CN1883861A - Method for preparing carbon-base material-copper connector used as thermonuclear reactor component under high heat flux - Google Patents

Method for preparing carbon-base material-copper connector used as thermonuclear reactor component under high heat flux Download PDF

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Publication number
CN1883861A
CN1883861A CNA2006100896429A CN200610089642A CN1883861A CN 1883861 A CN1883861 A CN 1883861A CN A2006100896429 A CNA2006100896429 A CN A2006100896429A CN 200610089642 A CN200610089642 A CN 200610089642A CN 1883861 A CN1883861 A CN 1883861A
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carbon
solder
copper
layer
brazing
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CN100436019C (en
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周张健
钟志宏
都娟
宋书香
葛昌纯
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Beijing University of Technology
University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/10Nuclear fusion reactors

Abstract

Provided is a preparation of carbon-based material-copper connector used for hybrid reactor high-heat load member, belonging to high-heat load member carbon-based material and copper base alloy system integration technical field. The process comprises selecting amorphous Ti-based active solder as a connecting material at the mass percent for each component of 40 to 50% Ti, 25 to 35% Zr, 20 to 10% Cu, 15 to 5% Ni with the thickness of 20 to 30mu, inserting an interlayer between the carbon-based material and the copper for stress release, shining flatly the solder, copper block and interlayer material after machining, followed by cleaning with acetone, sintering and putting the carbon-based material into a vacuum furnace after its pending welding surface is machined and polished and soldering in vacuum in resistance radiation heating method. The method is characterized in using the high activity of the amorphous Ti-based active solder, reducing the joining temperature while improving the wetting property of solder to the carbon-based material and solving the problem of thermal stress between the carbon-based material and the copper due to mismatching of coefficient of thermal expansion.

