CN104060298A - Ceramic alloy inert anode with equipotential plane and preparation method thereof - Google Patents
Ceramic alloy inert anode with equipotential plane and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 64
- 229910002110 ceramic alloy Inorganic materials 0.000 title abstract description 5
- 238000005260 corrosion Methods 0.000 claims abstract description 102
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000007797 corrosion Effects 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 18
- 239000002184 metal Substances 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims description 46
- 238000000465 moulding Methods 0.000 claims description 31
- 238000003825 pressing Methods 0.000 claims description 31
- 229910045601 alloy Inorganic materials 0.000 claims description 23
- 239000000956 alloy Substances 0.000 claims description 23
- 239000000919 ceramic Substances 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 229910052759 nickel Inorganic materials 0.000 claims description 18
- 238000010792 warming Methods 0.000 claims description 17
- 238000004512 die casting Methods 0.000 claims description 16
- 238000002347 injection Methods 0.000 claims description 16
- 239000007924 injection Substances 0.000 claims description 16
- 238000001746 injection moulding Methods 0.000 claims description 16
- 229910052742 iron Inorganic materials 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- 229910052750 molybdenum Inorganic materials 0.000 claims description 13
- 229910052727 yttrium Inorganic materials 0.000 claims description 13
- 229910052804 chromium Inorganic materials 0.000 claims description 12
- 230000006698 induction Effects 0.000 claims description 12
- 229910052746 lanthanum Inorganic materials 0.000 claims description 11
- 229910052684 Cerium Inorganic materials 0.000 claims description 10
- 239000012267 brine Substances 0.000 claims description 10
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 10
- 229910017563 LaCrO Inorganic materials 0.000 claims description 9
- 229910008336 SnCo Inorganic materials 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 229910052718 tin Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910000684 Cobalt-chrome Inorganic materials 0.000 claims description 8
- 229910015372 FeAl Inorganic materials 0.000 claims description 8
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims description 8
- 229910000943 NiAl Inorganic materials 0.000 claims description 8
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 8
- 239000010952 cobalt-chrome Substances 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 229910052748 manganese Inorganic materials 0.000 claims description 7
- 229910003321 CoFe Inorganic materials 0.000 claims description 6
- 241000877463 Lanio Species 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 230000005611 electricity Effects 0.000 claims description 5
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- 238000009826 distribution Methods 0.000 claims description 3
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 abstract description 9
- 150000003839 salts Chemical class 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- -1 ferrous metals Chemical class 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000005422 blasting Methods 0.000 description 6
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
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- Powder Metallurgy (AREA)
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Abstract
The invention discloses a ceramic alloy inert anode with an equipotential plane and a preparation method thereof, relates to a fused salt electrolysis process extracting inert anode of non-ferrous metals, and particularly relates to an aluminum electrolysis inert anode and a preparation method thereof. The ceramic alloy inert anode is characterized in that the anode is of a sandwich structure, and composed of a corrosion-resistant housing and a conductive connecting core body, wherein the corrosion-resistant housing is consistent in thickness; the conductive connecting core body tightly contacts with the inner surface of the housing, so that the outer housing surface forms the equipotential plane, and therefore, current passing through the anode is distributed uniformly. The ceramic alloy inert anode with the equipotential plane, which is disclosed by the invention, effectively realizes uniform control on thickness of the corrosion-resistant outer layer, solves tight combination of the corrosion-resistant housing and the connecting core body, and is simple in preparation process and capable of realizing industrial application.
Description
Technical field
A kind of ceramal inert anode with equipotential plane and preparation method thereof, relates to a kind of fused salt electrolysis process extraction inert anode of non-ferrous metal, particularly inert anode for aluminium electrolysis and preparation method thereof.
