CN109014661A - A kind of high nitrogen steel soldering solder additive - Google Patents
A kind of high nitrogen steel soldering solder additive Download PDFInfo
- Publication number
- CN109014661A CN109014661A CN201811133488.XA CN201811133488A CN109014661A CN 109014661 A CN109014661 A CN 109014661A CN 201811133488 A CN201811133488 A CN 201811133488A CN 109014661 A CN109014661 A CN 109014661A
- Authority
- CN
- China
- Prior art keywords
- graphene
- high nitrogen
- parts
- nitrogen steel
- plating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
A kind of high nitrogen steel soldering solder additive, the solder additive is made of reinforcing agent, water-base adhesive and BJQ mixture with the mass ratio of 1:7~8:3~5, the reinforcing agent is the mixing of any mass ratio of Ni-coated graphite alkene or plating vanadium graphene or both, and the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the mass ratio of 1:3.5:1.It additive disclosed by the invention is added into when being brazed in solder, 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
The present invention relates to the brazing solder of metal welding field, specifically a kind of high nitrogen steel soldering is added with solder
Agent.
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 high nitrogen steel soldering solder additives, by the way that reinforcing agent of the invention to be added to
High nitrogen steel is brazed again in brazing solder, high nitrogen steel base material is almost non-fusible, so that nitrogen is not lost, overcomes tradition
The stomata disadvantage of welding manner, so that nitrogen almost free of losses, and the bonding strength of connector is improved to a certain extent
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: a kind of high nitrogen steel soldering is added with solder
Agent, the solder additive is made of reinforcing agent, water-base adhesive and BJQ mixture with the mass ratio of 1:7~8:3~5, described
Reinforcing agent is Ni-coated graphite alkene or the mixing for plating any mass ratio of vanadium graphene or both, the BJQ mixture be barium glass powder,
Fumed silica and tartaric acid are mixed with the mass ratio of 1:3.5:1.
In the present invention, the 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.
High nitrogen steel of the present invention, the preferably high nitrogen steel of following component, 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.
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.
Additive of the invention is suitable for general brazing solder, it is preferred to use following composite soldering should according to weight ratio
The group of effective components of composite soldering become 25~28 parts of Pd, 8~13 parts of Ni, 36~41 parts of Cr, 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, and additive plus
Enter 2~4% that amount is composite soldering weight.
The synergistic effect of each element is as follows in the composite soldering:
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.
The method that additive is added in above-mentioned composite soldering is as follows:
1) alloy powder containing mentioned component is weighed, and it is uniformly mixed shape with reinforcing agent, the BJQ mixture in additive
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, the water based adhesive in additive 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.
Unique effect of the water based adhesive played in composite soldering in the present invention, in additive 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.
BJQ mixture each component role in additive of 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.
In the present invention, effect of the Ni-coated graphite alkene in composite soldering in additive 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.
Effect of the vanadium graphene in composite soldering is plated in the present invention, in additive 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；
Compared with prior art, the invention has the following beneficial effects:
1) can optimize containing the particle that main body is composite graphite alkene when it is added in solder in additive of the invention
Solder structure property, the strength of joint of enhancing solder connection high nitrogen steel, extends the service life of high nitrogen steel device；
2) high nitrogen steel is brazed again in it additive disclosed by the invention is added into brazing solder, high nitrogen steel base material is hardly molten
Change, so that nitrogen is not lost, the stomata disadvantage of prior welding mode is overcome, so that nitrogen almost free of losses, Er Qie
The bonding strength and mechanical property of connector are improved to a certain extent, and welding joint shaping is very good；
3) it is carried out in brazing process using currently preferred composite soldering, high nitrogen steel base material is almost non-fusible, so that nitrogen
It is not lost, overcomes the stomata disadvantage of prior welding mode, so that nitrogen almost free of losses；And since high nitrogen steel base material is several
It is non-fusible, that is, deformation will not be generated, the bonding strength and mechanical property of connector are improved to a certain extent, and welding connects
Head forming is very good；And soldering is implemented under vacuum conditions, so that impurity element, ambient atmos in solder preparation process
It can not participate in, thus the solder cleanliness obtained is high, has excellent performance；The use temperature of composite soldering of the present invention is lower, Ke Yiyou
Effect prevents the generation of nitride in soldered fitting, carbide, carbonitride to reduce its performance；At high temperature due to high nitrogen steel
It is easy to produce high-temerature creep, phase transformation etc., structure property will change, and reduce the performance of welding point, use pricker of the present invention
Expect that high nitrogen steel is almost non-fusible in brazing process, it can be to avoid above-mentioned structure property variation issue；
It 4), not only can be with effective wetting high nitrogen steel base material, Er Qieyu containing elements such as palladium, nickel, manganese, chromium in solder used in the present invention
The virtually limitless solid solution of base material, efficiently forms metallurgical bonding, enhances the mechanical property of connector.
Specific embodiment
Technical solution of the present invention is described in further detail combined with specific embodiments below.
