CN106271179A - A kind of ZrB2crB2duplex heat treatment deposition rod and preparation method thereof - Google Patents
A kind of ZrB2crB2duplex heat treatment deposition rod and preparation method thereof Download PDFInfo
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- CN106271179A CN106271179A CN201610782535.8A CN201610782535A CN106271179A CN 106271179 A CN106271179 A CN 106271179A CN 201610782535 A CN201610782535 A CN 201610782535A CN 106271179 A CN106271179 A CN 106271179A
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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
The present invention provides a kind of ZrB2‑CrB2Duplex heat treatment deposition rod and preparation method thereof.The present invention with Zr powder, Cr powder and B powder that gross mass content is 70～95wt%, gross mass content be 5～30wt% Si powder and Mn powder be raw material, by high-energy ball milling and sinter molding, obtain ZrB2‑CrB2Duplex heat treatment deposition rod.The present invention, by the composition of appropriate design deposition rod, controls the phase composition of powder simultaneously by ball milling and sintering process, and the deposition rod prepared forms ZrB in use2‑CrB2Duplex heat treatment, it is possible to realize and the basic metallurgical binding of chromium-zirconium-copper spot-wedling electrode, improves the bond strength of coating and chromium-zirconium-copper spot-wedling electrode matrix, improves the chromium-zirconium-copper Spot Welding Electrode during Spot Welding of Zinc Coated Steels life-span further.
Description
Technical field
The present invention relates to technical field of metal, particularly to a kind of ZrB2-CrB2Duplex heat treatment deposition rod and system thereof
Preparation Method.
Background technology
Along with developing rapidly and people's raising to environmental requirement of auto industry, coating (zinc-plated, aluminize) steel plate and aluminum
Plate application on automobile gets more and more；Spot welding is most important process in Hyundai Motor process industry, and it has production
Efficiency is high, welding cost is low, it is easy to accomplish automatization and be widely used in machine-building and automobile production.Spot-wedling electrode is a little
Easily-consumed products during weldering, in pinpoint welding procedure, the major function of electrode is transmission electric current, pressurizes and dispels the heat.Between this, spot welding
Electrode mainly produces material using copper alloy as it, most widely used with chromium-zirconium-copper (ZrCrCu) again.
Owing to temperature when electrode and absorption surface is higher, and spot-wedling electrode self has certain resistance, in spot welding
Also can produce resistance heat under the effect of electric current, therefore the temperature rise of spot-wedling electrode head is quickly, has reached to be slightly less than nugget
High temperature, makes electrode head lose efficacy under the common effect of high temperature and high pressure, especially during spot welding automobile clad steel sheet, and eutectic
The coating material of point reduces contact resistance, compared with spot welding general steel plate (non-clad steel sheet), needs increase of weld current or prolongs
Long weld interval guarantee point quality, electrode working portion is under spot welded hot and power synergy, the lowest with surface of steel plate
Fusing point coating material reacts, and forms the alloy of low melting point, and this will accelerate electrode failure.Electricity when spot welding clad steel sheet and aluminium sheet
The life-span of pole than spot welding non-coating steel plate time electrode life-span want much shorter, this increase also make while spot-wedling electrode consumption raw
Product cost increases, but also because frequently changing electrode, reduces productivity ratio.
At present, mainly the surface peening optimizing design and electrode by electrode shape reduces the abrasion of electrode, extends
The life-span of electrode.Though the electrode selecting Reasonable Shape can improve electrode life to a certain extent, but when welding galvanized steel plain sheet,
The essential problem of electrode failure cannot be solved, thus the raising of electrode life is the most limited.The welding plating of chromium-zirconium-copper spot-wedling electrode
During zinc steel plate, its dominant failure mode becomes the alloying reaction shown as between spot-wedling electrode material and steel plate coating, therefore needs
Taking rational technique to stop or the chromium-zirconium-copper spot-wedling electrode alloying that slows down, the surface peening of electrode is to improve the electrode longevity at present
Order ideal means.
