallization effect；（4）It is arranged based on its unique electron orbit, alloy surface oxidation film layer can also be enhanced
Stability and compactness.（5）Inhibit to corrode by improving matrix current potential.Report that more is to utilize light rare earth in document at present
Lanthanum（La）And cerium（Ce）, application of the heavy rare earth in copper alloy and report are less.103740976 A of patent CN and patent
CN103740977 A individually discloses a kind of White Copper Tubes for ocean engineering, is wherein added in ingredient design a certain amount of
Light rare earth La and Ce is to improve its corrosive nature.Patent US4749548 and patent US4872048 are individually disclosed high-strength
Height, which is led, adds heavy rare earth Y to improve its intensity and electric conductivity in CuCrZr alloy.However, having no using heavy rare earth Y improves
The related patents of the corrosive nature of White brass alloy are reported.
The active outline of heavy rare earth Y is higher than light rare earth La and Ce, therefore is easier to form complex inclusion in conjunction with O, S, and
And formed YOxSy complex inclusion is easier to float in copper liquid compared with La (Ce) OxSy, therefore large inclusions are easier to remove
It goes, and fine particle field trash can be retained in Copper substrate and promote heterogeneous nucleation, to refine crystal grain.Meanwhile heavy rare earth Y adds
Add the stacking fault energy that can also improve copper alloy, can effectively activate the twin in deformation or annealing process, to greatly improve twin
Brilliant ratio.Therefore, this patent proposes the corrosive nature for improving corronil system using yttrium-base heavy rare earth.
Other than ingredient design, another focused protection behave of this patent is the thermomechanical treatment process after hot rolling is rolled.For
White brass alloy, the Grain Boundary Character of a-Cu matrix are one of the principal elements for influencing its corrosive nature.Different deformation and heat treatments
Process combination influences whether that the crystal grain recrystallization of copper-nickel alloy and crystal grain are grown up behavior, to generate a fixing to Grain Boundary Character distribution
It rings.It is well known that low energy coincidence lattice grain boundary（low-ΣCSL）Because having the higher degree of order, low crystal boundary energy and low work
Property and be not easy to be corroded, therefore, the CSL crystal boundary ratio of copper-nickel alloy matrix can be improved by optimizing heat treatment process, thus into one
Step improves its corrosive nature.In addition, grain boundary corrosion or crack propagation are often carried out along crystal boundary, and therefore, the connection of free crystal boundary
Influence of the property for material property is also most important.Free crystal boundary ratio is higher, not fully represents it and resists external world energy
Power is with regard to poor, and also related to the connectivity of free crystal boundary, connecting degree is higher, and correlated performance can be worse.Therefore, through this patent public affairs
The corronil for the bounding engineering technical treatment opened not only has low special grain boundary ratio, and more crucially free crystal boundary connects
The general character is interrupted, and corrosion path is suppressed, and finally will further improve the corrosion resistance of corronil.
Summary of the invention
The present invention provides a kind of high anti-corrosion CuNi system alloys of yttrium-base heavy rare earth addition, by adding micro heavy rare earth
Y can effectively purify matrix, activate twin, increase temperature in short-term in combination with thermomechanical treatment twice, especially second of small deformation
Annealing process can sufficiently improve special grain boundary ratio, the connectivity of free crystal boundary be destroyed, so as to improve its corrosion resistance.
In order to achieve the above objectives, the technical scheme is that：
A kind of high anti-corrosion CuNi system alloy of yttrium-base heavy rare earth addition of the present invention, each component chemical quality percentage is such as
Under：Ni:9~12%；Fe:1~2%；Mn:0.5~1.5%；S<0.01%； P<0.01%；C<0.01%； Y（Yttrium）：50~
300ppm, other impurity contents<0.1%, surplus Cu.
On the basis of above scheme, the yttrium-base heavy rare earth adds Cu-Ni system alloy, each component chemical quality percentage
It is as follows：Ni:9~11%；Fe:1.3~1.8%；Mn:0.8~1.3%；S<0.008%； P<0.008%；C<0.008%； Y
（Yttrium）：80~250ppm, other impurity contents<0.1%, surplus Cu.
