CN101270489B - Method for quick electrodeposition of foam iron with low energy consumption - Google Patents
Method for quick electrodeposition of foam iron with low energy consumption Download PDFInfo
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- CN101270489B CN101270489B CN2008100645487A CN200810064548A CN101270489B CN 101270489 B CN101270489 B CN 101270489B CN 2008100645487 A CN2008100645487 A CN 2008100645487A CN 200810064548 A CN200810064548 A CN 200810064548A CN 101270489 B CN101270489 B CN 101270489B
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Abstract
A method for fast and electrically depositing foamed irons with low-energy consumption relates to a preparation method for the foamed irons. The invention solves the problem of high power consumptionin the current foamed iron preparing technology and that problems that the foamed irons manufactured by the existing foamed iron liquid have burrs, are rough, loosen, have remarkably increased brittleness and are not beneficial to wind. The preparation method of the invention include: 1, obtaining a conductive sponge after carrying out physical vapour deposition on metals on the surface of a sponge skeleton, then coating black lead conductive glue on the surface of the conductive sponge; 2, putting the conductive sponge into plating liquid for electric deposition, rinsing and dipping into sodium carbonate liquid, rinsing and then drying; 3, sintering; 4, carrying out reductive heat treatment to obtain the foamed iron. The method of the invention has the advantages of low energy consumption, environment protection, high manufacture efficiency, low cost, dense plating layer, good flexibility and easy winding. The iron content of the foamed iron prepared by the invention is over 99 percent; the surface density is 300 to 1500g/m<2>, the aperture is 30 to 110 PPI, the hole rate is more than or equal to 90 percent, the thickness is 1 to 10mm, the longitudinal tensile strength is more than or equal to 1.0N/mm<2>, the transverse tensile strength is 1.0N/mm<2> and the winding property is more than or equal to Phi 30mm.
Description
Technical field
The present invention relates to a kind of preparation method of foam iron.
Background technology
Therefore characteristics such as foam iron has low price, specific surface area is big, ultimate compression strength is high, thermal expansivity is low, Heat stability is good become the focus of research.At present, adopt the sulfate type iron plating liquid to electroplate preparation foam iron mostly, but the power consumption height that this method consumes.Though chloride type plating bath good conductivity, specific conductivity are 2.5 times of the sulfate type plating bath, existing chloride type iron plating liquid resistance of oxidation is relatively poor, when plating bath contacts with air, and ferrous iron (Fe
2+) easily oxidation become ferric iron (Fe
3+), ferric iron forms ironic hydroxide at coating surface easily and is entrained in the coating, makes foam iron produce burr, becomes coarse, loose, and fragility obviously increases and is unfavorable for reeling; So also few people are used for actual production with the chloride type iron plating liquid.
Summary of the invention
The objective of the invention is to have the power consumption height in order to solve present preparation foam iron, and the foam iron that existing iron plating liquid is produced is jagged, and become coarse, loose, the problem that fragility obviously increases and is unfavorable for reeling, and a kind of method of quick electrodeposition of foam iron with low energy consumption is provided.
