CN102383147B - Sandwich biscuit type graphite/titanium diboride electrode and manufacturing method thereof - Google Patents
Sandwich biscuit type graphite/titanium diboride electrode and manufacturing method thereof Download PDFInfo
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- CN102383147B CN102383147B CN201110230612.6A CN201110230612A CN102383147B CN 102383147 B CN102383147 B CN 102383147B CN 201110230612 A CN201110230612 A CN 201110230612A CN 102383147 B CN102383147 B CN 102383147B
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Abstract
The invention discloses a sandwich biscuit type graphite/titanium diboride electrode and a manufacturing method thereof. The graphite/titanium diboride electrode is prepared by proportioning different raw materials for a surface layer and a central layer. The technical process comprises the following steps: laying powder in lamination in a graphite hot pressing mould, covering with a graphite plate after completing the powder laying of one electrode, then repeating the laminated powder laying process, covering a graphite plate again, then repeating the laminated powder laying until the graphite hot pressing mould is full, then covering a graphite pressure head, and sintering for 1-4 hours under the hot pressing conditions with the temperature of 1600-1900 DEG C and the pressure of 20-30MPa; and cooling the sintered product to room temperature along with a furnace, opening the mould to take out the product, processing the product to a given size according to the requirements by a surface grinder and a diamond wheel, and then drilling and tapping specified side surfaces to complete product manufacture. The invention has good product performance, a simple process and remarkable economic and social benefits.
Description
Technical field
The present invention relates to the manufacture method of efficient inert cathode for New Electrolytic Aluminium, be specifically related to a kind of graphite/titanium diboride electrode and manufacture method thereof.
Background technology
Metallic aluminium is large common metal material, and the basic product electrolytic aluminum of metal aluminium mainly adopts the aluminum oxide of electrolytic dissolution in cryolite melts to produce.In electrolytic process, metal aluminium liquid generates at the negative electrode of electrolyzer, and the resistance to metallic aluminium of wettability, cathode material of aluminium liquid anticathode material, the corrosive nature of cryolite melts greatly affect the key issues such as the pole effect of electrolytic process, current efficiency, electrolyzer work-ing life.
TiB2, as a kind of new ceramic material, has good conductivity, good with liquid aluminum wets, and the aluminium of resistance to liquid and cryolite melts corrosion, be very good aluminium slot electrode inert cathode material.
TiB2, as a kind of high-melting-point boride ceramics, adopts ordinary method to be difficult to sintering, generally adopts the way of hot pressed sintering.But as the cathode material of electrolyzer key part, must be able to be processed into the device of unified size, and every cube electrode must have can tie cable interface (bolt hole).TiB2 extreme hardness, if adopt the TiB2 sintered compact of single component, will cause bolt hole to process.Therefore need to adopt to add the good graphite of processibility to make graphite/titanium diboride composite ceramics electrode.But graphite and liquid aluminium wettability are poor, if content of graphite is higher, although processibility has very big improvement, product performance also decline to a great extent, and if TiB2 content is higher, later stage boring, tapping are very difficult again.In order to address this problem, we have invented Sandwich biscuit type composite ceramics and the preparation technology thereof who mentions in this patent.
Summary of the invention
The object of the present invention is to provide a kind of graphite/titanium diboride electrode and manufacture method thereof.Product performance are good, and technique is simple, have significant economic and social benefit.
For achieving the above object, the present invention adopts following technical scheme:
(1) titanium diboride powder is evenly mixed in proportion with crystalline flake graphite powder, a kind of TiB2 content below claims A powder at 85 ~ 99%(), another kind of TiB2 content below claims B powder at 70-78%().
(2) in hot pressing die, first pack A powder into, opened up even paving, compacting, forms lower top layer.As Fig. 3
(3) on the A powder compacted lift of having completed, cover a certain amount of B powder again, opened up equally even paving, note not destroying the lower top layer A bisque of having completed, compacting, forms central core (or claiming sandwich layer).As Fig. 4
The laying of central core also can be taked another method: first on the A of the lower floor powder of compacting, put a U-shaped division board (making with the thin slice of sheet iron or other materials) completing, make the opening of U-shaped division board be close to the sidewall of hot pressing die, then the interior space-filling B powder forming at U-shaped plate, in the space forming, fill A powder between U-shaped plate and hot pressing die sidewall, as even the paving of preceding method exhibition, and make two kinds of powder be laid to same thickness; Then carefully take out from the bottom up U-shaped plate, make A, two kinds of powder of B be connected to form the sandwich layer of sandwich biscuit, then appropriate compacting (not destroying the distribution situation of A, B powder).As Fig. 5
(4) on the central core of completing, re-lay A powder, open up the even compacting of paving, form upper epidermis.As Fig. 6
(5) 10 ~ 30 millimeters of high-strength graphite plates in the upper epidermis A powder upper cover of completing.
(6) repeating step (2) (3) (4) (5), until install mould.
(7) mould that installs is moved in hot-pressed sintering furnace, under vacuum environment (or nitrogen, argon shield), 1600 ~ 1900 ℃ of sintering temperatures, under pressure 20 ~ 30MPa, heat-insulation pressure keeping sintering is 1 ~ 4 hour, burns till densification product.