Description

Be used as the preparation method of the carbon-based material-copper connector of fusion reactor high heat load parts
Technical field
The invention belongs to high heat load parts carbon-based material and acid bronze alloy system integration technology field, a kind of preparation method who is used as the carbon-based material-copper connector of fusion reactor high heat load parts particularly is provided.
Background technology
Carbon-based material (carbon/carbon compound material and doped graphite etc.) is to be used widely in the fusion assay device in the face of the important candidate material of plasma parts in the magnetic constraint fusion reactor.Except its low atomic number, carbon-based material has other excellent performances, comprises superior anti-thermal shock ability, high-melting-point, and high thermal conductivity and thermal fatigue property are good etc.Copper (Cu) and alloy thereof then are that a kind of fusing point is lower but the extraordinary metal of thermal conductivity is selected as heat sink material in nuclear fusion experimental device.In actual use, carbon-based material and copper need be combined as using in the face of the plasma parts.But because the two physical property is widely different, the connector that obtain practical and effective carbon-based material/copper is not a thing easily.Countries such as U.S., day, method, Russia, moral, English all take much count of the connection research of these materials, have obtained remarkable progress.China also takes much count of the work of this respect, in national high-tech research Outline Development Plan, newly conceive the exploration problem specially to " solder technology of tungsten, graphite and copper alloy " project verification, as sub-problem that needs exploration in the energy technology theme as new ideas.But the work that China carries out at present in this respect also seldom.People such as the Zou Guisheng of Tsing-Hua University have made two kinds of Ag bases of crystalline state and amorphous state solder by oneself high-strength graphite and being connected of copper have been carried out Primary Study.
Preparing the effective a kind of method of this material is the active soldering method, promptly inserts solder between carbon-based material and copper (alloy), is heated to certain temperature under certain atmospheric condition solder is dissolved, and both are coupled together.Technology is simple, bonding strength good owing to having, as a result good reproducibility, size for connection and shape restricted less, have medium resistance to elevated temperatures, relative cost low, adapt to series of advantages such as industrial-scale production and become the prefered method that metal and pottery are connected, present great vitality.
People such as H.Ise adopt Ag-Cu-Ti and two kinds of active solders of Ag-Cu-Ti-In that carbon/carbon compound material is connected with copper alloy, but ban use of Ag in the nuclear fusion device, and the Cd that can be transformed into high vapour pressure because of Ag behind the irradiation pollutes plasma.People such as P.W.Trester thereby used Cu base solder, people such as P.Appendino then select 70Ti-15Cu-15Ni (wt%) alloy to be used to connect C/C composite and copper.
But because physics, the chemical property of carbon-based material and copper have very big-difference, the subject matter that method for brazing exists is: a) wetability of reaction interface is poor, compatibility is poor, is difficult to obtain the good interface combination; B) interfacial reaction complexity, it is many to generate the phase kind, and the butt joint Effect on Performance is bigger; C) because the thermal expansion coefficient difference of carbon-based material and copper is very big and the inhomogeneities of structure, joint often exists very big residual stress, thereby has had a strong impact on the intensity of joint, even causes connection failure.Thereby influenced the actual use of this material.This also is the greatest problem that this material faces in actual applications.Therefore should note the stress at carbon-based material-transition zone-copper (alloy) three interface when preparing this material, design rational structure more.
Realize that another kind of effective ways that carbon-based material is connected with copper are reactive metal casting (Active Metal Casting, the AMC that introduce in the patent by Austrian Plansee company ).Because the wetability of copper and carbon is very poor, therefore can not directly go up cast copper liquid toward CFC.Handle the surface of CFC earlier with special laser treatment technique, do like this is in order to obtain funnelform duck eye (about 50~500 μ m of diameter of a large amount of sealings on the surface of CFC, about 100~750 μ m of the degree of depth), reach the purpose that increases contact area and stop the crackle expansion.Then the fine copper of liquid state is cast in the surface of CFC, after solidifying, the surface of processing fine copper.In order to make technology oversimplify and reduce the cost of reactive metal casting technique, J.J.Cordier has avoided laser processing technique, and elder generation through chemical erosion, carries out surface modification treatment on the surface of C/C again before the casting, directly pours into a mould copper liquid then.
Though the connector remelting temperature height (1083 ℃) and the degree of reliability height that adopt the reactive metal casting technique to obtain,, this method technology more complicated, cost height.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who is used as the carbon-based material-copper connector of fusion reactor high heat load parts.According to work characteristics and performance requirement, adopt not amorphous Ti base solder active soldering carbon-based material and copper under vacuum condition of argentiferous as nuclear fusion stack limiter parts.
Of the present invention constituting:
1, adopts amorphous Ti base solder brazing technology to connect carbon-based material and copper, adopt sheet metals such as fine copper, molybdenum as the intermediate layer relief of thermal stress.Comprise following main points:
A, solder composition: in order to improve wetability between carbon-based material and the copper, to improve the adhesion between the interface and reduce and be connected temperature, select commercial amorphous Ti based active solder as connecting material, its composition weight is Ti (40~50%), Zr (25~35%), Cu (20~10%), Ni (15~5%), thickness are 20~30 μ m.Therefore Cu, Ni, Zr and Ti can form eutectic, can be used as the element that reduces the solder fusing point and add, and can obtain Ti-Zr-Cu-Ni is alloy.Compare with common crystalline state solder of the same race, the amorphous filler metal composition is even, intensity height, good toughness, the diffusion that helps heating atom in the connection procedure and interfacial reaction, with carbon-based material have better wetability.
B, intermediate layer material: for reducing the residual stress that carbon-based material and copper cause owing to thermal coefficient of expansion does not match, the intermediate layer that needs between carbon-based material and copper, to insert 1-3 kind relieve stresses.Intermediate layer material can adopt Mo, Cu, Ni, Ti, W etc. to have certain thickness (0.1~0.5mm) thin slice.
Prepare before c, the weldering: solder, copper billet and intermediate layer material is after machined, smooth with sand papering, clean up with acetone, dry standby; To be welded of carbon-based material after machined, polishing, in sintering furnace, handled 5~6 hours in 250 ℃~350 ℃ degassings.Der group according to Cu → solder → (intermediate layer → solder) → carbon-based material installs from the bottom to top, is placed in the weld jig then, and puts into vacuum drying oven.
D, soldering: adopt resistance radiation heating mode to carry out vacuum brazing, technological parameter is: vacuum is not less than 10-2Pa, heating rate Tr=10~20K/min, and insulation 5min~10min is so that the temperature of weldment is even when 1023K~1123K; Brazing temperature T=1153K~1223K, holding time of brazing t=5min~15min, rate of temperature fall T d=4K/min~10K/min.In order to make the thickness that weld seam is fine and close and control weld seam, can apply certain pressure during soldering, scope is between 0.01~0.1MPa.
