CN103286473A - TiZr base amorphous alloy with low Cu and Ni contents and preparation method thereof - Google Patents
TiZr base amorphous alloy with low Cu and Ni contents and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a TiZr base amorphous alloy with low Cu and Ni contents and a preparation method thereof, and belongs to the technical field of welding. The TiZr base amorphous alloy is suitable for brazed connection of one kind of material or dissimilar materials such as titanium alloy, TiAl intermetallic compound, steel and ceramic. The components of brazing filler metal comprises, by mass percent, Cu accounts for 3-15%, Ni accounts for 1-10%, Si accounts for 0.1-2%, X accounts for 0.5-8%, Y accounts for 0.1-8%, and Ti and Zr account for the rest, wherein the X represents Co or Fe or Co and Fe, Y represents Al or Sn or Al and Sn. Thin band-shaped amorphous alloy brazing filler metal as thick as 20-50 microns is obtained through the rapid solidification technology. Compared with the prior titanium base brazing filler metal and TiZr base amorphous alloy brazing filler metal, the brazing filler metal made of the TiZr base amorphous alloy with low Cu and Ni contents has the advantages that the fusing point is low, the contents of Cu and Ni are low (lower than 20%), and soldered joints are good in property, high in reliability and wide in application range.
Description
Technical field
The invention belongs to welding technology field, specifically disclose TiZr base noncrystal alloy solder of a kind of low Cu and Ni content and preparation method thereof.
Background technology
Soldering has become one of accurate important solder technology that connects of high-technology field parts as a kind of metal fever method of attachment.In the numerous factors that determine brazing quality, solder is in critical role.Advantages such as the titanium-base alloy solder has active height, hear resistance, corrosion resistance is good, antioxygenic property is excellent, the soldering processes performance is good are a kind of solders that has application prospect.Early stage in the titanium-base alloy Solders Research, people attempt adding elements such as Cu, Ni, Zr, Be, Co, V in alloy, and to reduce the solder fusing point, the main alloy element of existing titanium-base alloy solder is Cu, Ni, Zr, Be etc.The unlimited solid solution of Zr and Ti can not produce the fragility phase among the adding Ti, allow addition more, and Zr can improve the intensity of alloy under the situation that does not significantly reduce titanium alloy plasticity.Secondly, it is neutral that Zr is in titanium alloy, very little to its α/beta transus temperature influence; In addition, Zr can form eutectic with Cu, Ni, and being expected to obtain low-melting Ti-Zr-Cu-Ni is alloy.Therefore, Zr is one of main adding elements of titanium-base alloy solder.Adding alloying element cu, Ni etc. in the Ti base solder alloy, is to reduce alloy melting point on the one hand, is the combination property that improves joint by the effect of alloying on the other hand.But existing titanium-base alloy solder Cu and Ni content are higher, generate the frangible compounds phase after the soldering, as Ti
2Cu, Ti
2Ni, δ-TiCu and Ti
3Cu
4Deng, soldered fitting is easy to generate fragility in various degree, and the performance of soldered fitting is reduced.And the poor processability of titanium-base alloy solder own, foil preparation be difficulty, has limited the type of service of solder.
Therefore, develop a kind of low melting point, the novel high-performance TiZr base noncrystal alloy solder of low Cu and Ni content has very important meaning for high-technology fields such as Aero-Space.
Summary of the invention
Technical problem to be solved by this invention is: overcome the deficiencies in the prior art, provide a kind of fusing point low, Cu and Ni content are low, the soldered fitting performance is good, reliability is high, cost is low, TiZr base noncrystal alloy solder applied widely, and a kind of corresponding preparation method is provided.
The technology of the present invention solution: TiZr base noncrystal alloy solder of a kind of low Cu and Ni content and preparation method thereof, wherein solder becomes to be grouped into elements such as relating to Ti, Zr, Cu, Ni, Co, Fe, Al, Sn, Si.Wherein, except Ti, Zr, Cu, Ni, Si element, all the other alloying elements are trace to be added.By mass percentage, solder consists of: Cu3～15%, and Ni1～10%, Si0.1～2%, X0.5～8%, Y0.1～8%, surplus is Ti and Zr, and wherein X represents Co or Fe or Co and Fe, and Y represents Al or Sn or Al and Sn.Compare with existing titanium based solder, under Cu, Ni content situation still less, thereby can reduce the mechanical property that improves soldered fitting of separating out of compound between brittle metal; Do not contain precious metal element and poisonous element in the composition, reduced use cost, the Safety and Environmental Protection height.