Chinese patent ZL201310684586.3, ZL201310683068.X, ZL201310684856.0 individually disclose
A kind of deposition rod of spot-wedling electrode electric spark on surface deposition coating and preparation method thereof, final goal in above-mentioned granted patent
It is to obtain TiB on chromium-zirconium-copper spot-wedling electrode surface respectively2-ZrB2、TiB2-TiC、Al2O3-TiB2Duplex heat treatment, carries with this
The high chromium-zirconium-copper spot-wedling electrode life-span.Though above-mentioned patent improves the spot-wedling electrode life-span the most to a certain extent, but coating and matrix
Between metallurgical binding ratio relatively low, or be entirely mechanical bond, thus it be strong to improve the combination between coating and matrix
Degree, makes increase substantially electrode life.
Summary of the invention
It is an object of the invention to provide a kind of ZrB2-CrB2Duplex heat treatment deposition rod and preparation method thereof.The present invention carries
ZrB prepared by the preparation method of confession2-CrB2Duplex heat treatment deposition rod, it is possible to realize coating and the basic smelting of chromium-zirconium-copper spot-wedling electrode
Gold combines, and improves the bond strength of coating and chromium-zirconium-copper spot-wedling electrode matrix, improves chromium-zirconium-copper spot-wedling electrode spot welding plating further
The zinc steel plate life-span.
The invention provides a kind of ZrB2-CrB2The duplex heat treatment preparation method of deposition rod, comprises the following steps:
(1) Zr powder, Cr powder, B powder, Si powder and Mn powder being mixed, ball milling obtains mixed material；Described Zr powder, Cr powder and B powder
Gross mass is mixed material quality 70～95wt%, described Si powder and gross mass is mixed material quality the 5 of Mn powder～
30wt%；
(2) being mixed with binding agent by the mixed material that described step (1) obtains, cold moudling obtains green compact；
(3) the green compact defat described step (2) obtained and sintering, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
Preferably, in described step (1), the mol ratio of Zr powder, Cr powder and B powder is 1:0.8～1.2:3.5～4.5.
Preferably, in described step (1), the mass ratio of Si powder and Mn powder is 1:0.5～1.5.
Preferably, in described step (1), the ratio of grinding media to material of ball milling is 10～30:1.
Preferably, in described step (1), the rotating speed of ball milling is 300～500r/min.
Preferably, in described step (1), the time of ball milling is 24～48h.
Preferably, the ball milling in described step (1) is carried out under vacuum or inert gas shielding.
Preferably, in described step (3), the temperature of defat is 700～800 DEG C, and the time of defat is 0.5～1h.
Preferably, in described step (3), the temperature of sintering is 1000～1100 DEG C, and the time of sintering is 1～2h.
Present invention also offers the ZrB prepared according to technique scheme2-CrB2Duplex heat treatment deposition rod, phase composition is not
Containing ZrB2And CrB2Phase.
The present invention is 5～30wt% with Zr powder, Cr powder and B powder that gross mass content is 70～95wt%, gross mass content
Si powder and Mn powder be raw material, by high-energy ball milling and sinter molding, obtain ZrB2-CrB2Duplex heat treatment deposition rod.The present invention
By the composition of appropriate design deposition rod, with Zr, Cr, B as ZrB2-CrB2The duplex heat treatment material of main part of deposition rod, with Si and
Mn, as metal adhesive, improves alloying ratio between coating and matrix；Control powder by ball milling and sintering process simultaneously
Phase composition, it is to avoid in deposition rod preparation process produce ZrB2And CrB2Phase, can to reduce Zr-Cr-B system anti-for ball milling simultaneously
ZrB should be generated2-CrB2Activation energy, obtain ZrB for electric spark in situ deposition during using2-CrB2Duplex heat treatment provides energy
Preparation in terms of amount and phase composition；The deposition rod prepared forms ZrB in use2-CrB2Duplex heat treatment, it is possible to realize with
The basic metallurgical binding of chromium-zirconium-copper spot-wedling electrode, improves the bond strength of coating and chromium-zirconium-copper spot-wedling electrode matrix, improves further
The chromium-zirconium-copper Spot Welding Electrode during Spot Welding of Zinc Coated Steels life-span.Test result indicate that, ZrB prepared by the preparation method that the present invention provides2-
CrB2Duplex heat treatment deposition rod can in-situ preparation ZrB2-CrB2Duplex heat treatment, electrode life is up to 4000 points.