(8) heat-insulation pressure keeping finishes, after (draught of take is less than 0.2mm/10min and completes condition as differentiating sintering), to close heating power supply, product furnace cooling.
(9) after completely cooling in stove, hot pressing die is taken out in blow-on, takes mould apart and takes out the base substrate sintering, and then grinds, the processing such as brill, tapping, finally makes Sandwich biscuit type graphite/titanium diboride combined electrode.
The invention has the advantages that:
(1) this electrode adopts TiB2/graphite powder mix lamination paving powder in hot pressing die of different proportionings, then utilize high temperature hot pressing sintering make outside high TiB2 content, high hard, high conductivity, with the top layer of aluminium liquid high wettability, inner lower TiB2 content, the central core that material is softer, workability is good.
(2) product performance are good, and technique is simple, have significant economic and social benefit.
Accompanying drawing explanation
Fig. 1 and Fig. 2 are two kinds of different graphite/titanium diboride electrodes that the present invention makes.
Fig. 3 is the schematic diagram on the lower top layer of paving.
Fig. 4 and Fig. 5 are the schematic diagram of two kinds of different methods paving central cores.
Fig. 6 is the schematic diagram of spreading top layer.
Note: in figure, 1 is hot pressing die push-down head, the 2nd, hot pressing die former, the 3rd, lower top layer A powder, the 4th, central core B powder, the 5th, U-shaped dividing plate, the 6th, central core A powder, the 7th, upper epidermis A powder.
Embodiment
(1) titanium diboride powder is evenly mixed in proportion with crystalline flake graphite powder, a kind of TiB2 content below claims A powder at 85%(), another kind of TiB2 content 70%(below claims B powder).
(2) in hot pressing die, first pack A powder into, opened up even paving, compacting, forms lower top layer.
(3) on the A powder compacted lift of having completed, cover a certain amount of B powder again, opened up equally even paving, note not destroying the lower top layer A bisque of having completed, compacting, forms central core (or claiming sandwich layer).
(4) on the central core of completing, re-lay A powder, open up the even compacting of paving, form upper epidermis.
(5) 10 millimeters of high-strength graphite plates in the upper epidermis A powder upper cover of completing.
(6) repeating step (2) (3) (4) (5), until install mould.
(7) mould that installs is moved in hot-pressed sintering furnace, under vacuum environment (or nitrogen, argon shield), 1600 ℃ of sintering temperatures, under pressure 20MPa, heat-insulation pressure keeping sintering is 1 hour, burns till densification product.
(8) heat-insulation pressure keeping finishes, after (draught of take is less than 0.2mm/10min and completes condition as differentiating sintering), to close heating power supply, product furnace cooling.
(9) after completely cooling in stove, hot pressing die is taken out in blow-on, takes mould apart and takes out the base substrate sintering, and then grinds, the processing such as brill, tapping, finally makes Sandwich biscuit type graphite/titanium diboride combined electrode.
(1) titanium diboride powder is evenly mixed in proportion with crystalline flake graphite powder, a kind of TiB2 content below claims A powder at 99%(), another kind of TiB2 content 78%(below claims B powder).
(2) in hot pressing die, first pack A powder into, opened up even paving, compacting, forms lower top layer.
(3) on the A powder compacted lift of having completed, cover a certain amount of B powder again, opened up equally even paving, note not destroying the lower top layer A bisque of having completed, compacting, forms central core (or claiming sandwich layer).
(4) on the central core of completing, re-lay A powder, open up the even compacting of paving, form upper epidermis.
(5) 30 millimeters of high-strength graphite plates in the upper epidermis A powder upper cover of completing.
(6) repeating step (2) (3) (4) (5), until install mould.
(7) mould that installs is moved in hot-pressed sintering furnace, under vacuum environment (or nitrogen, argon shield), 1900 ℃ of sintering temperatures, under pressure 30MPa, heat-insulation pressure keeping sintering is 4 hours, burns till densification product.
(8) heat-insulation pressure keeping finishes, after (draught of take is less than 0.2mm/10min and completes condition as differentiating sintering), to close heating power supply, product furnace cooling.
(9) after completely cooling in stove, hot pressing die is taken out in blow-on, takes mould apart and takes out the base substrate sintering, and then grinds, the processing such as brill, tapping, finally makes Sandwich biscuit type graphite/titanium diboride combined electrode.
(1) titanium diboride powder is evenly mixed in proportion with crystalline flake graphite powder, a kind of TiB2 content below claims A powder at 92%(), another kind of TiB2 content 75%(below claims B powder).
(2) in hot pressing die, first pack A powder into, opened up even paving, compacting, forms lower top layer.
(3) on the A powder compacted lift of having completed, cover a certain amount of B powder again, opened up equally even paving, note not destroying the lower top layer A bisque of having completed, compacting, forms central core (or claiming sandwich layer).
(4) on the central core of completing, re-lay A powder, open up the even compacting of paving, form upper epidermis.
