CN109570669A - A kind of preparation method of multilayer high temperature resistant composite anode - Google Patents
A kind of preparation method of multilayer high temperature resistant composite anode Download PDFInfo
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- CN109570669A CN109570669A CN201811585145.7A CN201811585145A CN109570669A CN 109570669 A CN109570669 A CN 109570669A CN 201811585145 A CN201811585145 A CN 201811585145A CN 109570669 A CN109570669 A CN 109570669A
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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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
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Abstract
The invention discloses a kind of preparation method of multilayer high temperature resistant composite anode, this method comprises: one, the first metal layer, second metal layer and non-metallic layer prepared according to target product composite anode respectively, and successively stack from top to bottom;Two, the first solder is added between face in stacking for the first metal layer and second metal layer;Three, the second solder is added between face obtain composite anode clip in bimetallic stack of the after stating non-metallic layer and adding the first solder;Four, composite anode clip is subjected to high-temperature vacuum thermal compression welding, makes to form transition zone between second metal layer and non-metallic layer, then processed obtain composite anode.The present invention first processes each layer of composite anode, then each layer is successively stacked and addition solder carries out vacuum hotpressing welding between the layers, obtain composite anode, it is connected using the High temperature diffusion of each interlayer, so that transition rule between each bed boundary, interface is clear, ensure that the high temperature resistance of composite anode, reduces the dynamic balancing deviation of composite anode.
Description
Technical field
The invention belongs to anode material preparation technical fields, and in particular to a kind of preparation side of multilayer high temperature resistant composite anode
Method.
Background technique
When CT machine X-ray tube works, about 98% or more energy will change while anode target is generated X-ray by electron bombardment
For thermal energy, and heat is concentrated mainly on anode.This heat is distributed in the anode with certain tilt angle being rotating
On target surface, a circular heating surface area is formed.Due to rotary anode in vacuum environment and under conditions of alternation thermic load
It uses, in continuous load, entire anode target temperature can rise very high, and environment temperature when X-ray tube works is at 1300 DEG C
More than, heat dissipation relies primarily on heat radiation.Tungsten has many advantages, such as that fusing point is high, steam forces down, density is big and atomic number is high,
It can guarantee and generate a large amount of X-rays under beam bombardment, can be used as anode material;But the thermal capacity of pure tungsten is small, heat dissipation performance
Difference.Graphite has very high thermal capacity and heat-sinking capability and high thermal stress resistance ability.By W/Mo composite layer and different thickness
Three high joining of graphite of degree as a whole, can largely reduce anode volume and weight, improve anode service life.
In terms of x-ray anode preparation, the relevant technologies intellectual property and document are delivered seldom both at home and abroad,
CN101290852A is using powder metallurgical technique together with graphite once sintered molding at high temperature;US4119879 is in tungsten interlayer
Addition rare earth element does transition zone;CN102124537A, CN103050357A, CN 104350574A are with basic material and knot
Structure design is illustrated as emphasis.In refractory metal molybdenum and molybdenum alloy and joining of graphite technical aspect, CN102240836B adds foil
Material solder, the method for increasing graphite surface roughness are welded;US2002/0085678A1,US2011/0103553A1,
In the foreign patents such as US2011/0103553A1, US2011/008059785B2, JP2010-140879A involved molybdenum and
Its alloy and graphite welding method, to add different elements, in the form of different additions, including powder, foil, coating etc. are brazed.
Above method products obtained therefrom dynamic balancing yields is poor, and the introducing of new element is bound to cause product dirt under hot operation
The problems such as dye, material at high temperature service life reduction.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, provide a kind of multilayer high temperature resistant
The preparation method of composite anode.This method first processes each layer of composite anode, then successively stacks each layer and between the layers
It adds solder and carries out vacuum hotpressing welding, finally obtain composite anode, due to being connected between each layer of composite anode by High temperature diffusion
It connects, transition rule between each bed boundary, interface is clear, ensure that the high temperature resistance of composite anode, avoids after filling powder because of compacting
Discontinuity generates a large amount of irregular bumps, sawtooth, oval interface, so that the dynamic balancing deviation of composite anode is reduced,
Improve the yields of composite anode.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of system of multilayer high temperature resistant composite anode
Preparation Method, which is characterized in that method includes the following steps:
Step 1: the first metal layer, second metal layer and non-metallic layer are prepared according to target product composite anode respectively, and
It successively stacks from top to bottom;The ingredient of the first metal layer is tungsten or tungsten alloy, the ingredient of the second metal layer be molybdenum or
Molybdenum alloy, the ingredient of the non-metallic layer are graphite;
Step 2: the first metal layer described in step 1 and stacking for second metal layer add the first solder between face;
Step 3: adding bimetallic stacking after the first solder in the non-metallic layer described in step 1 and step 2
The second solder is added between face, obtains composite anode clip;
Step 4: composite anode clip obtained in step 3 is carried out high-temperature vacuum thermal compression welding, second after welding
Transition zone is formed between metal layer and non-metallic layer, then the processed multilayer for obtaining the high-temperature degassing volatilization without exception at 1600 DEG C
High temperature resistant composite anode.
The present invention is first machining by each layer for forming composite anode according to target product composite anode, then by each layer
It successively stacks and addition solder carries out vacuum hotpressing welding between the layers, composite anode is finally obtained, since composite anode is each
It is connected between layer by High temperature diffusion, transition rule between each bed boundary, interface is clear, ensure that the heat-resisting quantity of composite anode
Can, compared with prior powder metallurgy, successively compression moulding prepares composite anode, produced after avoiding dress powder because suppressing discontinuity
Raw a large amount of irregular bumps, sawtooth, oval interface improve compound sun to reduce the dynamic balancing deviation of composite anode
The yields of pole.
A kind of preparation method of above-mentioned multilayer high temperature resistant composite anode, which is characterized in that the first gold medal described in step 1
Belong to the surface roughness for stacking face of layer and second metal layer, the rough surface for stacking face of second metal layer and the first metal layer
Surface roughness Ra≤1.6 for stacking face of degree, second metal layer and non-metallic layer, the non-metallic layer and second metal layer
Stack surface roughness Ra≤3.2 in face.By the restriction to the above-mentioned surface roughness for stacking face, subsequent weldering is effectively reduced
Foreign gas in termination process enters, and is conducive to reduce each atom diffusion length for being laminated and putting between face, while guaranteeing that weldment combines
Face does not generate hole.
A kind of preparation method of above-mentioned multilayer high temperature resistant composite anode, which is characterized in that the first pricker described in step 2
Material is nanometer powder, and the nanometer powder is nano-tungsten powder or nano Mo powder, and the granularity of the nanometer powder is no more than 200nm;
The mode of the first solder of the addition is to brush or apply cream, and the thickness of first solder is no more than 0.1mm.Nanometer powder conduct
Solder has the characteristics that high activity, solid phase metallurgy can be realized in lower temperature, to realize the solid diffusivity of two matrixes.The present invention
Using nano-tungsten powder or nano Mo powder as the first solder, the connection between the first metal layer and second metal layer is effectively increased
Effect, while avoiding introducing impurity element, it ensure that composite anode high temperature cleanliness and hot operation stability;Using brush or
It applies herbal paste formula and is conducive to the uniform addition of the first solder, be that both ensure that the no more than 0.1mm by the thickness control of the first solder
Being bonded between one metal layer and second metal layer, the metallurgical hole in turn avoiding the blocked up formation of the first solder are unfavorable for
Connection between one metal layer and second metal layer.
A kind of preparation method of above-mentioned multilayer high temperature resistant composite anode, which is characterized in that the second pricker described in step 3
Material is graphene or superfine graphite powder, and the granularity of second solder is no more than 1 μm;The mode of the second solder of the addition is spray
Cream is applied or applies, the thickness of second solder is no more than 0.1mm.The present invention uses graphene or ultra-fine stone with greater activity
Ink powder reduces diffusion activation energy as the second solder, effect, has got through diffusion admittance, and induction promotes the carbon in non-metallic layer
It is quickly spread to second metal layer, promotes being bonded between second metal layer and non-metallic layer;Using spraying or apply cream
Mode is conducive to the uniform addition of the second solder, while being that both ensure that non-no more than 0.1mm by the thickness control of the second solder
Being bonded between metal layer and second metal layer, in turn avoid be in so that carbide the second solder layer as main component is blocked up
Now apparent Brittleness adversely affects the weld strength and processing performance of subsequent composite anode.
The preparation method of above-mentioned a kind of multilayer high temperature resistant composite anode, which is characterized in that high temperature described in step 4 is true
The vacuum degree of empty thermal compression welding is no more than 10-1Pa, pressure are 10MPa~30MPa, and temperature is 1700 DEG C~2000 DEG C, when heat preservation
Between be 1h~3h, the heating rate of the high-temperature vacuum thermal compression welding is 5 DEG C/min~10 DEG C/min, the rate of temperature fall after heat preservation
No more than 15 DEG C/min.By stringenter vacuum level requirements, guarantee O, N existing for weld seam during high-temperature vacuum thermal compression welding
And effective discharge of the oxidizing gas of reaction generation, improve the quality of composite anode;The temperature of high-temperature vacuum thermal compression welding and
Pressure ensure that the diffusion effect between the first metal layer and second metal layer, between second metal layer and non-metallic layer, simultaneously
Welding temperature of 1300 DEG C much higher than composite anode service temperature, effectively prevent composite anode be on active service during occur liquid phase,
The problem of phase transformation;The vacuum degree of above-mentioned high-temperature vacuum thermal compression welding, pressure, temperature, soaking time and temperature rate mutual
Match, finally realizes going on smoothly for high-temperature vacuum thermal compression welding process.
Compared with the prior art, the present invention has the following advantages:
1, the present invention is first machining by each layer for forming composite anode according to target product composite anode, then will be each
Layer successively stacks and addition solder carries out vacuum hotpressing welding between the layers, composite anode is finally obtained, due to composite anode
It is connected between each layer by High temperature diffusion, transition rule between each bed boundary, interface is clear, ensure that the heat-resisting quantity of composite anode
Can, compared with prior powder metallurgy, successively compression moulding prepares composite anode, produced after avoiding dress powder because suppressing discontinuity
Raw a large amount of irregular bumps, sawtooth, oval interface improve compound sun to reduce the dynamic balancing deviation of composite anode
The yields of pole.
2, the present invention is using nano-tungsten powder or nano Mo powder as first connected between the first metal layer and second metal layer
Solder can realize solid phase metallurgy, to be effectively reduced since above-mentioned nanometer powder has the characteristics that high activity at a lower temperature
Metallurgical temperature between the first metal layer and second metal layer improves the efficiency of subsequent vacuum hotpressing welding, simultaneously because
The ingredient of above-mentioned nanometer powder is identical as the ingredient of the first metal layer or second metal layer, does not introduce the element of low melting point, also not
The element molten there may be eutectic drop is introduced, the high temperature cleanliness and hot operation stability of composite anode has been effectively ensured, from
And extend the service life of composite anode.
3, the present invention is connected using Activated Graphite alkene or active superfine graphite powder as between second metal layer and non-metallic layer
The second solder, under the high-temperature and high-pressure conditions of subsequent vacuum hotpressing welding, Activated Graphite alkene or active superfine graphite powder and the
Molybdenum or molybdenum alloy in two metal layers react, and diffuse into second metal layer matrix cystal by interstitial diffusion mechanism C element
Inside, while the microdefects portions such as second metal layer matrix crystal boundary, hole are diffused by express passway flooding mechanism C element
Position quickly opens diffusion admittance and plays induction diffusion, non-metallic layer is enable quickly to form diffusion connection with second metal layer,
It realizes effective connection of non-metallic layer and second metal layer, and the addition without new element, does not introduce impurity, welding surface is effectively ensured
Weld strength.
