CN106583967A - TiH2-Ni-Cu-TiC composite welding flux as well as preparing method and application thereof - Google Patents
TiH2-Ni-Cu-TiC composite welding flux as well as preparing method and application thereof Download PDFInfo
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- CN106583967A CN106583967A CN201710028946.2A CN201710028946A CN106583967A CN 106583967 A CN106583967 A CN 106583967A CN 201710028946 A CN201710028946 A CN 201710028946A CN 106583967 A CN106583967 A CN 106583967A
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- graphite
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Classifications
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- 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
-
- 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
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
-
- 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
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Ceramic Products (AREA)
Abstract
The invention relates to a TiH2-Ni-Cu-TiC novel composite welding flux as well as a preparing method and an application thereof. The novel composite welding flux is prepared by ball-milling the following raw materials in a percent by weight: 13-17% of Cu powder, 58-62% of TiH2 powder, 23-27% of Ni powder and 1-5% of TiC powder. The obtained composite welding flux is mainly used for the preparation of a graphite and copper alloy connector in nuclear fusion and automobile industries. The preparing method of the connector comprises the following steps: mixing the TiH2-Ni-Cu-TiC novel composite welding flux and glycerol, preparing into a paste, coating the to-be-connected surfaces of treated graphite and copper alloy with the paste, connecting the to-be-connected surfaces, applying load, and carrying out brazing. Brazing is carried out under the conditions that heat is preserved at 890-940DEG C for 8-13min, and applied pressure is 10kPa. The preparing method of the composite welding flux, which is provided by the invention, is simple, and the cost of the raw materials is low. A graphite and copper alloy joint which is prepared by using the composite welding flux has the advantages that the interface layer of the joint is well bonded, is free of cracks, is porous and the like. The average shear strength of the joint can reach 15.2MPa and is 81.7% of the strength of a graphite base material.
Description
Technical field
The invention belongs to carbon-based material technical field, and in particular to a kind of TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder and its
Preparation method and application.
Background technology
Material with carbon element stable chemical performance, it is difficult to other substance reactions, be the brush that prepared in direct current generator at present or change
One of preferred material to device copper work surface, but the preparation of this new carbon commutator is related to the connection of carbon/copper.Additionally,
Facing plasma material is very important material in nuclear fusion stack, and material with carbon element has good compatibility with plasma,
Be connected with copper alloy can by irradiation produce a large amount of conduction of heat go out, so towards plasma bias filter component be also required to by
Material with carbon element and Cu alloys are attached.
Copper is difficult to moistening in graphite surface, also there is larger hot mispairing between graphite and copper.These difficult points cause to adopt
When the graphite and Cu alloys of general solder connection, connector failure or bonding strength are relatively low.The solder of research is mainly wrapped at present
Include AgCuTi, NiCrP, NiCrPCu, CuSiAlTi and amorphous state TiZrCuNi solder etc..But existing solder is present
Problem.For example, AgCuTi solders effect when fine vacuum soldering graphite is connected with copper is preferable but expensive；TiZrCuNi is welded
Expect for amorphous state, preparation is more bothered；Additionally, the P element addition contained in solder can reduce the electric conductivity of joint.
The content of the invention
The purpose of the present invention is for problems of the prior art, there is provided a kind of TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE
Solder and its preparation method and application.The TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders can be used to connect graphite and Cu alloys,
Its preparation method is simple, easy to use, safe and reliable.
For achieving the above object, the present invention adopts following technical proposals：
A kind of TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that prepared by following raw material by weight percentage
Form：
Cu powder：13%～17%；
TiH2Powder：58%～62%；
Ni powder：23%～27%；
TiC powder：1%～5%.
The present invention is also provided and prepares above-mentioned TiH2The preparation method of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that
Comprise the steps：By Cu powder, TiH2Powder, Ni powder and ball milling is formed during TiC powder is put into ball mill.
By such scheme, it is preferable that the Cu powder, TiH2Powder, the particle diameter of Ni powder are 45～55 μm, the grain of the TiC powder
Footpath is 1～5 μm.
