CN108149072A - A kind of zinc foil material and preparation process - Google Patents

A kind of zinc foil material and preparation process Download PDF

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Publication number
CN108149072A
CN108149072A CN201810110503.2A CN201810110503A CN108149072A CN 108149072 A CN108149072 A CN 108149072A CN 201810110503 A CN201810110503 A CN 201810110503A CN 108149072 A CN108149072 A CN 108149072A
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pure
zinc
tin
magnesium
manganese chloride
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不公告发明人
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NANTONG XINXIANG ZINC INDUSTRY Co Ltd
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NANTONG XINXIANG ZINC INDUSTRY Co Ltd
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Priority to CN201810110503.2A priority Critical patent/CN108149072A/en
Publication of CN108149072A publication Critical patent/CN108149072A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C18/00Alloys based on zinc
    • C22C18/04Alloys based on zinc with aluminium as the next major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21BROLLING OF METAL
    • B21B1/00Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/40Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/06Making non-ferrous alloys with the use of special agents for refining or deoxidising

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of zinc foil material and preparation processes, include the raw material of following parts by weight:Pure zinc, aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier;Its preparation flow is:Stock, melting:Pure zinc is added in by being preheated in 600 800 DEG C of smelting furnace, after stirring evenly, smelting furnace is warming up to 1,200 1300 DEG C, sequentially adding aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier, after stirring to complete melt, 20 30min are stood, zinc alloy solution, injection molding, hot-forming and cooling storage is made;The present invention in zinc by adding a certain amount of aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier, effectively increase the intensity and corrosion resistance of kirsite, the quality of zinc foil after molding is effectively ensured, while shaping efficiency is high, it is suitable for large-scale promotion.

Description

A kind of zinc foil material and preparation process
Technical field
The present invention relates to zinc foil field shaping technique, specially a kind of zinc foil material and preparation process.
Background technology
The characteristics of purposes of foil is very extensive, this is foliation metal and foil feature itself determine.Such as steel and conjunction Goldleaf is mainly used for the departments such as electronics, aerospace, instrument and meter;Fe-Ni soft magnetic alloy foil is used to make novel high-frequency pulse The iron core of transformer, switch coil, magnetic recorder, magnetic amplifier etc.;Titanium alloy foil is used to make jet engine combustion tube Decorations net, the composite thermal protection tile in space shuttle heat-protection system and titanium compound wall;The foils such as tungsten are used for special electron tube And heater element;Cupro-nickel and Jellif foil are used to make between dynamometry foil gauge, precision resistance and video and audio recording magnetic head Feeler;Stainless steel foil is used to make in precision instrument the partition on highly sensitive pressure elements, main in steam turbine engines Structural material and heat exchange material etc..Aluminium foil, lead foil, copper foil and constantan foil purposes see aluminium foil production, lead foil production, cathode copper Foil produces and the production of constantan foil.Pure zinc is more crisp, at 100~150 DEG C, softens, after 200 DEG C, and becomes fragile, is not suitable for system Into zinc foil.
So how to design a kind of zinc foil material and preparation process, becoming us will currently solve the problems, such as.
Invention content
It is mentioned above in the background art to solve the purpose of the present invention is to provide a kind of zinc foil material and preparation process Problem.
To achieve the above object, the present invention provides following technical solution:A kind of zinc foil material includes the original of following parts by weight Material:Pure zinc 75.0-83.0 parts, 13.4-16.5 parts of aluminium, 2.3-4.3 parts of copper, magnesium 1.9-3.6 parts pure, 0.01-0.03 parts of pure tin, chlorine Change 0.2-0.6 parts of manganese, pure boron 0.03-0.08 parts and 0.13-0.34 parts of composite modifier.