The method of less energy-consumption quick electrodeposition realizes by following step among the present invention: one, the composite conducting processing of sponge: be to obtain conductive sponge behind the sponge skeleton surface gas phase physical deposition metal of 30～110PPI in the aperture, wherein metal is nickel, copper or titanium, then at conductive sponge surface-coated graphite conductive adhesive; Two, galvanic deposit: will the sponge after step 1 is handled put into behind the acid chloride plating bath galvanic deposit 3～10 minutes, keep pH value=1.0～1.5 in the electrodeposition process, wash then three to five times, again with pH=7～8 (preventing that foam iron from getting rusty) that are dipped in sodium carbonate solution or the sodium hydroxide solution through the sponge of electrodeposition process, wash again three to five times, then under 100～120 ℃ of conditions, dry; Three, sintering: the conductive sponge after step 2 is handled is put into the sintering oven that blasts air, and the temperature in the sintering oven is heated to 750 ℃ continuously by room temperature, continuously 3～5 minutes heating-up times, is cooled to 200 ℃ more continuously, and temperature fall time is 3～5 minutes continuously; Four, reduction heat is handled: in the continuous tunnel furnace that feeds decomposed ammonia, the product behind the sintering is carried out reduction heat handle; Make foam iron; Every square metre of sponge skeleton surface deposition metal 5～10g in the step 1 wherein, the consumption of graphite conductive adhesive is 30～60g/m
2Every liter of acid chloride plating bath is by 400～500gFeCl in the step 2
24H
2The muriate of O, 0.5～5g Succinic Acid, 0.1～1g vanadium and the water of surplus are made; The processing parameter of galvanic deposit in the step 2: the temperature of galvanic deposit is 40～70 ℃, and conductive sponge is made negative electrode, and the negative electrode apparent current density is 3 * 10
3～3 * 10
4A/m
2Anode material is soft steel or technically pure iron below No. 20, and anode and negative electrode apparent area are 1～2: 1; Reduction heat treated temperature continuous change procedure in the step 4 continuous tunnel furnace: be warming up to 1150 ℃ continuously from about 200 ℃, the heating-up time is 3～5 minutes continuously, keeps 1150 ℃ 3～5 minutes, be cooled to 100 ℃ more continuously, be 15～20 minutes continuous cooling time.
Sponge is the open-cell polyurethane sponge in the step 1, also can adopt cloth or fibrefelt to substitute sponge and prepare foam iron.The muriate of the vanadium described in the acid chloride plating bath of step 2 is vanadium trichloride and/or vanadium tetrachloride.The concentration of sodium carbonate solution or sodium hydroxide solution is 50～100g/L in the step 2.
Compared with prior art, the present invention has the following advantages.
1, the present invention's iron level of making foam iron surpasses 99%, and area density is 300～1500g/m
2, the aperture is 30～110PPI, porosity 〉=90%, thickness are 1～10mm, endwise tensile strength 〉=1.0N/mm
2Transverse tensile strength 1.0N/mm
2, coiling performance 〉=Ф 30mm.
2, the good conductivity of chloride plate liquid of the present invention, its specific conductivity are 2.5 times of sulfate type plating bath, and allow the high current density galvanic deposit.Therefore, adopt chloride type plating bath electrodeposition of foam iron at normal temperatures, to voltage of supply require low, voltage has only 1/2 of sulfate type plating bath, has the saving electric energy, the characteristics that sedimentation velocity is fast, and iron ion and chlorion are all free from environmental pollution, meet the overall policy of China's energy-saving and emission-reduction and Sustainable development.
3, the resistance of oxidation of existing muriate iron plating liquid is relatively poor, when plating bath contacts with air, and ferrous ion (Fe
2+) easily oxidation become ferric ion (Fe
3+), ferric ion forms ironic hydroxide at coating surface easily and is entrained in the coating, makes foam iron produce burr, becomes coarse, loose, and fragility obviously increases.Therefore, the ferric ion content that suppresses in the muriate iron plating liquid is crucial, and the present invention increases with the ferric ion content in the muriate inhibition iron plating liquid of vanadium.Because the muriate of vanadium generates V in cathodic reduction
2+, V
2+Fe in the reducible solution
3+Be Fe
2+, self be oxidized to high price V
3+Ion, the V of generation
3+Compare Fe
3+Arrive easily and be reduced to V on the surface of foam iron cathode
2+, so move in circles, suppress the Fe in the plating bath
3+Accumulation.Its reaction is:
V
2+-e
-→ V
3+(in the solution)
Fe
3++ e
-→ Fe
2+(in the solution)
V
3++ e
-→ V
2+(cathode surface)
Fe
3+Self being difficult to arrive foam iron cathode surface reduction is Fe
2+, be because Fe
3+Do not wait the arrival cathode surface just to form oxyhydroxide, and Fe
3+Oxyhydroxide form colloid easily, be not easy to arrive cathode surface.
