CN1472367A - Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent - Google Patents
Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent Download PDFInfo
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- CN1472367A CN1472367A CNA031352464A CN03135246A CN1472367A CN 1472367 A CN1472367 A CN 1472367A CN A031352464 A CNA031352464 A CN A031352464A CN 03135246 A CN03135246 A CN 03135246A CN 1472367 A CN1472367 A CN 1472367A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims description 21
- 239000003795 chemical substances by application Substances 0.000 title claims description 10
- 229910000906 Bronze Inorganic materials 0.000 title 1
- 239000010974 bronze Substances 0.000 title 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 title 1
- 238000004513 sizing Methods 0.000 title 1
- 239000002002 slurry Substances 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000004020 conductor Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims description 36
- 238000002360 preparation method Methods 0.000 claims description 27
- 150000001875 compounds Chemical class 0.000 claims description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 14
- 230000004048 modification Effects 0.000 claims description 14
- -1 polyoxyethylene Polymers 0.000 claims description 11
- 230000002829 reductive effect Effects 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 235000013312 flour Nutrition 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 235000012054 meals Nutrition 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 3
- 229910001316 Ag alloy Inorganic materials 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 19
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000010953 base metal Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000004840 adhesive resin Substances 0.000 description 1
- 229920006223 adhesive resin Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
Abstract
An electrically conductive composite copper powder and composite slurry for copper conductor is prepared through preparing superfine copper powder, depositing a silver alloy layer on the surface of copper particle for modifying its surface, preparing electronic slurry by adding reducing agent, and direct sintering without protective atmosphere. Its advantages are good electric conductivity and low cost.
Description
Technical field
The present invention relates to microelectronics or technical fields such as electrochemistry and chemical industry, especially a kind of conduction is with the preparation method of compound copper powder and compound copper conductor slurry.
Background technology
Electric slurry has been widely used in the every field of electron trades such as wafer capacitance device, potentiometer, thick film hybrid integrated circuit, sensor, surface installation technique.The electrode of electronic ceramics element is many to be raw material with precious metals such as gold and silver, palladiums, making the ceramic capacitor electrode with silver slurry has good characteristic such as the simple and electrical condenser high frequency of technology and is widely used, but the premium properties of ceramic dielectic often moves destroyed because of silver ions and causes electrical condenser to lose efficacy, in addition, when welding, capacitor lead wire can be made electrode for capacitors have latent defect by the tin corrode easily because of silver again.Given this, people consider to use the base metal slurry.
In base metal, copper is as the main starting material of electric slurry, because it has ideal as the due characteristic of conductor paste, the electrode of making the electronic ceramics element of it can reach service requirements, and price is more much lower than precious metal, is the high electrode materials of a kind of cost performance.Existing copper slurry is made up of copper powder and thermosetting resin, but when the copper slurry thermofixation constitutes rete, the easy copper of oxidation and airborne oxygen and adhesive resin chemical combination mutually, and at the surface of copper powder particle formation layer oxide film, thus its electroconductibility influenced greatly.And As time goes on, the copper conductor rete of being made up of this copper slurry finally can completely lose its electroconductibility.
Since the seventies, scientific and technical personnel and manufacturer adopt high purity nitrogen protection sintering process usually both at home and abroad.But the copper electrocondution slurry of nitrogen protective sintering requires: (1) research unit and user must possess the nitrogen sintering oven of the costliness of being worth; (2) sufficient source nitrogen supply must be arranged, per hour consume the about 5m of high pure nitrogen
3(3) in sintering process, the charcoal that requires organic carrier to remain in the conductor must be removed, and therefore must allocate suitable oxygen in nitrogen, and nitrogen, oxygen cooperate the control of ratio comparatively difficult.Therefore adopt non-cheaply protection sintering technology and specific equipment to have great importance.
The copper electrocondution slurry of air calcination forms commercialization finally at the end of the seventies in last century, its representative brand is 9535 of a du pont company.Be better than gold owing to the electroconductibility of copper is only second to silver, thereby people study the technology of coalesced copper electrocondution slurry in the air at all costs, the patent of invention of announcement is countless, but fails to promote until today.Its major cause is: existing technology is agglomerating technology instability in air, still can't realize commercialization.