4, the present invention takes into account the first metal layer and second metal layer, the second metal during high-temperature vacuum thermal compression welding
The welding temperature of layer and non-metallic layer, using 1700 DEG C or more high temperature, using specified pressure, temperature rate and soaking time into
Row welding, welding temperature are much higher than composite anode service temperature (1300 DEG C), the applied at elevated temperature of composite anode have been effectively ensured
Energy;And the pressure and soaking time that high-temperature vacuum thermal compression welding uses solve welding process driving force deficiency, interface hole etc.
Caused indiffusion or diffusion are inadequate, so that the temperature rate of use improves welding process the problems such as influencing weld strength
Middle weld strength avoids weld seam from generating cracking, the soldering of composite anode has been effectively ensured.
Technical solution of the present invention is described in further detail below by drawings and examples.
Detailed description of the invention
Fig. 1 is the vacuum hotpressing welding schematic diagram of the composite anode clip in the embodiment of the present invention 1.
Fig. 2 is Mo-C binary alloy phase diagram in composite anode in the embodiment of the present invention 1.
Fig. 3 is the partial cutaway view for the composite anode that the embodiment of the present invention 1 is prepared.
Fig. 4 is the vacuum hotpressing welding schematic diagram of the composite anode clip in the embodiment of the present invention 2.
Description of symbols
1-the first metal layer;2-second metal layers;3-non-metallic layers;
4-the first solder;5-the second solder;6-welding toolings.
Specific embodiment
Embodiment 1
The preparation method of the present embodiment the following steps are included:
Step 1: taking diameter to be machined out for 110mm, with a thickness of the tungsten plectane of 10mm according to target product composite anode
Obtain the first metal layer 1, and it be polished to roughness Ra=1.6 with the face that is superimposed of second metal layer, take diameter be 110mm,
Be machined out to obtain second metal layer 2 with a thickness of the molybdenum plectane of 10mm, and by its upper and lower surface be polished to roughness Ra=
1.6, to take diameter be 110mm, is machined out to obtain non-metallic layer 3 with a thickness of the three high graphite disks of 40mm, and by its surface
Roughness Ra=3.2 are polished to, are then successively stacked from top to bottom;
Step 2: the first solder 4 is adjusted to the upper surface that paste is applied to second metal layer 2, and controls smearing thickness and be
0.1mm;First solder 4 uses granularity for the nano Mo powder of 200nm;
Step 3: the second solder 5 is sprayed on the lower surface of second metal layer 2, and controlling smearing thickness is 0.05mm, is obtained
To composite anode clip;Second solder 5 uses granularity for 1 μm of superfine graphite powder;
Step 4: composite anode clip obtained in step 3 is placed in progress vacuum hotpressing welding in welding tooling 6,
As shown in Figure 1, arrow indicates the direction of pressure F in Fig. 1, transition zone is formed between second metal layer and non-metallic layer after welding,
It is processed to obtain composite anode;The vacuum degree of the vacuum hotpressing welding is 10-1Pa, pressure 30MPa, temperature are 1700 DEG C,
Soaking time is 3h, and the heating rate of the vacuum hotpressing welding is 5 DEG C/min, and the rate of temperature fall after heat preservation is 15 DEG C/min.
Fig. 2 is Mo-C binary alloy phase diagram in composite anode in the embodiment of the present invention 1, figure it is seen that C and Mo
Have good reaction interval and solid solution section, carbon content be within the scope of 10wt% in Mo-C bianry alloy with MoC, β solid solution,
β ' solid solution, β " solid solution are primary product, which becomes molybdenum and provide good theoretical basis in conjunction with graphite.
Fig. 3 is the partial cutaway view for the composite anode that the present embodiment is prepared, from figure 3, it can be seen that the present embodiment system
Standby obtained composite anode appearance is good, and the binder course of tungsten layer and molybdenum layer is smooth clear, between molybdenum layer and the binder course of graphite linings
There are transition zones, and the transition between molybdenum layer and graphite linings is good, and interface is smooth clear.