Embodiment 1
A kind of high nitrogen steel soldering solder additive, the solder additive by reinforcing agent, water-base adhesive and BJQ mixture with
The mass ratio of 1:7:3 mixes, and the reinforcing agent is the mixed of any mass ratio of Ni-coated graphite alkene or plating vanadium graphene or both
It closes, the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the mass ratio of 1:3.5:1.
In the present embodiment, the 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 parts of trbasic zinc phosphate, 45 parts of ammonium chloride, 15 parts of poly- second two
Pure and mild 14 parts of Tisuacryl mixes.
High nitrogen steel described in the present embodiment, the preferably high nitrogen steel of following component, according to weight ratio, the composition of the high nitrogen steel
Ingredient 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 of C, 0.3 part of Si, 0.2
Nb, 0.05 part of the Al, S and 0.05 of 0.02 part part of P of part.
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.
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.
Embodiment 2
A kind of high nitrogen steel soldering solder additive, the solder additive by reinforcing agent, water-base adhesive and BJQ mixture with
The mass ratio of 1:8:5 mixes, and the reinforcing agent is the mixed of any mass ratio of Ni-coated graphite alkene or plating vanadium graphene or both
It closes, the BJQ mixture is that barium glass powder, fumed silica and tartaric acid are mixed with the mass ratio of 1:3.5:1.
In the present embodiment, the 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 36 parts of trbasic zinc phosphate, 61 parts of ammonium chloride, 23 parts of poly- second two
Pure and mild 22 parts of Tisuacryl mixes.
High nitrogen steel described in the present embodiment, the preferably high nitrogen steel of following component, according to weight ratio, the composition of the high nitrogen steel
Ingredient 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 of C, 0.5 part of Si, 0.35
Nb, 0.06 part of the Al, S and 0.08 of 0.05 part part of P of part.
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.
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.
Embodiment 3
A kind of high nitrogen steel soldering solder additive, the solder additive by reinforcing agent, water-base adhesive and BJQ mixture with
The mass ratio of 1:7.5:4 mixes, and the reinforcing agent is any mass ratio of Ni-coated graphite alkene or plating vanadium graphene or both
Mixing, the BJQ mixture are that barium glass powder, fumed silica and tartaric acid are mixed with the mass ratio of 1:3.5:1.
In the present embodiment, the 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 30 parts of trbasic zinc phosphate, 53 parts of ammonium chloride, 19 parts of poly- second two
Pure and mild 18 parts of Tisuacryl mixes.
High nitrogen steel described in the present embodiment, the preferably high nitrogen steel of following component, according to weight ratio, the composition of the high nitrogen steel
Ingredient 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 part of C, 0.4 part of Si,
0.275 part of Nb, 0.055 part of Al, S and 0.065 of 0.035 part part of P.
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.
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.
Claims (5)
1. a kind of high nitrogen steel soldering solder additive, it is characterised in that: the solder additive is by reinforcing agent, water-base adhesive
It is formed with BJQ mixture with the mass ratio of 1:7~8:3~5, the reinforcing agent is Ni-coated graphite alkene or plating vanadium graphene or both
The mixing of any mass ratio, the BJQ mixture are barium glass powder, fumed silica and tartaric acid with the quality of 1:3.5:1
Than mixing.
2. a kind of high nitrogen steel soldering solder additive according to claim 1, it is characterised in that: according to weight ratio, institute
Water-base adhesive is stated by 24~36 parts of trbasic zinc phosphate, 45~61 parts of ammonium chloride, 15~23 parts of polyethylene glycol and 14~22 parts
Tisuacryl mix.
3. a kind of high nitrogen steel soldering solder additive according to claim 1, it is characterised in that: according to weight ratio, institute
State the constituent of 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.
4. a kind of high nitrogen steel soldering solder additive 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.