Summary of the invention
The objective of the invention is to avoid above-mentioned deficiency of the prior art; the preparation method of a kind of conduction with compound copper powder and compound copper conductor slurry proposed; this method becomes composite powder at superfine cupper powder surface deposition one deck silver alloys; in the slurry preparation, add reductive agent; become composite mortar; thereby be implemented in direct sintering in the air, do not need nitrogen protection atmosphere, save nitrogen gas generating device and accessory facility investment.
The present invention realizes by following technical scheme.
Conduction with the technical process of compound copper powder and compound copper conductor pulp preparation is: preparation superfine cupper powder → copper powder surface modification → preparation conductor paste → sintering slurry → manufacture a finished product.
One, preparation superfine cupper powder: adopt Cu-CATH-1 as anode, with copper coin or stainless steel plate as negative electrode, under the effect of the pulse power, on negative electrode, separate out copper powder,, isolate and to enter next step surface modification operation by 500 purpose superfine cupper powders through washing, dry, screening.
The prescription and the processing condition of preparation superfine cupper powder are: copper sulfate: 10～40g/L; Sulfuric acid: 100～200g/L; Additive A: 5～10g/L, current density: 5～9A/dm
2Temperature: 25～30 ℃.
Two, copper powder surface modification: satisfactory superfine cupper powder is placed container, add the surface modification solution for preparing, fully stir, can obtain compound copper powder.The prescription and the processing condition of surface modification solution are: Silver Nitrate 10～60g/L; Reductive agent B 50～100g/L; Addition of C 10～20g/L; Temperature normal temperature; Time 10～30min.
Three, preparation conductor paste: at first that compound copper powder and various medium is composite by following mass percent; Compound copper powder 45～60%; Glass powder 5～20%; Reductive agent D5～10%, organic adhesive 10～45%, stirring promptly obtains conductor paste.
Four, sintering slurry: adopt the method for silk screen printing to be coated to workpiece surface in slurry, carry out sintering circuit.Sintering process is carried out in the air calcination stove of self design, and sintering temperature is controlled at 700～800 ℃, is incubated 10～30 minutes.
Five, manufacture a finished product: the workpiece behind the sintering can be processed as finished product according to the specific requirement of producer.
Additive A in compound copper powder and the complex copper slurry preparation method is one or more the mixture in polyoxyethylene glycol, polyvinyl alcohol, sodium polydithio-dipropyl sulfonate, sodium lauryl sulphate, thiocarbamide, the hydrochloric acid; Reductive agent B is one or more the mixture in formaldehyde, hydrazine hydrate, inferior sodium phosphate, glucose, the Seignette salt; Addition of C is one or more the mixture in polyvinylpyrrolidone, polyvinyl alcohol, the polyoxyethylene glycol; Reductive agent D is one or more the mixture in bismuth meal, zinc powder, aluminium powder, silica flour, the magnesium powder.
The sintering of complex copper slurry is to carry out under the condition that is incubated 10～30 minutes in 700～800 ℃ temperature range.
Fig. 1 is preparation technology's schema of the present invention.
The present invention compared with prior art has following advantage or good effect:
1, compound copper conductor slurry of the present invention is compared with traditional silver paste, and electric conductivity is suitable, and direct sintering problem of oxidation can not take place in air, burnt in a heap can bonding die, and small investment, instant effect, method is simple, can large-scale production:
2, omitted in the sintering process of compound copper conductor slurry of the present invention nitrogen protection operation that known technology generally adopts and Its equipment can carry out in the general sintering furnace that adopts, and has significantly reduced production cost.
Embodiment
Embodiment 1:
Adopt the inventive method to prepare superfine cupper powder.
Adopt stainless steel plate as negative electrode, as anode, under the effect of the pulse power, prepare superfine cupper powder,, isolate by 500 purpose superfine cupper powders through washing, dry, screening with copper coin.The adjusting process parameter can obtain the copper powder of different-grain diameter.For example: copper sulfate 40g/L, sulfuric acid 200g/L, the mixture 5g/L of polyoxyethylene glycol and hydrochloric acid, current density 9A/dm
2, 30 ℃ of temperature.The particle diameter that obtains copper powder is 10～20 μ m, after cleaning, drying, screening, promptly can be used as finished product.
Embodiment 2:
Adopt the inventive method to prepare compound copper powder.