Through detecting, the composite anode that the present embodiment is prepared is in 1600 DEG C of high-temperature degassing volatilizations without exception, base material tissue
Without exception to grow up without significant change, free from admixture pollution, interface is without obvious hole, and computing ballance correction is 1.3g.cm before duplicate removal, moves flat
It weighs functional.
Embodiment 2
The preparation method of the present embodiment the following steps are included:
Step 1: taking diameter according to target product composite anode is 110mm, with a thickness of the tungsten-rhenium alloy plectane progress of 10mm
Machining obtains the first metal layer 1 of annular, and it is polished to roughness Ra=0.8 with the face that is superimposed of second metal layer, takes
Diameter is 110mm, is machined out to obtain second metal layer 2 with a thickness of the TZM plectane of 40mm, and its upper and lower surface is polished to
Roughness Ra=0.8 takes diameter to be machined out to obtain non-metallic layer 3 for 110mm, with a thickness of the three high graphite disks of 40mm,
And by its surface polishing to roughness Ra=1.6, then successively stack from top to bottom;
Step 2: the first solder 4 is adjusted to the upper surface that paste is applied to second metal layer 2, and controls smearing thickness and be
0.05mm;First solder 4 uses granularity for the nano-tungsten powder of 100nm;
Step 3: the second solder 5 is adjusted to the lower surface that paste is applied to second metal layer 2, and controls smearing thickness and be
0.1mm obtains composite anode clip;Second solder 5 uses granularity for 0.2 μm of graphene;
Step 4: composite anode clip obtained in step 3 is placed in progress vacuum hotpressing welding in welding tooling 6,
As shown in figure 4, arrow indicates the direction of pressure F in Fig. 4, transition zone is formed between second metal layer and non-metallic layer after welding,
It is processed to obtain composite anode;The vacuum degree of the vacuum hotpressing welding is 10-2Pa, pressure 20MPa, temperature are 1900 DEG C,
Soaking time is 1.5h, and the heating rate of vacuum hotpressing welding is 6 DEG C/min, the rate of temperature fall after heat preservation is 10 DEG C/
min。
Through detecting, the composite anode that the present embodiment is prepared is in 1600 DEG C of high-temperature degassing volatilizations without exception, base material tissue
Without exception to grow up without significant change, free from admixture pollution, interface is without obvious hole, and computing ballance correction is 1.4g.cm before duplicate removal, moves flat
It weighs functional.
Embodiment 3
The preparation method of the present embodiment the following steps are included:
Step 1: taking diameter according to target product composite anode is 150mm, with a thickness of the tungsten-rhenium alloy plectane progress of 10mm
Machining obtains the first metal layer 1 of annular, and it is polished to roughness Ra=0.8 with the face that is superimposed of second metal layer, takes
Diameter is 150mm, is machined out to obtain second metal layer 2 with a thickness of the TZM plectane of 30mm, and its upper and lower surface is polished to
Roughness Ra=0.8 takes diameter to be machined out to obtain non-metallic layer 3 for 150mm, with a thickness of the three high graphite disks of 60mm,
And by its surface polishing to roughness Ra=1.6, then successively stack from top to bottom;
Step 2: the first solder 4 is adjusted to emulsus brushing in the upper surface of second metal layer 2, and controls smearing thickness and be
0.05mm;First solder 4 uses granularity for the nano-tungsten powder of 100nm;
Step 3: the second solder 5 is adjusted to the lower surface that paste is applied to second metal layer 2, and controls smearing thickness and be
0.1mm obtains composite anode clip;Second solder 5 uses granularity for 0.5 μm of superfine graphite powder;
Step 4: composite anode clip obtained in step 3 is placed in progress vacuum hotpressing welding in welding tooling 6,
As shown in figure 4, arrow indicates the direction of pressure F in Fig. 4, transition zone is formed between second metal layer and non-metallic layer after welding,
It is processed to obtain composite anode;The vacuum degree of the vacuum hotpressing welding is 10-2Pa, pressure 10MPa, temperature are 2000 DEG C,
Soaking time is 1h, and the heating rate of the vacuum hotpressing welding is 10 DEG C/min, and the rate of temperature fall after heat preservation is 10 DEG C/min.