According to above-mentioned technical proposal, the preparation method of the pure magnesium for first by the φ 300 being placed in black-fead crucible × Three layers every layer 5 pieces of 130mm magnesium ingots point are placed in vacuum distilling apparatus, and one block of aluminium sheet is placed above in every layer of magnesium ingot;Then vacuum is steamed Device is evaporated to be put into vacuum distillation furnace;Then by between vacuum distilling apparatus and condenser between vacuum distilling apparatus and vacuum distillation furnace It vacuumizes;Again to stove heat being evaporated in vacuo 2 hours, the heating temperature of epimere is 650 DEG C, and the heating temperature of hypomere is 660 DEG C;It connects It in the cyclic annular water jacket above the ring-shaped water jacket of condenser and the sealing rubber ring of vacuum distilling apparatus and is passed through cooling water circulation, make Magnesium steam condenses 3 hours on condenser;Finally stop vacuumizing, and be filled with argon gas into vacuum distilling apparatus, it is cold to release vacuum But after, the pure magnesium that vacuum distilling apparatus takes out condensation is opened.
According to above-mentioned technical proposal, the preparation method of the pure tin for first by granulated metal tin with through distilled water wash bottle and The chlorine reaction of concentrated sulfuric acid wash bottle generates butter of tin;Obtained butter of tin is then added in the tin of 1-2% weight, is filtered, Supernatant liquor is taken, is fractionated in oil bath, intercepts boiling temperature 114 DEG C of distillates of steady component, adds in the 4-5% of distillate weight Pure ammonium oxalate is analyzed to stay overnight;Distillate will be obtained again and is passed through ammonia, be obtained stannic hydroxide precipitation, be washed with distilled water 2-3 times, clear liquid It pours out, obtains precipitation stannic hydroxide, drying;Stannic hydroxide will be finally obtained, moves to quartz boat, quartz boat is put into quartz ampoule In, with hydrogen reducing, temperature slowly heats 100-120 DEG C, time 30-40 minute, heats 150-170 DEG C, constant temperature, time 1- 1.5 hours, 400-450 DEG C is heated, constant temperature, time 1-1.2 hour heats 570-600 DEG C, and heating time 2-3 hour stops adding Heat, cooling, taking-up obtain high purity tin.
According to above-mentioned technical proposal, the preparation method of the manganese chloride is obtained first to react manganese powder with hydrochloric acid Manganese chloride solution;Then hydrogen peroxide is added in manganese chloride solution and carries out oxidation reaction, oxidation reaction terminal pH is controlled in 4-5.5 In the range of, solid-liquor separation I obtains liquid phase I and iron hydroxide impurity, and sulfide precipitation agent is added in liquid phase I, precipitate anti- Should, solid-liquor separation II obtains liquid phase II and metal sulfide impurity, and it is molten to get removal of impurities manganese chloride that liquid phase II is adjusted pH to 4-5 Liquid;Finally removal of impurities manganese chloride solution is spray-dried, dry obtained solid is dissolved using alcohols solvent, filtering, gained filter Liquid is dried using spray drying-vacuum rotating tray drying group technology, obtains manganese chloride powder.
According to above-mentioned technical proposal, the preparation method of the pure boron is to mix thick boron by 1: 2-3 mass ratio with magnesium, into After row ball milling mixing 8-16 hours, mixed material is placed in mold and is compacted under the pressure of 10-60MPa, is put on its surface Up-igniting agent, is then reacted in autoclave, excludes air therein, Deng Daorong with argon gas purging autoclave at room temperature Device temperature is vented again when rising to 180 DEG C, and the argon gas for then passing to 1-6MPa continues increase container temperature;As container Nei Wenduda Start to react to detonator at 260 DEG C or so and release a large amount of heat, so as to the reaction of initiation reaction storeroom, protected in argon gas It cools to room temperature under shield with the furnace and pure boron powder is made.
According to above-mentioned technical proposal, the preparation method of the composite modifier is mixed for ingredient A, B and C are weighed in proportion It closes, adds in graphite crucible, intermediate frequency furnace or resistance stove heat, be warming up to 200-300 DEG C of heat preservation 1-3h, be then warming up to again 300-600 DEG C, 0.5-3h is kept the temperature, is stirred evenly;Cooling obtains composite modifier, the ingredient in injection punching block or graphite crucible One or more combinations of the A in rare earth oxide;The ingredient B is selected from ZrO2And TiO2One or both of combination;Institute It is 1 that ingredient C, which is stated, by weight ratio:(3-5):(4-6):NaF, KCl, the NH of (0.5-1.2)4F and CaCl2The salt-mixture of composition.
