CN103978219B - One can soldering nickel conductor electrode and preparation method thereof - Google Patents
One can soldering nickel conductor electrode and preparation method thereof Download PDFInfo
- Publication number
- CN103978219B CN103978219B CN201410220467.7A CN201410220467A CN103978219B CN 103978219 B CN103978219 B CN 103978219B CN 201410220467 A CN201410220467 A CN 201410220467A CN 103978219 B CN103978219 B CN 103978219B
- Authority
- CN
- China
- Prior art keywords
- nickel
- conductor electrode
- preparation
- soldering
- electrode
- 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.)
- Active
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 260
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 126
- 239000004020 conductor Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 55
- 238000005476 soldering Methods 0.000 title claims abstract description 35
- 238000007747 plating Methods 0.000 claims abstract description 43
- 239000000126 substance Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 28
- 239000000428 dust Substances 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- 229910000990 Ni alloy Inorganic materials 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 239000000853 adhesive Substances 0.000 claims abstract description 14
- 230000001070 adhesive effect Effects 0.000 claims abstract description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 11
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 11
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 11
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052796 boron Inorganic materials 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229910000679 solder Inorganic materials 0.000 claims description 9
- 241000080590 Niso Species 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 6
- KIMPPGSMONZDMN-UHFFFAOYSA-N sodium;dihydrogen phosphite Chemical compound [Na+].OP(O)[O-] KIMPPGSMONZDMN-UHFFFAOYSA-N 0.000 claims description 6
- 206010070834 Sensitisation Diseases 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 230000008313 sensitization Effects 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000009713 electroplating Methods 0.000 claims 2
- 101150003085 Pdcl gene Proteins 0.000 abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 229910000510 noble metal Inorganic materials 0.000 description 7
- 238000001994 activation Methods 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Conductive Materials (AREA)
Abstract
The open one of the present invention can soldering nickel conductor electrode and preparation method thereof, described method is: nickel, boron, aluminium, zinc powder are mixed by predetermined ratio, by compound with the pressure of 6.0-9.0 ton/cm2 pressure knot, by pressure caking at 2.40-3.33 handkerchief, 8-10 hour is incubated in 1200-1300 DEG C, after cooling, pressure caking is crushed to 80-120nm, obtained nickel alloy powder; Nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive are obtained nickel slurry by predetermined ratio mixed rolling; Be printed onto on alumina substrate by obtained nickel slurry and dry, in air, sintering obtains nickel electrode.Compared to existing nickel electrode, nickel electrode of the present invention has high electrical conductivity, simultaneously nickel electrode acid-alkali-corrosive-resisting of the present invention, and without the need to plating piece alligatoring before chemical nickel plating, also without the need to PdCl
2activation procedure, makes preparation method of the present invention not only simplify operation, also greatly reduces cost, improve the competitiveness of product in market.
Description
Technical field
The present invention relates to powder metallurgy and chemical preparation field, particularly relating to one can soldering nickel conductor electrode and preparation method thereof.
Background technology
Along with the development of electronic information technology, electronic information material is also along with development.Electric slurry belongs to a part in electronic information material.The conductor paste of electric slurry is much made up of noble metal (as Au Ag Pt Pd).Noble metal one is shortage of resources, and two is expensive, and thus it becomes one of factor of restriction electric slurry widespread adoption.
In recent years, the semiconductor cooler electrode grown up, a kind of is make with the copper conductor slurry of high-purity gas protection sintering, can soldering, but cost is too high; Another kind is with W-Mn(Mo) starch in 1500-1600 DEG C of molybdenum sheet stove, sinter at Al under hydrogen shield
2o
3on substrate.Because temperature is too high, Al
2o
3substrate is out of shape, need 800 DEG C of corrections.The electrode resistance obtained is large, and can not soldering.Can soldering for solving, chemical nickel plating be carried out (by electrode clean, SnCl
2sensitization, PdCl
2the operations such as activation process), the electrode conductivuty after process improves greatly, soldering (Pb
36sn
62ag
2scolding tin), adhesive force also can meet use.But said method prepares the complex procedures of nickel coating electrode, equipment and material are (as PdCl
2) expensive, consuming time, power consumption work consuming time.In sum, noble metal needs to find substitute, although copper conductor slurry can soldering manufacturing cost high, W-Mn(Mo) cost of sizing agent is cheap, but sintering method is complicated, consuming time, manufacturing cost is high.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide one can soldering nickel conductor electrode and preparation method thereof, be intended to solve current nickel electrode manufacturing process complex procedures, the problem that consuming time, manufacturing cost is high.
