CN109108522A - A kind of composite soldering and preparation method thereof for being brazed high nitrogen steel - Google Patents
A kind of composite soldering and preparation method thereof for being brazed high nitrogen steel Download PDFInfo
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- CN109108522A CN109108522A CN201811131827.0A CN201811131827A CN109108522A CN 109108522 A CN109108522 A CN 109108522A CN 201811131827 A CN201811131827 A CN 201811131827A CN 109108522 A CN109108522 A CN 109108522A
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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
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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
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
A kind of composite soldering and preparation method thereof for high nitrogen steel soldering, the group of effective component become Pd, Ni, Cr, Ni-coated graphite alkene or plating vanadium graphene, Mo, Mn, Re, Si, B and Nb.It is carried out in brazing process using composite soldering of the present invention, high nitrogen steel base material is almost non-fusible, so that nitrogen is not lost, the stomata disadvantage of prior welding mode is overcome, so that nitrogen almost free of losses；And since high nitrogen steel base material is almost non-fusible, that is, deformation will not be generated, improve the bonding strength and mechanical property of connector to a certain extent, welding joint shaping is very good.
Description
Technical field
It is specifically a kind of for the compound of high nitrogen steel soldering the present invention relates to the brazing solder of metal welding field
Solder and preparation method thereof.
Background technique
There are high nitrogen steel performances, these excellent performances such as corrosion-resistant, resistance to oxidation, wear-resistant and excellent in mechanical performance to make
It becomes one of the important materials in the equipment manufacturings such as aviation, ship and weapons, and welding technique is to determine its application category
Important process link.Since high nitrogen steel itself nitrogen content is high, weld blowhole often is generated because of the precipitation of base material nitrogen in welding process and is asked
Topic, it is to be dissolved a kind of main loss mode of nitrogen, and induce other hard crisp phases and occur that heat affected area nitride, which is precipitated, to weaken
Material property reduces the comprehensive performance of welding point.Currently, the research of high nitrogen steel welding technique is mainly rubbed with friction welding (FW), stirring
It wipes based on weldering, TIG weldering, MIG weldering, explosion weldering, gas shield welding, laser and its Combined Welding etc., but there are still nitrogen content losses, nitride
Or the defects of Carbide Precipitation and weld blowhole problem.
Chinese patent " a kind of double-layer air-flow protection TIG welding method of high nitrogen steel " (application number 201210250419.3),
Try hard to solve the problems, such as that high nitrogen steel pool depth when gas tungsten arc welding connects is shallower and weld seam nitrogen is overflowed, but deposits
In pool width and the wider problem of welding seam deep width ratio；Patent " high nitrogen steel laser MIG arc hybrid welding method "
(201210385839.2), laser-MIG electric arc compound welding technology is disclosed in the application in high nitrogen steel field；Patent is " a kind of high
The welding method of nitrogen steel " (201510885543.0) discloses instantaneous supercooled liquid phase diffusion and is connected to answering in high nitrogen steel welding
With, disclose using non-crystalline material supercooling liquid phase region superplasticity realize connection, then by raising temperature spread amorphous layer
The welding of metallurgical bonding is realized into base material；" solve high nitrogen steel weld blowhole and improve strength of joint welder and
Its welding method " (201610363272 .7) provides a kind of new approaches of improved high nitrogen steel laser-arc hybrid welding in industry,
Solve the problems, such as that high nitrogen steel weld blowhole and welding heat influence area toughness are poor " high simultaneously by the compound method of magnetic control and temperature control
Method nitrogen steel pressurization device for welding and weld high nitrogen steel using the device " (201610976054 .0) discloses a kind of logical
Crossing control welding protective gas composition, gross pressure and cooling parameter can achieve nitrogen content in fixed high nitrogen steel weld seam, improve
High nitrogen steel weld joint mechanical performance.
But the weldering of previous friction welding (FW), agitating friction, TIG weldering, MIG weldering, explosion weldering, gas shield welding, laser and its Combined Welding etc.
Welding method has that nitrogen is lost serious in weld penetration and width ratio selection hardly possible, base material high nitrogen steel, at present state
It is inside and outside also without the open source information of this respect, be badly in need of developing new welding material and solve the problems, such as this.
Summary of the invention
In order to solve high nitrogen steel using friction welding (FW), agitating friction weldering, TIG weldering, MIG weldering, explosion weldering, gas shield welding, laser
And its there are nitrogens in weld penetration and width ratio selection hardly possible, base material high nitrogen steel to be lost when the welding of the welding methods such as Combined Welding
Serious problem, the present invention provides a kind of composite soldering and preparation method thereof for high nitrogen steel soldering, using of the invention
When composite soldering is brazed high nitrogen steel, high nitrogen steel base material is almost non-fusible, so that nitrogen is not lost, overcomes traditional weldering
Connect the stomata disadvantage of mode so that nitrogen almost free of losses, and improve to a certain extent connector bonding strength and
Mechanical property, welding joint shaping are very good.