Background technology
Existing fused salt electrolysis is prepared in the technique of metallic aluminium and is mostly adopted carbon annode material, not only consumes the carbon materials of a large amount of high-qualitys, produces a large amount of CO
2greenhouse gases and have carcinogenic substance bitumen flue gas, sour gas sulfurous gas and a strong greenhouse gas CF
n, cause serious environmental pollution, and the poor electric conductivity of carbon anode, electric energy efficiency is low, power consumption is large especially, be the major cause of existing aluminum electrolysis process high energy consumption, the problem such as expensive, and inert anode is because addressing the above problem the revolution that is expected to realize fused salt electrolysis technology.
There are three class materials studied as fused salt electrolysis inert anode: oxide ceramics, alloy and sintering metal.Though oxide ceramics has excellent electrolyte-resistant dissolved corrosion and nascent oxygen oozes erosion performance, its electroconductibility is low, fragility is high, heat-shock resistance is poor, be difficult to be connected with metal guide rod, alloy anode intensity is high, good toughness, the opposite sex that is applicable to maximize equips, are connected easily, conduct electricity very well with metal guide rod, develop the main bugbear of alloy anode and be the control that how to reduce its erosion rate, oxidation film layer thickness with and with the conjugation of matrix, sintering metal in ideal can have both the strong erosion resistance of metal oxide ceramic and good electroconductibility and the mechanical property of metal, can overcome the heat-shock resistance of metal oxide anode poor and be connected the problems such as difficulty with guide rod, there is better erosion resistance and oxidation-resistance than metal or alloy anode simultaneously, but due to learning from other's strong points to offset one's weaknesses of also failing to realize ideal between metal oxide ceramic at present used and metal, make the cermet material of preparing be difficult to fully have the advantage of metallographic phase and ceramic phase simultaneously, even also introduce shortcoming separately, particularly due to metallic conductor connectivity problem, engineering is amplified difficulty, at present also cannot industrial applications.
Patent CN 101255577B has described a kind of metal ceramic inert anode for molten salt electrolysis and preparation method thereof, by adjusting the oxygen level in atmosphere, material is carried out to selective oxidation, there is corrosion-resistant skin and high-strength, high-ductility to form, the function gradient structure of high conduction internal layer, the method need to regulate oxygen levels different in atmosphere, be difficult to control, and after its selective oxidation, corrosion-resistant outer field thickness is difficult to regulation and control.
Patent CN 1548586A has described a kind of ceramet material with gradient function for electrolyzing Al, and the method complicated process of preparation is difficult to realize industrialization.
Summary of the invention
The deficiency that the object of the invention exists for above-mentioned prior art, provide the corrosion-resistant outer field thickness of a kind of effectively solution to be difficult to regulation and control, metallic conductor connects, preparation technology is simple, can realize industrial applications, corrosion resistance and good there is ceramal inert anode of equipotential plane and preparation method thereof.
The object of the invention is to be achieved through the following technical solutions.
A ceramal inert anode for equipotential plane, is characterized in that this anode is for " sandwich " structure, is connected core body forms by anti-corrosion shell with conduction; The consistency of thickness of its anti-corrosion shell, conduction connects the close contact of core body and inner surface of outer cover, makes case surface form equipotential plane, impels by the distribution of current of anode even.
The ceramal inert anode of a kind of equipotential plane of the present invention, that the cross section that it is characterized in that described anti-corrosion shell can be is square, circular, any one in ellipse, and shell sidepiece and bottom are arc or square, and shell wall thickness is 0.5 ~ 3cm; It is any one in square, circular, ellipse that conduction connects core body cross section, and linker sidepiece and bottom are arc or square, and linker and shell are combined closely, and linker is wrapped among shell, or part is exposed.
The ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that described anti-corrosion shell is by pottery-alloy composition, and wherein the massfraction of ceramic phase is 10%-80%, and composition can be NiFe
2o
4, CoFe
2o
4, CoCr
2o
4, SnCo
2o
4, ZnAl
2o
4, NiAl
2o
4, ZnFe
2o
4, FeAl
2o
4, ZrSnO
4, LaCrO
3, LaNiO
3, NiO, FeO, Fe
2o
3, ZnO, CuO, Cu
2o, SnO
2, Sb
2o
3, Bi
2o
3, CeO
2, Cr
2o
3, Li
2o, Ag
2o, TiO
2, Y
2o
3in one or more combinations; The mass percent content of metallographic phase is 20%-90%, and composition can be one or more metallic combinations in Ni, Al, Cu, Fe, Co, Si, Ti, Sn, Y, Mn, Cr, Mo, Zn, Nb, La, Ce.
The ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that described conduction connects core body by ceramic-metal or alloy composition, and wherein the ceramic phase massfraction content of linker is 0-40%, consists of NiFe
2o
4, CoFe
2o
4, CoCr
2o
4, SnCo
2o
4, NiAl
2o
4, ZnFe
2o
4, FeAl
2o
4, ZrSnO
4, LaCrO
3, LaNiO
3, NiO, FeO, Fe
2o
3, ZnO, CuO, Cu
2o, SnO
2, Sb
2o
3, Bi
2o
3, CeO
2, Cr
2o
3, Li
2o, Ag
2o, TiO
2, Y
2o
3in one or more combinations; The massfraction of metallographic phase is 60-100%, and composition can be one or more combinations in Ni, Al, Cu, Fe, Co, Ti, Sn, Y, Mn, Cr, Mo, Zn, Nb, La, Ce.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation
First obtain the green compact of shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, then in inertia or weak oxide atmosphere, at 1200 DEG C-1500 DEG C, after 1-20 h sintering, obtain the finished product of refractory brine corrosion shell;
(2) anti-corrosion shell is connected core body combination with conduction
Anti-corrosion shell is preheated to 500 DEG C-1000 DEG C in inert atmosphere protection, linker is cast in anti-corrosion shell by after proportioning fusing, conduction connection-core body divides that exposed stove is chilled to room temperature outside anti-corrosion shell, obtains " sandwich " inert anode.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation
First obtain the green compact of refractory brine corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, then in inertia or weak oxide atmosphere in 1200 DEG C-1500 DEG C base substrates that obtain anti-corrosion shell after 1-20 h sintering;
(2) anti-corrosion shell preparation is connected core body combination with conduction
Prepare the alloy pig of required linker by vacuum induction melting, be processed as suitable size, shell is put into after clearing up in surface, keeps vacuum tightness 1.0 × 10
-3-1.0 × 10
-2pa, is warming up to insulation at the temperature of above 10 DEG C-50 DEG C of conduction connection-core bulk melting point and spread connection 1h-15h, obtains " sandwich shape " inert anode, and the connection-core body that wherein conducts electricity divides exposed.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation
First obtain the green compact of refractory brine corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, then in inert atmosphere in 500 DEG C-1000 DEG C through 2-10 h pre-burnings;
(2) anti-corrosion shell preparation is connected core body combination with conduction
Prepare by vacuum induction melting the alloy pig that required conduction connects core body component, after processing, put into anti-corrosion shell, in inertia or weak oxide atmosphere, be first warming up to conduction connection-core bulk melting point insulation 1h-5h, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min again, obtain " sandwich shape " inert anode, the connection-core body that wherein conducts electricity divides exposed.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation
First obtain the green compact of refractory brine corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed;
(2) anti-corrosion shell preparation is connected core body combination with conduction
Prepare by vacuum induction melting the alloy pig that required conduction connects core body, be processed as suitable size, anti-corrosion shell is put on surface after clearing up, in inertia or weak oxide atmosphere, be first warming up to linker fusing point insulation 1h-5h, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min again, obtain " sandwich shape " inert anode, anti-corrosion housing parts is exposed.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that the step of its preparation process comprises:
(1) conduction connects the preparation of core body
Prepare the alloy pig of required linker by vacuum induction melting, be processed as suitable size, surface is cleared up;
(2) preparation of " sandwich " inert anode
By die design, carry out global formation shell being connected to core body with conduction with isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, wherein conduction connection core body wraps up in the enclosure completely, in inertia or weak oxide atmosphere, be first warming up to linker melting temperature insulation 1h-5h, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min again, obtain " sandwich shape " inert anode.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that the step of its preparation process comprises:
(1) conduction connects the preparation of core body
First conduction is connected to core body powder and obtain by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed the green compact that conduction connects core body;
(2) preparation of " sandwich " inert anode
By die design, carry out global formation anti-corrosion shell being connected to core body with conduction with isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, wherein linker is wrapped in anti-corrosion shell completely, in lazy or weak oxide atmosphere, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min, obtain " sandwich shape " inert anode.