The advantage of this technology is: by adopting the high activity of amorphous Ti based active solder, reduced the connection temperature when improving solder to the carbon-based material wetability, solved the problem that carbon-based material is difficult to soldering; Utilize the mode of inserting the intermediate layer, solved the thermal stress issues that carbon-based material and copper cause owing to thermal coefficient of expansion does not match.
Description of drawings
Fig. 1 is the joint pattern of doped graphite of the present invention/TiZrCuNi/ copper, T=1173K, t=5min.
Fig. 2 is the joint pattern of doped graphite of the present invention/TiZrCuNi/ copper, T=1173K, t=15min.
Fig. 3 is the X-ray diffraction spectrum at linkage interface of the present invention place, solder/copper interface.
Fig. 4 is the X-ray diffraction spectrum at linkage interface of the present invention place, solder/graphite interface.
Fig. 5 for the joint pattern of doped graphite/solder of the present invention/intermediate layer/copper and elemental line scan figure (T=1173K, t=15min), the joint pattern.
Fig. 6 for the joint pattern of doped graphite/solder of the present invention/intermediate layer/copper and elemental line scan figure (T=1173K, t=15min), elemental line scan.
The specific embodiment
Embodiment: do not add the comparison of the doped graphite/copper mold piece of intermediate layer and adding composite interlayer
The no intermediate layer that utilized method for preparing and insert the doped graphite/copper mold piece of composite interlayer.The size of doped graphite and copper is respectively 30mm * 30mm * 6mm and 30mm * 30mm * 1.5~30mm.
(1) do not add direct soldered fitting pattern in intermediate layer and constituent analysis
Fig. 1 is 1173K with copper being connected temperature to doped graphite for adopting the Ti-Zr-Ni-Cu amorphous brazing filler metal, carries out the pattern that soldering is connected copper and doped graphite interblock brazing layer under the condition of contact of insulation 5min and 15min.As can be seen: linkage interface is high-visible, and whole joint is not found tangible crackle and pore.In inner irregular black patch, grey piece, white portion and the thread zone of hair of occurring of solder.The X-ray energy spectrometer constituent analysis that each zone among the figure is carried out shows and has occurred multiple intermetallic compound in the brazed seam that copper content in brazed seam improves, and illustrates that dissolving and diffusion to a certain degree taken place in solder copper in brazing process; And it is higher at the junction of graphite and solder Ti content.Illustrate bigger affinity is arranged between C and the Ti.In the joint pattern photo of Fig. 1 (b) as can be seen: brazed seam thickness is about 140 μ m, and whole joint is not found tangible crackle and pore yet.Solder and graphite are having tangible conversion zone to occur at the interface, black patch that the size that distributing in the conversion zone is similar and the grey piece that adheres to interface growth, and these materials are linked to be elongated black-tape in the graphite side; On the interface of solder and copper, do not find tangible conversion zone, but combine relatively goodly, do not find tangible pore and not seam phenomenon with copper; Comparison diagram 1 (a) and (b) as can be known, when temperature retention time more in short-term, the active element in the solder is that partial zones is poly-partially or evenly distribute in solder basically, and is less to the interfacial diffusion of graphite, almost do not have the formation of carbide, fails to form metallurgical the connection; C in solder and Ti in graphite, spread and react to each other and need time enough.After prolonging temperature retention time, help improving the activity and the diffusivity of active element, promote the generation of chemical reaction.
In order to determine the interfacial reaction phase, adopt X-ray diffraction successively to peel off method and determined that weld seam reaches the existence form of newborn compound at the interface.Fig. 2 is brazing temperature T=1173K, the X-ray diffraction spectrum at linkage interface place under the temperature retention time t=15min condition.Wherein Fig. 2 (a) is the joint face XRD figure spectrum of solder and copper, from Fig. 3 (a) as can be seen, CuTi wherein 2, CuTi, Cu 3Ti, CuZr 2, CuZr, Ni 3Ti, TiNi are that solder reaction generates phase, and Cu is a mother metal.By the relative intensity and the half-peak breadth size of each product characteristic peak, CuTi in the product as can be known 2, Cu 3Ti, CuZr 2, the content of TiNi is higher.Because the performance of metal and intermetallic compound is more approaching, can infer that solder and Cu have formed the intracrystalline metallurgical binding.Fig. 2 (b) is solder and doped graphite joint face XRD figure spectrum, as we can see from the figure, at the interface except there being multiple intermetallic beyond the region of objective existence, also find to have TiC and a spot of ZrC, and making that forming the metallurgical principal element that is connected between solder and the graphite is the formation of newborn compound TiC, it is to be formed by the C atom combination of Ti in the solder and graphite.Intermetallic compound is the compound of solder inside, in survey place at the interface their existence, two kinds of possibilities are described: 1) carbide lamella of Xing Chenging is discontinuous, therefore, directly contact or the solder of molten condition is penetrated into by capillarity in the hole and capillary channel of graphite at the regional area intermetallic compound with graphite; 2) carbide lamella is very thin, and X ray has certain penetration power, and the multiple intermetallic compound in the solder tissue of carbide lower floor may be measured simultaneously.This result is consistent in the result of interface phase counterdiffusion with Ti and C that the scanning of electron probe face records.
Though find in the experiment that microexamination shows that being connected of carbon-based material and copper is good, macroscopic view goes up the soldering sample and is prone to cracking phenomena in four edges and corners of doped graphite, does not meet the requirement of actual use.This is because the physics between carbon-based material and copper the two and the interface product, mechanical property different, the thermal coefficient of expansion between them particularly than big-difference, make the bigger residual thermal stress of generation in the cooling procedure center tap, the existence of this internal stress, when serious weld seam inside is cracked, reduced the bonding strength of joint even directly caused the cracking of graphite, needed to add the intermediate layer to relax thermal stress.
(2) add Mo/Cu composite interlayer joint pattern and constituent analysis
In order to relax the residual stress of joint, doped graphite is connected with copper by adopting the Mo/Cu composite interlayer.Flawless occurs on the soldering sample macroscopic view.Fig. 3 is the joint pattern and the elemental line scan figure of doped graphite/solder/intermediate layer/copper.After using the Mo/Cu composite interlayer as can be seen from Fig. 3 (a), joint is not found crackle and pore equally.By electron probe the interface microcell is carried out line sweep, from Fig. 3 (b) as can be seen: the Ti element is near graphite curve low curve ripple when high when occurring, illustrating that the Ti element is alternately distributed herein, might be that this zone has the compound of Ti or solid solution to generate in brazing process.About 50 μ m places still can see the distribution of Ti element at distance graphite/solder interface, and diffusion has to a certain degree taken place in graphite Ti as can be known; What is interesting is that the Zr element has carried out fairly large diffusion in Mo, illustrate that the diffusivity of Zr in Mo is more intense; Distribution curve explanation Ni and the Cu of Ni and Cu almost do not spread in graphite.Adopt shearing method that the soldering sample is tested, it is as shown in the table for the result, as can be known: at 950 ℃, under the condition of insulation 10min, use the shear strength of 0.23mmCu/0.2mmMo/0.23mmCu composite interlayer acquisition sample the highest.