4, the internal stress of existing muriate iron plating liquid causes the foam iron snappiness of galvanic deposit poor greatly, cause brittle rupture easily, can not satisfy the galvanized rolling demand of serialization, the present invention's stress relieving agent of binary organic acid as foam iron, make the foam iron of galvanic deposit before thermal treatment, can be wound into web-like, thereby solved plating foam iron speed and the unmatched problem of foam iron thermal treatment rate, realized plating foam iron, foam iron thermal treatment independently serialization production mutually.
5, the concentration height of the main salt of chloride plate liquid of the present invention, and be acid, guarantee that plating bath has best electroconductibility, reduces the power consumption of electrodeposition of foam iron; And the current density of this plating bath permission electrodeposition of foam iron is big, the production efficiency height; And coating hardness is low, the good toughness of foam iron.
6, the present invention adopts soft steel to do soluble anode, and material cost is low.
Description of drawings
Fig. 1 is 40 times of enlarged views of foam iron microscopic appearance that embodiment 11 makes, and Fig. 2 is 200 times of enlarged views of foam iron microscopic appearance that embodiment 13 makes.
Embodiment
Embodiment one: the method for less energy-consumption quick electrodeposition realizes by following step in the present embodiment: one, the composite conducting processing of sponge: in the aperture is that (PPI is a sponge aperture unit to 30～110PPI, the number in sponge hole in referring to one inch) obtains conductive sponge behind the sponge skeleton surface gas phase physical deposition metal, wherein metal is nickel, copper or titanium, then at conductive sponge surface-coated graphite conductive adhesive; Two, galvanic deposit: will the sponge after step 1 is handled put into behind the acid chloride plating bath galvanic deposit 3～10 minutes, keep pH value=1.0～1.5 in the electrodeposition process, wash then three to five times, be dipped to pH=7～8 (preventing that foam iron from getting rusty) again in the solution with yellow soda ash or sodium hydroxide through the sponge of electrodeposition process, wash again three to five times, then under 100～120 ℃ of conditions, dry; Three, sintering: the conductive sponge after step 2 is handled is put into the sintering oven that blasts air, and the temperature in the sintering oven is heated to 750 ℃ continuously by room temperature, continuously 3～5 minutes heating-up times, is cooled to 200 ℃ more continuously, and temperature fall time is 3～5 minutes continuously; Four, reduction heat is handled: feeding decomposed ammonia (H
2: N
2Mol ratio be 3: 1 mixed gas) continuous tunnel furnace in, the product behind the sintering is carried out reduction heat handles; Make foam iron; Every square metre of sponge skeleton surface deposition metal 5～10g in the step 1 wherein, the consumption of graphite conductive adhesive is 30～60g/m
2Every liter of acid chloride plating bath is by 400～500g FeCl in the step 2
24H
2O, 0.5～5g Succinic Acid (doing the stress relieving agent), the muriate (making antioxidant) of 0.1～1g vanadium and the water of surplus are made; The processing parameter of galvanic deposit in the step 2: the temperature of galvanic deposit is 40～70 ℃, and conductive sponge is made negative electrode, and the negative electrode apparent current density is 3 * 10
3～3 * 10
4A/m
2Anode material is soft steel or technically pure iron below No. 20, and anode and negative electrode apparent area are 1～2: 1; Reduction heat treated temperature continuous change procedure in the step 4 continuous tunnel furnace: be warming up to 1150 ℃ continuously from about 200 ℃, the heating-up time is 3～5 minutes continuously, keeps 1150 ℃ 3～5 minutes, be cooled to 100 ℃ more continuously, be 15～20 minutes continuous cooling time.
Graphite conductive adhesive is the graphite conductive adhesive TL-10 that Shenyang Tian Run chemical industry company limited produces in the step 1, and described graphite conductive adhesive has acid resistance.Yellow soda ash or concentration sodium hydroxide are 50～100g/L in the step 2.