The preparation method of the ceramal inert anode of a kind of equipotential plane of the present invention, is characterized in that sintering atmosphere is Ar or N
2rare gas element, wherein in atmosphere oxygen level at 20-500ppm.
The ceramal inert anode of a kind of equipotential plane of the present invention, efficiently solves corrosion-resistant outer field thickness and is difficult to regulation and control, and metallic conductor connects, and preparation technology is simple, can realize industrial applications.
Brief description of the drawings
Fig. 1 is the structural representation of the ceramal inert anode of a kind of equipotential plane of the present invention.
Fig. 2 is the structural representation of the ceramal inert anode of another kind of equipotential plane of the present invention.
Fig. 3 is the structural representation of the ceramal inert anode of another kind of equipotential plane of the present invention.
In figure, 1 is anti-corrosion shell, and 2 is conduction connection core body.
Embodiment
A ceramal inert anode for equipotential plane, this anode is " sandwich " structure, is connected core body forms by anti-corrosion shell with conduction; The consistency of thickness of its anti-corrosion shell, conduction connects the close contact of core body and inner surface of outer cover, makes case surface form equipotential plane, impels by the distribution of current of anode even.
(1) preparation of corrosion-resistant ceramic alloy shell
Anti-corrosion shell is made up of ceramic phase and metallographic phase, because metal content is wherein more than or equal to 20%, higher than the sintering metal anode (metal content <20%) of tradition research, shows better thermal shock resistance, therefore claim ceramal.Metallographic phase is one or more combinations in Ni, Al, Cu, Fe, Co, Si, Ti, Sn, Y, Mn, Cr, Mo, Zn, Nb, La, Ce, the massfraction of metallographic phase is 20-90%, and metallographic phase can form rapidly against corrosion and oxidation resistant oxide membranous layer under electrolytic process or oxidizing atmosphere; Ceramic phase is NiFe
2o
4, CoFe
2o
4, CoCr
2o
4, SnCo
2o
4, NiAl
2o
4, ZnFe
2o
4, FeAl
2o
4, ZrSnO
4, LaCrO
3, LaNiO
3, NiO, FeO, Fe
2o
3, ZnO, CuO, Cu
2o, SnO
2, Sb
2o
3, Bi
2o
3, CeO
2, Cr
2o
3, Li
2o, Ag
2one or more combinations in O, the massfraction of ceramic phase is 10%-80%; Add a small amount of additive as ZrO simultaneously
2, TiO
2, Y
2o
3and the one or more combination such as other rare earth oxides is with acceleration of sintering, ensures anti-corrosion shell thing phase and density uniformity from inside to outside.First obtain the green compact of anti-corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, after oversintering, obtain the finished product of anti-corrosion shell, sintering temperature is 1200 DEG C-1500 DEG C, sintering atmosphere is maintained weak oxide atmosphere (oxygen level remains 20-500ppm), and sintering time is 1-20 h.
That cross-sectional outer can be is square, circular, any one in ellipse, and sidepiece and bottom can be designed to arc or square, and wall thickness is 0.5 ~ 3cm.