The present invention to solve above-mentioned technical problem used by technical solution are as follows: it is a kind of for high nitrogen steel soldering compound pricker
Material, according to weight ratio, the group of effective component become 25~28 parts of Pd, 8~13 parts of Ni, 36~41 parts of Cr, 2.5~
3.9 parts of Ni-coated graphite alkene or plating vanadium graphene, 5.6~6.8 parts of Mo, 23~27 parts of Mn, 7~11 parts of Re, 3~6 parts
Si, B and 0.35~0.6 of 2~4.5 parts part of Nb.
Composite soldering of the invention can be suitble to all high nitrogen steels, it is preferred that the high nitrogen steel of following component, according to weight
Than the constituent of the high nitrogen steel are as follows: 1.2~2.8 parts of N, 51~65 parts of Fe, 24~29 parts of Cr, 21~26 parts
Mn, 5.2~6.5 parts of Mo, 0.2~0.3 part of C, 0.3~0.5 part of Si, 0.2~0.35 part of Nb, 0.05~0.06 part
Al, S and 0.05~0.08 of 0.02~0.05 part part of P.
In the present invention Ni-coated graphite alkene used the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent is preferably hydrazine hydrate or sodium borohydride；
3) nickel plating is carried out on reduced graphene surface using electrodeposition process, Ni-coated graphite alkene is made, it is spare；The parameter of electrodeposition process
It is preferred that as follows: current density: 2.5~3.7A/dm2, temperature: 35~46 DEG C, pH value is 4.5~6.8,61~81g/ of nickel sulfate
L, 41~50g/L of nickel chloride, boric acid: 28~36g/L, 5.2~6.8g/L of dodecyl sodium sulfate, deposition rate: 1.3~1.75
μm/min；
4) nickel plating that load has molybdenum ion is made in Ni-coated graphite alkene surface deposited metal molybdenum ion using direct current magnetron sputtering process
Graphene, it is spare；The parameter of direct current magnetron sputtering process is preferably as follows: target be purity 99.99% nickel molybdenum (nickel molybdenum ratio be 3:
7) alloys target, substrate are glass slide, 0.8~0.95kV of voltage power, vacuum degree (0.8~1.3) × 10-4When Pa, it is passed through purity
99.99% argon gas is 2~2.5min as electric discharge and sputter gas, 110~140W of sputtering power, sedimentation time；
5) there is the Ni-coated graphite alkene of molybdenum ion to be put into ball grinder load to clay into power, Ni-coated graphite alkene powder, powder is made
Partial size be preferably 86~112 μm.
In the present invention it is used plating vanadium graphene the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent preferentially selects hydrazine hydrate；
3) plating vanadium is carried out on reduced graphene surface using conventional electrodeposition process, plating vanadium graphene is made；The ginseng of electrodeposition process
Number is preferably as follows: current density: 1.5~3A/dm2, temperature: 32~39 DEG C, pH value is 5.5~7.2, the sulphur of divalent vanadium ion
58~81g/L of hydrochlorate, 6.2~7.9g/L of lauryl sodium sulfate, 33~48g/L of nickel chloride, 2.5~4 μm/h of deposition rate；
4) the plating vanadium that load has nickel ion is made in plating vanadium graphene surface deposited metal nickel ion using direct current magnetron sputtering process
Graphene；The parameter of direct current magnetron sputtering process is preferably as follows, and target is the vanadium nickel of purity 99.99% (vanadium nickel mass ratio is 2:3)
Alloys target, substrate are glass slide, 0.6~0.8kV of voltage power, vacuum degree (1.5~2.1) × 10-4When Pa, it is passed through purity
99.99% argon gas is 3~4.5min as electric discharge and sputter gas, 120~160W of sputtering power, sedimentation time；
5) there is the plating vanadium graphene of nickel ion to be put into ball grinder load to clay into power, obtain plating vanadium graphene powder, powder
The partial size at end is preferably 86~112 microns.
The BJQ that Ni-coated graphite alkene or 3~5 times of vanadium graphene weight of plating can also be added in composite soldering of the present invention is mixed
Object is closed, the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the weight ratio of 1:3.5:1.
Composite soldering of the present invention the preparation method is as follows:
1) alloy powder containing mentioned component is weighed, and it is uniformly mixed shape with Ni-coated graphite alkene or plating vanadium graphene powder
At mixed-powder, and in mixed-powder, the weight ratio of each component meets above-mentioned requirement；
2) according to weight ratio, it is mixed that 15~30 parts of distilled water, 15~30 parts of water based adhesive and 5~12 parts of acetone are weighed
It closes, and is evenly stirred until and is generated without precipitating, form mixed solution, weigh the mixed powder prepared in 45~70 parts of step 1) later
End, and add it in mixed solution and stir evenly, 0.5 × 10 is evacuated in diffusion in vacuum furnace later-5MPa is obtained
Composite soldering.