A kind of preparation process of zinc foil material, includes the following steps:
1) it stocks up:Each material component is weighed by composition of raw materials ratio, it is spare;
2) melting:Pure zinc is added in by being preheated in 600-800 DEG C of smelting furnace, after stirring evenly, smelting furnace is warming up to 1200- 1300 DEG C, aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier are being sequentially added, is being stirred to complete melt, it is quiet 20-30min is put, zinc alloy solution is made;
3) injection molding:Manufactured zinc alloy solution is injected in metal die, kirsite block is made after cooling and shaping;
4) it is hot-forming:Kirsite block is put into compacting by rolling in duo mill, zinc foil is made;
5) cooling storage:After the cooling of zinc foil will be made, storage.
According to above-mentioned technical proposal, the roller temperature of the duo mill is 90-110 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows:The present invention by added in zinc a certain amount of aluminium, Copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier effectively increase the intensity and corrosion resistance of kirsite, effectively protect The quality of zinc foil after molding is demonstrate,proved, while shaping efficiency is high, it is suitable for large-scale promotion.
Description of the drawings
Fig. 1 is the molding flow diagram of the zinc foil material of the present invention;
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work Embodiment shall fall within the protection scope of the present invention.
Embodiment 1:Referring to Fig. 1, the present invention provides a kind of zinc foil material, include the raw material of following parts by weight:Pure zinc 75.0 parts, 13.4 parts of aluminium, 2.3 parts of copper, 1.9 parts of pure magnesium, 0.01 part of pure tin, 0.2 part of manganese chloride, 0.03 part of pure boron and composite inoculating 0.13 part of agent.
According to above-mentioned technical proposal, the preparation method of pure magnesium is the φ 300 × 130mm magnesium that will be placed in black-fead crucible first Three layers every layer 5 pieces of ingot point is placed in vacuum distilling apparatus, and one block of aluminium sheet is placed above in every layer of magnesium ingot;Then vacuum distilling apparatus is put into In vacuum distillation furnace;Then it will be vacuumized between vacuum distilling apparatus and vacuum distillation furnace between vacuum distilling apparatus and condenser; Again to stove heat being evaporated in vacuo 2 hours, the heating temperature of epimere is 650 DEG C, and the heating temperature of hypomere is 660 DEG C;Then cold Cooling water circulation is passed through in cyclic annular water jacket above the ring-shaped water jacket of condenser and the sealing rubber ring of vacuum distilling apparatus, makes magnesium steam It is condensed 3 hours on condenser;Finally stop vacuumizing, and be filled with argon gas into vacuum distilling apparatus, after releasing vacuum cooled, beat Open the pure magnesium that vacuum distilling apparatus takes out condensation.
According to above-mentioned technical proposal, the preparation method of pure tin is first by granulated metal tin and through distilled water wash bottle and dense sulphur The chlorine reaction of pickling bottle generates butter of tin;Obtained butter of tin is then added in the tin of 1-2% weight, filtering takes Layer clear liquid, is fractionated in oil bath, intercepts boiling temperature 114 DEG C of distillates of steady component, adds in the 4-5% analyses of distillate weight Pure ammonium oxalate is stayed overnight;Distillate will be obtained again and is passed through ammonia, be obtained stannic hydroxide precipitation, be washed with distilled water 2-3 times, clear liquid falls Go out, obtain precipitation stannic hydroxide, drying;Stannic hydroxide will be finally obtained, moves to quartz boat, quartz boat will be put into quartz ampoule, With hydrogen reducing, temperature slowly heats 100-120 DEG C, and time 30-40 minute heats 150-170 DEG C, and constant temperature, the time, 1-1.5 was small When, 400-450 DEG C is heated, constant temperature, time 1-1.2 hour heats 570-600 DEG C, and heating time 2-3 hour stops heating, cold But, it takes out and obtains high purity tin.