(2) conduction connects the preparation of core body
Linker is made up of ceramic phase and metallographic phase.Ceramic phase is NiFe
2o
4, CoFe
2o
4, CoCr
2o
4, SnCo
2o
4, NiAl
2o
4, ZnFe
2o
4, FeAl
2o
4, ZrSnO
4, LaCrO
3, LaNiO
3, NiO, FeO, Fe
2o
3, ZnO, CuO, Cu
2o, SnO
2, Sb
2o
3, Bi
2o
3, CeO
2, Cr
2o
3, Li
2o, Ag
2o, TiO
2, Y
2o
3in one or more combination, massfraction is 0-40%; Metallographic phase is one or more combinations in Ni, Al, Cu, Fe, Co, Ti, Sn, Y, Mn, Cr, Mo, Zn, Nb, La, Ce, and massfraction is 60-100%.Prepare linker with casting or the method for powder metallurgy.
Linker and shell are combined closely, and that its cross section can be is square, circular, any one in ellipse, and sidepiece and bottom can be designed to arc or square, and linker can be wrapped among shell, also can part exposed.
(3) combination of resistance to shell and linker
Anti-corrosion shell can be totally enclosed, and linker is wrapped in anti-corrosion shell completely, can be also semi-enclosed, and linker has part exposed.
The method of anti-corrosion shell and linker combination has casting, infiltration, diffusion welding, sintering.
For the totally-enclosed inert anode of refractory brine corrosion shell, its preparation method is in anti-corrosion shell moulding process, linker to be put into wherein, and a step sintering combines refractory salt shell and linker by infiltration or sintering.
For the semiclosed inert anode of anti-corrosion shell, its preparation method is the anti-corrosion shell first obtaining after sintering, then mode by casting, infiltration, diffusion welding or sintering is by anti-corrosion shell and linker combination.Also can, by linker and anti-corrosion shell one step sintering, by infiltration or sintering, anti-corrosion shell and linker be combined.
Embodiment 1
Melting 5 kg linker alloy pigs in vacuum induction furnace, contained each constituent mass mark respectively: 75%Cu, 19.5%Ni, 1.5%Ti, 1%Co, 1%CuO, 1.5%Cu
2o, 0.5%CeO
2, alloy pig is processed as to 50 × 50 × 200(mm) block, Shot Blasting is carried out on surface.In anti-corrosion shell, metallographic phase accounts for 20 wt%, and its constituent mass mark is respectively 6%Co, 40%Ni, 40%Fe, 14%Cu; ; Ceramic phase accounts for 80 wt%, and its component is 70%NiFe
2o
4, 10%NiO, 10%ZnFe
2o
4, 5%Fe
2o
3, 4%TiO
2, 1%Y
2o
3; Anti-corrosion shell component is mixed; add 1% PVA; in isostatic pressing (forming pressure 100Mpa) process, be pressed in corrosion-resistant shell using linker as inner core; under argon shield; at 1200 DEG C of sintering 4 h; obtain totally-enclosed inert anode (a step sintering), schematic diagram as shown in Figure 1.
Embodiment 2
Melting 5 kg metal connector alloy pigs in vacuum induction furnace, contained each element massfraction respectively: 70%Cu, 20%Ni, 5%Fe, 1%Al, 1%Mn, 1%Cr, 1%NiO, 0.5%Y
2o
3, 0.5%La, is processed as 50 × 50 × 200(mm by alloy pig) block, Shot Blasting is carried out on surface.The metallographic phase content of anti-corrosion shell is 60 wt%, and the each element massfraction of metallographic phase is respectively 5%Al, 40%Ni, and 40%Fe, 14%Cu, 1%Mo; Anti-corrosion shell ceramic content 40 wt%, ceramic phase consists of 70%NiAl
2o
4, 10%CoCr
2o
4, 10%FeAl
2o
4, 4%FeO, 4%Sb
2o
3, 1%Li
2o, 1%CeO
2; Anti-corrosion shell component is mixed; add 1% PVA; after isostatic pressing (forming pressure 200Mpa), under argon shield, at 1000 DEG C of sintering 2 h, obtain anti-corrosion shell; linker after Shot Blasting is put into the corrosion-resistant shell after sintering; under vacuum, at 1300 DEG C of sintering 10h, linker and corrosion-resistant shell are combined; obtain the semi-enclosed inert anode of refractory brine corrosion shell, schematic diagram as shown in Figure 2.