By such scheme, it is preferable that the ball milling speed of the ball mill is 250～350rpm, and Ball-milling Time is 2～3h.
Present invention also offers above-mentioned TiH2The application of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that made
It is used to connect graphite and Cu alloys for solder, to prepare graphite/Cu alloy brazed joints.
The TiH2The schematic diagram of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solder connection graphite and Cu alloys is shown in Fig. 1.
Present invention also offers the soldered fitting of a kind of graphite and Cu alloys, it is characterised in that it is using above-mentioned TiH2-
Ni-Cu+TiC NEW TYPE OF COMPOSITE solder connection is obtained.
By such scheme, it is preferable that the Cu alloys are CuCrZr alloys or red copper.
Present invention also offers the preparation method of the soldered fitting of above-mentioned graphite and Cu alloys, it is characterised in that under including
State step：By TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder is applied to graphite or Cu alloys with glycerol hybrid modulation into paste
Face to be connected on, the face to be connected of close graphite and Cu alloys, soldering.
By such scheme, it is preferable that the graphite passes through polishing, washing and drying treatment with the face to be connected of Cu alloys；
Wherein, the cleaning is to be cleaned by ultrasonic 30min with acetone or ethanol.
By such scheme, it is preferable that the condition of the soldering is：In the vacuum under pressure soldering of 10kPa, the temperature of soldering
For 890～940 DEG C, the temperature retention time of soldering is 8～13min.
By such scheme, it is preferable that before the temperature for reaching the soldering, also comprise the steps：First with 10 DEG C/
The ramp of min is incubated 1h to 500 DEG C, makes the ethanol or glycerol volatilization in solder；Again with the ramp of 10 DEG C/min
To 800 DEG C, be incubated 30min, make solder before melting with mother metal with sufficiently contact；Then added with the ramp of 5 DEG C/min
Heat is to the brazing temperature.
By such scheme, it is preferable that when carrying out the soldering, the graphite for closing and the face to be connected of Cu alloys are placed in graphite
In mould.
The ultimate principle of the present invention is as follows：
TiH2Powder decomposes the Ti elements of generation at high temperature, can improve wettability of the solder in graphite surface very well.TiC
Can be as phase reinforcing joint be strengthened, additionally, the TiC of low thermal coefficient of expansion can reduce the thermal expansion between solder layer and graphite
Difference of coefficients, alleviates the residual thermal stress of joint, so as to improve graphite/Cu alloy-junction performances.
Compared to prior art, main advantages of the present invention are：
(1) present invention is by TiH2Adding TiC in-Ni-Cu solders strengthens phase, and articulamentum is strengthened, obtained
TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders can be used for the connector for preparing graphite and Cu alloys.
(2) TiH that the present invention is provided2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders preparation method is simple, easy to use, safely may be used
Lean on.
(3) present invention prepares TiH2In the method for-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, powder body material used is commercially available
Commodity, it is with low cost.
(4) TiH that the present invention is obtained2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder is used to connect graphite and Cu alloys, gained
The joint interface layer of connector is well combined, not it was observed that the defect such as crackle and hole, mean intensity is up to graphite strength of parent
81.7%.
Description of the drawings
Cu alloys/TiH that Fig. 1 is provided for the present invention2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldering connection sample dress
With schematic diagram.
Fig. 2 is CuCrZr alloys/TiH obtained in Application Example 12- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldering
The SEM figures in the joint interface region of joint, wherein left part are CuCrZr alloys, and right part is graphite, and zone line is
Thick about 80 μm solder layer.
Fig. 3 is CuCrZr alloys/TiH obtained in Application Example 12- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldering
The XRD spectrum in the joint interface region of joint.
Specific embodiment
For a better understanding of the present invention, present disclosure is further elucidated with reference to embodiment, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
TiH2The preparation of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, comprises the following steps that：
By Cu powder that particle diameter is 45～55 μm, TiH2Powder, Ni powder and the TiC powder that particle diameter is 1～5 μm, according to quality percentage
Than for Cu powder 14.7%, TiH2Powder 59%, Ni powder 24.3%, 2% dispensing of TiC powder are simultaneously put in ball mill, with the speed of 300rpm
Rate ball milling 2.5h, is obtained TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders.
Embodiment 2
TiH2The preparation of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, comprises the following steps that：
By Cu powder that particle diameter is 45～55 μm, TiH2Powder, Ni powder and the TiC powder that particle diameter is 1～5 μm, according to quality percentage
Than for Cu powder 14%, TiH2Powder 58%, Ni powder 24%, 4% dispensing of TiC powder are simultaneously put in ball mill, with the speed ball of 350rpm
Mill 2h, is obtained TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders.
Application Example 1
By obtained TiH in embodiment 12- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder is used to connect graphite and CuCrZr alloys,
Prepare CuCrZr alloys/TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldered fitting, comprises the following steps that：
1) by the face to be connected of graphite and CuCrZr alloys sand paper grinding and polishing step by step, then it is cleaned by ultrasonic in acetone
30min, dries up stand-by.
2) TiH obtained in Example 12- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, are added thereto to a small amount of glycerol, modulation
Into paste, uniform application is Jing step 1) process after graphite and CuCrZr alloys face to be connected on, face to be connected of closing obtains
To " CuCrZr alloys-NEW TYPE OF COMPOSITE solder-graphite " connector in " sandwich " shape.
3) by step 2) obtained " CuCrZr alloys-NEW TYPE OF COMPOSITE solder-graphite " connector is placed in graphite jig, then
It is put in vacuum drying oven, intensification soldering is carried out under 10kPa pressure：First, it is heated to from room temperature with the heating rate of 10 DEG C/min
, then 1h is incubated at 500 DEG C, make the ethanol and glycerol volatilization in solder by 500 DEG C；Again will with the heating rate of 10 DEG C/min
Sample is heated to 800 DEG C from 500 DEG C, and 800 DEG C be incubated 30min, make solder before melting with mother metal be fully contacted；Then
900 DEG C are heated to the heating rate of 5 DEG C/min and 10min is incubated；Finally, stop heating, take out after cooling to room temperature with the furnace
Sample, obtains CuCrZr alloys/TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldered fitting.
By CuCrZr alloys/TiH obtained in the present embodiment2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldered fitting exists
The test of shear strength is carried out on electronic universal tester, is as a result shown：The average shear strength of the joint is reachable
15.2MPa, is the 81.7% of graphite strength of parent (18.6MPa).
As it is clear from fig. 2 that CuCrZr alloys/TiH obtained in the present embodiment2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite pricker
The solder layer shape appearance figure even compact of plumb joint, solder are combined very well with graphite and CuCrZr alloys, not it was observed that space and splitting
Stricture of vagina.
From figure 3, it can be seen that CuCrZr alloys/TiH obtained in the present embodiment2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/stone
The joint interface region of black soldered fitting is mainly by the intermetallic compound such as Cu (s, s), TiC, Ti-Cu-Ni, Cu-Ti and Ti-Ni
Composition.
Application Example 2
By obtained TiH in embodiment 22- Ni-Cu+TiC composite solders are used to connect graphite and red copper, prepare red copper/
TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldered fitting, comprises the following steps that:
1) by the face to be connected of graphite and red copper sand paper grinding and polishing step by step, then it is cleaned by ultrasonic 30min in acetone,
Dry up stand-by.
2) TiH obtained in Example 22- Ni-Cu+TiC composite solders, are added thereto to a small amount of glycerol, are modulated into cream
Shape, uniform application is Jing step 1) process after graphite and red copper face to be connected on, face to be connected of closing, is in " Sanming City
Control " " red copper-NEW TYPE OF COMPOSITE solder-graphite " connector of shape.
3) by step 2) obtained " red copper-NEW TYPE OF COMPOSITE solder-graphite " connector is placed in graphite jig, places into true
In empty stove, intensification soldering is carried out under 10kPa pressure：First, 500 DEG C are heated to from room temperature with the heating rate of 10 DEG C/min,
Then 1h is incubated at 500 DEG C, make the ethanol and glycerol volatilization in solder；Again with the heating rate of 10 DEG C/min by sample from
500 DEG C are heated to 800 DEG C, and 800 DEG C be incubated 30min, make solder before melting with mother metal with sufficiently contact；Then with 5
DEG C/heating rate of min is heated to 910 DEG C and is incubated 9min；Finally, stop heating, after cooling to room temperature with the furnace, take out sample,
Obtain red copper/TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldered fitting.