In above-mentioned preparation method, water based adhesive can select conventional bonding agent, but preferentially select following component
Water based adhesive: according to weight ratio, the water based adhesive is by 24~36 parts of trbasic zinc phosphate, 45~61 parts of ammonium chloride, 15~23
The polyethylene glycol and 14~22 parts of Tisuacryl of part mix.
In the present invention, effect of the Ni-coated graphite alkene in composite soldering are as follows:
It joined the Ni-coated graphite alkene that area load has molybdenum ion, one side graphene has excellent electricity, calorifics, mechanics etc.
Property, while density is low, structural stability is good, addition enter the wetability that solder can be obviously improved in solder, thermal conductivity and
Soldering property, by nickel plating on the surface of graphene, not only prevent graphene floated in solder paste and liquid solder it is indefinite, make pricker
There is the problem of oxide in material ingredient unevenness and tissue, and the tensile strength for preparing composite soldering has been greatly enhanced, makes
The tensile strength for obtaining composite soldering connection high nitrogen steel is more than 750MPa；On the other hand in Ni-coated graphite alkene area load molybdenum ion,
When composite soldering in use, molybdenum ion is released slowly, since molybdenum ion is under extremely low concentration, it will be able to press down
Appearance and generation in high nitrogen steel processed the defects of nitride, carbide, improve the mechanical property of connector.
In the present invention, effect of the vanadium graphene in composite soldering is plated are as follows:
One side graphene has the properties such as excellent electricity, calorifics, mechanics, while density is low, structural stability is good, is added to
The wetability, thermal conductivity and soldering property for entering to be obviously improved solder in solder, by plating vanadium on the surface of graphene, not only prevent
That graphene floats in solder paste and liquid solder is indefinite, make solder ingredient uneven and tissue in there is the problem of oxide,
And the tensile strength for preparing composite soldering has been greatly enhanced, so that the tensile strength of connector is much higher than it has been reported that another
Aspect plating vanadium graphene area load nickel ion, when composite soldering in use, nickel ion is released slowly, by
In nickel ion under extremely low concentration, it will be able to which the appearance and generation for the defects of inhibiting nitride in high nitrogen steel, carbide improve
The mechanical property of connector；
The unique effect played in composite soldering preparation process of water based adhesive used in the present invention are as follows:
On the one hand it can improve the wetability between solder particle and bonding agent, mainly wellability, since brazing filler metal compositions useful contains plating
Nickel graphene, graphene are easy to appear floating and oxidizing slag during granulate mixture and molten state solder brazing high nitrogen steel
Defect not only makes Ni-coated graphite alkene particle be evenly distributed in solder paste and liquid solder by water-base adhesive, but also has
There is slagging-off effect, to improve the uniformity of bonding agent attachment solder particle, Quick-forming and the connection for facilitating solder paste are high
On the other hand the brazing filler metal efficiency (ratio of brazing area) of nitrogen steel can guarantee solder particle, especially Ni-coated graphite alkene, metal alloy powder, glue
It connects agent to be uniformly mixed, while promoting the volatilization of moisture, improve the forming quality of solder paste and at cream efficiency；In addition, the present invention mentions
The bonding agent of confession, especially Tisuacryl, at room temperature can rapid link composite soldering particle, bonding force is strong, nontoxic
It is harmless, avoid pollution caused by organic solvent.
The synergistic effect of each element is as follows in composite soldering of the present invention:
Pd: dissolving each other with elements such as nickel, silicon, rhenium, manganese, can form solid solution, improves the intensity resistant to high temperatures of solder and connector；It is connection
The one of the chief elements of high nitrogen steel；
Ni: improving solder wetting, improve soldering joint strength, corrosion resistance, and purification brazed seam crystal boundary improves solder processing performance,
It is one of connection most important element of high nitrogen steel steel；
Cr: being infinitely dissolved with nickel, manganese, and solder and strength of joint, corrosion resistance can be improved, be connection the most important element of high nitrogen steel it
One；
Mo: high elastic modulus, close with the intensity of steel, the mechanical property of composite soldering connection high nitrogen steel can be improved in addition molybdenum element
Energy；
Mn: it reduces fusion temperature, improve solder wetting, there is secondary deoxidation；Simultaneously can be improved solder microhardness and
Elevated temperature strength；
Re: rhenium added in solder it is seldom, be rarely reported, solder of the present invention adds rhenium element, improve the seam-filling ability of solder,
Improve the joint capacity of solder.