The diversification of alloying element is added main effect with trace among the present invention: the one, reduce the solder liquidus temperature; The 2nd, the amorphous formation ability of raising brazing filler metal alloy; The 3rd, the combination property of enhancing soldered fitting.Wherein, each alloying element of trace interpolation mainly acts on as follows:
Cu: improve the wetability of brazing filler metal alloy, the flowability after the fusing, be conducive to strengthen the soldered fitting corrosion resistance;
Ni: reduce the activity of Ti, improve soldered fitting high temeperature chemistry and mechanical property;
Co: suppress or reduce the diffusion of Cu, Ni, improve soldered fitting mechanical behavior under high temperature and serviceability temperature;
Fe: strengthen the flowability of brazing filler metal alloy, improve soldered fitting hardness;
Al: as the grain refinement element, improve mechanical property and the non-oxidizability of soldered fitting;
Sn: reduce the solder fusing point, crystal grain thinning;
Si: the wetability that strengthens brazing filler metal alloy; Room temperature and elevated temperature strength, non-oxidizability and corrosion resistance as grain refinement element raising soldered fitting reduce fracture toughness.
In the present invention, for reducing production costs, pure titanium, pure zirconium can be substituted by titanium sponge, the sponge zirconium of purifying through electric arc melting, with further reduction use cost.
As shown in Figure 1, the preparation method of the TiZr base noncrystal alloy solder of the low Cu of the present invention and Ni content is as follows:
(1) take by weighing each element simple substance:
According to mass percent Cu3～15%, Ni1～10%, Si0.1～2%, X0.5～8%, Y0.1～8%, surplus is Ti and Zr, and wherein X represents Co or Fe or Co and Fe, and Y represents Al or Sn or Al and Sn, takes by weighing the metal simple-substance raw material of respective quality;
(2) melting prepares alloy:
The metal simple-substance raw material that takes by weighing is placed electric arc melting equipment, and being evacuated to vacuum is 4 * 10
-3～6 * 10
-3Pa charges into high-purity Ar gas, and the mode molten alloy of employing electric arc heated at least 4 times treats that alloy cooling back from the smelting equipment taking-up, makes alloy;
(3) the melt spinning method legal system is equipped with amorphous alloy ribbon:
Adopting the mode of Mechanical Crushing with step 2) alloy that makes is preset in the quartz ampoule that exit width is 0.2～0.3mm after being broken into fritter, and integral body places the liquid quench solidification equipment, regulates quartz ampoule lowermost end and copper wheel surface 1.5～5mm apart;
Be 9 * 10 with being evacuated to vacuum in the liquid quench coagulation system cavity
-2Pa charges into high-purity Ar gas;
Regulate liquid quench solidification device the copper wheel rotating speed (30～50m/s), expulsion pressure (0.03～0.06MPa), (0.02～0.04MPa) to suitable numerical value, and wherein gas jet, strip gas all adopt high-purity Ar gas for gas stripping pressure;
Adopt the alloy of the mode fused quartz Guan Zhongyi fragmentation of eddy-current heating, treat that alloy melts fully and after fluctuating appears in liquid level, close heating power supply, start injection apparatus immediately, after under the gas jet effect alloy liquation being injected into the copper wheel surface rapidly cooling obtain continuously, toughness and the good amorphous alloy ribbon of surface quality.
Adopting the resulting amorphous alloy thin tape thickness of above-mentioned preparation method is 20～50 μ m, and continuously, any surface finish, strip edge be smooth, good-toughness.And the non-crystaline amorphous metal solder can be prepared into highly purified powdered filler metal or other type of service.