Technical scheme of the present invention is as follows:
Can the preparation method of soldering nickel conductor electrode, wherein, said method comprising the steps of:
By nickel, boron, aluminium, zinc powder by predetermined ratio mixing, compound is carried out pressure knot with the pressure of 6.0-9.0 ton/cm2, pressure is tied the pressure obtained to lump in 2.40-3.33 handkerchief vacuum environment, 8-10 hour is incubated in 1200-1300 DEG C of temperature, after cooling, pressure caking is crushed to 80-120nm, obtained nickel alloy powder;
Nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive are obtained nickel slurry by predetermined ratio mixed rolling, and wherein said glass dust is by MgO, CaO, Al
2o
3, SiO
2, B
2o
3, PbO founds rear pulverizing and makes;
Being printed onto by obtained nickel slurry on alumina substrate and drying, finally sintering obtains nickel conductor electrode in atmosphere.
Described can the preparation method of soldering nickel conductor electrode, wherein, the predetermined ratio of described nickel, boron, aluminium, zinc powder mixing is: by weight percentage, boron powder 1.0-8.0, aluminium powder 0.1-1.0, zinc powder 0.3-3.0 and aequum nickel powder, each component sum is 100%.
Described can the preparation method of soldering nickel conductor electrode, wherein, described sintering temperature is 850-1000 DEG C.
Described can the preparation method of soldering nickel conductor electrode, wherein, granularity≤30 μm of described nickel powder.
Described can the preparation method of soldering nickel conductor electrode, wherein, the predetermined ratio of described nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive mixing is: by weight percentage, nickel alloy powder 70-80, glass dust 5-10, ethyl cellulose and terpinol adhesive 10-25.
Described can the preparation method of soldering nickel conductor electrode, wherein, described glass dust is by MgO, CaO, Al
2o
3, SiO
2, B
2o
3, PbO founds rear pulverizing and makes and be specially: by weight percentage, by the Al of CaO, 5-10% of MgO, 3-5% of 2-5%
2o
3, 10-23% SiO
2, 13-20% B
2o
3, 37-67% PbO mix, after founding at 1300 DEG C of temperature pulverize obtain glass dust.
Described can the preparation method of soldering nickel conductor electrode, wherein, described method also comprises: carry out acid chemical plating nickel or alkaline chemical nickel-plating to after the nickel conductor electrode pre-treatment of preparation, wherein said pre-treatment is specially: the Na first using 1% weight percent concentration
2cO
3cleaning nickel conductor electrode nickel film surface, the stannous chloride sensitization of rear 10-20% weight percent concentration 5 minutes.
Described can the preparation method of soldering nickel conductor electrode, wherein, containing NiSO in the plating solution that acid chemical plating nickel is used
47H
2o30g/L, sodium dihydrogen phosphite 10g/L, sodium acetate 10g/L, asccharin 1-1.5g/L, plating solution pH value is 4-6, and bath temperature is 90 DEG C.
Described can the preparation method of soldering nickel conductor electrode, wherein, containing NiSO in the plating solution that alkaline chemical nickel-plating is used
47H
2o30g/L, sodium dihydrogen phosphite 10g/L, NH
4cl20g/L, ammonium citrate 50g/L, plating solution pH value is 8-10, and bath temperature is 90 DEG C.
One can soldering nickel conductor electrode, wherein, describedly can method as above be adopted to prepare by soldering nickel conductor electrode.
Beneficial effect: the invention provides one can soldering nickel conductor electrode and preparation method thereof, compared to existing nickel electrode, nickel conductor electrode alloying level of the present invention and compactness have and significantly improve, simultaneously, nickel conductor electrode acid and alkali-resistance reagent corrosion of the present invention, and without the need to carrying out alligatoring to plating piece before chemical nickel plating, also without the need to carrying out PdCl
2activation procedure, thus the preparation method of nickel conductor electrode of the present invention not only simplify operation, but also reduces processing cost, correspondingly improves the competitiveness of product in market.