Claims (1)

1, a kind of preparation method who is used as the carbon-based material-copper connector of fusion reactor high heat load parts is characterized in that:
A, solder composition: select amorphous Ti based active solder as connecting material, its composition weight is Ti:40~50%, Zr:25~35%, and Cu:20~10%, Ni:15~5%, thickness are 20~30 μ m; Cu, Ni, Zr and Ti form eutectic, and obtaining Ti-Zr-Cu-Ni is alloy;
B, intermediate layer material: the intermediate layer of between carbon-based material and copper, inserting 1~3 kind of relieve stresses; Intermediate layer material has Mo, Cu, Ni, Ti or W to have the thin slice of thickness 0.1~0.5mm;
Prepare before c, the weldering: solder, copper billet and intermediate layer material is after machined, smooth with sand papering, clean up with acetone, dry standby; To be welded of carbon-based material after machined, polishing, in sintering furnace, handled 5~6 hours in 250 ℃~350 ℃ degassings; Der group according to Cu → solder → intermediate layer → solder → carbon-based material installs from the bottom to top, is placed on then in the weld jig, puts into vacuum drying oven;
D, soldering: adopt resistance radiation heating mode to carry out vacuum brazing, technological parameter is: vacuum is not less than 10 -2Pa, heating rate Tr=10~20K/min, insulation 5min~10min is so that the temperature of weldment is even when 1023K~1123K; Brazing temperature T=1153K~1223K, holding time of brazing t=5min~15min, rate of temperature fall T d=4K/min~10K/min; Apply the pressure of 0.01~0.1MPa during soldering.
CNB2006100896429A 2006-07-07 2006-07-07 Method for preparing carbon-base material-copper connector used as thermonuclear reactor component under high heat flux Expired - Fee Related CN100436019C (en)