Adopt stainless steel as negative electrode, as anode, under the effect of the pulse power, prepare superfine cupper powder,, isolate by 500 purpose superfine cupper powders and enter next step surface modification through washing, dry, screening with copper coin.The prescription and the processing condition of preparation copper powder are: copper sulfate 20g/L, sulfuric acid: 100g/L, the mixture 5g/L of thiocarbamide and polyoxyethylene glycol, current density 5A/dm
2, 30 ℃ of temperature.
Satisfactory superfine cupper powder is inserted in the container, add the surface modification solution for preparing, fully stir, can obtain compound copper powder.Prescription and processing condition are: Silver Nitrate 50g/L, glucose 50g/L, the mixture 10g/L of polyoxyethylene glycol and polyvinyl alcohol, temperature normal temperature, time 20min.
The compound copper powder that obtains, promptly can be used as conductive powder and uses after the screening through super-dry.For example, be applied in rubber and prepare in the industry, add in the rubber as conductive powder, rolling with three-high mill, uniform mixing gets final product.
Embodiment 3:
Utilize the foregoing description 1 method to obtain superfine cupper powder, join Silver Nitrate 20g/L, inferior sodium phosphate 50g/L in the surface modification solution of the mixture 10g/L of polyvinylpyrrolidone and polyoxyethylene glycol, fully stirs 10min at normal temperatures, promptly obtains compound copper powder.
Compound copper powder after the modification and medium is composite by following mass percent; Composite powder 45%, glass powder 20%, zinc powder 10%, organic adhesive 25%, and stir and obtain conductor paste.
Sintering slurry: adopt the method for silk screen printing to be coated to workpiece surface in slurry, carry out sintering circuit.Sintering process is carried out in tube type resistance furnace, and sintering temperature is 700 ℃, is incubated 20 minutes.
Slurry behind the sintering promptly can be used as the inspection after construction warehouse-in, and the film performance index that obtains is: side's resistance 5m Ω/, sticking power is greater than 10N/mm
2
Embodiment 4:
Utilize the foregoing description 1 method to obtain superfine cupper powder, join Silver Nitrate 10g/L, hydrazine hydrate 50ml/L in the mixture 10g/L solution of polyvinylpyrrolidone and polyvinyl alcohol, stirs 20min at normal temperatures, can obtain composite powder.
Composite powder and medium are prepared slurry by following mass percent: composite powder 50%, glass powder 15%, the mixture 10% of aluminium powder and silica flour, organic binder bond 25%.The finished product of printing is sent into sintering in the tube furnace (750 ℃ of top temperatures, insulation 15min), and prepared thick film rete resistance is 7m Ω/, and sticking power is greater than 15N/mm
2
Embodiment 5:
Obtain the copper composite conductive powder by the foregoing description 2 methods, prepare slurry with medium according to following mass percent: composite powder 60%, glass powder 10%, the mixture 5% of zinc powder and magnesium powder, silica flour, organic binder bond 25%.The finished product of printing is sent into sintering in the tube furnace (800 ℃ of top temperatures, insulation 10min), and prepared thick film rete resistance is 7m Ω/, and sticking power is greater than 10N/mm
2
By above embodiment as seen, adopt the ultra-fine compound copper powder of the inventive method preparation, granularity and electroconductibility are all better.Electric slurry of the present invention, every performance index have reached the level of silver paste, and equipment can adopt the agglomerating plant of original silver slurry simultaneously.
Claims (9)
1, a kind of conduction is with the preparation method of compound copper powder and compound copper conductor slurry, and preparation technology's flow process is gone on foot by preparation superfine cupper powder → copper powder surface modification → preparation conductor paste → sintering slurry → manufacture a finished product five to be formed.
2, preparation method according to claim 1 is characterized in that: adopt electrolytic method, prepare copper powder under the effect of the pulse power, through washing, dry, screening, isolate and can enter next step surface modification operation by 500 purpose copper powders.The prescription and the processing condition of preparation superfine cupper powder are: copper sulfate: 10～40g/l; Sulfuric acid: 100～200g/l; Additive A: 5～10g/l, current density: 5～9A/dm
2Temperature: 25～30 ℃, anode adopts the fine copper plate, and negative electrode can adopt copper coin or stainless steel plate.