According to above-mentioned technical proposal, the preparation method of manganese chloride obtains chlorination first to react manganese powder with hydrochloric acid Manganese solution;Then hydrogen peroxide is added in manganese chloride solution and carries out oxidation reaction, oxidation reaction terminal pH is controlled in 4-5.5 ranges Interior, solid-liquor separation I obtains liquid phase I and iron hydroxide impurity, and sulfide precipitation agent is added in liquid phase I, carries out precipitation reaction, liquid Admittedly detaching II, liquid phase II and metal sulfide impurity are obtained, liquid phase II is adjusted into pH to 4-5 to get removal of impurities manganese chloride solution;Most Removal of impurities manganese chloride solution is spray-dried afterwards, dry obtained solid is dissolved using alcohols solvent, and filtering, gained filtrate uses Spray drying-vacuum rotating tray drying group technology is dried, and obtains manganese chloride powder.
According to above-mentioned technical proposal, the preparation method of pure boron carries out ball for thick boron is mixed with magnesium by 1: 2-3 mass ratio After mill mixing 8-16 hours, mixed material is placed in mold and is compacted under the pressure of 10-60MPa, puts and draws on its surface Agent is fired, is then reacted in autoclave, air therein is excluded with argon gas purging autoclave at room temperature, until container temperature Degree is vented again when rising to 180 DEG C, and the argon gas for then passing to 1-6MPa continues increase container temperature;When temperature reaches in container Detonator starts to react and releases a large amount of heat at 260 DEG C or so, so as to the reaction of initiation reaction storeroom, is protected in argon gas Under cool to room temperature with the furnace pure boron powder be made.
According to above-mentioned technical proposal, the preparation method of composite modifier is mixed, is added for ingredient A, B and C are weighed in proportion Enter in graphite crucible, intermediate frequency furnace or resistance stove heat, be warming up to 200-300 DEG C of heat preservation 1-3h, be then warming up to 300- again 600 DEG C, 0.5-3h is kept the temperature, is stirred evenly;Cooling obtains composite modifier in injection punching block or graphite crucible, and ingredient A is selected from dilute One or more combinations in native oxide;Ingredient B is selected from ZrO2And TiO2One or both of combination;Ingredient C is by weight ratio It is 1:(3-5):(4-6):NaF, KCl, the NH of (0.5-1.2)4F and CaCl2The salt-mixture of composition.
A kind of preparation process of zinc foil material, includes the following steps:
1) it stocks up:Each material component is weighed by composition of raw materials ratio, it is spare;
2) melting:Pure zinc is added in by being preheated in 600-800 DEG C of smelting furnace, after stirring evenly, smelting furnace is warming up to 1200- 1300 DEG C, aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier are being sequentially added, is being stirred to complete melt, it is quiet 20-30min is put, zinc alloy solution is made;
3) injection molding:Manufactured zinc alloy solution is injected in metal die, kirsite block is made after cooling and shaping;
4) it is hot-forming:Kirsite block is put into compacting by rolling in duo mill, zinc foil is made;
5) cooling storage:After the cooling of zinc foil will be made, storage.
According to above-mentioned technical proposal, the roller temperature of duo mill is 90-110 DEG C.
Embodiment 2:Referring to Fig. 1, the present invention provides a kind of zinc foil material, include the raw material of following parts by weight:Pure zinc 83.0 parts, 16.5 parts of aluminium, 4.3 parts of copper, 3.6 parts of pure magnesium, 0.03 part of pure tin, 0.6 part of manganese chloride, 0.08 part of pure boron and composite inoculating 0.34 part of agent.