Detailed description of the invention
The invention provides one can soldering nickel conductor electrode and preparation method thereof, and for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The invention provides a kind of can the preparation method of soldering nickel conductor electrode, wherein, said method comprising the steps of:
The preparation of nickel alloy powder: by nickel, boron, aluminium, zinc powder by predetermined ratio mixing, compound is loaded punching block and carry out pressure knot with the pressure of 6.0-9.0 ton/cm2, pressure is tied the pressure caking obtained and load alumina crucible, be sealed in quartz ampoule and be evacuated down to 2.40-3.33 handkerchief, 8-10 hour is incubated in 1200-1300 DEG C of temperature, after cooling, pressure caking is crushed to 80-120nm(and is preferably crushed to 100nm), obtained nickel alloy powder.
The pressure of 6.0-9.0 ton/cm2 pressure is tied and is incubated 8-10 hour reaction condition in 1200-1300 DEG C of temperature and can ensure that the solid state reaction of nickel alloy is thorough, more be conducive to its alloying, and it is high just because of nickel alloy degree of the present invention, reacted alloyed powder could be broken to about 100nm, and finally make prepared nickel conductor electrode finer and close, finally make its electric conductivity be improved.
Wherein, the predetermined ratio of described nickel, boron, aluminium, zinc powder mixing is: by weight percentage, boron powder 1.0-8.0, aluminium powder 0.1-1.0, zinc powder 0.3-3.0 and aequum nickel powder (granularity≤30 μm of nickel powder), each component sum is 100%.
Prepared by nickel slurry: nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive are mixed rolling by predetermined ratio and obtain nickel slurry.Wherein, the predetermined ratio of described nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive mixing is: by weight percentage, nickel alloy powder 70-80, glass dust 5-10, ethyl cellulose and terpinol adhesive 10-25.
In addition, described glass dust is by MgO, CaO, Al
2o
3, SiO
2, B
2o
3, PbO founds rear pulverizing and makes.Be specially: by weight percentage, by the Al of CaO, 5-10% of MgO, 3-5% of 2-5%
2o
3, 10-23% SiO
2, 13-20% B
2o
3, 37-67% PbO mix, obtain glass dust through mechanical crushing after founding at 1300 DEG C of temperature.The nickel conductor electrode acid and alkali-resistance reagent that the glass dust added in nickel slurry is conducive to sintering soaks and is not corroded, and is conducive to the raising of the nickel electrode adhesive force of chemical nickel plating.
The preparation of nickel conductor electrode: by obtained nickel slurry by be screen-printed on alumina substrate and to dry, finally sintering obtains nickel conductor electrode in 850-1000 DEG C of air.
Surveying nickel conductor electrode sheet resistance with electric bridge is 30-40m Ω/.Use Pb
36sn
62ag
2scolding tin is 225-240 DEG C of immersed solder, and nickel conductor electrode of the present invention is not infiltrated by scolding tin.
In addition, carry out acid chemical plating nickel or alkaline chemical nickel-plating to after the nickel conductor electrode pre-treatment of preparation, wherein said pre-treatment is specially: the Na first using 1% weight percent concentration
2cO
3cleaning nickel conductor electrode nickel film surface, the stannous chloride sensitization of rear 10-20% weight percent concentration 5 minutes.
If nickel conductor electrode adopts acid chemical plating nickel, then containing NiSO in plating solution used
47H
2o30g/L, sodium dihydrogen phosphite 10g/L, sodium acetate 10g/L, asccharin 1-1.5g/L, plating solution pH value is 4-6, and bath temperature is 90 DEG C.
If nickel conductor electrode adopts alkaline chemical nickel-plating, containing NiSO in the plating solution that alkaline chemical nickel-plating is used
47H
2o30g/L, sodium dihydrogen phosphite 10g/L, NH
4cl20g/L, ammonium citrate 50g/L, plating solution pH value is 8-10, and bath temperature is 90 DEG C.
Nickel conductor electrode deionized water wash clean after chemical nickel plating, dries, obtains nickel conductor electrode, then be 12-18m Ω/ by bridge measurement sheet resistance in 100-120 DEG C. use Pb
36sn
62ag
2scolding tin carries out immersed solder at 225-240 DEG C, and pad scolding tin infiltrates full.
The present invention also provides one can soldering nickel conductor electrode, wherein, describedly can method as above be adopted to prepare by soldering nickel conductor electrode.Nickel conductor electrode of the present invention can do general conductor and use, and its electric conductivity doubles left and right than the Ni-based conductor of traditional boracic and aluminium-nickel base contained conductor.