(5) 20 millimeters of high-strength graphite plates in the upper epidermis A powder upper cover of completing.
(6) repeating step (2) (3) (4) (5), until install mould.
(7) mould that installs is moved in hot-pressed sintering furnace, under vacuum environment (or nitrogen, argon shield), 1750 ℃ of sintering temperatures, under pressure 25MPa, heat-insulation pressure keeping sintering is 2.5 hours, burns till densification product.
(8) heat-insulation pressure keeping finishes, after (draught of take is less than 0.2mm/10min and completes condition as differentiating sintering), to close heating power supply, product furnace cooling.
(9) after completely cooling in stove, hot pressing die is taken out in blow-on, takes mould apart and takes out the base substrate sintering, and then grinds, the processing such as brill, tapping, finally makes Sandwich biscuit type graphite/titanium diboride combined electrode.
(1) titanium diboride powder is evenly mixed in proportion with crystalline flake graphite powder, a kind of TiB2 content below claims A powder at 90%(), another kind of TiB2 content 70%(below claims B powder).
(2) in hot pressing die, first pack A powder into, opened up even paving, compacting, forms lower top layer.
(3) first on the A of the lower floor powder of compacting, put a U-shaped division board (making with the thin slice of sheet iron or other materials) completing, make the opening of U-shaped division board be close to the sidewall of hot pressing die, then the interior space-filling B powder forming at U-shaped plate, in the space forming, fill A powder between U-shaped plate and hot pressing die sidewall, as even the paving of preceding method exhibition, and make two kinds of powder be laid to same thickness; Then carefully take out from the bottom up U-shaped plate, make A, two kinds of powder of B be connected to form the sandwich layer of sandwich biscuit, then appropriate compacting (not destroying the distribution situation of A, B powder).
(4) on the central core of completing, re-lay A powder, open up the even compacting of paving, form upper epidermis.
(5) 20 millimeters of high-strength graphite plates in the upper epidermis A powder upper cover of completing.
(6) repeating step (2) (3) (4) (5), until install mould.
(7) mould that installs is moved in hot-pressed sintering furnace, under vacuum environment (or nitrogen, argon shield), 1800 ℃ of sintering temperatures, under pressure 25MPa, heat-insulation pressure keeping sintering is 3 hours, burns till densification product.
(8) heat-insulation pressure keeping finishes, after (draught of take is less than 0.2mm/10min and completes condition as differentiating sintering), to close heating power supply, product furnace cooling.
(9) after completely cooling in stove, hot pressing die is taken out in blow-on, takes mould apart and takes out the base substrate sintering, and then grinds, the processing such as brill, tapping, finally makes Sandwich biscuit type graphite/titanium diboride combined electrode.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. a manufacture method for Sandwich biscuit type graphite/titanium diboride electrode, is characterized in that: top layer and central core adopt the graphite/titanium diboride matrix material of different ratios of raw materials;
Top layer comprises upper and lower two surfaces; Central core comprises at least one side;
The TiB2 content on top layer is 80% ~ 99%, and sintered density is 95% ~ 99%; The TiB2 content of central core is at 70%-78%, and sintered density is 85% ~ 99%;
The concrete steps of manufacture method are as follows:
(1) titanium diboride powder is evenly mixed in proportion with crystalline flake graphite powder, a kind of TiB2 content, 85 ~ 99%, is called A powder, and another kind of TiB2 content, at 70-78%, is called B powder;
(2) in hot pressing die, first pack A powder into, opened up even paving, compacting, forms lower top layer;
(3) on the A powder compacted lift of having completed, cover a certain amount of B powder again, opened up equally even paving, note not destroying the lower top layer A bisque of having completed, compacting, forms central core;
Or first on the A of the lower floor powder of compacting, put a U-shaped division board made from sheet iron completing, make the opening of U-shaped division board be close to the sidewall of hot pressing die, then the interior space-filling B powder forming at U-shaped plate, in the space forming, fill A powder between U-shaped plate and hot pressing die sidewall, open up even paving, and make two kinds of powder be laid to same thickness; Then carefully take out from the bottom up U-shaped plate, make A, two kinds of powder of B be connected to form the central core of sandwich biscuit, then at appropriate compacting;
(4) on the central core of completing, re-lay A powder, open up the even compacting of paving, form upper epidermis;
(5) 10 ~ 30 millimeters of high-strength graphite plates in the upper epidermis A powder upper cover of completing;
(6) repeating step (2) (3) (4) (5), until install mould;
(7) mould that installs is moved in hot-pressed sintering furnace, in vacuum environment, or under nitrogen, argon shield, 1600 ~ 1900 ℃ of sintering temperatures, under pressure 20 ~ 30MPa, heat-insulation pressure keeping sintering is 1 ~ 4 hour, burns till densification product;
(8) after heat-insulation pressure keeping finishes, close heating power supply, product furnace cooling;
(9) after completely cooling in stove, hot pressing die is taken out in blow-on, takes mould apart and takes out the base substrate sintering, and then grinds, brill, tapping processing, finally makes Sandwich biscuit type graphite/titanium diboride electrode.
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