Detailed description of the invention
The invention provides a kind of ZrB2-CrB2The duplex heat treatment preparation method of deposition rod, comprises the following steps:
(1) Zr powder, Cr powder, B powder, Si powder and Mn powder being mixed, ball milling obtains mixed material；Described Zr powder, Cr powder and B powder
Gross mass is mixed material quality 70～95wt%, described Si powder and gross mass is mixed material quality the 5 of Mn powder～
30wt%；
(2) being mixed with binding agent by the mixed material that described step (1) obtains, cold moudling obtains green compact；
(3) the green compact defat described step (2) obtained and sintering, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
Zr powder, Cr powder, B powder, Si powder and Mn powder are mixed by the present invention, and ball milling obtains mixed material；Described Zr powder, Cr powder and
The gross mass of B powder is the 70～95wt% of mixed material quality, described Si powder and gross mass is mixed material quality the 5 of Mn powder
～30wt%.In the present invention, the gross mass of described Zr powder, Cr powder and B powder is preferably the 75～90wt% of mixed material quality,
More preferably 80～85wt%.In the present invention, the mol ratio of described Zr powder, Cr powder and B powder is preferably 1:0.8～1.2:3.5
～4.5, more preferably 1:0.9～1.1:3.8～4.2.In the present invention, described Zr powder, Cr powder and B powder are based on chromium-zirconium-copper spot welding
Electrode elementary composition (Zr, Cr, Cu), obtains ZrB in situ for electric spark2-CrB2Duplex heat treatment provides the preparation on element, carries
Alloying ratio between high coating and matrix, thus improve coating and basal body binding force.
In the present invention, the gross mass of described Si powder and Mn powder is preferably the 10～25wt% of mixed material quality, more excellent
Elect 15～20wt% as.In the present invention, the mass ratio of described Si powder and Mn powder is preferably 1:0.5～1.5, and more preferably 1:
0.8～1.2.In the present invention, described Si powder and Mn powder are as metal adhesive, with ZrB2And CrB2Angle of wetting the least, energy
Enough ensure the integrity after deposition rod sintering and intensity.
In the present invention, the granularity of described Zr powder is preferably 200～400 mesh, more preferably 250～350 mesh；Described Cr powder
Granularity be preferably 200～400 mesh, more preferably 250～350 mesh；The granularity of described B powder is preferably 200～400 mesh, more excellent
Elect 250～350 mesh as；The granularity of described Si powder is preferably 200～400 mesh, more preferably 250～350 mesh；The grain of described Mn powder
Degree is preferably 200～400 mesh, more preferably 250～350 mesh.
In the present invention, the purity of described Zr powder is preferably not lower than 99wt%；The purity of described Cr powder is preferably the lowest
In 99wt%；The purity of described B powder is preferably not lower than 99wt%；The purity of described Si powder is preferably not lower than 99wt%；Institute
The purity stating Mn powder is preferably not lower than 99wt%.