Through detecting, the composite anode that the present embodiment is prepared is in 1600 DEG C of high-temperature degassing volatilizations without exception, base material tissue
Without exception to grow up without significant change, free from admixture pollution, interface is without obvious hole, and computing ballance correction is 2.7g.cm before duplicate removal, moves flat
It weighs functional.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (5)
1. a kind of preparation method of multilayer high temperature resistant composite anode, which is characterized in that method includes the following steps:
Step 1: preparing the first metal layer (1), second metal layer (2) and non-metallic layer respectively according to target product composite anode
(3), it and from top to bottom successively stacks;The ingredient of the first metal layer (1) is tungsten or tungsten alloy, the second metal layer (2)
Ingredient be molybdenum or molybdenum alloy, the ingredient of the non-metallic layer (3) is graphite;
Step 2: the first metal layer described in step 1 (1) and stacking for second metal layer (2) add the first solder between face
(5);
Step 3: adding the second metal (2) after the first solder (5) in the non-metallic layer described in step 1 (3) and step 2
Stack and add the second solder (6) between face, obtain composite anode clip;
Step 4: composite anode clip obtained in step 3 is carried out high-temperature vacuum thermal compression welding, the second metal after welding
Transition zone is formed between layer (2) and non-metallic layer (3), it is then processed to obtain in the more of 1600 DEG C of high-temperature degassing volatilizations without exception
Layer high temperature resistant composite anode.
2. a kind of preparation method of multilayer high temperature resistant composite anode according to claim 1, which is characterized in that in step 1
The surface roughness for stacking face of the first metal layer (1) and second metal layer (2), second metal layer (2) and the first metal
The surface roughness Ra for stacking face of the layer surface roughness for stacking face of (1), second metal layer (2) and non-metallic layer (3)≤
1.6, surface roughness Ra≤3.2 for stacking face of the non-metallic layer (3) and second metal layer (2).
3. a kind of preparation method of multilayer high temperature resistant composite anode according to claim 1, which is characterized in that in step 2
First solder (5) is nanometer powder, and the nanometer powder is nano-tungsten powder or nano Mo powder, the granularity of the nanometer powder
No more than 200nm;The mode of the addition the first solder (5) is to brush or apply cream, and the thickness of first solder (5) is no more than
0.1mm。
4. a kind of preparation method of multilayer high temperature resistant composite anode according to claim 1, which is characterized in that in step 3
Second solder (6) is graphene or superfine graphite powder, and the granularity of second solder (6) is no more than 1 μm;The addition the
The mode of two solders (6) is to spray or apply cream, and the thickness of second solder (6) is no more than 0.1mm.
5. a kind of preparation method of multilayer high temperature resistant composite anode according to claim 1, which is characterized in that in step 4
The vacuum degree of the high-temperature vacuum thermal compression welding is no more than 10-1Pa, pressure are 10MPa~30MPa, and temperature is 1700 DEG C~2000
DEG C, soaking time is 1h~3h, and the heating rate of the high-temperature vacuum thermal compression welding is 5 DEG C/min~10 DEG C/min, after heat preservation
Rate of temperature fall be not more than 15 DEG C/min.
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CN113770467A (en) * | 2021-09-07 | 2021-12-10 | 合肥工业大学 | SPS (spark sintering) pressureless brazing method for TZM alloy and graphite |
CN113770467B (en) * | 2021-09-07 | 2023-06-20 | 安徽尚欣晶工新材料科技有限公司 | SPS pressureless brazing method for TZM alloy and graphite |
CN114682896A (en) * | 2022-04-13 | 2022-07-01 | 安泰天龙钨钼科技有限公司 | Method for preparing anode substrate by diffusion bonding |
CN114799460A (en) * | 2022-04-13 | 2022-07-29 | 安泰天龙钨钼科技有限公司 | Method for preparing multilayer composite anode matrix by diffusion bonding |
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