Provided by the invention can soldering nickel conductor electrode and preparation method thereof, compared to existing nickel electrode, nickel conductor electrode compactness of the present invention and electric conductivity have and significantly improve, simultaneously, the acidproof alkaline agent corrosion of nickel conductor electrode of the present invention, and without the need to carrying out alligatoring (mechanical coarsening, chemical attack alligatoring) to plating piece before chemical nickel plating, also without the need to carrying out PdCl
2activation procedure, save time power saving, due to without the need to PdCl
2activation procedure, has saved precious metals pd Cl
2
The base metal that preparation method of the present invention is cheap replaces noble metal.Therefore, when electrode sheet resistance is 20-30m Ω/, AgPd20 can be replaced; When electrode sheet resistance is 10-20m Ω/, AgPd10 can be replaced; Can improve by an enterprising step process on the basis of preparation method of the present invention in addition, increase thickness of coating, sheet resistance can be less than 10m Ω/, and at this moment nickel conductor electrode can replace pure Ag electrode to use.Prepared nickel electrode electric conductivity is good, can with leaded or Pb-free solder immersed solder, qualified to the adhesive force of matrix.This saves noble metal, greatly reduce cost.
Preparation method of the present invention can substitute the preparation method using W-Mn (Mo) slurry completely.After using nickel slurry of the present invention instead, only need be once sintered at 850-1000 DEG C.Eliminate expensive molybdenum sheet stove, simultaneously without the need to using protective gas, the Al also without the need to correcting at about 800 DEG C
2o
3substrate, without PdCl during chemical plating
2activation, in a word, nickel conductor electrode preparation method of the present invention enormously simplify existing preparation technology, power saving, saves time, and its preparation cost is only 20% of traditional handicraft.
Meanwhile, the copper that preparation method of the present invention can replace protective atmosphere to sinter completely is starched.The present invention adopts air calcination nickel conductor electrode, and without the need to special stove, without high pure protective gas (as nitrogen), thus compared to the traditional handicraft of protective atmosphere sintered copper slurry, technique of the present invention simplifies greatly, and cost also significantly reduces.
The present invention carries out process modification to nickel alloy powder preparation, uses acid and alkali-resistance glass dust to be combined with nickel alloy powder simultaneously, makes prepared nickel conductor electrode partly can replace noble metal electrode, W-Mn (Mo) electrode and copper electrode.
The solution of the present invention is set forth further below by embodiment
Embodiment 1
1. the preparation of nickel alloy powder
(1) raw material components prepared is as shown in table 1:
The component of table 1, preparation nickel alloy powder and content
| Boron powder | 4.02g |
| Aluminium powder | 0.53g |
| Zinc powder | 2.10g |
| Nickel powder (particle diameter≤30 μm) | 93.35g |
(2) nickel alloy powder is prepared
After in table 1, component V-type machine fully mixes, dress punching block, with 8.5 Dun/㎝
2pressure carry out pressure knot, must press caking to load after quartz ampoule and sealing, being evacuated to 2.67 handkerchiefs, heating 9 hours at 1250 DEG C, with the Ni alloy powder of mechanical crushing to 0.1 μm after cooling.
2. glass dust preparation
(1) component and the content of preparing glass dust are as shown in table 2:
Table 2, the component preparing glass dust and content
| PbO | 55g |
| MgO | 2g |
| CaO | 4g |
| Al 2O 3 | 6g |
| SiO 2 | 13g |
| B 2O 3 | 20g |
(2) glass dust is prepared
Mix in table 2 with V-type machine, load in corundum crucible, 1300 DEG C of meltings about 1 hour, shrend, pulverized the glass dust into about 5 μm.
3. the preparation of nickel slurry and nickel electrode
Take the nickel alloy powder 7.7 grams in step 1,0.6 gram, the glass dust in step 2, ethyl cellulose and 1.7 grams, terpinol adhesive, obtain nickel slurry with three-high mill rolling.With the labyrinthine pattern Al of 250 order silk screen processes at 1 × 102mm
2o
3on substrate, sinter after oven dry in the stove of 950 DEG C, obtain the nickel conductor electrode sintered in air, be 36.4m Ω/mouth by bridge measurement sheet resistance, conductor is to Al
2o
3matrix attachment is good.Use Pb
36sn
62ag
2scolding tin immersed solder, nickel conductor can not weld.