Si: improving solder wetting, refines solder tissue, improves the intensity of solder and soldered fitting；It can be formed with aluminium
Eutectic, the mass fraction of eutectic point Si are 11.7%, are the connection most important elements of high nitrogen steel；
B: improving the plasticity of solder, enhances the spreadability and mobility of solder, is one of connection most important element of high nitrogen steel.
Nb: improving the plasticity and processability of composite soldering, refines brazing seam structure, can prevent going out for soldering high nitrogen steel nitride
It is existing.
Ni-coated graphite alkene: regulation solder tissue and Weld Performance improve the tensile strength of connector, so that the mechanical property of solder
Can be more excellent, it is to guarantee one of most important material of high nitrogen steel bonding strength；
Plating vanadium graphene: being obviously improved the wetability of solder, thermal conductivity and soldering property, meanwhile, prevent graphene in solder paste and
Floated in liquid solder it is indefinite, make solder ingredient uneven and tissue in there is the problem of oxide, and be greatly enhanced
The tensile strength of composite soldering is prepared, is had been reported so that the tensile strength of connector is much higher than；And nickel ion is in use process
In be released slowly, since nickel ion is under extremely low concentration, it will be able to inhibit nitride in high nitrogen steel, carbide etc. lack
Sunken appearance and generation, improves the mechanical property of connector；
The effect for the BJQ mixture mixed by barium glass powder, fumed silica and tartaric acid being added in the present invention
Are as follows:
Barium glass powder: partial size is small, good dispersion, transparency is high, has good result of prevention；Facilitate alloyed powder, bonding agent,
Deposit-free generates after Ni-coated graphite alkene is uniformly dispersed, stirs, and improves the homogeneity of solder paste；Meanwhile having affinity strong,
It can easily be scattered in solder paste；
Fumed silica: non-toxic and tasteless pollution-free, porosity, high temperature resistant, large specific surface area, superficial attractive forces are strong, dispersibility
It is good, as the thickener and dispersing agent of preparation solder paste, effectively control alloyed powder, bonding agent, Ni-coated graphite alkene rheological characteristic and
Homogeneity prevents the floating of Ni-coated graphite alkene indefinite, guarantees that the structural homogenity, adhesion, continuity of solder paste (prevent from smearing
Interrupt, fall off), improve high-temperature oxidation resistance, Testing Tensile Strength at Elevated Temperature, tear resistance and the wearability of solder paste；
Tartaric acid: as the auxiliary element of bonding agent, the cementability of bonding agent can be improved, facilitate water-base adhesive, third
Fused, the guarantee mixing uniformity of ketone.
Compared with prior art, the invention has the following beneficial effects:
1) it being carried out in brazing process using composite soldering of the present invention, high nitrogen steel base material is almost non-fusible, so that nitrogen is not lost,
The stomata disadvantage of prior welding mode is overcome, so that nitrogen almost free of losses；And since high nitrogen steel base material is hardly molten
Change, that is, deformation will not be generated, improves the bonding strength and mechanical property of connector, welding joint shaping to a certain extent
It is very good；
2) implement under vacuum conditions when being brazed using composite soldering of the invention, so that impurity member in solder preparation process
Element, ambient atmos can not participate in, thus the solder cleanliness obtained is high, has excellent performance；
3) solder of the present invention is lower using temperature, can effectively prevent nitride in soldered fitting, carbide, carbonitride
It generates to reduce its performance；
4) high nitrogen steel is easy to produce high-temerature creep, phase transformation etc. at high temperature, and structure property will change, and reduces welding point
Performance, it is almost non-fusible using high nitrogen steel during solder brazing of the present invention, can be to avoid above-mentioned structure property variation issue；
5) used in the present invention in solder paste containing elements such as palladium, nickel, manganese, chromium, not only can with effective wetting high nitrogen steel base material, but also
With the virtually limitless solid solution of base material, metallurgical bonding is efficiently formed, enhances the mechanical property of connector；
6) solder provided by the invention optimizes solder structure property by composite graphite alkene particle, and enhancing solder connects high nitrogen steel
Strength of joint, extend high nitrogen steel device service life.
Specific embodiment
Technical solution of the present invention is described in further detail combined with specific embodiments below.
Embodiment 1
A kind of composite soldering for high nitrogen steel soldering, according to weight ratio, the group of effective component as 25 parts Pd, 8 parts
Ni, 36 parts of Cr, 2.5 parts of Ni-coated graphite alkene or plating vanadium graphene, 5.6 parts of Mo, 23 parts of Mn, 7 parts of Re, 3 parts of Si,
2 parts of B and 0.35 part of Nb；
Above-mentioned composite soldering the preparation method is as follows:
1) alloy powder containing mentioned component is weighed, and it is uniformly mixed shape with Ni-coated graphite alkene or plating vanadium graphene powder
At mixed-powder, and in mixed-powder, the weight ratio of each component meets above-mentioned requirement；
2) according to weight ratio, 15 parts of distilled water, 15 parts of water based adhesive and the mixing of 5 parts of acetone are weighed, and is stirred evenly
It is generated to without precipitating, forms mixed solution, weigh the mixed-powder prepared in 45 parts of step 1) later, and add it to mixing
It is stirred evenly in solution, is evacuated to 0.5 × 10 in diffusion in vacuum furnace later-5MPa obtains composite soldering.