According to above-mentioned technical proposal, the preparation method of pure magnesium is the φ 300 × 130mm magnesium that will be placed in black-fead crucible first Three layers every layer 5 pieces of ingot point is placed in vacuum distilling apparatus, and one block of aluminium sheet is placed above in every layer of magnesium ingot;Then vacuum distilling apparatus is put into In vacuum distillation furnace;Then it will be vacuumized between vacuum distilling apparatus and vacuum distillation furnace between vacuum distilling apparatus and condenser; Again to stove heat being evaporated in vacuo 2 hours, the heating temperature of epimere is 650 DEG C, and the heating temperature of hypomere is 660 DEG C;Then cold Cooling water circulation is passed through in cyclic annular water jacket above the ring-shaped water jacket of condenser and the sealing rubber ring of vacuum distilling apparatus, makes magnesium steam It is condensed 3 hours on condenser;Finally stop vacuumizing, and be filled with argon gas into vacuum distilling apparatus, after releasing vacuum cooled, beat Open the pure magnesium that vacuum distilling apparatus takes out condensation.
According to above-mentioned technical proposal, the preparation method of pure tin is first by granulated metal tin and through distilled water wash bottle and dense sulphur The chlorine reaction of pickling bottle generates butter of tin;Obtained butter of tin is then added in the tin of 1-2% weight, filtering takes Layer clear liquid, is fractionated in oil bath, intercepts boiling temperature 114 DEG C of distillates of steady component, adds in the 4-5% analyses of distillate weight Pure ammonium oxalate is stayed overnight;Distillate will be obtained again and is passed through ammonia, be obtained stannic hydroxide precipitation, be washed with distilled water 2-3 times, clear liquid falls Go out, obtain precipitation stannic hydroxide, drying;Stannic hydroxide will be finally obtained, moves to quartz boat, quartz boat will be put into quartz ampoule, With hydrogen reducing, temperature slowly heats 100-120 DEG C, and time 30-40 minute heats 150-170 DEG C, and constant temperature, the time, 1-1.5 was small When, 400-450 DEG C is heated, constant temperature, time 1-1.2 hour heats 570-600 DEG C, and heating time 2-3 hour stops heating, cold But, it takes out and obtains high purity tin.
According to above-mentioned technical proposal, the preparation method of manganese chloride obtains chlorination first to react manganese powder with hydrochloric acid Manganese solution;Then hydrogen peroxide is added in manganese chloride solution and carries out oxidation reaction, oxidation reaction terminal pH is controlled in 4-5.5 ranges Interior, solid-liquor separation I obtains liquid phase I and iron hydroxide impurity, and sulfide precipitation agent is added in liquid phase I, carries out precipitation reaction, liquid Admittedly detaching II, liquid phase II and metal sulfide impurity are obtained, liquid phase II is adjusted into pH to 4-5 to get removal of impurities manganese chloride solution;Most Removal of impurities manganese chloride solution is spray-dried afterwards, dry obtained solid is dissolved using alcohols solvent, and filtering, gained filtrate uses Spray drying-vacuum rotating tray drying group technology is dried, and obtains manganese chloride powder.
According to above-mentioned technical proposal, the preparation method of pure boron carries out ball for thick boron is mixed with magnesium by 1: 2-3 mass ratio After mill mixing 8-16 hours, mixed material is placed in mold and is compacted under the pressure of 10-60MPa, puts and draws on its surface Agent is fired, is then reacted in autoclave, air therein is excluded with argon gas purging autoclave at room temperature, until container temperature Degree is vented again when rising to 180 DEG C, and the argon gas for then passing to 1-6MPa continues increase container temperature;When temperature reaches in container Detonator starts to react and releases a large amount of heat at 260 DEG C or so, so as to the reaction of initiation reaction storeroom, is protected in argon gas Under cool to room temperature with the furnace pure boron powder be made.
According to above-mentioned technical proposal, the preparation method of composite modifier is mixed, is added for ingredient A, B and C are weighed in proportion Enter in graphite crucible, intermediate frequency furnace or resistance stove heat, be warming up to 200-300 DEG C of heat preservation 1-3h, be then warming up to 300- again 600 DEG C, 0.5-3h is kept the temperature, is stirred evenly;Cooling obtains composite modifier in injection punching block or graphite crucible, and ingredient A is selected from dilute One or more combinations in native oxide;Ingredient B is selected from ZrO2And TiO2One or both of combination;Ingredient C is by weight ratio It is 1:(3-5):(4-6):NaF, KCl, the NH of (0.5-1.2)4F and CaCl2The salt-mixture of composition.