Jing is tested, red copper/TiH obtained in the present embodiment2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder/graphite soldered fitting interface
It is well combined.
Claims (12)
1. a kind of TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that prepared by following raw material by weight percentage and
Into：
Cu powder：13%～17%；
TiH2Powder：58%～62%；
Ni powder：23%～27%；
TiC powder：1%～5%.
2. the TiH described in claim 12The preparation method of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that including following
Step：By Cu powder, TiH2Powder, Ni powder and ball milling is formed during TiC powder is put into ball mill.
3. TiH according to claim 22The preparation method of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that described
Cu powder, TiH2Powder, the particle diameter of Ni powder are 45～55 μm, and the particle diameter of the TiC powder is 1～5 μm.
4. TiH according to claim 22The preparation method of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that described
The ball milling speed of ball mill is 250～350rpm, and Ball-milling Time is 2～3h.
5. the TiH described in claim 12The application of-Ni-Cu+TiC NEW TYPE OF COMPOSITE solders, it is characterised in that as solder
For connecting graphite and Cu alloys, to prepare graphite/Cu alloy brazed joints.
6. the soldered fitting of a kind of graphite and Cu alloys, it is characterised in that it is using the TiH described in claim 12-Ni-Cu+
TiC NEW TYPE OF COMPOSITE solder connection is obtained.
7. the soldered fitting of graphite according to claim 6 and Cu alloys, it is characterised in that the Cu alloys are CuCrZr
Alloy or red copper.
8. graphite described in claim 6 or 7 and the preparation method of the soldered fitting of Cu alloys, it is characterised in that including following
Step：
By TiH2- Ni-Cu+TiC NEW TYPE OF COMPOSITE solder and glycerol hybrid modulation are applied to treating for graphite or Cu alloys into paste
On joint face, the face to be connected of close graphite and Cu alloys, soldering.
9. the preparation method of the soldered fitting of graphite according to claim 8 and Cu alloys, it is characterised in that the graphite
Polishing, washing and drying treatment are passed through with the face to be connected of Cu alloys；Wherein, the cleaning is to be cleaned by ultrasonic with acetone or ethanol
30min。
10. the preparation method of the soldered fitting of graphite according to claim 8 and Cu alloys, it is characterised in that the pricker
The condition of weldering is：In the vacuum under pressure soldering of 10kPa, the temperature of soldering is 890～940 DEG C, the temperature retention time of soldering is 8～
13min。
The preparation method of the soldered fitting of 11. graphite according to claim 10 and Cu alloys, it is characterised in that reaching
Before the temperature of the soldering, also comprise the steps：
First with the ramp of 10 DEG C/min to 500 DEG C, 1h is incubated；Again with the ramp of 10 DEG C/min to 800 DEG C, insulation
30min；Then the brazing temperature is heated to the ramp of 5 DEG C/min.
The preparation method of the soldered fitting of 12. graphite according to claim 8 and Cu alloys, it is characterised in that carry out institute
When stating soldering, the graphite for closing and the face to be connected of Cu alloys are placed in graphite jig.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710028946.2A CN106583967B (en) | 2017-01-16 | 2017-01-16 | A kind of TiH2- Ni-Cu+TiC composite solder and its preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710028946.2A CN106583967B (en) | 2017-01-16 | 2017-01-16 | A kind of TiH2- Ni-Cu+TiC composite solder and its preparation method and application |
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| CN106583967A true CN106583967A (en) | 2017-04-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113600947A (en) * | 2021-07-28 | 2021-11-05 | 西安理工大学 | Method for improving strength of copper-graphite joint through waveform interface |
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| CN113600947B (en) * | 2021-07-28 | 2023-03-10 | 西安理工大学 | Method for improving strength of copper-graphite joint through waveform interface |
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| CN106583967B (en) | 2018-12-14 |
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