Implementation column 3
Linker is by 60% Ni, 20% Cu, 5% Mo, 2% Cr, 2% Y, 1% Sn, 1% Ce, 5% NiFe
2o
4, 2% SnO
2, 2% Bi
2o
3composition, linker raw material is mixed, adopt dry-pressing formed 60 × 60 × 250(mm for preparing) base substrate, in anti-corrosion shell, metallographic phase content is 30 wt%, the each element massfraction of metallographic phase is respectively 5% Al, 60% Ni, 10% Fe, 14% Cu, 2% Mo, 1% Y, 1% Nb, 1% La, 1% Ce, 1% Co, 1% Zn, 1% Sn, 1% Si, 1% Cr; Ceramic content 30 wt% in anti-corrosion shell, ceramic phase consists of 70% ZnFe
2o
4, 10% ZrSnO
4, 5% LaCrO
3, 5% SnCo
2o
4, 4% FeO, 4%Sb
2o
3, 1%Li
2o, 1%CeO
2; Corrosion-resistant shell component is mixed; add 1% PVA; in isostatic pressing (forming pressure 200Mpa) process, previously prepared linker base substrate is pressed into shell base substrate; and on shell green compact, process a hole; linker part is exposed, then under argon shield, at 1250 DEG C of sintering 2 h; obtain " sandwich " inert anode, schematic diagram as shown in Figure 3.
Embodiment 4
In anti-corrosion shell, metallographic phase content is 50 wt%, and the each element massfraction of metallographic phase is respectively 65% Ni, 10% Fe, 14% Cu, 2% Mo, 1% Y, 1% Nb, 1% La, 1% Ce, 1% Co, 1% Zn, 1% Sn, 1% Si, 1% Cr; Ceramic content 50 wt% in anti-corrosion shell, ceramic phase consists of 70% ZnAl
2o
4, 10% ZrSnO
4, 5% LaCrO
3, 5% SnCo
2o
4, 4% FeO, 4%Sb
2o
3, 1%Li
2o, 1%CeO
2; Anti-corrosion shell component is mixed, adopt injection molding to obtain shell green compact, under inert atmosphere, obtain shell in 1400 DEG C of sintering 5 h.Linker composition is 70%Cu, 25%Ni, 1.5%Ti, 1%Co, 1%Ag
2o, 1.5%Cu
2o is preheated to shell 1000 DEG C in inert atmosphere protection, after linker is melted by proportioning, is cast in shell, and stove is chilled to room temperature, obtains " sandwich " inert anode, as shown in Figure 2.
Embodiment 5
In anti-corrosion shell, metallographic phase content is 25 wt%, and the each element massfraction of metallographic phase is respectively 55% Ni, 10% Fe, 25% Cu, 2% Mo, 1% Y, 1% Nb, 1% La, 1% Ce, 1% Co, 1% Zn, 1% Si, 1% Cr; Ceramic content 75 wt% in anti-corrosion shell, ceramic phase is 80% ZnAl
2o
4, 5% ZrSnO
4, 5% LaCrO
3, 3% SnCo
2o
4, 2% FeO, 2% Cr
2o
3, 2% Fe
2o
3, 1% CeO
2; Anti-corrosion shell component is mixed, adopt injection forming to obtain shell green compact, under inert atmosphere, obtain shell in 1400 DEG C of sintering 7 h.Linker composition is 65% Cu, 25% Ni, 5% Al, 1.5% Ti, 1% Co, 1% Ag
2o, 1.5% Cu
2o, in vacuum induction furnace, melting 5 kg metal connector alloy pigs, are processed as 50 × 50 × 200(mm) block, Shot Blasting is carried out on surface.Linker after processing is put into shell, 1.0 × 10
-3under Pa vacuum tightness, be warming up to above 50 DEG C of linker fusing point and spread connection 5 h, obtain " sandwich " inert anode, as shown in Figure 2.
