CN107160059A - A kind of preparation of Ni base solders for soldering Nb Ti high temperature alloys and method for welding - Google Patents
A kind of preparation of Ni base solders for soldering Nb Ti high temperature alloys and method for welding Download PDFInfo
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- CN107160059A CN107160059A CN201710347319.5A CN201710347319A CN107160059A CN 107160059 A CN107160059 A CN 107160059A CN 201710347319 A CN201710347319 A CN 201710347319A CN 107160059 A CN107160059 A CN 107160059A
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- Prior art keywords
- solder
- soldering
- temperature
- alloys
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/008—Soldering within a furnace
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/20—Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3033—Ni as the principal constituent
Abstract
A kind of preparation of Ni base solders for soldering Nb Ti high temperature alloys and method for welding, belong to field of welding material.The component and content of solder are by atomic percentage in the present invention：Ni：60~70%, Ti：20~30%, Nb：5~15%.Ni Ti Nb high-temp solders are prepared using vacuum arc melting technology, using the solder vacuum brazing Nb Ti high temperature alloys, brazing temperature is 1050~1200 DEG C, and the holding time is 5 20min, and soldered fitting room temperature shear strength is up to more than 550MPa.Ni Ti Nb solders in the present invention are higher than traditional Ag bases, Al bases and Au base solder brazing temperature, can give full play to the high-temperature behavior of Nb Ti alloys.Using Ni Ti Nb solder brazing Nb based high-temperature alloys, its room temperature shear strength reaches more than 550MPa.The solder that the present invention is described can be additionally used in the soldering connection of other Ni bases, Ti bases and Nb based high-temperature alloys.
Description
Technical field
Prepared and method for welding the present invention relates to the solder for soldering Nb based high-temperature alloys, belong to field of welding material.
Background technology
Nb-Ti high temperature alloys are a kind of new (β Ti, Nb) solid solution alloys with body-centered cubic structure, and it has
The fusing point higher than nickel-base alloy, good temperature-room type plasticity and medium temperature intensity.Not only mechanical property is good for Nb-Ti alloys, Er Qie
The antioxygenic property that substantial amounts of Ti is greatly improved Nb alloys is added in Nb.According to the difference of Ti additions, these alloys it is close
Degree is generally 6.2-6.9g/cm3, and the density of high temperature alloy is generally 8.1-8.6g/cm3, therefore, Nb-Ti high temperature alloys can be with
Replace Ni and high temperature alloy and be applied on the critical component of spacecraft.As a kind of new high-temperature material, Nb-Ti is realized
The practical application of high temperature alloy, its Material Joining Technology is most important.At present, the interconnection technique of common high temperature alloy mainly has
Three kinds, respectively melting welding, diffusion welding (DW) and soldering.Wherein, soldering has many advantages, as brazing temperature is relatively low, can be right
The structure of complicated shape is attached, high accuracy connection can be achieved, and can realize dissimilar material joining, and technique is simple.
Therefore, soldering tech is widely applied in the connection area of high-temperature material.
At present, in common commercial solder, Ag bases, Al bases and Au base solder brazing temperature are relatively low, the reality of soldered fitting
Service temperature is generally lower than 500 DEG C, is not suitable for soldering (the Materials Science and of Nb-Ti high temperature alloys
Engineering A,2012,551:133-139).In high-temp solder, mainly based on Ni bases or Ti base solders, this kind of pricker
The brazing temperature of material is normally at 1000~1300 DEG C.Such as Ni-Cr, Ni-Cr-Si and Ni-Cr-B solder, Ti bases solder is such as
The solders such as Ti-Ni, Ti-Zr-Cu-Ni-Co, Ti-Cu-Ni, Ti-Ni-V and Ni-Ti-Nb are used for solder Ti3Al, TiNi, nickel
Based high-temperature alloy and Cf(the Journal of the European Ceramic Society 2003,23 such as/SiC ceramic matrix composite material:
547-553,Science and Technology of Welding and Joining,2011,16(2):193-198,
Materials Science and Engineering:A,2015,636:522-528).Use the soldered fitting of above-mentioned solder
Typically there is higher bond strength and good antioxygenic property, meanwhile, the element such as Ti, Cr and Nb is active element, can be with
Interfacial reaction occurs for common ceramics, improves the shear strength of soldered fitting.