4. the preparation of acid chemical plating nickel electrode
(1) acid chemical plating nickel formula of liquid is as shown in table 3
Table 3, acid chemical plating nickel liquid (g/L)
| NiSO 4·7H2O | 30 |
| NaH 2PO 2 | 10 |
| Sodium acetate | 10 |
| Asccharin | 1.5 |
| PH value | 5 |
(2) chemical nickel plating
By the 1% weight concentration Na of the labyrinthine pattern in step 3
2cO
3cleaning, washes away the alkali of disbud, the SnCl of rear use 10% weight concentration
2solution soaks sensitization about 5 minutes, cleans up.Put into the acidic nickel plating solution of (1), be heated to 90 DEG C, about 60 minutes, nickel plating completed, and cleans up, and drying, is 16.3m Ω/mouth with electric bridge measuring resistance.Pb
36sn
62ag
2solder bath about 230 DEG C, in 4 seconds, nickel conductor is by scolding tin immersed solder, and lead-in wire of burn-oning (area 1 × 2mm), surveying vertical Fracture Force with tensile testing machine is 9.5N.
Embodiment 2
1. nickel alloy powder component and preparation, the preparation of glass dust component and preparation and nickel slurry and nickel electrode is with embodiment 1.
2. the preparation of alkaline electroless plating nickel electrode:
(1) alkaline chemical nickel-plating formula of liquid is as shown in table 4
Table 4, alkaline chemical nickel-plating liquid (g/L)
| NiSO 4·7H 2O | 30 |
| NaH 2PO 2 | 10 |
| NH 4CL | 20 |
| Ammonium citrate | 50 |
| PH value | 9 |
(2) chemical nickel plating
The labyrinthine pattern 1% weight concentration Na that step 3 in embodiment 1 is obtained
2cO
3solution cleans, and washes away residual alkali, the SnCl of rear use 10% weight concentration
2solution soaks sensitization 5 minutes, and clean up, put into the alkali electroless plating solution of (1), be heated to 90 DEG C, about 60 minutes, nickel plating completed, and cleans up, and drying, is 13.7m Ω/, Pb with electric bridge measuring resistance
36sn
62ag
2tin bath groove about 230 DEG C, in 4 seconds, nickel conductor is by scolding tin immersed solder, and lead-in wire of burn-oning (area 1 × 2mm), surveying vertical tension Fracture Force with tensile testing machine is 9.1N.
Nickel conductor electrode in embodiment 1 and preparation method thereof and existing conductor electrode and preparation method thereof are compared.Obtain result as shown in table 5.
Preparation method, the performance test of table 5, the present invention and existing conductor electrode
As can be seen from Table 5, the nickel conductor electrode electric conductivity prepared by the inventive method is good, reaches 13.7-16.3m Ω/, reach the conductivity level of Ag20Pd and Ag10Pd in test.
Starch semiconductor cooler technique relative to W-Mn, chemical plating of the present invention is without the need to PdCl simultaneously
2activation procedure can carry out soldering, thus saves noble metal.
The conductor refrigeration copper sizing process that preparation method of the present invention sinters relative to protective atmosphere, only need sinter, in atmosphere without the need to protective gas, and its cost is well below conductor refrigeration copper sizing process.Therefore the combination property of nickel conductor electrode preparation technology of the present invention is better than existing several nickel electrode preparation method, and thus making prepared nickel conductor electrode possess extremely strong is the market competitiveness.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (6)
1. can the preparation method of soldering nickel conductor electrode, it is characterized in that, said method comprising the steps of:
By nickel, boron, aluminium, zinc powder by predetermined ratio mixing, compound is carried out pressure knot with the pressure of 6.0-9.0 ton/cm2, pressure is tied the pressure obtained to lump in 2.40-3.33 handkerchief vacuum environment, 8-10 hour is incubated in 1200-1300 DEG C of temperature, after cooling, pressure caking is crushed to 80-120nm, obtained nickel alloy powder;
Nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive are obtained nickel slurry by predetermined ratio mixed rolling, and wherein said glass dust is by MgO, CaO, Al
2o
3, SiO
2, B
2o
3, PbO founds rear pulverizing and makes;
Being printed onto by obtained nickel slurry on alumina substrate and drying, finally sintering obtains nickel conductor electrode in atmosphere;