The above are the basic embodiments of the present embodiment, can be improved further, optimize and limit on the basis of above:
Such as, the composite soldering of the present embodiment can be suitble to all high nitrogen steels, it is preferred that the high nitrogen steel of following component, according to weight
Than the constituent of the high nitrogen steel are as follows: 1.2 parts of N, 51 parts of Fe, 24 parts of Cr, 21 parts of Mn, 5.2 parts of Mo, 0.2 part
C, 0.3 part of Si, 0.2 part of Nb, 0.05 part of Al, S and 0.05 of 0.02 part part of P.
For another example, in the present embodiment Ni-coated graphite alkene used the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent is preferably hydrazine hydrate or sodium borohydride；
3) nickel plating is carried out on reduced graphene surface using electrodeposition process, Ni-coated graphite alkene is made, it is spare；The parameter of electrodeposition process
It is preferred that as follows: current density: 2.5A/dm2, temperature: 35 DEG C, pH value 4.5, nickel sulfate 61g/L, nickel chloride 41g/L, boric acid:
28g/L, dodecyl sodium sulfate 5.2g/L, deposition rate: 1.3 μm/min；
4) nickel plating that load has molybdenum ion is made in Ni-coated graphite alkene surface deposited metal molybdenum ion using direct current magnetron sputtering process
Graphene, it is spare；The parameter of direct current magnetron sputtering process is preferably as follows: target be purity 99.99% nickel molybdenum (nickel molybdenum ratio be 3:
7) alloys target, substrate are glass slide, voltage power 0.8kV, vacuum degree 0.8 × 10-4When Pa, the argon gas for being passed through purity 99.99% is made
For electric discharge and sputter gas, sputtering power 110W, sedimentation time 2min；
5) there is the Ni-coated graphite alkene of molybdenum ion to be put into ball grinder load to clay into power, Ni-coated graphite alkene powder, powder is made
Partial size be preferably 86 μm.
For another example, in the present embodiment it is used plating vanadium graphene the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent preferentially selects hydrazine hydrate；
3) plating vanadium is carried out on reduced graphene surface using conventional electrodeposition process, plating vanadium graphene is made；The ginseng of electrodeposition process
Number is preferably as follows: current density: 1.5A/dm2, temperature: 32 DEG C, pH value 5.5, the sulfate 58g/L of divalent vanadium ion, ten
Sodium dialkyl sulfate 6.2g/L, nickel chloride 33g/L, 2.5 μm/h of deposition rate；
4) the plating vanadium that load has nickel ion is made in plating vanadium graphene surface deposited metal nickel ion using direct current magnetron sputtering process
Graphene；The parameter of direct current magnetron sputtering process is preferably as follows, and target is the vanadium nickel of purity 99.99% (vanadium nickel mass ratio is 2:3)
Alloys target, substrate are glass slide, voltage power 0.6kV, vacuum degree 1.5 × 10-4When Pa, it is passed through the argon gas conduct of purity 99.99%
Electric discharge and sputter gas, sputtering power 120W, sedimentation time 3min；
5) there is the plating vanadium graphene of nickel ion to be put into ball grinder load to clay into power, obtain plating vanadium graphene powder, powder
The partial size at end is preferably 86 microns.
Ni-coated graphite alkene or 3 times of vanadium graphene weight of plating can also be added for another example, in composite soldering described in the present embodiment again
BJQ mixture, the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the weight ratio of 1:3.5:1
It closes.
Finally, water based adhesive can select conventional bonding agent in the preparation method of composite soldering, but preferentially choosing
With the water based adhesive of following component: according to weight ratio, the water based adhesive is by 24 parts of trbasic zinc phosphate, 45 parts of ammonium chloride, 15
The polyethylene glycol and 14 parts of Tisuacryl of part mix.