For different matrix materials, the composition and content of solder also should be different, but relevant to Nb based high-temperature alloys at present
Welding report seldom, it is welded without suitable brazing material and related process, present invention mainly solves Nb-Ti
The problem of high temperature alloy correlation solder and soldering processes lack.
Realize that, to Nb-Ti high temperature alloy good connections, solder should meet the following aspects requirement with soldered fitting：①
Need to seek fusing point high solder as far as possible, with good antioxygenic property, to meet its applied at elevated temperature demand；2. solder with
Nb-Ti alloys have good wettability；3. the internal stress of soldered fitting should be than relatively low, with sufficiently high intensity.
The content of the invention
The problem of lacking present invention mainly solves the related solder of Nb-Ti high temperature alloys and soldering processes, there is provided a kind of vacuum
The preparation method and soldering processes of the solder of soldering Nb-Ti high temperature alloys, solder and method for welding of the invention can also be used for it
Its Ni base, Ti bases and Nb based high-temperature alloys.
Suitable solder is selected to be on active service under given conditions to pass again to obtaining high performance joint to meet matrix material
Will.Need to consider physics and chemical compatibility between solder and matrix material, wetability and the thermal expansion matched
The factors such as coefficient.
In order to strengthen the wettability of solder and Nb-Ti matrix alloys, make soldered fitting that there is higher intensity and antioxygen
Change performance, present invention selection Ni-Ti-Nb alloys are solder system.The solder system has the following aspects advantage：1. solder
In Ti elements and Nb elements be matrix essential element, it is ensured that solder and matrix have good wetability；2. pricker
Ni members in material have two aspect effects, are to adjust element as fusing point first, to adjust the fusing point of solder；Next to that Ni is first
Element can react with the Ti and Nb in matrix, generate NiTi2、NiTi、Ni3Ti、Ni3The intermetallic compounds such as Nb and NiNb, can be with
Reach good interface cohesion；3. Ni-Ti-Nb solders have good plasticity, this be conducive to soldered fitting plastic deformation and
The release of stress, while the alloy has excellent high temperature oxidation resistance.
A kind of preparation method of Ni base solders for soldering Nb-Ti high temperature alloys, it is characterised in that the component of solder and
Content is by atomic percentage：Ni：60~70%, Ti：20~30%, Nb：5~15%.The preferred component of above-mentioned solder is：
Ni：63~67%, Ti：20~25%, Nb：8~12%.
Above-mentioned solder is to follow these steps to be prepared from technique：
(1) preparatory stage：Electrolytic nickel (Ni) is chosen, titanium sponge (Ti), niobium block (Nb) is raw material, Ni purity exists
More than 99.95%, Ti and Nb purity reach more than 99.9%；Raw material acetone soln and alcoholic solution difference ultrasonic wave are clear
10~15min is washed, is dried at room temperature for；
(2) smelt stage：Before melting, vacuum in stove is evacuated to 0.1Pa first with mechanical pump, is kept for 2-4 minutes, beaten afterwards
Drive molecular pump and vacuum in stove is evacuated to 6 × 10-2More than Pa, is re-filled with high-purity argon gas；During melting, in order that alloying component is uniform
Change, alloy at least melt back more than 5 times, vacuum casting under function composite by electromagnetic stirring；Weighed after melting, sample weight loss exists
Within 0.1%, it is believed that alloy actual constituent and nominal composition are basically identical.
The solder microstructure prepared using the above method is as shown in Figure 1, it can be seen that solder Elemental redistribution is uniform, wherein
White chrysanthemum shape is (β Ti, Nb) continuous solid solution, and greyish white alternate sheet is eutectic structure { (β Ti, Nb)+Ti2Ni }, ash
Form and aspect are Ti2Ni phases, black is mutually rich-Ti phases.From the DSC curve (Fig. 2) of brazing filler metal alloy, the fusing point of the solder is about
945.7℃.Brazing temperature should be higher than that solder fusing point in brazing process, therefore set brazing temperature range as 1050~1200 DEG C.