Embodiment 6
Melting 5 kg metal connector alloy pigs in vacuum induction furnace, contained each element massfraction respectively: 80%Cu, 15%Ni, 1%Al, 1%Co, 1%Mo, 1%NiO, 0.5%Y
2o
3, 0.5%La, is processed as 50 × 50 × 200(mm by alloy pig) block, Shot Blasting is carried out on surface.In anti-corrosion shell, metallographic phase content is 35 wt%, and the each element massfraction of metallographic phase is respectively 5%Al, 40%Ni, and 40%Fe, 14%Cu, 1%Mo; Ceramic content 65 wt% in anti-corrosion shell, ceramic phase consists of 70%NiAl
2o
4, 10%CoCr
2o
4, 10%FeAl
2o
4, 4%FeO, 4%Sb
2o
3, 1%Li
2o, 1%CeO
2; Anti-corrosion shell component is mixed, adopt hot die-casting molding to obtain shell green compact, the linker after Shot Blasting is put into the anti-corrosion shell after sintering, in inert atmosphere, at 1300 DEG C of sintering 5 h, obtain " sandwich " inert anode, as shown in Figure 2.
Claims (11)
1. a ceramal inert anode for equipotential plane, is characterized in that this anode is for " sandwich " structure, is connected core body forms by anti-corrosion shell with conduction; The consistency of thickness of its anti-corrosion shell, conduction connects the close contact of core body and inner surface of outer cover, makes case surface form equipotential plane, impels by the distribution of current of anode even.
2. the ceramal inert anode of a kind of equipotential plane according to claim 1, that the cross section that it is characterized in that described anti-corrosion shell can be is square, circular, any one in ellipse, shell sidepiece and bottom are arc or square, and shell wall thickness is 0.5 ~ 3cm; It is any one in square, circular, ellipse that conduction connects core body cross section, and linker sidepiece and bottom are arc or square, and linker and shell are combined closely, and linker is wrapped among shell, or top part is exposed.
3. the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that described anti-corrosion shell is by pottery-alloy composition, and wherein the massfraction of ceramic phase is 10%-80%, and composition can be NiFe
2o
4, CoFe
2o
4, CoCr
2o
4, SnCo
2o
4, ZnAl
2o
4, NiAl
2o
4, ZnFe
2o
4, FeAl
2o
4, ZrSnO
4, LaCrO
3, LaNiO
3, NiO, FeO, Fe
2o
3, ZnO, CuO, Cu
2o, SnO
2, Sb
2o
3, Bi
2o
3, CeO
2, Cr
2o
3, Li
2o, Ag
2o, TiO
2, Y
2o
3in one or more combinations; The mass percent content of metallographic phase is 20%-90%, and composition can be one or more metallic combinations in Ni, Al, Cu, Fe, Co, Si, Ti, Sn, Y, Mn, Cr, Mo, Zn, Nb, La, Ce.
4. the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that described conduction connects core body by ceramic-metal or alloy composition, and wherein the ceramic phase massfraction content of conduction connection core body is 0-40%, consists of NiFe
2o
4, CoFe
2o
4, CoCr
2o
4, SnCo
2o
4, NiAl
2o
4, ZnFe
2o
4, FeAl
2o
4, ZrSnO
4, LaCrO
3, LaNiO
3, NiO, FeO, Fe
2o
3, ZnO, CuO, Cu
2o, SnO
2, Sb
2o
3, Bi
2o
3, CeO
2, Cr
2o
3, Li
2o, Ag
2o, TiO
2, Y
2o
3in one or more combinations; The massfraction of metallographic phase is 60-100%, and composition can be one or more combinations in Ni, Al, Cu, Fe, Co, Ti, Sn, Y, Mn, Cr, Mo, Zn, Nb, La, Ce.