Present embodiment makes in the foam iron iron level, and to surpass 99% area density be 300～1500g/m
2, the aperture is 30～110PPI, porosity 〉=90%, thickness are 1～10mm, endwise tensile strength 〉=1.0N/mm
2Transverse tensile strength 1.0N/mm
2, coiling performance 〉=Ф 30mm.The reaction process of present embodiment can be the operation of continous way, also can be the operation of discontinuous.Applying graphite conductive adhesive in the step 1, is that nickel or copper dissolve in acidic bath and under the effect of dissolved oxygen and reduces the electroconductibility of sponge and pollute plating bath for before preventing that conductive sponge from entering negative electrode plating district.Temperature rising automatically in the galvanic deposit iron process in the step 2; The specific conductivity height of the plating bath that present embodiment is used, the electric energy of reaction consumes is low, thereby has improved production efficiency; Soft steel is done soluble anode, and material cost is low.The method that step 3 heats up and lowers the temperature has continuously solved the cracking problem in foam iron sintering, the reduction process.Add the antioxidant of plating bath and the stress relieving agent of foam iron in the iron plating liquid, make the snappiness of electrodeposition of foam iron good, before thermal treatment, web-like be can be wound into, foam iron speed and the unmatched separate serialization production of foam iron thermal treatment rate realized electroplating.Neutralizing treatment has been avoided the corrosion problem of foam iron.The sintering of foam iron, reduction process adopt the method that heats up and lower the temperature continuously, can prevent that foam iron from ftractureing because of unexpected temperature variation.
Embodiment two: what present embodiment and embodiment one were different is: the pH value of acid chloride plating bath is regulated with 1: 1 hydrochloric acid in the step 1.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: sponge open-cell polyurethane sponge, cloth or fibrefelt in the step 1.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: the aperture of sponge is 40～80PPI.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is: the aperture of sponge is 60PPI.Other is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is: the consumption of graphite conductive adhesive is 40～50g/m in the step 1
2Other is identical with embodiment one.
Embodiment seven: what present embodiment and embodiment one were different is: the consumption of graphite conductive adhesive is 45g/m in the step 1
2Other is identical with embodiment one.
Embodiment eight: what present embodiment and embodiment one were different is: every liter of acid chloride plating bath is by 420～480gFeCl in the step 2
24H
2The muriate of O, 1～4g Succinic Acid, 0.2～0.8g vanadium and the water of surplus are made.
Embodiment nine: what present embodiment and embodiment one were different is: every liter of acid chloride plating bath is by 450gFeCl in the step 2
24H
2The muriate of O, 3g Succinic Acid, 0.5g vanadium and the water of surplus are made.
Embodiment ten: what present embodiment and embodiment one were different is: the muriate of the vanadium described in the acid chloride plating bath of step 2 is vanadium trichloride and/or vanadium tetrachloride.
When the muriate of present embodiment vanadium was composition, vanadium trichloride can be by any than mixing with vanadium tetrachloride.
Embodiment 11: the method for quick electrodeposition of foam iron with low energy consumption realizes by following step in the present embodiment: one, the composite conducting processing of sponge: obtain conductive sponge behind the gas phase physical deposition nickel of open-cell polyurethane sponge skeleton surface, wherein the aperture of sponge is 110PPI, every square metre of sponge skeleton surface deposition nickel 5g; Then at conductive sponge surface-coated graphite conductive adhesive 50g/m
2Two, galvanic deposit: will the sponge after step 1 is handled put into behind the acid chloride plating bath galvanic deposit 3 minutes, keep pH value=1.0～1.5 in the electrodeposition process, wash then three to five times, in solution, be dipped to pH=7～8 through the sponge of electrodeposition process with concentration 50g/L yellow soda ash, wash again three to five times, then under 120 ℃ of conditions, dried by the fire 5 minutes; Three, sintering: the foam iron that contains conductive sponge after step 2 is handled is put into the sintering oven that blasts air, foam iron is heated to 750 ℃ continuously by room temperature in stove, the continuous heating-up time 3-5 of foam iron minute, be cooled to 200 ℃ more continuously, temperature fall time is 3～5 minutes continuously; Four, reduction heat is handled: in the continuous tunnel furnace that feeds decomposed ammonia, sponge behind the sintering is carried out reduction heat handles, reduce the continuous change procedure of heat treated temperature: be warming up to 1150 ℃ continuously from about 200 ℃, heating-up time is 3～5 minutes continuously, keep 1150 ℃ 3～5 minutes, be cooled to 100 ℃ more continuously, be 15～20 minutes cooling time continuously; Make foam iron; Wherein every liter of acid chloride plating bath is by 400g FeCl in the step 2
24H
2The water of O, 0.5g Succinic Acid, 0.1g vanadium trichloride and surplus is made; The processing parameter of galvanic deposit in the step 2: the temperature of galvanic deposit is 50 ℃, and sponge makes negative electrode, and the apparent current density of sponge is 1 * 10
4A/m
2Anode material is No. 10 soft steel, and anode and negative electrode apparent area are 2: 1.
The about 500g/m of area density of the foam iron that present embodiment obtains
2, and do not have cracking phenomena (as shown in Figure 1).
Embodiment 12: what present embodiment and embodiment 11 were different is: the metal of gas phase physical deposition is a copper in step 1, every square metre of sponge skeleton copper-depositing on surface 5g.Other is identical with embodiment 11.
Embodiment 13: what present embodiment and embodiment 11 were different is: the thickness of sponge is 10mm in the step 1, and the aperture of sponge is 30PPI; Every liter of acid chloride plating bath is by 500g FeCl in the step 2
24H
2The water of O, 5.0g Succinic Acid, 1.0g vanadium tetrachloride and surplus is made; The temperature of galvanic deposit is 63 ℃, and the apparent current density of sponge is 3 * 10
4A/m
2, galvanic deposit 3 minutes.Other is identical with embodiment 11.
The about 1500g/m of the untouchable density of the foam that present embodiment obtains
2, and do not have cracking phenomena (as shown in Figure 2).
Embodiment 14: what present embodiment and embodiment 11 were different is: the thickness of sponge is 5mm in the step 1, and the aperture of sponge is 60PPI; Every liter of acid chloride plating bath is by 450g FeCl in the step 2
24H
2The water of O, 2.5g Succinic Acid, 0.2g vanadium trichloride and surplus is made; The temperature of galvanic deposit is 55 ℃, and the apparent current density of sponge is 2 * 10
4A/m
2Anode material is No. 20 soft steel.Other is identical with embodiment 11.
Embodiment 15: what present embodiment and embodiment 11 were different is: step 4 is reduced the continuous change procedure of heat treated temperature: be warming up to 1150 ℃ continuously from about 200 ℃, heating-up time is 3 minutes continuously, keep 1150 ℃ 3 minutes, be cooled to 100 ℃ more continuously, be 20 minutes cooling time continuously.Other is identical with embodiment 11.
The foam iron of present embodiment preparation does not have cracking phenomena.
Embodiment 16: what present embodiment and embodiment 11 were different is: step 4 is reduced the continuous change procedure of heat treated temperature: be warming up to 1150 ℃ continuously from about 200 ℃, heating-up time is 5 minutes continuously, keep 1150 ℃ 5 minutes, be cooled to 100 ℃ more continuously, be 15 minutes cooling time continuously.Other is identical with embodiment 11.
The foam iron of present embodiment preparation does not have cracking phenomena.
Claims (9)
1. the method for a quick electrodeposition of foam iron with low energy consumption, the method that it is characterized in that the less energy-consumption quick electrodeposition realizes by following step: one, the composite conducting processing of sponge: be to obtain conductive sponge behind the sponge skeleton surface gas phase physical deposition metal of 30～110PPI in the aperture, wherein metal is nickel, copper or titanium, then at conductive sponge surface-coated graphite conductive adhesive; Two, galvanic deposit: will the sponge after step 1 is handled put into behind the acid chloride plating bath galvanic deposit 3～10 minutes, keep pH value=1.0～1.5 in the electrodeposition process, wash then three to five times, be dipped to pH=7～8 with sodium carbonate solution or sodium hydroxide solution again through the sponge of electrodeposition process, wash again three to five times, then under 100～120 ℃ of conditions, dry; Three, sintering: the conductive sponge after step 2 is handled is put into the sintering oven that blasts air, and the temperature in the sintering oven is heated to 750 ℃ continuously by room temperature, continuously 3～5 minutes heating-up times, is cooled to 200 ℃ more continuously, and temperature fall time is 3～5 minutes continuously; Four, reduction heat is handled: in the continuous tunnel furnace that feeds decomposed ammonia the product behind the sintering is carried out reduction heat and handle; Make foam iron; Every square metre of sponge skeleton surface deposition metal 5～10g in the step 1 wherein, the consumption of graphite conductive adhesive is 30～60g/m
2Every liter of acid chloride plating bath is by 400～500g FeCl in the step 2
24H
2The muriate of O, 0.5～5g Succinic Acid, 0.1～1g vanadium and the water of surplus are made; The processing parameter of galvanic deposit in the step 2: the temperature of galvanic deposit is 40～70 ℃, and conductive sponge is made negative electrode, and the negative electrode apparent current density is 3 * 10
3～3 * 10
4A/m
2, the galvanic deposit anode material is soft steel or technically pure iron below No. 20, anode and negative electrode apparent area are 1～2: 1; Reduction heat treated temperature continuous change procedure in the step 4 continuous tunnel furnace: be warming up to 1150 ℃ continuously from about 200 ℃, the heating-up time is 3～5 minutes continuously, keeps 1150 ℃ 3～5 minutes, be cooled to 100 ℃ more continuously, be 15～20 minutes continuous cooling time.
2. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1 is characterized in that sponge is the open-cell polyurethane sponge in the step 1.
3. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1, the aperture that it is characterized in that sponge in the step 1 is 40～80PPI.
4. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1, the aperture that it is characterized in that sponge in the step 1 is 60PPI.
5. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1 is characterized in that the concentration of sodium carbonate solution in the step 2 or sodium hydroxide solution is 50～100g/L.
6. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1 is characterized in that every liter of acid chloride plating bath is by 420～480g FeCl in the step 2
24H
2The muriate of O, 1～4g Succinic Acid, 0.2～0.8g vanadium and the water of surplus are made.
7. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1 is characterized in that every liter of acid chloride plating bath is by 450g FeCl in the step 2
24H
2The muriate of O, 3g Succinic Acid, 0.5g vanadium and the water of surplus are made.
8. according to the method for claim 1 or 6 described a kind of quick electrodeposition of foam iron with low energy consumption, it is characterized in that the muriate of the vanadium described in the acid chloride plating bath of step 2 is vanadium trichloride and/or vanadium tetrachloride.
9. the method for a kind of quick electrodeposition of foam iron with low energy consumption according to claim 1 is characterized in that the negative electrode apparent current density in the step 2 is 2 * 10
4A/m
2
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| CN104593844A (en) * | 2013-10-31 | 2015-05-06 | 上海众汇泡沫铝材有限公司 | Preparation method of cathode shield for super-thick open-cell foam iron nickel filter material |
| CN106797164B (en) * | 2014-09-03 | 2019-07-23 | 广东肇庆爱龙威机电有限公司 | The method for reducing EMI of motor based on ring varistor |
| CN107419243B (en) * | 2017-07-03 | 2020-03-20 | 西北工业大学 | Preparation method of open-cell foam copper-nickel composite material |
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