The structure and the hot property that adopt X-ray diffractometer and differential scanning calorimeter to test above-mentioned strip, the liquidus temperature scope of TiZr base noncrystal alloy solder is 860 ℃～920 ℃, brazing temperature range is 900 ℃～950 ℃.Before the soldering, titanium alloy uses 60#, 200#, 600# sand papering surface successively, and amorphous alloy ribbon and titanium alloy adopt ultrasonic wave to clean to remove impurity such as surface and oil contaminant successively in acetone, absolute ethyl alcohol, distilled water then, take out dry.Soldered fitting adopts overlapping mode, amorphous alloy ribbon is preset in forms titanium alloy/non-crystaline amorphous metal solder/titanium alloy sandwich between the titanium alloy sheet.Above-mentioned soldering work piece is placed vacuum brazing furnace.Treat that vacuum reaches 1.0 * 10
-3～5.0 * 10
-3Pa begins to be warming up to 600 ℃ with 20 ℃/min programming rate, insulation 5～10min, and the programming rate with 10 ℃/min is warming up to required brazing temperature then, closes heating system behind insulation 5～15min, and braze-welded structure cools to room temperature with the furnace.In brazing process, the vacuum system continuous firing also keeps vacuum to be better than 1 * 10
-2Pa.
The present invention compared with prior art has the following advantages:
(1) Cu of the present invention and Ni content are low, and two element mass percent sums are lower than 20%, and compound is few between soldered fitting place generation brittle metal, have improved the mechanical property of soldered fitting greatly, particularly adopt Ti
50Zr
27Cu
8Ni
4Co
3Fe
2Al
3Sn
2Si
1The maximum shear strength of the soldered fitting that (atomic percent %) soldering TC4 alloy obtains can reach 428MPa.
(2) diversification of solder alloy and element trace adds has good action to the preparation of solder and the performance of soldered fitting, and the first, aspect non-crystaline amorphous metal formation, improved the amorphous formation ability of TiZr base noncrystal alloy solder; The second, aspect hot property, reduced alloy melting point, solved that Cu and Ni content reduce and problem that fusing point is raise; The 3rd, aspect weldingmetallurgy, improved the performance of joint.
(3), thickness continuous according to composition among the present invention, the resulting non-crystaline amorphous metal solder of preparation method strip evenly, toughness and surface quality be good.
Description of drawings
Fig. 1 is the preparation flow figure of the inventive method.
Fig. 2 is non-crystaline amorphous metal solder Ti in the embodiment of the invention 1
50Zr
27Cu
8Ni
4Co
3Fe
2Al
3Sn
2Si
1X-ray diffraction (XRD) collection of illustrative plates of (atomic percent %).
Fig. 3 is non-crystaline amorphous metal solder Ti in the embodiment of the invention 1
50Zr
27Cu
8Ni
4Co
3Fe
2Al
3Sn
2Si
1The DSC curve that the employing difference formula scanning amount method of (atomic percent %) obtains.
The specific embodiment
Introduce the present invention in detail below in conjunction with drawings and the specific embodiments.But following embodiment only limits to explain the present invention, and protection scope of the present invention should comprise the full content of claim, is not limited only to present embodiment.
Embodiment 1:
Composition (mass percent): Ti38.40%, Zr39.50%, Cu8.15%, Ni3.77%, Co2.84%, Fe1.79%, Al1.30%, Sn3.81%, Si0.44%, i.e. Ti
50Zr
27Cu
8Ni
4Co
3Fe
2Al
3Sn
2Si
1(atomic percent %).
The preparation method:
(1) takes by weighing each element simple substance: the metal simple-substance raw material that takes by weighing respective quality according to mass percent;
(2) melting prepares alloy: the metal simple-substance raw material that step (1) is taken by weighing places electric arc melting equipment, and being evacuated to vacuum is 5 * 10
-3Pa charges into high-purity Ar gas, and the mode molten alloy of employing electric arc heated 4 times treats that alloy takes out from smelting equipment with stove cooling back, makes alloy;
(3) the melt spinning method method prepares amorphous alloy ribbon: be preset in the quartz ampoule that exit width is 0.2mm after the alloy that the mode of employing Mechanical Crushing makes step (2) is broken into fritter, and integral body places the liquid quench coagulation system, regulates quartzy mouth of pipe lowermost end and copper wheel surface at a distance of 1.5mm; Be 9 * 10 with being evacuated to vacuum in the liquid quench coagulation system cavity
-2Pa charges into high-purity Ar gas; The copper wheel rotating speed of regulating liquid quench solidification device is 40m/s, sprays and press to 0.05MPa, gas stripping pressure are 0.03MPa that wherein gas jet, strip gas all adopt high-purity Ar gas; Adopt the alloy of pulverizing in the mode fused quartz pipe of eddy-current heating, treat that alloy melts fully and after fluctuating appears in liquid level, close heating power supply, start injection apparatus immediately, after under the gas jet effect alloy liquation being injected into the copper wheel surface rapidly cooling obtain continuously, toughness and the good strip of surface quality.