3, preparation method according to claim 1 is characterized in that: superfine cupper powder must pass through surface modification, and copper powder is placed container, adds surface modification solution, fully stirs, and promptly obtains compound copper powder.Surface modification solution prescription and processing condition are: Silver Nitrate: 10～60g/l; Reductive agent B:50～100g/l; Addition of C: 10～20g/l; Temperature is a normal temperature; Time: 10～30min.
4, preparation method according to claim 1 is characterized in that: earlier with compound copper powder and medium by the composite composite powder that obtains of following mass percent, compound copper powder 45～60%; Glass powder 5～20%; Reductive agent D5～10%, organic adhesive 10～45% obtains conductor paste after fully stirring.
5, preparation method according to claim 1 and 2, it is characterized in that: additive A is one or more the mixture in polyoxyethylene glycol, polyvinyl alcohol, sodium polydithio-dipropyl sulfonate, sodium lauryl sulphate, thiocarbamide, the hydrochloric acid, and consumption is 5～10g/l.
6, according to claim 1 or 3 described preparation methods, it is characterized in that: reductive agent B is one or more the mixture in formaldehyde, hydrazine hydrate, inferior sodium phosphate, glucose, the Seignette salt, and its consumption is 50～100g/l.
7, according to claim 1 or 3 described preparation methods, it is characterized in that: addition of C is one or more the mixture in polyvinylpyrrolidone, polyvinyl alcohol, the polyoxyethylene glycol, and its consumption is 10-20g/l.
8, according to claim 1 or 4 described preparation methods, it is characterized in that: reductive agent D is one or more the mixture in bismuth meal, zinc powder, aluminium powder, silica flour, the magnesium powder, and its consumption is 5-10% (mass percent).
9, preparation method according to claim 1 is incubated 10～30 minutes when it is characterized in that the sintering slurry in 700～800 ℃ of temperature ranges.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031352464A CN1300381C (en) | 2003-06-16 | 2003-06-16 | Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031352464A CN1300381C (en) | 2003-06-16 | 2003-06-16 | Preparing method for conductive composite bronze powder and composite bronze conductive sizing agent |
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| CN1472367A true CN1472367A (en) | 2004-02-04 |
| CN1300381C CN1300381C (en) | 2007-02-14 |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100429727C (en) * | 2005-06-16 | 2008-10-29 | 沈阳工业大学 | Copper-silver alloy conductor size and its preparing method |
| CN100493781C (en) * | 2007-04-06 | 2009-06-03 | 深圳市危险废物处理站 | Method of producing sheet shaped silver-plated copper powder |
| CN101339821B (en) * | 2008-08-15 | 2010-09-01 | 深圳市圣龙特电子有限公司 | Copper paste without lead and cadmium and manufacturing method therefor |
| CN102133636A (en) * | 2011-03-10 | 2011-07-27 | 昆明理工大学 | Method for preparing anti-migration flaky silver coated copper powder |
| CN101818365B (en) * | 2009-09-23 | 2012-04-04 | 兰州理工大学 | Method for preparing nano stibium powder |
| CN102601355A (en) * | 2012-03-20 | 2012-07-25 | 昆明理工大学 | Surface modification method for improving corrosion resistance of bronze powder |
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| US4122232A (en) * | 1975-04-21 | 1978-10-24 | Engelhard Minerals & Chemicals Corporation | Air firable base metal conductors |
| JPH07107168B2 (en) * | 1987-01-27 | 1995-11-15 | 田中貴金属工業株式会社 | Method for producing fine copper particles |
| CN1022468C (en) * | 1992-02-19 | 1993-10-20 | 北京市印刷技术研究所 | Surface treating method for electric conducting copper powder |
| US5820653A (en) * | 1993-04-19 | 1998-10-13 | Electrocopper Products Limited | Process for making shaped copper articles |
| JP3002379B2 (en) * | 1994-04-08 | 2000-01-24 | 新日本製鐵株式会社 | Manufacturing method of high-strength cold-rolled galvannealed steel sheets for automobiles with excellent formability, paint bake hardenability and little change in paint bake hardenability |
| CN1060982C (en) * | 1997-11-17 | 2001-01-24 | 北京有色金属研究总院 | Preparation of ultrafine metal powders |
| CN1074331C (en) * | 1998-03-03 | 2001-11-07 | 浙江大学 | Preparation of nanometer silver-copper alloy powder |
| CN1401819A (en) * | 2002-09-23 | 2003-03-12 | 北京工业大学 | Inorganic powder surface metallizing method |
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