CN107052569A - A kind of preparation method of high-activity nano thermite - Google Patents
A kind of preparation method of high-activity nano thermite Download PDFInfo
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- CN107052569A CN107052569A CN201710132841.1A CN201710132841A CN107052569A CN 107052569 A CN107052569 A CN 107052569A CN 201710132841 A CN201710132841 A CN 201710132841A CN 107052569 A CN107052569 A CN 107052569A
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- aluminium
- thermite
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- ball milling
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K23/00—Alumino-thermic welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The present invention relates to a kind of preparation method of high-activity nano thermite, belong to thermite technical field.The present invention is relatively low for the thermal efficiency that conventional thermite is produced at present, it is also easy to produce welded rate low, the problem of shrinkage cavity, base-material is used as using aluminium chloride and aluminium powder the invention provides one kind, disperseed by being put into after ball milling in isopropanol, reacted using tri-butyl aluminum with aluminium isopropoxide, it is aided with ultrasonic vibration, flow back ageing under acidity regulation, obtain Alumina gel, complexing agent is then used as using ammonium citrate, it is combined with iron ion, it is aided with surfactant to be modified, improve activity, addition platinum ion is used as catalyst, ferrum collosol is obtained by ultrasonic vibration and wraps up Alumina gel, it is freeze-dried again, obtain the material that iron containing compoundses wrap up aluminium compound, finally by electrolyzing fused, pass through platinum catalysis, reduce the partial oxidation aluminium of parcel, obtain the high-activity nano thermite of oxidation Fe2O3 doping platinum coated alumina and aluminium.
Description
Technical field
The present invention relates to a kind of preparation method of high-activity nano thermite, belong to thermite technical field.
Background technology
In many welding methods, electric resistance welding（Including spot welding, projection welding）It is considered as most important connection method and is answered
In manufacture for body structure and parts.But, compared with other welding methods, electric resistance welding energy consumption is of a relatively high.Entering
During row aluminium alloy electric welding resistance, because aluminium alloy has higher heat conduction, electric conductivity.Therefore, resistance heat phase is produced under similarity condition
To less, and substantial amounts of welding heat is transmitted to rapidly in metallic matrix and surrounding environment and lost, and phase is needed during welding
The high-quality welding of this kind of material could be realized to higher welding energy effect.In actual welding production, in order to provide foot
Enough resistance heats, the resistance spot welding welding current of the light-alloy thin-slab structure such as aluminium alloy is usually the 3 of identical thickness of slab mild steel
~5 times.Therefore, in order to realize the high-quality welding of the light-alloy light sheet material such as aluminium alloy, it is necessary to the resistance spot welding of powerful
Machine.This can no doubt realize the reliable welding of aluminum alloy materials, but in the manufacturing link of product, but need consumption more
Electric energy.This undoubtedly increases energy resource consumption, adds the energy cost in production.
Conventional thermite is generally made up of aluminium powder and brown iron oxide, in the exothermic welding for being mainly used in the materials such as steel.For
Thermite is used for point of resistance, projection welding aluminum alloy materials, reduction power consumption is played, the effect of welding efficiency is improved, before
Literature various in and have no relevant report.Conventional thermite is used for point of resistance, projection welding aluminum alloy materials, due to resistance heat
Instantaneous, heat point source characteristic, the thermal efficiency for producing conventional thermite is relatively low, it is difficult to play the larger efficiency of thermite, easily
The defects such as the low, shrinkage cavity of welded rate are produced, so that it is poor applied to resistance welding aluminium alloy effect.
The content of the invention
The technical problems to be solved by the invention：The thermal efficiency produced for current conventional thermite is relatively low, is also easy to produce weldering
Conjunction rate is low, shrinkage cavity the problem of, the invention provides one kind using aluminium chloride and aluminium powder as base-material, by being put into isopropanol after ball milling
It is middle to be disperseed, reacted using tri-butyl aluminum with aluminium isopropoxide, be aided with ultrasonic vibration, flow back ageing under acidity regulation,
Alumina gel is obtained, then using ammonium citrate as complexing agent, is combined with iron ion, is aided with surfactant and is modified,
Activity is improved, addition platinum ion obtains ferrum collosol as catalyst, by ultrasonic vibration and wraps up Alumina gel, then is freeze-dried, and obtains
The material that iron containing compoundses wrap up aluminium compound is obtained, finally by electrolyzing fused, passes through platinum catalysis, reduces the partial oxidation of parcel
Aluminium, obtains the high-activity nano thermite of oxidation Fe2O3 doping platinum coated alumina and aluminium.Nanometer thermite prepared by the present invention is lived
Property it is high, the thermal efficiency is high, and welded rate is high, no shrinkage cavity phenomenon.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