Fig. 3 be Ni-Ti-Nb solders at 1150 DEG C Nb-Ti high-temperature alloy surfaces wetting dynamic curve, it can be seen that solder and
Nb-Ti high temperature alloys have good wetability, and wetting time is about 3min, and final angle of wetting is about 3.8 °.
The soldering processes of solder brazing Nb-Ti high temperature alloys prepared by the above method and technique are as follows：
(1) by wire cutting method by solder be cut into base shape identical thin slice to be welded, then using No. 2000 sand paper
It is about 200 μm to be polishing to thickness；Matrix surface to be welded is polished using No. 2000 sand paper simultaneously, matrix surface is removed
Oxide layer, be cleaned by ultrasonic with alcohol after solder and matrix material and dried up.
(2) solder is positioned between Nb based high-temperature alloys, is assembled into the structure of Nb-Ti/Ni-Ti-Nb/Nb-Ti alloys；
The structural member is put into vacuum brazing furnace, it is 3.0 × 10 to be then evacuated to vacuum-3More than Pa, with 5 DEG C/min speed liters
Temperature is to 1050~1200 DEG C of brazing temperature, 5~20min of soldering connection；Then with stove vacuum cooled to room temperature, welding is completed.
In the present invention, it is ensured that the key of Nb-Ti/Ni-Ti-Nb soldered fitting shear strengths is crisp in control soldered fitting
The generation of property phase.Fig. 4 is the microstructure photo of soldering 15min Nb-Ti/Ni-Ti-Nb soldered fittings at 1150 DEG C, can be with
Find out can there is four kinds of phases, (β Ti, Nb) continuous solid solution, (β of chrysanthemum shape of respectively bright grey simultaneously in seam organization
Ti, Nb)+TiNi eutectic structures, the Ti of Dark grey2The rich Ti phases of Ni intermetallic compounds, black.Wherein first two is mutually toughness
Phase, latter two is mutually brittlement phase.When the holding time is shorter, in seam organization be mainly (β Ti, Nb) continuous solid solution, (β Ti,
, also there is the brittle Ti in part in Nb)+TiNi eutectic structures2Ni intermetallic compounds, with the extension of holding time, weld seam group
(β Ti, Nb) continuous solid solution, (β Ti, Nb)+TiNi eutectic structures in knitting all disappear, and are only left brittle Ti2Ni metals
Between compound, richness Ti phases, therefore the holding time is long, and can cause the shear strength of soldered fitting reduces.But when holding time mistake
In short-term, although solder has good wettability, the time too short alloying element and base that can cause in solder with matrix
Precursor reactant and diffusion are insufficient, make the intensity of welding point equally relatively low.Therefore the preferred scope of above-mentioned process conditions is：Soldering
1100~1150 DEG C of temperature, 10~15min of soldering connection.
The beneficial effects of the invention are as follows：Ni-Ti-Nb solders in the present invention are than traditional Ag bases, Al bases and Au base solders
Brazing temperature is high, can give full play to the high-temperature behavior of Nb-Ti alloys.Closed using Ni-Ti-Nb solder brazing Nb bases high temperature
Gold, its room temperature shear strength reaches more than 550MPa.It is high that the solder that the present invention is described can be additionally used in other Ni bases, Ti bases and Nb bases
The soldering connection of temperature alloy.
Brief description of the drawings
The Ni-Ti-Nb solder as-cast structure photos that Fig. 1 is prepared for the present invention；
The DSC curve figure for the solder that Fig. 2 is prepared for the present invention；
Wetting dynamic curves of the Fig. 3 for the solder of the invention prepared at 1150 DEG C in Nb-Ti high-temperature alloy surfaces；
Fig. 4 is that Ni-Ti-Nb solders are 1150 DEG C in brazing temperature, the soldering connection time be 15min under conditions of, welding
The electron backscattered photo of joint；
Embodiment
The solder of soldering Nb based high-temperature alloys is prepared, the component and content of solder are by atomic percentage：Ni：65%, Ti：
25%, Nb：10%.