On the basis of above scheme, selected yttrium-base heavy rare earth intermediate alloy is using yttrium iron alloy, and wherein Y is accounted for
65%, Fe account for 35%.It using yttrium iron alloy, can make the Y in CuNi alloy under the premise of higher recovery rate, stablize and add
Enter, be evenly distributed, it is ensured that the efficient melting of Yttrium base rare earth CuNi system alloy.
A kind of high anti-corrosion Cu-Ni system alloy of yttrium-base heavy rare earth addition of the present invention, technology of preparing scheme are as follows：
（1）Vacuum induction melting is protected using nitrogen or argon gas, is heated to keeping the temperature 3-5 minutes addition yttrium base weights after high-temperature liquid-phase dilute
Native alloy, then ingot of casting after keeping the temperature 1 minute.
（2）Hot rolling is carried out again after the hot forging of ingot casting high temperature.Forging stock is heated to 950 DEG C of heat preservation 1h, and finishing temperature is not less than 750
DEG C, hot rolling deformation amount is greater than 50%.
（3）Once cold rolling deflection is not less than 70%, and between 7%-14%, total deformation is greater than secondary cold-rolling deflection
75%。
（4）The soft annealing between cold rolling carries out in protection annealing furnace twice, and whole process uses nitrogen protection, heating temperature
Degree is 800~900 DEG C, and the time is 5-10 minutes；Finished products also carry out in protection annealing furnace, and whole process is protected using nitrogen
Shield；Temperature is 850~900 DEG C, and the time is 10-15 minutes, and using the technique of water cooling to room temperature after finished products.
On the basis of above scheme, the yttrium-base heavy rare earth corronil tissue is mainly α-Cu phase, crystallite dimension（No
Consider twin）Adhere to sub-micron and nanoscale heavy rare earth complex inclusion in 40-60 μm and phase and on phase crystal boundary.
On the basis of above scheme, the yttrium-base heavy rare earth corronil, low energy dot matrix coincident grain boundary ratio is more than
75%, wherein twin boundary ratio is more than 60%.Maximum is freely connected to the ratio of crystal boundary length and free crystal boundary total length less than 0.3
（Lmax/Ltoal <0.3）.
Compared with prior art, advantage of the invention is that：
（1）Yttrium-base heavy rare earth disclosed in this invention adds Cu-Ni system alloy, and added rare earth alloy is yttrium iron alloy, no
With traditional light rare earth alloy and yttrium copper alloy, recovery rate height is added, stability is high, it is ensured that low-cost design.Together
When, Yttrium base rare earth is more likely formed sub-micron or nano-scale rare earth complex inclusion, and size is at 5 μm hereinafter, part reaches nanoscale.
Under the premise of not deteriorating matrix mechanical property, matrix is adequately purified, improves matrix grain size, optimizes corrosion resistance.
（2）Yttrium-base heavy rare earth disclosed in this invention adds CuNi system alloy, on the basis of adding Yttrium base rare earth, uses
Large deformation, two passage small deformations is cold worked in two passage thermomechanical treatment process, a time, and finished products use high temperature, short time work
Skill can be sufficiently formed big crystal grain cluster, it is ensured that low energy dot matrix coincident grain boundary ratio is greater than 75%, especially twin boundary ratio
More than 60%, more it is essential that the connectivity of free crystal boundary is effectively interrupted, maximum is freely connected to crystal boundary length and free crystal boundary
The ratio of total length is less than or equal to 0.3（Lmax/Ltoal is less than or equal to 0.3）.
（3）Its preparation of CuNi alloy disclosed in this invention and cost of alloy are lower, and processing technology operation is feasible, has excellent
Different corrosion resistance is especially adaptable to the briny environment of chloride ion-containing and sodium ion.
Detailed description of the invention
Fig. 1 is the electron probe photo after 1 finished products of embodiment；
Fig. 2 is the electron probe photo after 2 finished products of comparative example；
Fig. 3 is that the Grain Boundary Character distribution map of embodiment 1 is freely connected to crystal boundary with maximum（MRCB）Extract figure；
Fig. 4 is that the Grain Boundary Character distribution map of comparative example 3 is freely connected to crystal boundary with maximum（MRCB）Extract figure.
Specific embodiment
The present invention is made a more thorough explanation below with embodiment.The present invention can be presented as a variety of different forms,
It should not be construed as limited to the exemplary embodiments described herein.