5. the preparation method of the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation:
First obtain the green compact of shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, then in inertia or weak oxide atmosphere, at 1200 DEG C-1500 DEG C, after 1-20 h sintering, obtain the finished product of refractory brine corrosion shell;
(2) anti-corrosion shell is connected core body combination with conduction:
Anti-corrosion shell is preheated to 500 DEG C-1000 DEG C in inert atmosphere protection, linker is cast in anti-corrosion shell by after proportioning fusing, conduction connection-core body divides that exposed stove is chilled to room temperature outside anti-corrosion shell, obtains " sandwich " inert anode.
6. the preparation method of the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation:
First obtain the green compact of refractory brine corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, then in inertia or weak oxide atmosphere in 1200 DEG C-1500 DEG C base substrates that obtain anti-corrosion shell after 1-20 h sintering;
(2) anti-corrosion shell preparation is connected core body combination with conduction:
Prepare the alloy pig of required linker by vacuum induction melting, be processed as suitable size, shell is put into after clearing up in surface, keeps vacuum tightness 1.0 × 10
-3-1.0 × 10
-2pa, is warming up to insulation at the temperature of above 10 DEG C-50 DEG C of conduction connection-core bulk melting point and spread connection 1h-15h, obtains " sandwich shape " inert anode, and the connection-core body that wherein conducts electricity divides exposed.
7. the preparation method of the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation:
First obtain the green compact of refractory brine corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, then in inert atmosphere in 500 DEG C-1000 DEG C through 2-10 h pre-burnings;
(2) anti-corrosion shell preparation is connected core body combination with conduction:
Prepare by vacuum induction melting the alloy pig that required conduction connects core body component, after processing, put into anti-corrosion shell, in inertia or weak oxide atmosphere, be first warming up to conduction connection-core bulk melting point insulation 1h-5h, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min again, obtain " sandwich shape " inert anode, the connection-core body that wherein conducts electricity divides exposed.
8. the preparation method of the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that the step of its preparation process comprises:
(1) anti-corrosion shell preparation:
First obtain the green compact of refractory brine corrosion shell by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed;
(2) anti-corrosion shell preparation is connected core body combination with conduction:
Prepare by vacuum induction melting the alloy pig that required conduction connects core body, be processed as suitable size, anti-corrosion shell green compact are put on surface after clearing up, in inertia or weak oxide atmosphere, be first warming up to connection-core bulk melting point insulation 1h-5h, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min again, obtain " sandwich shape " inert anode, anti-corrosion housing parts is exposed.
9. the preparation method of the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that the step of its preparation process comprises:
(1) conduction connects the preparation of core body:
Prepare the alloy pig of required linker by vacuum induction melting, be processed as suitable size, surface is cleared up;
(2) preparation of " sandwich " inert anode:
By die design, carry out global formation shell being connected to core body with conduction with isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, wherein conduction connection core body wraps up in the enclosure completely, in inertia or weak oxide atmosphere, be first warming up to linker melting temperature insulation 1h-5h, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min again, obtain " sandwich shape " inert anode.
10. the preparation method of the ceramal inert anode of a kind of equipotential plane according to claim 1, is characterized in that the step of its preparation process comprises:
(1) conduction connects the preparation of core body:
First conduction is connected to core body powder and obtain by isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed the green compact that conduction connects core body;
(2) preparation of " sandwich " inert anode:
By die design, carry out global formation anti-corrosion shell being connected to core body with conduction with isostatic cool pressing, injection molding, hot die-casting molding, injection forming, one or more moulding processs in dry-pressing formed, wherein connecting core body is wrapped in anti-corrosion shell completely, in inertia or weak oxide atmosphere, be warming up to 1200 DEG C-1500 DEG C sintering 1-20 h sintering with the temperature rise rate of 1 DEG C/min-10 DEG C/min, obtain " sandwich shape " inert anode.
The preparation method of the ceramal inert anode of 11. a kind of equipotential planes according to claim 1, is characterized in that sintering atmosphere is Ar or N
2rare gas element, wherein in atmosphere oxygen level at 20-500ppm.
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