Embodiment 2
A kind of composite soldering for high nitrogen steel soldering, according to weight ratio, the group of effective component as 28 parts Pd, 13 parts
Ni, 41 parts of Cr, 3.9 parts of Ni-coated graphite alkene or plating vanadium graphene, 6.8 parts of Mo, 27 parts of Mn, 11 parts of Re, 6 parts
Si, B and 0.6 of 4.5 parts part of Nb；
Above-mentioned composite soldering the preparation method is as follows:
1) alloy powder containing mentioned component is weighed, and it is uniformly mixed shape with Ni-coated graphite alkene or plating vanadium graphene powder
At mixed-powder, and in mixed-powder, the weight ratio of each component meets above-mentioned requirement；
2) according to weight ratio, 30 parts of distilled water, 30 parts of water based adhesive and the mixing of 12 parts of acetone are weighed, and is stirred evenly
It is generated to without precipitating, forms mixed solution, weigh the mixed-powder prepared in 70 parts of step 1) later, and add it to mixing
It is stirred evenly in solution, is evacuated to 0.5 × 10 in diffusion in vacuum furnace later-5MPa obtains composite soldering.
The above are the basic embodiments of the present embodiment, can be improved further, optimize and limit on the basis of above:
Such as, the composite soldering of the present embodiment can be suitble to all high nitrogen steels, it is preferred that the high nitrogen steel of following component, according to weight
Than the constituent of the high nitrogen steel are as follows: 2.8 parts of N, 65 parts of Fe, 29 parts of Cr, 26 parts of Mn, 6.5 parts of Mo, 0.3 part
C, 0.5 part of Si, 0.35 part of Nb, 0.06 part of Al, S and 0.08 of 0.05 part part of P.
For another example, in the present embodiment Ni-coated graphite alkene used the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent is preferably hydrazine hydrate or sodium borohydride；
3) nickel plating is carried out on reduced graphene surface using electrodeposition process, Ni-coated graphite alkene is made, it is spare；The parameter of electrodeposition process
It is preferred that as follows: current density 3.7A/dm2, 46 DEG C of temperature, pH value 6.8, nickel sulfate 81g/L, nickel chloride 50g/L, boric acid
36g/L, dodecyl sodium sulfate 6.8g/L, 1.75 μm/min of deposition rate；
4) nickel plating that load has molybdenum ion is made in Ni-coated graphite alkene surface deposited metal molybdenum ion using direct current magnetron sputtering process
Graphene, it is spare；The parameter of direct current magnetron sputtering process is preferably as follows: target be purity 99.99% nickel molybdenum (nickel molybdenum ratio be 3:
7) alloys target, substrate are glass slide, voltage power 0.95kV, vacuum degree 1.3 × 10-4When Pa, it is passed through the argon gas of purity 99.99%
As electric discharge and sputter gas, sputtering power 140W, sedimentation time 2.5min；
5) there is the Ni-coated graphite alkene of molybdenum ion to be put into ball grinder load to clay into power, Ni-coated graphite alkene powder, powder is made
Partial size be preferably 112 μm.
For another example, in the present embodiment it is used plating vanadium graphene the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent preferentially selects hydrazine hydrate；
3) plating vanadium is carried out on reduced graphene surface using conventional electrodeposition process, plating vanadium graphene is made；The ginseng of electrodeposition process
Number is preferably as follows: current density 3A/dm2, 39 DEG C of temperature, pH value 7.2, the sulfate 81g/L of divalent vanadium ion, dodecane
Base sodium sulphate 7.9g/L, nickel chloride 48g/L, 4 μm/h of deposition rate；
4) the plating vanadium that load has nickel ion is made in plating vanadium graphene surface deposited metal nickel ion using direct current magnetron sputtering process
Graphene；The parameter of direct current magnetron sputtering process is preferably as follows, and target is the vanadium nickel of purity 99.99% (vanadium nickel mass ratio is 2:3)
Alloys target, substrate are glass slide, voltage power 0.8kV, vacuum degree 2.1 × 10-4When Pa, it is passed through the argon gas conduct of purity 99.99%
Electric discharge and sputter gas, sputtering power 160W, sedimentation time 4.5min；
5) there is the plating vanadium graphene of nickel ion to be put into ball grinder load to clay into power, obtain plating vanadium graphene powder, powder
The partial size at end is preferably 86~112 microns.
Ni-coated graphite alkene or 5 times of vanadium graphene weight of plating can also be added for another example, in composite soldering described in the present embodiment again
BJQ mixture, the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the weight ratio of 1:3.5:1
It closes.
Finally, water based adhesive can select conventional bonding agent in the preparation method of composite soldering, but preferentially choosing
With the water based adhesive of following component: according to weight ratio, the water based adhesive is by 36 parts of trbasic zinc phosphate, 61 parts of ammonium chloride, 23
The polyethylene glycol and 22 parts of Tisuacryl of part mix.