A kind of preparation process of zinc foil material, includes the following steps:
1) it stocks up:Each material component is weighed by composition of raw materials ratio, it is spare;
2) melting:Pure zinc is added in by being preheated in 600-800 DEG C of smelting furnace, after stirring evenly, smelting furnace is warming up to 1200- 1300 DEG C, aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier are being sequentially added, is being stirred to complete melt, it is quiet 20-30min is put, zinc alloy solution is made;
3) injection molding:Manufactured zinc alloy solution is injected in metal die, kirsite block is made after cooling and shaping;
4) it is hot-forming:Kirsite block is put into compacting by rolling in duo mill, zinc foil is made;
5) cooling storage:After the cooling of zinc foil will be made, storage.
According to above-mentioned technical proposal, the roller temperature of duo mill is 90-110 DEG C.
Based on above-mentioned, it is an advantage of the current invention that the present invention in zinc by adding a certain amount of aluminium, copper, pure magnesium, pure Tin, manganese chloride, pure boron and composite modifier effectively increase the intensity and corrosion resistance of kirsite, after molding has been effectively ensured Zinc foil quality, while shaping efficiency is high, suitable for large-scale promotion.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace And modification, the scope of the present invention is defined by the appended.

Claims (8)

1. a kind of zinc foil material, it is characterised in that:Include the raw material of following parts by weight:Pure zinc 75.0-83.0 parts, aluminium 13.4- 16.5 parts, 2.3-4.3 parts of copper, magnesium 1.9-3.6 parts pure, 0.01-0.03 parts of pure tin, 0.2-0.6 parts of manganese chloride, pure boron 0.03- 0.08 part and 0.13-0.34 parts of composite modifier.
2. a kind of zinc foil material according to claim 1, it is characterised in that:The preparation method of the pure magnesium is will be placed on stone first Three layers every layer 5 pieces of 300 × 130mm of φ magnesium ingots point in black crucible are placed in vacuum distilling apparatus, and every layer of magnesium ingot is placed above one piece Aluminium sheet;Then vacuum distilling apparatus is put into vacuum distillation furnace;Then it between vacuum distilling apparatus and condenser and will be evaporated in vacuo It is vacuumized between device and vacuum distillation furnace;Again to stove heat being evaporated in vacuo 2 hours, the heating temperature of epimere is 650 DEG C, hypomere Heating temperature is 660 DEG C;Then the cyclic annular water jacket above the sealing rubber ring of the ring-shaped water jacket of condenser and vacuum distilling apparatus In be passed through cooling water circulation, magnesium steam is made to be condensed on condenser 3 hours;Finally stop vacuumizing, and into vacuum distilling apparatus Argon gas is filled with, after releasing vacuum cooled, opens the pure magnesium that vacuum distilling apparatus takes out condensation.
3. a kind of zinc foil material according to claim 1, it is characterised in that:The preparation method of the pure tin is first by granular gold Belong to tin and the chlorine reaction through distilled water wash bottle and concentrated sulfuric acid wash bottle, generate butter of tin;Then obtained butter of tin is added Enter the tin of 1-2% weight, filter, take supernatant liquor, be fractionated in oil bath, 114 DEG C of interception boiling temperature steady component evaporates Liquid, the pure ammonium oxalate of 4-5% analyses for adding in distillate weight are stayed overnight;Distillate will be obtained again and is passed through ammonia, obtain stannic hydroxide precipitation, It is washed with distilled water 2-3 times, clear liquid is poured out, and obtains precipitation stannic hydroxide, drying;Stannic hydroxide will be finally obtained, moves to quartz Quartz boat is put into quartz ampoule by boat, and with hydrogen reducing, temperature slowly heats 100-120 DEG C, and time 30-40 minute heats 150-170 DEG C, constant temperature, time 1-1.5 hour heats 400-450 DEG C, and constant temperature, time 1-1.2 hour heats 570-600 DEG C, Heating time 2-3 hour, stop heating, cooling, taking-up obtains high purity tin.