The predetermined ratio of described nickel, boron, aluminium, zinc powder mixing is: by weight percentage, boron powder 1.0-8.0, aluminium powder 0.1-1.0, zinc powder 0.3-3.0 and aequum nickel powder, and each component sum is 100%;
The predetermined ratio of described nickel alloy powder, glass dust, ethyl cellulose, terpinol adhesive mixing is: by weight percentage, nickel alloy powder 70-80, glass dust 5-10, ethyl cellulose and terpinol adhesive 10-25;
Described glass dust is by MgO, CaO, Al
2o
3, SiO
2, B
2o
3, PbO founds rear pulverizing and makes and be specially: by weight percentage, by the Al of CaO, 5-10% of MgO, 3-5% of 2-5%
2o
3, 10-23% SiO
2, 13-20% B
2o
3, 37-67% PbO mix, after founding at 1300 DEG C of temperature pulverize obtain glass dust;
Described method also comprises: carry out acid chemical plating nickel or alkaline chemical nickel-plating to after the nickel conductor electrode pre-treatment of preparation, wherein said pre-treatment is specially: the Na first using 1% weight percent concentration
2cO
3cleaning nickel conductor electrode nickel film surface, the stannous chloride sensitization of rear 10-20% weight percent concentration 5 minutes;
Nickel conductor electrode deionized water wash clean after chemical nickel plating, dries, obtains nickel conductor electrode, then be 12-18m Ω/ by bridge measurement sheet resistance, use Pb in 100-120 DEG C
36sn
62ag
2scolding tin carries out immersed solder at 225-240 DEG C, and pad scolding tin infiltrates full.
2. according to claim 1 can the preparation method of soldering nickel conductor electrode, it is characterized in that, described sintering temperature is 850-1000 DEG C.
3. according to claim 1 can the preparation method of soldering nickel conductor electrode, it is characterized in that, granularity≤30 μm of described nickel powder.
4. according to claim 1 can the preparation method of soldering nickel conductor electrode, it is characterized in that, containing NiSO in the electroplate liquid that acid chemical plating nickel is used
47H
2o30g/L, sodium dihydrogen phosphite 10g/L, sodium acetate 10g/L, asccharin 1-1.5g/L, electroplate liquid pH value is 4-6, and electroplating temperature is 90 DEG C.
5. according to claim 1 can the preparation method of soldering nickel conductor electrode, it is characterized in that, containing NiSO in the electroplate liquid that alkaline chemical nickel-plating is used
47H
2o30g/L, sodium dihydrogen phosphite 10g/L, NH
4cl20g/L, ammonium citrate 50g/L, electroplate liquid pH value is 8-10, and electroplating temperature is 90 DEG C.
6. can a soldering nickel conductor electrode, it is characterized in that, describedly can the method as described in any one of claim 1-5 be adopted to prepare by soldering nickel conductor electrode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410220467.7A CN103978219B (en) | 2014-05-21 | 2014-05-21 | One can soldering nickel conductor electrode and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410220467.7A CN103978219B (en) | 2014-05-21 | 2014-05-21 | One can soldering nickel conductor electrode and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103978219A CN103978219A (en) | 2014-08-13 |
| CN103978219B true CN103978219B (en) | 2016-03-23 |
Family
ID=51270521
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410220467.7A Active CN103978219B (en) | 2014-05-21 | 2014-05-21 | One can soldering nickel conductor electrode and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103978219B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541367B (en) * | 2015-12-11 | 2018-06-29 | 湖北大学 | A kind of ceramic discharge tube low temperature nickel metallization method for sealing |
| CN108922652A (en) * | 2018-05-23 | 2018-11-30 | 江苏时瑞电子科技有限公司 | A kind of Zinc-oxide piezoresistor corrosion-resistant electrode slurry and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100475A (en) * | 1987-01-26 | 1988-06-01 | 中国有色金属工业总公司昆明贵金属研究所 | Composition of nickel base conductive pulp and preparation |
| CN1598969A (en) * | 2004-09-06 | 2005-03-23 | 云南大学 | Resistance material containing nichrome base capable of sintering in air and preparation method thereof |
| CN1871728A (en) * | 2003-10-21 | 2006-11-29 | 瑞沃特科技有限公司 | Electrode, method of its production, metal-air fuel cell and metal hydride cell |
| EP2055419A1 (en) * | 2007-11-05 | 2009-05-06 | Magtech Technology Co., Ltd | Method of soldering a magnesium alloy workpiece with electroless plating with Nickel-Phosphrous, fluxing and use of a leadfree tin alloy solder |