In the present invention, the ratio of grinding media to material of described ball milling is preferably 10～30:1, more preferably 15～25:1, and most preferably 18
～22:1；The rotating speed of described ball milling is preferably 300～500r/min, more preferably 350～450r/min, most preferably 380～
420r/min；The time of described ball milling is preferably 24～48h, more preferably 30～40h, most preferably 32～36h.In the present invention
In, described ball milling is preferably carried out under inert gas shielding；Described noble gas is preferably nitrogen or argon.In the present invention,
Described ball milling can control the phase composition of powder, it is to avoid produces ZrB in deposition rod preparation process2And CrB2Phase, reduces simultaneously
The reaction of Zr-Cr-B system generates ZrB2-CrB2Activation energy, obtain ZrB for electric spark in situ deposition during using2-CrB2Multiple
Phase coating provides the preparation in terms of energy and phase composition.
After obtaining mixed material, described mixed material is mixed by the present invention with binding agent, and cold moudling obtains green compact.At this
In invention, the Functionality, quality and appealing design of described binding agent elects the 0.5～1% of mixed material quality, more preferably 0.6～0.8% as.The present invention
The kind of described binding agent is not had special requirement, uses powder used in metallurgy binding agent well known to those skilled in the art i.e.
Can.In the present invention, described binding agent is preferably liquid paraffin or zinc stearate.
The present invention does not has special restriction to the operation of described cold moudling, uses well known to those skilled in the art colding pressing
The technical scheme of molding.In the present invention, the pressuring method of described cold moudling is preferably two-phase pressure；Described it is cold-pressed into
The pressure of type is preferably 4000～6000N, more preferably 4500～5500N.
The present invention does not has special restriction to the size of described green compact, uses deposition well known to those skilled in the art rod
Size.In the present invention, the diameter of described green compact is preferably 6～8mm；The length of described green compact is preferably 30～40mm.
After obtaining green compact, the present invention, by described green compact defat and sintering, obtains ZrB2-CrB2Duplex heat treatment deposition rod.?
In the present invention, described defat is preferably carried out under inert gas shielding；Described noble gas is preferably nitrogen or argon.At this
In bright, the temperature of described defat is preferably 700～800 DEG C, more preferably 720～780 DEG C, most preferably 740～760 DEG C；Institute
The time stating defat is preferably 0.5～1h, more preferably 0.6～0.8h.
Temperature is preferably warming up to sintering temperature after defat completes and is sintered by the present invention, obtains ZrB2-CrB2Complex phase is coated with
Layer deposition rod.In the present invention, described sintering is preferably carried out under inert gas shielding；Described noble gas is preferably nitrogen
Or argon.In the present invention, described in be warming up to the heating rate of sintering temperature and be preferably 10～20 DEG C/min, more preferably 14～
16℃/min.In the present invention, the temperature of described sintering is preferably 1000～1100 DEG C, more preferably 1020～1080 DEG C,
It is preferably 1040～1060 DEG C；The time of described sintering is preferably 1～2h, more preferably 1.4～1.6h.
The present invention preferably cools down after completing described sintering.In the present invention, described cooling is preferably furnace cooling.
Present invention also offers ZrB prepared by preparation method described in a kind of technique scheme2-CrB2Duplex heat treatment is with molten
Applying rod, phase composition does not contains ZrB2And CrB2Phase.In the present invention, described ZrB2-CrB2Duplex heat treatment deposition rod preferably includes
Zr, Cr and B simple substance phase.
In order to further illustrate the present invention, the ZrB present invention provided below in conjunction with embodiment2-CrB2Duplex heat treatment is with molten
Apply rod and preparation method thereof to be described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1:
By 75 grams of (Zr+Cr+B) powder (mol ratio of Zr, Cr and B is 1:1:4), 25 grams of (Si+Mn) powder (Si and Mn matter
Amount is than being 1:1) uniformly after mixing, by the ratio of grinding media to material of 20:1, with 400r/min speed ball milling 32 hours；
Above-mentioned mixed-powder good for ball milling is added 1 gram of liquid paraffin and is pressed into diameter 7mm, the bar of long 35mm；
In argon atmosphere, bar is incubated 0.5 hour at 750 DEG C, then with the heating rate of 15 DEG C/min
It is incubated 1.5 hours to 1050 DEG C, last furnace cooling, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
The ZrB obtained after the present embodiment sintering2-CrB2Duplex heat treatment is with deposition rod outside drawing such as Fig. 1 (a) Suo Shi.From figure
It can be seen that deposition rod prepared by the present embodiment is in the most bar-shaped.