By XRD collection of illustrative plates shown in Figure 2 as can be seen, adopt embodiment 1 strip of method for preparing to be shown as the diffuse scattering peak through the X-ray diffraction detection, can confirm as non crystalline structure.
DSC curve shown in Figure 3 represents to adopt differential scanning calorimeter test heat flow to the relation curve of temperature, and as shown in Figure 3, the solder liquidus temperature among the embodiment 1 is 907 ℃, and soldering can temperature be carried out more than it.
To adopt the non-crystaline amorphous metal solder of present embodiment preparation at vacuum brazing furnace brazing TC4 (Ti-6Al-4V) alloy.Before the soldering, the TC4 alloy uses 60#, 200#, 600# sand papering surface successively, and amorphous alloy ribbon and TC4 alloy adopt ultrasonic wave to clean to remove impurity such as surface and oil contaminant successively in acetone, absolute ethyl alcohol, distilled water then, take out dry.Soldered fitting adopts overlapping mode, the banded solder of amorphous alloy thin is preset in forms TC4/ non-crystaline amorphous metal solder/TC4 sandwich between the TC4 alloy sheets.This structure is placed the high temperature resistant stainless steel square box, with obtain evenly, temperature field accurately.Said apparatus is placed vacuum brazing furnace.Treat that vacuum reaches 1.5 * 10
-3Pa begins to be warming up to 600 ℃ with 20 ℃/min programming rate, insulation 10min, and the programming rate with 10 ℃/min is warming up to 930 ℃ then, closes heating system behind the insulation 15min, the vacuum system operate as normal, braze-welded structure cools to room temperature with the furnace.In brazing process, the vacuum system continuous firing also keeps vacuum 3 * 10
-3About Pa.To be cooled to room temperature, in vacuum brazing furnace, take out, test its relevant mechanical property.
The related data of non-crystaline amorphous metal solder and soldering processes sees the following form among the embodiment 1:
Have the part difference except element mass fraction, soldering standard, welding base metal among the embodiment 2～28, all the other conditions are identical with embodiment 1.Embodiment 2～28 related contents see the following form:
In the last table, soldering mother metal shape such as A, the expression welding base metal is same material A; Shape such as B/C, the expression welding base metal is foreign material B and C.Soldering mother metal Ti
3Al represents Ti
3Al base alloy Ti-24Al-15Nb-1Mo(atomic percent %), TiAl represents TiAl base alloy Ti-24Al-15Nb-1Mo(atomic percent %), Si
3N
4Expression Si
3N
4Pottery, Al
2O
3Expression Al
2O
3Pottery.
The above only is preferred example of the present invention, not in order to limit the present invention.All equivalence or simple change of doing according to the described composition design of patent of the present invention, preparation method are included in the scope of patent protection of the present invention.
Need to prove that though amorphous alloy component generally adopts atomic percent to represent, composition represents all to adopt mass percent in welding field, thereby amorphous alloy component all is scaled mass percent by atomic percent and is indicated among the present invention.
In addition, according to the various embodiments described above of the present invention, those skilled in the art are the four corners that can realize independent claims of the present invention and appurtenance fully, implementation procedure and method same the various embodiments described above; And the non-elaborated part of the present invention belongs to techniques well known.
The above; only for the part specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any those skilled in the art are in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (3)
1. the TiZr base noncrystal alloy solder of a low Cu and Ni content, it is characterized in that: described solder is made up of element more than seven kinds or seven kinds, and essential elements is: Ti, Zr, Cu, Ni, Si; The solder composition is Cu:3～15% by mass percentage, Ni:1～10%, and Si:0.1～2%, X:0.5～8%, Y:0.1～8%, surplus is Ti and Zr, and wherein X represents Co or Fe or Co and Fe, and Y represents Al or Sn or Al and Sn; Cu and Ni mass percent are below 20%, and Ti and Zr mass percent are more than 75%.