Embodiment 1：
A kind of high Niconmetal, specific chemical composition, by weight percent Ni：10.48%,Fe：1.61%, Mn：
0.99%, P：0.0054%, S：0.0047%, C：0.0074%, Y：0.021%, surplus is Cu ingredient.Wherein Y uses yttrium iron
Alloy is raw material；In yttrium iron alloy（By weight percent）Y should be controlled 60% to 70%；Y accounts for 65%, Fe and accounts for 35%；Manufactured conjunction
Golden performance is best.
Preparation process is as follows：
（1）Melting and casting is carried out by the ingredient of table 1, melting carries out in intermediate frequency furnace, and whole process is cast using nitrogen protection.Casting
Base is heated to 950 DEG C of heat preservation 1h, hot rolling is carried out on two roller hot-rolling mills, the start rolling temperature of hot rolling is 930 DEG C, and finishing temperature is
780 DEG C, deflection 55%, water cooling immediately after the completion of hot rolling；
（2）Once cold rolling technique：Cold rolling is carried out on 4-roller cold rolling mill, cold rolling reduction ratio is 72%；
（3）Intermediate annealing：Annealing temperature is 800 DEG C, annealing time 5min, and annealing atmosphere uses nitrogen protection；
（4）Secondary cold-rolling technique：Cold rolling is carried out on 4-roller cold rolling mill, cold rolling reduction ratio is 9%；
（5）Finished products：Annealing temperature is 800 DEG C, annealing time 10min, and annealing atmosphere uses nitrogen protection, after annealing
Water cooling.
Embodiment 2：
Difference from example 1 is that Ni by weight percent：10.09%,Fe：1.64%, Mn：0.89%, P：
0.0074%, S：0.0057%, C：0.0064%, Y：0.008%, surplus is Cu ingredient.
Embodiment 3：
Difference from example 1 is that Ni by weight percent：9.95%,Fe：1.66%, Mn：0.82%, P：
0.0054%, S：0.0052%, C：0.0074%, Y：0.017%, surplus is Cu ingredient.
Embodiment 4：
Difference from example 1 is that the deflection of secondary cold-rolling is 14% in the preparation process of CuNi system alloy.
Comparative example 1：
Difference from example 1 is that rare earth element is not added in CuNi system alloy, Ni by weight percent：10.38%,
Fe：1.76%, Mn：0.96%, P：0.0064%, S：0.0077%, C：0.0064%, surplus is Cu ingredient.
Comparative example 2：
Difference from example 1 is that content of rare earth increases in CuNi system alloy, Ni by weight percent：9.88%,Fe：
1.56%, Mn：1.02%, P：0.004%, S：0.0042%, C：0.0079%, Y：0.055%, surplus is Cu ingredient.
Comparative example 3：
The difference is that, secondary cold-rolling deflection is 3% with comparative example 1.
Comparative example 4：
The difference is that, secondary cold-rolling deflection is 32% with comparative example 1.
Based on above-mentioned, crystallite dimension, low energy dot matrix coincident grain boundary ratio have been carried out to the result of Examples and Comparative Examples（Packet
Include twin boundary）, it is maximum be freely connected to crystal boundary length and all free crystal boundary lenth ratios, as a result as shown in table 1 below：
The main Grain Boundary Character parameter and corrosive nature of 1 embodiment of table and comparative example
Remarks：The number of " * " is more, and representing alloy corrosion resistance can be better.
From the point of view of the comparison of Fig. 1 and Fig. 2, the content of rare earth in comparative example 2 is much higher than embodiment 1, therefore dilute in comparative example 2
Native complex inclusion（Black particle shape）It can increased significantly, and part inclusion distribution is in the position of crystal boundary.Work as the amount of inclusions
When increasing, on the one hand since size is larger, and it is distributed along crystal boundary, is easy to cause grain boundary corrosion；On the other hand, large inclusions
Quantity increases, and increases a possibility that regional area generates spot corrosion；Meanwhile, it is to be noted that crystal grain ruler can be refined to high rare-earth content
It is very little, so that crystal boundary ratio relative increase causes connectivity to enhance to improve the ratio of MRCB, so that alloy overall corrosion
It can decline.