Embodiment 2:
By 80 grams of (Zr+Cr+B) powder (mol ratio of Zr, Cr and B is 1:1:4), 20 grams of (Si+Mn) powder (Si and Mn matter
Amount is than being 1:1) uniformly after mixing, by the ratio of grinding media to material of 30:1, with 300r/min speed ball milling 34 hours；
Above-mentioned mixed-powder good for ball milling is added 5 grams of liquid paraffin pressures and is pressed into diameter 7mm, the bar of long 35mm；
In argon atmosphere, bar is incubated 0.5 hour at 750 DEG C, then with the heating rate of 15 DEG C/min
It is incubated 1.5 hours to 1100 DEG C DEG C, last furnace cooling, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
Embodiment 3:
By 85 grams of (Zr+Cr+B) powder (mol ratio of Zr, Cr and B is 1:1:4), 15 grams of (Si+Mn) powder (Si and Mn matter
Amount is than being 1:1) uniformly after mixing, by the ratio of grinding media to material of 10:1, with 500r/min speed ball milling 36 hours；
Above-mentioned mixed-powder good for ball milling is added 5 grams of liquid paraffin pressures and is pressed into diameter 7mm, the bar of long 35mm；
In argon atmosphere, bar is incubated 0.5 hour at 800 DEG C, then with the heating rate of 15 DEG C/min
It is incubated 1.5 hours to 1100 DEG C DEG C, last furnace cooling, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
Embodiment 4:
By 90 grams of (Zr+Cr+B) powder (mol ratio of Zr, Cr and B is 1:1:4), 10 grams of (Si+Mn) powder (Si and Mn matter
Amount is than being 1:1) uniformly after mixing, by the ratio of grinding media to material of 25:1, with 450r/min speed ball milling 38 hours；
Above-mentioned mixed-powder good for ball milling is added 5 grams of liquid paraffin pressures and is pressed into diameter 7mm, the bar of long 35mm；
In argon atmosphere, bar is incubated 0.5 hour at 800 DEG C, then with the heating rate of 15 DEG C/min
It is incubated 1.5 hours to 1100 DEG C DEG C, last furnace cooling, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
Comparative example 1:
By the method according to embodiment 1, Si and Mn is replaced with respectively Ni and Mo, prepares ZrB2-CrB2Duplex heat treatment
With deposition rod.
The ZrB obtained after this comparative example sintering2-CrB2Duplex heat treatment is excellent as shown in Fig. 1 (b) by deposition.Can from figure
Going out, the integrity after this comparative example deposition rod sintering cannot be ensured, more has no way of using.
Comparative example 2:
TiB is prepared according to the technical scheme disclosed in Chinese patent CN 103805988 A2-ZrB2Duplex heat treatment is used
Deposition rod.
Comparative example 3:
TiB is prepared according to the technical scheme disclosed in Chinese patent CN 103801858 A2-TiC duplex heat treatment is used
Deposition rod.
Comparative example 4:
Al is prepared according to the technical scheme disclosed in Chinese patent CN 103801851 A2O3-TiB2Duplex heat treatment is used
Deposition rod.
Respectively duplex heat treatment deposition rod prepared by embodiment 1 and comparative example 2～4 is used electric spark deposition technology in situ
Prepare coating on chromium-zirconium-copper spot-wedling electrode surface, obtain the microscopic appearance of coating as shown in Figure 2.It can be seen that use
Deposition rod chromium-zirconium-copper spot-wedling electrode surface in situ deposition gained coating prepared by the present invention not only has preferable integrity, and
Obvious break-off is not had between coating and matrix.