Embodiment 3
A kind of composite soldering for high nitrogen steel soldering, according to weight ratio, the group of effective component as 26.5 parts Pd, 10.5
Part Ni, 38.5 parts of Cr, 3.2 parts of Ni-coated graphite alkene or plating vanadium graphene, 6.2 parts of Mo, 25 parts of Mn, 9 parts of Re,
4.5 parts of Si, B and 0.45 of 3.25 parts part of Nb；
Above-mentioned composite soldering the preparation method is as follows:
1) alloy powder containing mentioned component is weighed, and it is uniformly mixed shape with Ni-coated graphite alkene or plating vanadium graphene powder
At mixed-powder, and in mixed-powder, the weight ratio of each component meets above-mentioned requirement；
2) according to weight ratio, 22.5 parts of distilled water, 22.5 parts of water based adhesive and the mixing of 8.5 parts of acetone are weighed, and is stirred
It mixes and is uniformly generated to without precipitating, form mixed solution, weigh the mixed-powder prepared in 57.5 parts of step 1) later, and added
Enter and stirred evenly into mixed solution, is evacuated to 0.5 × 10 in diffusion in vacuum furnace later-5MPa obtains composite soldering.
The above are the basic embodiments of the present embodiment, can be improved further, optimize and limit on the basis of above:
Such as, the composite soldering of the present embodiment can be suitble to all high nitrogen steels, it is preferred that the high nitrogen steel of following component, according to weight
Than the constituent of the high nitrogen steel are as follows: 2 parts of N, 58 parts of Fe, 26.5 parts of Cr, 23.5 parts of Mn, 5.85 parts of Mo, 0.25
C, 0.4 part of the Si, 0.275 part of Nb, 0.055 part of Al, S and 0.065 of 0.035 part part of P of part.
For another example, in the present embodiment Ni-coated graphite alkene used the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent is preferably hydrazine hydrate or sodium borohydride；
3) nickel plating is carried out on reduced graphene surface using electrodeposition process, Ni-coated graphite alkene is made, it is spare；The parameter of electrodeposition process
It is preferred that as follows: current density: 3.1A/dm2, temperature: 40.5 DEG C, pH value 5.65, nickel sulfate 71g/L, nickel chloride 45.5g/L,
Boric acid: 32g/L, dodecyl sodium sulfate 6g/L, deposition rate: 1.525 μm/min；
4) nickel plating that load has molybdenum ion is made in Ni-coated graphite alkene surface deposited metal molybdenum ion using direct current magnetron sputtering process
Graphene, it is spare；The parameter of direct current magnetron sputtering process is preferably as follows: target be purity 99.99% nickel molybdenum (nickel molybdenum ratio be 3:
7) alloys target, substrate are glass slide, voltage power 0.875kV, vacuum degree 1.05 × 10-4When Pa, it is passed through the argon of purity 99.99%
Gas is as electric discharge and sputter gas, sputtering power 125W, sedimentation time 2.25min；
5) there is the Ni-coated graphite alkene of molybdenum ion to be put into ball grinder load to clay into power, Ni-coated graphite alkene powder, powder is made
Partial size be preferably 99 μm.
For another example, in the present embodiment it is used plating vanadium graphene the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；Reducing agent preferentially selects hydrazine hydrate；
3) plating vanadium is carried out on reduced graphene surface using conventional electrodeposition process, plating vanadium graphene is made；The ginseng of electrodeposition process
Number is preferably as follows: current density: 2.25A/dm2, temperature: 35.5 DEG C, pH value 6.35, the sulfate of divalent vanadium ion
69.5g/L, lauryl sodium sulfate 7.05g/L, nickel chloride 40.5g/L, 3.25 μm/h of deposition rate；
4) the plating vanadium that load has nickel ion is made in plating vanadium graphene surface deposited metal nickel ion using direct current magnetron sputtering process
Graphene；The parameter of direct current magnetron sputtering process is preferably as follows, and target is the vanadium nickel of purity 99.99% (vanadium nickel mass ratio is 2:3)
Alloys target, substrate are glass slide, voltage power 0.7kV, vacuum degree 1.8 × 10-4When Pa, it is passed through the argon gas conduct of purity 99.99%
Electric discharge and sputter gas, sputtering power 140W, sedimentation time 3.75min；
5) there is the plating vanadium graphene of nickel ion to be put into ball grinder load to clay into power, obtain plating vanadium graphene powder, powder
The partial size at end is preferably 99 microns.
Ni-coated graphite alkene or 4 times of vanadium graphene weight of plating can also be added for another example, in composite soldering described in the present embodiment again
BJQ mixture, the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the weight ratio of 1:3.5:1
It closes.
Finally, water based adhesive can select conventional bonding agent in the preparation method of composite soldering, but preferentially choosing
With the water based adhesive of following component: according to weight ratio, the water based adhesive is by 30 parts of trbasic zinc phosphate, 53 parts of ammonium chloride, 19
The polyethylene glycol and 18 parts of Tisuacryl of part mix.