5. a kind of high nitrogen steel soldering solder additive according to claim 1, which is characterized in that the 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；
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811133488.XA CN109014661B (en) | 2018-09-27 | 2018-09-27 | Brazing filler metal additive for high-nitrogen steel brazing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811133488.XA CN109014661B (en) | 2018-09-27 | 2018-09-27 | Brazing filler metal additive for high-nitrogen steel brazing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109014661A true CN109014661A (en) | 2018-12-18 |
| CN109014661B CN109014661B (en) | 2020-07-10 |
Family
ID=64614685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811133488.XA Active CN109014661B (en) | 2018-09-27 | 2018-09-27 | Brazing filler metal additive for high-nitrogen steel brazing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109014661B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116000501A (en) * | 2022-12-30 | 2023-04-25 | 烟台精创力合科技有限公司 | Drying method for chloride salt used for brazing auxiliary agent |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140299231A1 (en) * | 2013-04-05 | 2014-10-09 | Samsung Electronics Co., Ltd. | Metal-based solder composite including conductive self-healing materials |
| WO2015004467A2 (en) * | 2013-07-10 | 2015-01-15 | Cambridge Enterprise Limited | Materials and methods for soldering, and soldered products |
| CN104400247A (en) * | 2014-09-29 | 2015-03-11 | 哈尔滨工业大学 | Preparation method of high-thermal conductivity graphene-Sn-Ag composite brazing filler metal |
| CN105643148A (en) * | 2016-03-07 | 2016-06-08 | 上海和伍复合材料有限公司 | Silver brazing paste and preparation method thereof |
| CN106475703A (en) * | 2016-11-30 | 2017-03-08 | 安徽华众焊业有限公司 | Lead-free pasty welding material and preparation method thereof |
| CN106695158A (en) * | 2016-12-28 | 2017-05-24 | 北京康普锡威科技有限公司 | Soft solder containing graphene and preparation method of soft solder |
| CN108340092A (en) * | 2018-03-02 | 2018-07-31 | 华北水利水电大学 | A kind of brazing material and preparation method thereof for anode steel claw reparation |
-
2018
- 2018-09-27 CN CN201811133488.XA patent/CN109014661B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140299231A1 (en) * | 2013-04-05 | 2014-10-09 | Samsung Electronics Co., Ltd. | Metal-based solder composite including conductive self-healing materials |
| WO2015004467A2 (en) * | 2013-07-10 | 2015-01-15 | Cambridge Enterprise Limited | Materials and methods for soldering, and soldered products |
| CN104400247A (en) * | 2014-09-29 | 2015-03-11 | 哈尔滨工业大学 | Preparation method of high-thermal conductivity graphene-Sn-Ag composite brazing filler metal |
| CN105643148A (en) * | 2016-03-07 | 2016-06-08 | 上海和伍复合材料有限公司 | Silver brazing paste and preparation method thereof |
| CN106475703A (en) * | 2016-11-30 | 2017-03-08 | 安徽华众焊业有限公司 | Lead-free pasty welding material and preparation method thereof |
| CN106695158A (en) * | 2016-12-28 | 2017-05-24 | 北京康普锡威科技有限公司 | Soft solder containing graphene and preparation method of soft solder |
| CN108340092A (en) * | 2018-03-02 | 2018-07-31 | 华北水利水电大学 | A kind of brazing material and preparation method thereof for anode steel claw reparation |
Non-Patent Citations (1)
| Title |
|---|
| 耿文范: "双相不锈钢的开发和应用现状", 《特殊钢》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN116000501A (en) * | 2022-12-30 | 2023-04-25 | 烟台精创力合科技有限公司 | Drying method for chloride salt used for brazing auxiliary agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109014661B (en) | 2020-07-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109108522A (en) | A kind of composite soldering and preparation method thereof for being brazed high nitrogen steel | |
| CN106944765B (en) | A kind of self-protection flux-cored wire for X80 pipe line steel | |
| CN108526752B (en) | Self-protection flux-cored wire for welding in wading environment | |
| CN109128583A (en) | A kind of solder and preparation method thereof for vacuum brazing high nitrogen steel | |
| CN109014661A (en) | A kind of high nitrogen steel soldering solder additive | |
| CN110369908A (en) | The excellent SA-508Gr.4N steel all position welding hydrogen controlled electrode of low-temperature impact toughness | |
| CN110587178A (en) | Self-protection flux-cored wire for welding aluminum and stainless steel and preparation method thereof | |
| CN104741834A (en) | Flux-cored wire for welding X90 pipeline steel and preparing method thereof | |
| CN110253172A (en) | A kind of high-strength steel Ar-CO2Metal powder core solder wire used for gas shield welding | |
| CN109014660A (en) | A kind of high nitrogen steel soldering reinforcing agent of solder | |
| CN116944734B (en) | Sintered flux for submerged arc welding of heat-resistant steel, and preparation method and application thereof | |
| CN109158780A (en) | It is a kind of to be brazed complex welding method for aluminium alloy/high nitrogen steel laser spot welding-electron beam | |
| CN115446499B (en) | Flux-cored powder, flux-cored aluminum welding wire with flux-cored powder and preparation method of flux-cored aluminum welding wire | |
| CN114905187B (en) | Low-hydrogen type welding rod applicable to austenitic light steel and preparation method | |
| CN112404788B (en) | Martensitic heat-resistant steel G115 matched welding rod for power station and preparation method thereof | |
| CN114346522B (en) | Stainless steel submerged arc welding wire welding flux capable of using alternating current for hydrogen energy and welding process | |
| JP3686545B2 (en) | A groove filler for simple single-sided submerged arc welding and a welding method using the same. | |
| CN115770973A (en) | Flux-cored wire | |
| CN112475661B (en) | Nickel-chromium-iron coating and welding rod for welding nickel-based alloy and preparation method thereof | |
| CN112809244B (en) | High-toughness high-efficiency welding rod | |
| CN112108791B (en) | Alkaline seamless flux-cored wire for improving low-temperature toughness of low-alloy high-strength steel welding joint | |
| CN108568614B (en) | Anti-coated red cracking nickel-based alloy welding rod and preparation method thereof | |
| KR102056637B1 (en) | Flux cored wire for gas shield | |
| JPH10180488A (en) | Flux cored wire for electro gas arc welding | |
| JPH0255696A (en) | Flux cored wire for gas shielded arc welding |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |