CN103556184A - Preparation method of all-wet nano NiFe2O4-NiO-Cu-Ni metal ceramic inert anode - Google Patents
Preparation method of all-wet nano NiFe2O4-NiO-Cu-Ni metal ceramic inert anode Download PDFInfo
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- CN103556184A CN103556184A CN201310561493.1A CN201310561493A CN103556184A CN 103556184 A CN103556184 A CN 103556184A CN 201310561493 A CN201310561493 A CN 201310561493A CN 103556184 A CN103556184 A CN 103556184A
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Abstract
The invention discloses a preparation method of an all-wet nano NiFe2O4-NiO-Cu-Ni metal ceramic inert anode. The method comprises the following steps: by taking ferric oxide, nickel protoxide or nickel oxide, copper powder, nickel powder and the like as main raw materials, one or mixture of more of titanium powder, manganese dioxide, vanadium pentoxide, magnesium oxide and calcium oxide as a dopant, and one or mixture of more of water, absolute ethyl alcohol and polyvinylpyrrolidone (PVP) as a surfactant, preparing the NiFe2O4-NiO-Cu-Ni metal ceramic inert anode of which the grain size is 53nm and the compactness is greater than 99% by adopting a planet-type ball milling technology, a cold isostatic pressing (CIP) technology and an atmosphere sintering technology. The metal ceramic inert anode can replace the traditional carbon anode at present to be applied to an aluminium cell. The inert anode produced by the preparation method disclosed by the invention does not generate a toxic and harmful gas, and is friendly to environment and low in production cost.
Description
Technical field
The invention belongs to powder metallurgy and molten-salt electrolytic aluminum anode material technical field,, be specifically related to a kind of full moist type nano-Ni/Fe
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode.
Background technology
Aluminum current electrolytic industry adopts fused salt electrolysis process, and the anode using is carbon anode, the carbon material that production process consumption is a large amount of and the energy, and electrolytic process produces a large amount of greenhouse gases CO
2, CF
4, C
2f
6, the material serious environment pollution such as bitumen flue gas and carbonyl sulfide (COS).Meanwhile, in electrolysis production process, because anode constantly consumes, need continuous antianode to adjust and change, increased workman's labour intensity, even cause producing being difficult to stablize and carry out, and then cause the phenomenons such as electrolysis of aluminum energy consumption is high, and current efficiency is low.Owing to there being above problem, by inert anode material, for aluminum electrolysis process, be current research heat subject, the important development direction that aluminium manufacture realizes energy-conserving and environment-protective, reduces discharging and raises the efficiency especially.At present both at home and abroad relevant fused salt electrolysis is reported often with inert anode patent and research, but still cannot reach the performances such as the high conductivity of existing aluminium electrolytic industry requirement, corrosion-resistant, high mechanical strength.At present relevant with the preparation of inert anode nano material main patent is the last NiFe that directly prepares Nano grade all
2o
4-NiO-Cu-Ni cermet inert anode, but by first preparing nano level NiFe
2o
4or NiO ceramics powder, then in inert anode, add a certain amount of nano-Ni/Fe
2o
4or the method for NiO ceramics powder prepares electroconductibility, erosion resistance and toughness etc. that inert anode improves anode material, but these methods fail to solve NiFe all the time
2o
4the wetting ceramic problem of metallographic phase in-NiO-Cu-Ni cermet inert anode.NiFe
2o
4in-NiO-Cu-Ni cermet inert anode, the wetting pottery of metallographic phase is to improve anode material electroconductibility, erosion resistance, the key of the performances such as heat-shock resistance and mechanical connection.For this reason, develop a kind of simple easy handling, energy-conserving and environment-protective, with low cost good dispersity, the NiFe that granularity is thinner of directly preparing
2o
4the method of-NiO-Cu-Ni nano-powder, tool is of great significance.
Summary of the invention
The object of the present invention is to provide preparation method and the technique of full moist type nanometer metal ceramic inert anode for a kind of molten-salt electrolytic aluminum, to solve problem nonwetting between metal and pottery or that wettability is poor, and overcome the poorly conductive that existing cermet inert anode exists, metal is isolated distribution and skewness in ceramic matrix, erosion resistance is poor, heat-shock resistance is poor, is difficult to the problem of processing and maximizing.
Another object of the present invention is to provide a kind of simple easy handling, energy-conserving and environment-protective, with low cost good dispersity, the NiFe that granularity is thinner of directly preparing
2o
4the method of-NiO-Cu-Ni nano-powder, makes it to be easy to realize suitability for industrialized production.
The object of the present invention is achieved like this, full moist type nano-Ni/Fe
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, is characterized in that comprising the steps:
A, the preparation of precursor ceramic powder: by Fe
2o
3with NiO or Ni
2o
3mixture, add water through wet ball grinding, dry after, be placed in sintering oven and calcine, control calcining temperature, be prepared into NiFe
2o
4-NiO precursor ceramic powder;
B, mix nano-powder preparation: by the ceramics powder of preparing in A step, one of be raw material, add Cu powder, Ni powder to mix, and add a small amount of Ti powder, MnO
2, V
2o
5, one or more materials such as MgO and CaO the hotchpotchs such as mixture, add one or more the mixture in water, dehydrated alcohol or polyvinylpyrrolidone (PVP) to carry out secondary planetary type ball-milling, dry, ball milling material is pulverized and is obtained containing NiFe
2o
4the mixing nano-powder of-NiO-Cu-Ni;
C, the mixing nano-powder of preparing in B step is placed in rubber package set, jolt ramming, vacuumizes after sizing, adopt cold isostatic compaction, obtain cylindrical shape green compact;
D, the green compact of preparing in C step are placed in and in vacuum oven or atmosphere furnace, carry out sintering, sintering temperature is 650 ℃～950 ℃, in vacuum or inert gas atmosphere, carry out sintering, finally obtain fused salt electrolysis use, metallographic phase and ceramic phase complete wetting, grain-size is 53nm, the NiFe that density is high
2o
4-NiO-Cu-Ni cermet inert anode.
Tool of the present invention has the following advantages:
(1) introduced polyvinylpyrrolidone (PVP), be dissolved in and in dehydrated alcohol, form composite grinding aids, dispersion agent, membrane-forming agent and cakingagent; PVP can disperse well levigate powder and form more stable coating film coated powder in addition, reduces the activity of nano-powder, improves the stability of nanometer powder;
(2) adopt cold isostatic compaction, the efficiency that has improved powder moulding with become work rate, reduced the consumption of powder, can reduce production costs;
(3) greatly reduced the sintering temperature of pressed compact, the sintering temperature of usual way is 1200 ℃～1400 ℃, and the sintering temperature of inert anode prepared by processing method of the present invention is only 650 ℃～900 ℃, has very large energy-saving and cost-reducing ability;
(4) inert anode that the sintering of nano-powder obtains has solved problem nonwetting between metal and pottery or that wettability is poor;
(5) by Ti, adulterate and substitute the TiO in usual way
2doping, no longer overflows the metal Cu in inert anode that sintering obtains, has realized the complete wetting between metal and pottery and reaches and sprawl;
(6) density of material is brought up to more than 99%, heat-shock resistance brings up to 185.71%, and static corrosion rate is reduced to below 2.046 mm/y.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but never in any form the present invention is limited, and any conversion of doing based on training centre of the present invention, all falls into protection domain of the present invention.
Full moist type nano-Ni/Fe of the present invention
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode comprises the following steps:
A, the preparation of precursor ceramic powder: by Fe
2o
3with NiO or Ni
2o
3mixture (be " Fe
2o
3mixture with NiO " or " Fe
2o
3and Ni
2o
3mixture "), add water through wet ball grinding, dry after, be placed in sintering oven and calcine, control calcining temperature, be prepared into NiFe
2o
4-NiO precursor ceramic powder;
B, mix nano-powder preparation: by the ceramics powder of preparing in A step, one of be raw material, add Cu powder, Ni powder to mix, and add a small amount of Ti powder, MnO
2, V
2o
5, one or more materials such as MgO and CaO the hotchpotchs such as mixture, add one or more the mixture in water, dehydrated alcohol or polyvinylpyrrolidone to carry out secondary planetary type ball-milling, dry, ball milling material is pulverized and is obtained containing NiFe
2o
4the mixing nano-powder of-NiO-Cu-Ni;
C, the mixing nano-powder of preparing in B step is placed in rubber package set, jolt ramming, vacuumizes after sizing, adopt cold isostatic compaction, obtain cylindrical shape green compact;
D, the green compact of preparing in C step are placed in and in vacuum oven or atmosphere furnace, carry out sintering, sintering temperature is 650 ℃～950 ℃, in vacuum or inert gas atmosphere, carry out sintering, finally obtain fused salt electrolysis use, metallographic phase and ceramic phase complete wetting, grain-size is 53nm, the NiFe that density is high
2o
4-NiO-Cu-Ni cermet inert anode.
The Fe of described A step
2o
3with NiO or Ni
2o
3weight ratio be 1:0.1 ~ 5.
The calcining temperature of described A step is 900 ~ 1200 ℃.
The weight percent of the presoma of described B step is that the weight percent of the mixture of 70 ~ 85%, Cu powder and Ni powder is 10 ~ 25%; Ti powder, MnO
2, V
2o
5, MgO, CaO the weight percent of mixture be 1 ~ 5%.
The water of described B step, dehydrated alcohol, polyvinylpyrrolidone (PVP) can be used as the tensio-active agent of preparing in powder process.
The full moist type nano-Ni/Fe of described D step
2o
4the massfraction of each component of-NiO-Cu-Ni cermet inert anode is: NiFe
2o
4powder 66.3%～75.6%, NiO powder 10%～15%, Cu powder 14%～17%, Ni powder 2%～5%; Trace doped thing content is respectively: Ti powder 0～2%, MnO
2powder 0～1%, V
2o
5powder 0～1.5%, MgO powder 0～1%, CaO powder 0～1%.
Embodiment 1
By weight 1:1, take technical grade brown iron oxide and nickel protoxide, and add 65% water, adopt ball mill mix grinding 6h, the slurry obtaining is dry 24h at 100 ℃, calcines the NiFe that obtains NiO excessive 10% after pulverizing at 1100 ℃
2o
4powder.With NiFe
2o
4-10%NiO powder is one of raw material, adds in proportion chemical pure 14%Cu powder, 3%Ni powder; Trace doped thing 0.5%Ti powder, 1%MnO
2powder, 1.5%V
2o
5powder, 1%MgO powder and 1%CaO powder, then adding massfraction is 60% dehydrated alcohol and 1% PVP, ball mill ball milling 12h, dehydrated alcohol is reclaimed in the mixed slurry evaporation obtaining, dry 12h at 80 ℃, and the material obtaining is pulverized and is prepared the mixing nano-powder that mean particle size is 43.7nm.Pack the nano-powder of preparation into plasticity-better, regularly after jolt ramming or compacting in the higher jacket of intensity go out desired shape, tentatively reserve size, first base vacuumizes the gas of removing in material, and then under 240MPa, cold isostatic compaction obtains required pressed compact.Pressed compact is in argon gas (Ar) protection, is incubated 12h sintering at 700 ℃, finally obtains NiFe
2o
4-NiO-Cu-Ni cermet inert anode.
Implementation result: inert anode material has substituted traditional carbon annode material completely.This inert anode material is applied to after Aluminum Electrolysis Production, and current efficiency has reached 95%, and bath voltage drops to 390mv, brings up to bath life more than 2000 days.
Embodiment 2
By weight 1:1.5, take technical grade brown iron oxide and nickel oxide powder, and add 65% water, adopt ball mill mix grinding 6h, the slurry obtaining is dry 24h at 100 ℃, calcines the NiFe that obtains NiO excessive 15% after pulverizing at 1200 ℃
2o
4powder.With NiFe
2o
4-15%NiO powder is one of raw material, adds in proportion chemical pure 10%Cu powder, 2%Ni powder; Trace doped thing 0.5%Ti powder, 0.5%MnO
2powder, 2%V
2o
5powder, 1.2%MgO powder and 0.8%CaO powder, then adding massfraction is 60% dehydrated alcohol and 1% PVP, ball mill ball milling 12h, dehydrated alcohol is reclaimed in the mixed slurry evaporation obtaining, dry 12h at 80 ℃, the material obtaining is pulverized and is prepared the mixing nano-powder that mean particle size is 43.7nm.Pack the nano-powder of preparation into plasticity-better, regularly after jolt ramming or compacting in the higher jacket of intensity go out desired shape, tentatively reserve size, first base vacuumizes the gas of removing in material, and then under 240MPa, cold isostatic compaction obtains required pressed compact.Pressed compact is in argon gas (Ar) protection, is incubated 12h sintering at 700 ℃, finally obtains the NiFe of good quality
2o
4-NiO-Cu-Ni cermet inert anode.
Implementation result: inert anode material has substituted traditional carbon annode material completely.This inert anode material is applied to after Aluminum Electrolysis Production, and current efficiency has reached 94%, and bath voltage drops to 385mv, brings up to bath life more than 2000 days.
Embodiment 3
1:2.0 takes technical grade brown iron oxide by weight proportion, and adds 70% water, adopts ball mill mix grinding 8h, and the slurry obtaining is dry 24h at 100 ℃, calcines the NiFe that obtains NiO excessive 12% after pulverizing at 1050 ℃
2o
4powder.With NiFe
2o
4-12%NiO powder is one of raw material, adds in proportion the 15%Cu powder of chemical grade, 3%Ni powder; Trace doped thing 1%Ti powder, 1%MnO
2powder, 1.0%V
2o
5powder, 1.5%MgO powder and 1%CaO powder, then adding massfraction is 70% dehydrated alcohol and 3% PVP, ball mill ball milling 30h, dehydrated alcohol is reclaimed in the mixed slurry evaporation obtaining, dry 12h at 80 ℃, the material obtaining is pulverized and is prepared the mixing nano-powder that mean particle size is 43.7nm.Pack the nano-powder of preparation into plasticity-better, regularly after jolt ramming or compacting in the higher jacket of intensity go out desired shape, thick step is reserved size, and first base vacuumizes the gas of removing in material, and then under 280MPa, cold isostatic compaction obtains required pressed compact.Pressed compact is in argon gas (Ar) protection, is incubated 12h sintering at 800 ℃, finally obtains NiFe2O4-NiO-Cu-Ni cermet inert anode.
Implementation result: inert anode material has substituted traditional carbon annode material completely.This inert anode material is applied to after Aluminum Electrolysis Production, and current efficiency has reached 94.5%, and bath voltage drops to 385mv, brings up to bath life more than 2000 days.
Claims (6)
1. a full moist type nano-Ni/Fe
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, is characterized in that comprising the steps:
A, the preparation of precursor ceramic powder: by Fe
2o
3with NiO or Ni
2o
3mixture, add water through wet ball grinding, dry after, be placed in sintering oven and calcine, control calcining temperature, be prepared into NiFe
2o
4-NiO precursor ceramic powder;
B, mix nano-powder preparation: by the ceramics powder of preparing in A step, one of be raw material, add Cu powder, Ni powder to mix, and add a small amount of Ti powder, MnO
2, V
2o
5, one or more materials such as MgO and CaO the hotchpotchs such as mixture, add one or more the mixture in water, dehydrated alcohol or polyvinylpyrrolidone to carry out secondary planetary type ball-milling, dry, ball milling material is pulverized and is obtained containing NiFe
2o
4the mixing nano-powder of-NiO-Cu-Ni;
C, the mixing nano-powder of preparing in B step is placed in rubber package set, jolt ramming, vacuumizes after sizing, adopt cold isostatic compaction, obtain cylindrical shape green compact;
D, the green compact of preparing in C step are placed in and in vacuum oven or atmosphere furnace, carry out sintering, sintering temperature is 650 ℃～950 ℃, carries out sintering in vacuum or inert gas atmosphere, finally obtains fused salt electrolysis use, metallographic phase and ceramic phase complete wetting, grain-size is 53nm, the NiFe that density is high
2o
4-NiO-Cu-Ni cermet inert anode.
2. full moist type nano-Ni/Fe according to claim 1
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, is characterized in that the Fe of described A step
2o
3with NiO or Ni
2o
3weight ratio be 1:0.1 ~ 5.
3. full moist type nano-Ni/Fe according to claim 1
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, the calcining temperature that it is characterized in that described A step is 900 ~ 1200 ℃.
4. full moist type nano-Ni/Fe according to claim 1
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, the weight percent that it is characterized in that the presoma of described B step is 70 ~ 85%; The weight percent of the mixture of Cu powder and Ni powder is 10 ~ 25%; Ti powder, MnO
2, V
2o
5, MgO, CaO the weight percent of mixture be 1 ~ 5%.
5. full moist type nano-Ni/Fe according to claim 1
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, is characterized in that the water, dehydrated alcohol, polyvinylpyrrolidone of described B step are as the tensio-active agent of preparing in powder process.
6. full moist type nano-Ni/Fe according to claim 1
2o
4the preparation method of-NiO-Cu-Ni cermet inert anode, is characterized in that the full moist type nano-Ni/Fe of described D step
2o
4the massfraction of each component of-NiO-Cu-Ni cermet inert anode is: NiFe
2o
4powder 66.3%～75.6%, NiO powder 10%～15%, Cu powder 14%～17%, Ni powder 2%～5%; Trace doped thing content is respectively: Ti powder 0～2%, MnO
2powder 0～1%, V
2o
5powder 0～1.5%, MgO powder 0～1%, CaO powder 0～1%.
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| CN108373326A (en) * | 2018-05-16 | 2018-08-07 | 东北大学 | A kind of preparation method of high-compactness nickel ferrite based magnetic loaded Ultra-fine Grained ceramic material |
| CN108947520A (en) * | 2018-06-26 | 2018-12-07 | 株洲冶炼集团股份有限公司 | A kind of preparation method of ITO sintering target |
| CN110854364A (en) * | 2019-10-28 | 2020-02-28 | 广州大学 | Iron-nickel composite particles with core-shell structure and preparation method and application thereof |
| CN112458523A (en) * | 2020-11-12 | 2021-03-09 | 南通创源电化学科技有限公司 | Ceramic anode electroplating bath |
| CN112827494A (en) * | 2020-12-31 | 2021-05-25 | 华中科技大学 | Nickel-iron composite oxygen carrier and preparation method and application thereof |
| CN113215429A (en) * | 2021-04-30 | 2021-08-06 | 中南大学 | Preparation method of high-density metal ceramic inert anode material for aluminum electrolysis |
| CN113308713A (en) * | 2021-05-25 | 2021-08-27 | 西部金属材料股份有限公司 | Metal ceramic anode and preparation method and application thereof |
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| US11996222B2 (en) | 2016-09-07 | 2024-05-28 | South Dakota Board Of Regents | Thermally stabilized redox materials and applications thereof |
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| CN112827494A (en) * | 2020-12-31 | 2021-05-25 | 华中科技大学 | Nickel-iron composite oxygen carrier and preparation method and application thereof |
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| CN113215429A (en) * | 2021-04-30 | 2021-08-06 | 中南大学 | Preparation method of high-density metal ceramic inert anode material for aluminum electrolysis |
| CN113308713A (en) * | 2021-05-25 | 2021-08-27 | 西部金属材料股份有限公司 | Metal ceramic anode and preparation method and application thereof |
| CN113430577A (en) * | 2021-07-21 | 2021-09-24 | 东北大学 | NiFe for aluminum electrolysis2O4Inert anode material of base cermet and its prepn |
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