Claims (7)
1. a kind of composite soldering for high nitrogen steel soldering, it is characterised in that: according to weight ratio, the group of effective component becomes 25
~28 parts of Pd, 8~13 parts of Ni, 36~41 parts of Cr, 2.5~3.9 parts of Ni-coated graphite alkene or plating vanadium graphene, 5.6~
6.8 parts of Mo, 23~27 parts of Mn, 7~11 parts of Re, 3~6 parts of Si, B and 0.35~0.6 of 2~4.5 parts part of Nb.
2. a kind of composite soldering for high nitrogen steel soldering according to claim 1, it is characterised in that: according to weight ratio,
The constituent of the high nitrogen steel are as follows: 1.2~2.8 parts of N, 51~65 parts of Fe, 24~29 parts of Cr, 21~26 parts of Mn,
5.2~6.5 parts of Mo, 0.2~0.3 part of C, 0.3~0.5 part of Si, 0.2~0.35 part of Nb, 0.05~0.06 part of Al,
0.02~0.05 part of S and 0.05~0.08 part of P.
3. a kind of composite soldering for high nitrogen steel soldering according to claim 1, which is characterized in that the Ni-coated graphite
Alkene the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；
3) nickel plating is carried out on reduced graphene surface using electrodeposition process, Ni-coated graphite alkene is made, it is spare；
4) nickel plating that load has molybdenum ion is made in Ni-coated graphite alkene surface deposited metal molybdenum ion using direct current magnetron sputtering process
Graphene, it is spare；
5) there is the Ni-coated graphite alkene of molybdenum ion to be put into ball grinder load to clay into power, Ni-coated graphite alkene powder is made.
4. a kind of composite soldering for high nitrogen steel soldering according to claim 1, which is characterized in that the plating scherbinaite ink
Alkene the preparation method comprises the following steps:
1) graphene oxide is taken, it is conventionally successively roughened, is sensitized and is activated；
2) graphene oxide after sensitized treatment is put into reducing agent and is restored, reduced graphene is made after washing, drying,
It is spare；
3) plating vanadium is carried out on reduced graphene surface using conventional electrodeposition process, plating vanadium graphene is made；
4) the plating vanadium that load has nickel ion is made in plating vanadium graphene surface deposited metal nickel ion using direct current magnetron sputtering process
Graphene；
5) there is the plating vanadium graphene of nickel ion to be put into ball grinder load to clay into power, obtain plating vanadium graphene powder.
5. a kind of composite soldering for high nitrogen steel soldering according to claim 1, it is characterised in that: the composite soldering
In also containing Ni-coated graphite alkene or plate 3~5 times of vanadium graphene weight BJQ mixture, the BJQ mixture be barium glass
Powder, fumed silica and tartaric acid are mixed with the weight ratio of 1:3.5:1.
6. a kind of composite soldering for high nitrogen steel soldering according to claim 1, which is characterized in that the composite soldering
The preparation method is as follows:
1) alloy powder containing ingredient described in claim 1 is weighed, and by itself and Ni-coated graphite alkene or plating vanadium graphene powder
It is uniformly mixed and forms mixed-powder, and the weight ratio of each component meets the requirement of claim 1 in mixed-powder；
2) according to weight ratio, it is mixed that 15~30 parts of distilled water, 15~30 parts of water based adhesive and 5~12 parts of acetone are weighed
It closes, and is evenly stirred until and is generated without precipitating, form mixed solution, weigh the mixed powder prepared in 45~70 parts of step 1) later
End, and add it in mixed solution and stir evenly, 0.5 × 10 is evacuated in diffusion in vacuum furnace later-5MPa is obtained
Composite soldering.
7. a kind of composite soldering for high nitrogen steel soldering according to claim 6, it is characterised in that: according to weight ratio,
The water based adhesive by 24~36 parts of trbasic zinc phosphate, 45~61 parts of ammonium chloride, 15~23 parts of polyethylene glycol and 14~
22 parts of Tisuacryl mixes.
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| CN110497116A (en) * | 2019-08-06 | 2019-11-26 | 华北水利水电大学 | A kind of mutative scale boron nitrogen graphene modified layer solder, Preparation method and use |
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| CN111843087A (en) * | 2020-07-07 | 2020-10-30 | 哈尔滨工业大学 | Vacuum brazing process method for inhibiting high-temperature nitrogen precipitation in high-nitrogen steel |
| CN111859642A (en) * | 2020-07-07 | 2020-10-30 | 哈尔滨工业大学 | Thermodynamic calculation method for optimizing high-nitrogen steel high-temperature brazing process |
| CN115464301A (en) * | 2022-10-08 | 2022-12-13 | 山东森峰激光装备有限公司 | Flux-cored wire for laser-arc hybrid welding of high-nitrogen steel |
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| CN115464301B (en) * | 2022-10-08 | 2023-05-23 | 山东森峰激光装备有限公司 | Flux-cored wire for high-nitrogen steel laser arc hybrid welding |
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