4. a kind of zinc foil material according to claim 1, it is characterised in that:The preparation method of the manganese chloride is first by metal Manganese powder is reacted with hydrochloric acid, obtains manganese chloride solution;Then hydrogen peroxide is added in manganese chloride solution and carries out oxidation reaction, oxidation is anti- Answering terminal pH controls, solid-liquor separation I obtains liquid phase I and iron hydroxide impurity, and vulcanization is added in liquid phase I in the range of 4-5.5 Precipitating reagent carries out precipitation reaction, and solid-liquor separation II obtains liquid phase II and metal sulfide impurity, and liquid phase II is adjusted pH to 4- 5 to get removal of impurities manganese chloride solution;Finally removal of impurities manganese chloride solution is spray-dried, dry obtained solid is molten using alcohols Agent is dissolved, and filtering, gained filtrate is dried using spray drying-vacuum rotating tray drying group technology, obtains manganese chloride Powder.
5. a kind of zinc foil material according to claim 1, it is characterised in that:Thick boron is is pressed by the preparation method of the pure boron with magnesium 1: 2-3 mass ratio mixing, carries out ball milling mixing after 8-16 hours, mixed material is placed in mold and with the pressure of 10-60MPa It is compacted under power, puts detonator on its surface, then reacted in autoclave, arranged at room temperature with argon gas purging autoclave It except air therein, is vented again until vessel temp rises to 180 DEG C, the argon gas for then passing to 1-6MPa continues increase container Temperature;Detonator starts to react and releases a large amount of heat when temperature reaches 260 DEG C or so in container, so as to initiation reaction object Reaction between material cools to room temperature with the furnace and pure boron powder is made under protection of argon gas.
6. a kind of zinc foil material according to claim 1, it is characterised in that:The preparation method of the composite modifier is by ingredient A, B and C weigh in proportion, and mixing is added in graphite crucible, and intermediate frequency furnace or resistance stove heat are warming up to 200-300 DEG C of guarantor Then warm 1-3h is warming up to 300-600 DEG C again, keep the temperature 0.5-3h, stir evenly;It cools down and obtains in injection punching block or graphite crucible Composite modifier, one or more combinations of the ingredient A in rare earth oxide;The ingredient B is selected from ZrO2And TiO2In One or two kinds of combinations;The ingredient C is 1 by weight ratio:(3-5):(4-6):NaF, KCl, the NH of (0.5-1.2)4F and CaCl2The salt-mixture of composition.
7. a kind of preparation process of zinc foil material, it is characterised in that:Include the following steps:
1) it stocks up:Each material component is weighed by composition of raw materials ratio, it is spare;
2) melting:Pure zinc is added in by being preheated in 600-800 DEG C of smelting furnace, after stirring evenly, smelting furnace is warming up to 1200-1300 DEG C, aluminium, copper, pure magnesium, pure tin, manganese chloride, pure boron and composite modifier are being sequentially added, is stirring to complete melt, stands 20- Zinc alloy solution is made in 30min;
3) injection molding:Manufactured zinc alloy solution is injected in metal die, kirsite block is made after cooling and shaping;
4) it is hot-forming:Kirsite block is put into compacting by rolling in duo mill, zinc foil is made;
5) cooling storage:After the cooling of zinc foil will be made, storage.
8. a kind of preparation process of zinc foil material according to claim 7, it is characterised in that:The roller temperature of the duo mill It is 90-110 DEG C.
CN201810110503.2A 2018-02-05 2018-02-05 A kind of zinc foil material and preparation process Withdrawn CN108149072A (en)

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CN112222188A (en) * 2020-09-27 2021-01-15 先导薄膜材料(广东)有限公司 Preparation method of high-purity indium foil

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Application publication date: 20180612