Solder preparation technology is as follows：
(1) preparatory stage：Electrolytic nickel (Ni) is chosen, titanium sponge (Ti), niobium block (Nb) is raw material, Ni purity exists
More than 99.95%, Ti and Nb purity reach more than 99.9%；Raw material acetone soln and alcoholic solution are successively ultrasonic respectively
Ripple cleans 10~15min, is dried at room temperature for；
(2) smelt stage：Before melting, vacuum in stove is evacuated to 0.1Pa first with mechanical pump, is kept for 3 minutes, opened afterwards
Vacuum in stove is evacuated to 6 × 10 by molecular pump-2More than Pa, is re-filled with high-purity argon gas；During melting, in order that alloying component is homogenized,
Alloy at least melt back more than 5 times, vacuum casting under function composite by electromagnetic stirring；Weighed after melting, sample weight loss 0.1% with
It is interior, it is believed that alloy actual constituent and nominal composition are basically identical.
Soldering process step is as follows：
(1) solder is cut into by the thick thin slices of 0.5mm, shape and Nb based high-temperature alloys table to be welded by Wire EDM method
Face is identical, and solder and matrix remove removing oxide layer with No. 2000 SiC sand paper polishings, then surpass solder and matrix in alcoholic solution
Sound wave cleans 10~15min, is dried at room temperature for；
(2) say that solder and matrix are assembled into Nb-Ti/Ni-Ti-Nb/Nb-Ti structure, be put into vacuum brazing furnace, then
It is 3.0 × 10 to be evacuated to vacuum-3More than Pa, 1050~1200 DEG C of brazing temperature, soldering connection 10 are warming up to 5 DEG C/min
~20min；Finally with stove vacuum cooled to room temperature, welding is completed.
Embodiment：
Brazing temperature chooses 1050 DEG C, 1100 DEG C, 1150 DEG C and 1200 DEG C respectively, the soldering connection time be 10min,
15min and 20min.Following table lists brazing temperature, the soldering connection that Ni-Ti-Nb solders in 12 groups of embodiments weld Nb based alloys
Time and the Mechanical test results of soldered fitting：
Above-described embodiment shows, is located at 1100-1150 DEG C in brazing temperature, the holding time is 10-15min, soldered fitting
Shear strength can reach more than 550MPa, the good welds of Nb-Ti high temperature alloys can be achieved.
Claims (4)
1. a kind of preparation method of Ni base solders for soldering Nb-Ti high temperature alloys, it is characterised in that the component of solder and contain
Measure and be by atomic percentage：Ni：60~70%, Ti：20~30%, Nb：5~15%；Specifically preparation process is：
(1) preparatory stage：Choose electrolytic nickel (Ni), titanium sponge (Ti), niobium block (Nb) is raw material, Ni purity 99.95% with
On, Ti and Nb purity reach more than 99.9%；Raw material clean 10 with acetone soln and alcoholic solution difference ultrasonic wave~
15min, is dried at room temperature for；
(2) smelt stage：Before melting, vacuum in stove is evacuated to 0.1Pa first with mechanical pump, is kept for 2-4 minutes, is opened divide afterwards
Vacuum in stove is evacuated to 6 × 10 by sub- pump-2More than Pa, is re-filled with high-purity argon gas；During melting, in order that alloying component is homogenized,
Alloy at least melt back more than 5 times, vacuum casting under function composite by electromagnetic stirring.
2. the preparation method of the Ni base solders for soldering Nb-Ti high temperature alloys described in claim 1, it is characterised in that Ni
Base solder is by the scope of atomic percentage：Ni：63~67%, Ti：20~25%, Nb：8~12%.