From the point of view of the comparison of Fig. 3 and Fig. 4, the thermomechanical treatment process after adding rare earth is particularly important, logical in embodiment 1
Suitable rare earth addition and secondary cold-rolling are crossed, not only increases the ratio of low energy dot matrix coincident grain boundary, while but also freely
The connectivity of crystal boundary is destroyed, and the maximum ratio for being freely connected to crystal boundary and total free crystal boundary significantly reduces, this is highly beneficial
In improving its corrosive nature, however, when secondary cold-rolling deflection increases to 32%, crystal grain is refined, low energy in comparative example 3
The decline of dot matrix coincident grain boundary ratio, and the connectivity of free crystal boundary increases, and causes the probability along grain boundary corrosion to increase, alloy corrosion resistant
Corrosion can decline.
Above-mentioned example is only intended to illustrate the present invention, and in addition to this, also there are many different embodiments, and these are implemented
Mode be all those skilled in the art after comprehension inventive concept it is also envisioned that therefore, will not enumerate herein.
Claims (3)
1. a kind of preparation method of yttrium-base heavy rare earth corronil, which is characterized in that each in the yttrium-base heavy rare earth corronil
Ingredient percent is Ni:9~12%；Fe:1~2%；Mn:0.5~1.5%；S<0.01%； P<0.01%；C<0.01%；
Y：10~300ppm, other impurity contents<0.1%, surplus Cu；It is prepared using following steps：
1）Raw material is uniformly mixed according to the ratio, ingredient is made；
2）Melting：Melting must be protected using vacuum gas, nitrogen or argon gas can be used in protective gas；
3）Processing technology：Forging stock carries out hot rolling in 900~950 DEG C of 1~3h of heat preservation, and finishing temperature is not less than 750 DEG C, hot rolling deformation
Amount is greater than 50%；Once cold rolling deflection is greater than 70%, and secondary cold-rolling deflection will be between 7%~14%, and cold rolling twice
Total deformation is greater than 75%；
4）Heat treatment process：800~900 DEG C of softening annealing temperature range between cold rolling twice, time are 5~10 minutes；Finished product
850~900 DEG C of annealing region, the time is 10~15 minutes, using water cooling to room temperature after finished products.
2. preparation method as described in claim 1, which is characterized in that step 1）Described in ingredient Y using in Yttrium base rare earth
Between alloy；Step 2）When melting, the Yttrium base rare earth intermediate alloy is first not added, melting to liquidus temperature area keeps the temperature 3~5 minutes
Afterwards, Yttrium base rare earth intermediate alloy is added, is cast after keeping the temperature 1 minute again.
3. preparation method as claimed in claim 2, which is characterized in that the Yttrium base rare earth is yttrium iron alloy, by mass fraction
Wherein Y accounts for 60-70%, surplus Fe.
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Cited By (5)
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| CN111575530A (en) * | 2020-05-29 | 2020-08-25 | 无锡隆达金属材料有限公司 | Preparation method of copper alloy pipe resistant to high-pollution seawater corrosion |
| CN112195362A (en) * | 2020-09-17 | 2021-01-08 | 宝钛集团有限公司 | Preparation method of white copper strip for heat exchange of ship engine |
| CN113136501A (en) * | 2021-04-20 | 2021-07-20 | 台州市通顺铸造有限公司 | Preparation method of high-density antioxidant nickel-copper alloy |
| CN113237821A (en) * | 2021-04-26 | 2021-08-10 | 江西科技师范大学 | Preparation and detection method of yttrium-doped Inconel625 alloy applied to oxidative high-temperature chlorine corrosion environment |
| CN116262954A (en) * | 2021-12-14 | 2023-06-16 | 上海理工大学 | Seawater scouring corrosion resistant Ce-containing copper-nickel alloy and preparation method thereof |
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| CN113237821A (en) * | 2021-04-26 | 2021-08-10 | 江西科技师范大学 | Preparation and detection method of yttrium-doped Inconel625 alloy applied to oxidative high-temperature chlorine corrosion environment |
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| CN116262954A (en) * | 2021-12-14 | 2023-06-16 | 上海理工大学 | Seawater scouring corrosion resistant Ce-containing copper-nickel alloy and preparation method thereof |
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