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Cited By (11)

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CN101845578A (en) * 2010-05-15 2010-09-29 徐州工程学院 First wall part made of doped tungsten-based composite material and preparation method thereof
CN102009239A (en) * 2010-10-15 2011-04-13 北京航空航天大学 Connection method used for carbon based materials and products thereof
CN101315814B (en) * 2008-06-28 2011-07-13 中国科学院等离子体物理研究所 Vacuum feed port ceramic sealing structure of ion-turbulent resonance heating antenna
CN102218594A (en) * 2011-06-24 2011-10-19 武汉理工大学 Low-temperature diffusion welding method for molybdenum alloy and copper alloy
CN102430874A (en) * 2011-11-01 2012-05-02 北京工业大学 Titanium-based amorphous brazing alloy foil strip for brazing and preparation method for foil strip
CN103658904A (en) * 2012-09-04 2014-03-26 核工业西南物理研究院 Vacuum brazing connection technology for tungsten copper composite block
CN103949802A (en) * 2014-04-23 2014-07-30 华南理工大学 Ti-Zr-Cu-Ni-Co-Mo amorphous brazing filler metal and preparing method thereof
CN106271213A (en) * 2015-05-22 2017-01-04 成都飞机工业(集团)有限责任公司 A kind of titanium-zirconium-copper-nickel-based solder for titanium alloy soldering
CN106392367A (en) * 2016-11-22 2017-02-15 江苏阳明船舶装备制造技术有限公司 Solder for brazing red copper and graphite and brazing method
CN106695043A (en) * 2016-12-22 2017-05-24 核工业西南物理研究院 Carbon base material and copper brazing connection method
CN111496414A (en) * 2020-04-01 2020-08-07 武汉工程大学 Graphite and copper joint and preparation method thereof

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US5855313A (en) * 1997-04-08 1999-01-05 Mcdonnell Douglas Corporation Two-step brazing process for joining materials with different coefficients of thermal expansion
CN100376353C (en) * 2005-11-29 2008-03-26 西北工业大学 Carbon/carbon composite and titanium alloy welding method

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101315814B (en) * 2008-06-28 2011-07-13 中国科学院等离子体物理研究所 Vacuum feed port ceramic sealing structure of ion-turbulent resonance heating antenna
CN101845578A (en) * 2010-05-15 2010-09-29 徐州工程学院 First wall part made of doped tungsten-based composite material and preparation method thereof
CN102009239B (en) * 2010-10-15 2012-09-05 北京航空航天大学 Connection method used for carbon based materials and products thereof
CN102009239A (en) * 2010-10-15 2011-04-13 北京航空航天大学 Connection method used for carbon based materials and products thereof
CN102218594A (en) * 2011-06-24 2011-10-19 武汉理工大学 Low-temperature diffusion welding method for molybdenum alloy and copper alloy
CN102430874A (en) * 2011-11-01 2012-05-02 北京工业大学 Titanium-based amorphous brazing alloy foil strip for brazing and preparation method for foil strip
CN103658904B (en) * 2012-09-04 2016-01-20 核工业西南物理研究院 A kind of tungsten copper composite block vacuum brazing Joining Technology
CN103658904A (en) * 2012-09-04 2014-03-26 核工业西南物理研究院 Vacuum brazing connection technology for tungsten copper composite block
CN103949802A (en) * 2014-04-23 2014-07-30 华南理工大学 Ti-Zr-Cu-Ni-Co-Mo amorphous brazing filler metal and preparing method thereof
CN103949802B (en) * 2014-04-23 2016-05-04 华南理工大学 A kind of Ti-Zr-Cu-Ni-Co-Mo amorphous brazing filler metal and preparation method thereof
CN106271213A (en) * 2015-05-22 2017-01-04 成都飞机工业(集团)有限责任公司 A kind of titanium-zirconium-copper-nickel-based solder for titanium alloy soldering
CN106392367A (en) * 2016-11-22 2017-02-15 江苏阳明船舶装备制造技术有限公司 Solder for brazing red copper and graphite and brazing method
CN106695043A (en) * 2016-12-22 2017-05-24 核工业西南物理研究院 Carbon base material and copper brazing connection method
CN111496414A (en) * 2020-04-01 2020-08-07 武汉工程大学 Graphite and copper joint and preparation method thereof

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