2. the method for the TiZr base noncrystal alloy solder of a low Cu who prepares claim 1 and Ni content is characterized in that performing step is as follows:
(1) take by weighing each element:
According to element mass percent Cu3～15%, Ni1～10%, Si0.1～2%, X0.5～8%, Y0.1～8%, surplus is Ti and Zr, and wherein X represents Co or Fe or Co and Fe, and Y represents Al or Sn or Al and Sn, takes by weighing respective metal simple substance raw material;
(2) melting prepares alloy:
The metal simple-substance raw material that step (1) is taken by weighing places electric arc melting equipment, and being evacuated to vacuum is 4 * 10
-3～6 * 10
-3Pa charges into high-purity Ar gas as protection gas, and the mode molten alloy of employing electric arc heated at least 4 times treats that alloy takes out from smelting equipment with stove cooling back, makes alloy;
(3) the melt spinning method method prepares amorphous alloy ribbon:
The alloy that adopts the mode of Mechanical Crushing that step (2) is made is broken into and is preset in outlet chi width behind the fritter is in the quartz ampoule of 0.2～0.3mm, and integral body places the liquid quench solidification equipment, regulates quartz ampoule lowermost end and copper wheel surface 1.5～5mm apart;
Be 9 * 10 with being evacuated to vacuum in the liquid quench solidification equipment cavity
-2Pa charges into high-purity Ar gas;
Regulate copper wheel rotating speed 30～50m/s, expulsion pressure 0.03～0.06MPa, the gas stripping pressure 0.02～0.04MPa of liquid quench solidification equipment, wherein gas jet, strip gas all adopt high-purity Ar gas;
Adopt the alloy of the mode fused quartz Guan Zhongyi fragmentation of eddy-current heating, broken alloy melts fully and occurs closing heating power supply after the fluctuation at liquid level, start injection apparatus immediately, under the gas jet effect, the alloy liquation is injected into the copper wheel surface by cooling rapidly obtain continuously, toughness and the good amorphous alloy ribbon of surface quality.
3. non-crystaline amorphous metal solder preparation method according to claim 2, it is characterized in that: enough obtain thickness at the amorphous alloy ribbon of 20～50 μ m by regulating the copper wheel rotating speed and spraying pressure energy in the described step (3), adjustments of gas is peeled off to press and is promoted that strip separates with copper wheel, and accelerates the cooling of copper wheel.
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| CN108356443A (en) * | 2018-02-07 | 2018-08-03 | 郑州大学 | Titanium-based amorphous solder and its preparation method and application |
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| CN108971801A (en) * | 2018-08-24 | 2018-12-11 | 华南理工大学 | A kind of Ti-Zr-Ni-Fe-Cu-Co-Mo-B solder and the preparation method and application thereof |
| CN109604861A (en) * | 2018-11-16 | 2019-04-12 | 南京理工大学 | For connecting the iron-based solder of TiAl alloy Yu Ni based high-temperature alloy |
| CN109500514A (en) * | 2019-01-15 | 2019-03-22 | 衢州学院 | For ZrO2With the preparation method and application technique of the brazing material of TC4 soldering |
| CN110172612A (en) * | 2019-05-10 | 2019-08-27 | 河北工业大学 | A kind of high-strength corrosion-resistant erosion titanium zirconium-base alloy and preparation method thereof |
| CN113134693A (en) * | 2021-04-30 | 2021-07-20 | 吉林大学 | Cu-based amorphous solder for brazing tungsten-based powder alloy and preparation method and application thereof |
| CN115592298A (en) * | 2022-11-04 | 2023-01-13 | 辽宁工业大学（Cn） | TiZr-based amorphous solder vacuum brazing Ti60 titanium alloy and preparation method thereof |
| CN116038174A (en) * | 2023-02-21 | 2023-05-02 | 北京航空航天大学 | Nickel-based amorphous alloy brazing material with high W content and preparation method and application thereof |
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