Respectively duplex heat treatment deposition rod prepared by embodiment 1 and comparative example 2～4 is used electric spark deposition technology in situ
Prepare coating on chromium-zirconium-copper spot-wedling electrode surface, in mensuration coating, boron element Gradient distribution is as shown in Figure 3.Can from figure
Go out, deposition rod prepared by the present invention by electric spark chromium-zirconium-copper spot-wedling electrode surface in situ deposit gained coating, its coating with
Matrix has the metallurgical binding of higher proportion.
Respectively duplex heat treatment deposition rod prepared by embodiment 1 and comparative example 2～4 is used electric spark deposition technology in situ
Prepare coating on chromium-zirconium-copper spot-wedling electrode surface, measure the bond strength of coating and matrix as shown in Figure 4.Can from figure
Going out, deposition rod prepared by the present invention has more preferable bond strength.
Respectively duplex heat treatment deposition rod prepared by embodiment 1 and comparative example 2～4 is used electric spark deposition technology in situ
Prepare coating on chromium-zirconium-copper spot-wedling electrode surface, test is as shown in table 1 for electrode life.
The welding electrode life-span prepared by table 1 embodiment of the present invention and comparative example duplex heat treatment deposition rod
By above comparative example and embodiment it can be seen that the ZrB for preparing of preparation method that provides of the present invention2-CrB2Complex phase is coated with
Layer deposition rod forms ZrB in use2-CrB2Duplex heat treatment, it is possible to realize and the basic metallurgical binding of chromium-zirconium-copper spot-wedling electrode,
Improve the bond strength of coating and chromium-zirconium-copper spot-wedling electrode matrix, improve the chromium-zirconium-copper Spot Welding Electrode during Spot Welding of Zinc Coated Steels longevity further
Life.
The above is only the preferred embodiment of the present invention, and the present invention not makees any pro forma restriction.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to if making
Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a ZrB2-CrB2The duplex heat treatment preparation method of deposition rod, comprises the following steps:
(1) Zr powder, Cr powder, B powder, Si powder and Mn powder being mixed, ball milling obtains mixed material；Described Zr powder, Cr powder and B powder total
Quality is the 70～95wt% of mixed material quality, described Si powder and gross mass is mixed material quality the 5 of Mn powder～
30wt%；
(2) being mixed with binding agent by the mixed material that described step (1) obtains, cold moudling obtains green compact；
(3) the green compact defat described step (2) obtained and sintering, obtain ZrB2-CrB2Duplex heat treatment deposition rod.
Preparation method the most according to claim 1, it is characterised in that in described step (1), Zr powder, Cr powder and B powder rubs
That ratio is 1:0.8～1.2:3.5～4.5.
Preparation method the most according to claim 1, it is characterised in that Si powder and the mass ratio of Mn powder in described step (1)
For 1:0.5～1.5.
4. according to the preparation method described in claims 1 to 3 any one, it is characterised in that the ball of ball milling in described step (1)
Material ratio is 10～30:1.
Preparation method the most according to claim 4, it is characterised in that in described step (1) rotating speed of ball milling be 300～
500r/min。
Preparation method the most according to claim 1 or 5, it is characterised in that in described step (1) time of ball milling be 24～
48h。
Preparation method the most according to claim 6, it is characterised in that the ball milling in described step (1) is in vacuum or inertia
Carry out under gas shield.
Preparation method the most according to claim 1, it is characterised in that in described step (3) temperature of defat be 700～
800 DEG C, the time of defat is 0.5～1h.
Preparation method the most according to claim 1, it is characterised in that in described step (3) temperature of sintering be 1000～
1100 DEG C, the time of sintering is 1～2h.
10. the ZrB that prepared by preparation method described in claim 1～9 any one2-CrB2Duplex heat treatment deposition rod, phase composition
Without ZrB2And CrB2Phase.
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| CN110000005A (en) * | 2019-02-13 | 2019-07-12 | 浙江润洁环境科技股份有限公司 | A kind of electric precipitator of the preparation process and application of electric precipitator the shell shell |
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