| CN102426925A (en) * | 2012-01-04 | 2012-04-25 | 黑龙江大学 | Method for preparing cobalt and zinc doped nickel hydroxide composite electrode material through electrodeposition |
-
2014
- 2014-05-21 CN CN201410220467.7A patent/CN103978219B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100475A (en) * | 1987-01-26 | 1988-06-01 | 中国有色金属工业总公司昆明贵金属研究所 | Composition of nickel base conductive pulp and preparation |
| CN1871728A (en) * | 2003-10-21 | 2006-11-29 | 瑞沃特科技有限公司 | Electrode, method of its production, metal-air fuel cell and metal hydride cell |
| CN1598969A (en) * | 2004-09-06 | 2005-03-23 | 云南大学 | Resistance material containing nichrome base capable of sintering in air and preparation method thereof |
| EP2055419A1 (en) * | 2007-11-05 | 2009-05-06 | Magtech Technology Co., Ltd | Method of soldering a magnesium alloy workpiece with electroless plating with Nickel-Phosphrous, fluxing and use of a leadfree tin alloy solder |
| CN102426925A (en) * | 2012-01-04 | 2012-04-25 | 黑龙江大学 | Method for preparing cobalt and zinc doped nickel hydroxide composite electrode material through electrodeposition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103978219A (en) | 2014-08-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102723142B (en) | Preparation method of nickel-based silver conductive slurry | |
| CN102126829B (en) | Lead-free glass powder, preparation method thereof, silver paste containing glass powder and crystal silicon solar cell manufactured by using silver paste | |
| CN101377966B (en) | Method for preparing leadless silver electrode slurry for glass substrates | |
| US7556747B2 (en) | Electrically conductive pastes | |
| CN110040968A (en) | A kind of glass powder and the silver-colored aluminium paste in N-type double-sided solar battery front including the glass powder | |
| CN104801709B (en) | Nickel-coated copper clad metal powder and preparation method and application thereof | |
| CN107274963B (en) | Silicon solar cell front side conductive silver paste and preparation method thereof | |
| CN102403049B (en) | Leadless electrode silver paste for lightning protection ZnO piezoresistor and preparation method thereof | |
| CN103540935A (en) | Gold-plating method of high silicon-aluminum composite material | |
| CN102592704B (en) | Aluminum paste for solar energy battery and preparation method thereof | |
| CN108118528B (en) | Flexible conductive textile | |
| CN108010601A (en) | Crystal silicon solar energy battery low contact resistance front electrode silver slurry and preparation method | |
| CN103978219B (en) | One can soldering nickel conductor electrode and preparation method thereof | |
| CN114530280A (en) | Low-cost thick-film conductor paste | |
| CN107863177A (en) | A kind of low-shrinkage crystal silicon solar energy battery front electrode silver slurry and preparation method | |
| CN105118873B (en) | Crystal silicon solar energy battery front electrode silver slurry | |
| CN102969082B (en) | The preparation method of Ag coated Ni composite nano powder electrocondution slurry | |
| CN108735341A (en) | Organically-modified solar cell low contact resistance electrode slurry and preparation method | |
| CN105489266A (en) | Composition of lead-free conductive slurry for crystalline silicon solar cell and preparation method for lead-free conductive slurry | |
| CN107887050A (en) | A kind of crystal silicon solar energy battery high solderability front electrode silver slurry and preparation method | |
| CN107993741A (en) | Silica flour modified crystal silicon solar cell front electrode silver slurry and preparation method | |
| CN108817376A (en) | A kind of electrically conductive graphite copper facing not method for oxidation | |
| CN116230289B (en) | Composition for P+ surface of solar cell, preparation method of composition and solar cell | |
| CN114530274B (en) | Silver migration resistant conductor paste | |
| CN108597641A (en) | The compound silver electrode paste of crystal silicon solar energy battery low contact resistance and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201229 Address after: 224300 No. 2 Industrial Road, Qianqiu Town Industrial Park, Sheyang County, Yancheng City, Jiangsu Province Patentee after: Chen Qingyong Address before: 518052 1st floor, building A3, fenghuanggang third industrial zone, Baoan District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN CHINA FULL POWER TECHNOLOGY Co.,Ltd. |
|
| TR01 | Transfer of patent right |