3. a kind of method of Ni bases solder brazing Nb-Ti high temperature alloys described in use claim 1 or 2, it is characterised in that soldering
Technique is as follows：
(1) solder is cut into and base shape identical thin slice to be welded, then No. 2000 sand paper polishings of use by wire cutting method
Thickness is polishing to for 200 μm；Matrix surface to be welded is polished using No. 2000 sand paper simultaneously, the oxidation of matrix surface is removed
Layer, is cleaned by ultrasonic solder with being dried up after matrix material with alcohol；
(2) solder is positioned between Nb based high-temperature alloys, is assembled into the structure of Nb-Ti/Ni-Ti-Nb/Nb-Ti alloys；Should
Structural member is put into vacuum brazing furnace, and it is 3.0 × 10 to be then evacuated to vacuum-3More than Pa, is warming up to 5 DEG C/min speed
1050~1200 DEG C of brazing temperature, 5~20min of soldering connection；Then with stove vacuum cooled to room temperature, welding is completed.
4. the method for soldering Nb-Ti high temperature alloys as claimed in claim 3, it is characterised in that brazing conditions technique is：Soldering temperature
Spend for 1100~1150 DEG C, the holding time is 10~15min, finally with stove vacuum cooled.
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| CN201710347319.5A CN107160059A (en) | 2017-05-17 | 2017-05-17 | A kind of preparation of Ni base solders for soldering Nb Ti high temperature alloys and method for welding |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110539048A (en) * | 2019-08-01 | 2019-12-06 | 航天材料及工艺研究所 | Brazing connection method of rhenium-carbon/carbon composite material and niobium |
| CN114131295A (en) * | 2021-11-26 | 2022-03-04 | 中国航发北京航空材料研究院 | Diffusion welding method adopting Ti-Nb alloy as intermediate layer |
| CN114346519A (en) * | 2022-03-04 | 2022-04-15 | 哈尔滨工业大学 | High-entropy brazing filler metal for TiAl alloy brazing and preparation method and application thereof |
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| CN101653884A (en) * | 2009-07-15 | 2010-02-24 | 哈尔滨工业大学 | High-temperature brazing filler metal |
| CN102489859A (en) * | 2011-12-16 | 2012-06-13 | 长春三友汽车部件制造有限公司 | Method for improving mechanical property of advanced high-strength steel spot welding joint |
| CN103567664A (en) * | 2013-10-30 | 2014-02-12 | 西安理工大学 | Ti-Ni welding wire for welding Ti-pipeline steel composite board and preparation method of Ti-Ni welding wire |
| CN105252169A (en) * | 2015-09-14 | 2016-01-20 | 安徽工程大学 | Active amorphous brazing filler metal for brazing ZrB2-SiC ceramic materials, preparation method for active amorphous brazing filler metal and brazing process |
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| US4883640A (en) * | 1988-06-17 | 1989-11-28 | Gte Products Corporation | Titanium-niobium-nickel brazing alloy |
| CN101653884A (en) * | 2009-07-15 | 2010-02-24 | 哈尔滨工业大学 | High-temperature brazing filler metal |
| CN102489859A (en) * | 2011-12-16 | 2012-06-13 | 长春三友汽车部件制造有限公司 | Method for improving mechanical property of advanced high-strength steel spot welding joint |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110539048A (en) * | 2019-08-01 | 2019-12-06 | 航天材料及工艺研究所 | Brazing connection method of rhenium-carbon/carbon composite material and niobium |
| CN110539048B (en) * | 2019-08-01 | 2021-08-10 | 航天材料及工艺研究所 | Brazing connection method of rhenium-carbon/carbon composite material and niobium |
| CN114131295A (en) * | 2021-11-26 | 2022-03-04 | 中国航发北京航空材料研究院 | Diffusion welding method adopting Ti-Nb alloy as intermediate layer |
| CN114346519A (en) * | 2022-03-04 | 2022-04-15 | 哈尔滨工业大学 | High-entropy brazing filler metal for TiAl alloy brazing and preparation method and application thereof |
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Application publication date: 20170915 |