（1）In mass ratio 1:3, take aluminium chloride and aluminium powder to be put into ball mill, a diameter of 20mm agate is added into ball mill
Ball, is protected using nitrogen, with 300r/min 40~50min of ball milling, ball milling thing is collected, by 7~9 times of ball milling thing and ball milling amount of substance
Isopropanol be put into container and stir, container is heated, 60~70 DEG C are heated to, 20~25min is incubated；
（2）After above-mentioned insulation terminates, tri-butyl aluminum is added dropwise into container with 0.1mL/s, dripping quantity is above-mentioned isopropanol volume
3~5%, then container is placed in ultrasonic oscillation device, setpoint frequency is 1.8~2.2MHz, shakes 30~40min, uses
Mass fraction for 70% salpeter solution regulation pH to 3.0~3.5, container is placed in reflux, design temperature be 60~
65 DEG C, flow back 23~25h；
（3）After above-mentioned backflow terminates, the residue in reflux is filtered, filtrate is collected, counts by weight,
Take 70~80 parts of absolute ethyl alcohols, 30~35 portions of ferric nitrates, 20~25 portions of filtrates, 12~16 portions of expoxy propane, 3~5 portions of lemons
Sour ammonium, 1~3 part of sucrose fatty ester and 0.9~1.2 part of platinum nitrate, first by absolute ethyl alcohol, ferric nitrate, ammonium citrate, sucrose
Fatty acid ester and platinum nitrate are put into glass container, and 10~15min is stirred with 160r/min；
（4）After above-mentioned stirring terminates, the filtrate and expoxy propane in above-mentioned parts by weight are put into glass container, then will
Glass container is placed in ultrasonic oscillation device, at 26~29 DEG C, is vibrated with 2.1~2.4MHz after 30~35min, glass is held
Device is placed in 2~3h of standing in 10~15 DEG C of refrigerating chambers, and then the mixture in glass container is put into vacuum freeze drier,
Design temperature -50~-45 DEG C, vacuum is 11~12Pa, is freeze-dried 2~3h；
（5）Above-mentioned dried object is put into electric smelting furnace, design temperature is 900~1100 DEG C, melts 3~5min, collects melting
Thing, you can obtain high-activity nano thermite.
The application process of the present invention：When carrying out electric resistance welding, setting electric current is 1.4 × 104~2.1 × 104A, then add this
The high-activity nano thermite prepared is invented, material is welded, weld interval is 0.12~0.15s, and welding material is examined
Measure, the solder joint tensile-sbear strength of the more traditional thermite of solder joint tensile-sbear strength improves 2~3 times, and firing temperature is 369~392K,
The thermal efficiency improves 1~3 times.
The present invention is compared with other method, and advantageous effects are：
（1）Nanometer thermite activity prepared by the present invention is high, and the thermal efficiency is high, and welded rate is high, no shrinkage cavity phenomenon；
（2）Nanometer thermite prepared by the present invention makes up the deficiency of welding kesistance heat, so that under relatively small welding current
Welding is that can obtain relatively bigger Joint Strength, efficient energy-saving.
Embodiment
In mass ratio 1:3, take aluminium chloride and aluminium powder to be put into ball mill, a diameter of 20mm agate is added into ball mill
Ball, is protected using nitrogen, with 300r/min 40~50min of ball milling, ball milling thing is collected, by 7~9 times of ball milling thing and ball milling amount of substance
Isopropanol be put into container and stir, container is heated, 60~70 DEG C are heated to, 20~25min is incubated；Above-mentioned
After insulation terminates, tri-butyl aluminum is added dropwise into container with 0.1mL/s, dripping quantity is the 3~5% of above-mentioned isopropanol volume, then will
Container is placed in ultrasonic oscillation device, and setpoint frequency is 1.8~2.2MHz, shakes 30~40min, and use quality fraction is 70%
Salpeter solution regulation pH to 3.0~3.5, container is placed in reflux, design temperature be 60~65 DEG C, backflow 23~
25h；
After above-mentioned backflow terminates, the residue in reflux is filtered, filtrate is collected, counts, take by weight
70~80 parts of absolute ethyl alcohols, 30~35 parts of ferric nitrates, 20~25 parts of filtrates, 12~16 parts of expoxy propane, 3~5 parts of citric acids
Ammonium, 1~3 part of sucrose fatty ester and 0.9~1.2 part of platinum nitrate, first by absolute ethyl alcohol, ferric nitrate, ammonium citrate, Sucrose Fatty Acid Ester
Fat acid esters and platinum nitrate are put into glass container, and 10~15min is stirred with 160r/min；, will be above-mentioned after above-mentioned stirring terminates
Filtrate and expoxy propane in parts by weight are put into glass container, then glass container is placed in ultrasonic oscillation device,
At 26~29 DEG C, with 2.1~2.4MHz vibrate 30~35min after, glass container be placed in 10~15 DEG C of refrigerating chambers stand 2~
3h, is then put into vacuum freeze drier, design temperature -50~-45 DEG C to the mixture in glass container, and vacuum is 11
~12Pa, is freeze-dried 2~3h；Above-mentioned dried object is put into electric smelting furnace, design temperature is 900~1100 DEG C, melting 3~
5min, collects fused mass, you can obtain high-activity nano thermite.
Example 1
In mass ratio 1:3, take aluminium chloride and aluminium powder to be put into ball mill, a diameter of 20mm agate ball is added into ball mill,
Protected using nitrogen, with 300r/min ball milling 40min, collect ball milling thing, 7 times of isopropanol of ball milling thing and ball milling amount of substance is put
Enter in container and stir, container is heated, be heated to 60 DEG C, be incubated 20min；After above-mentioned insulation terminates, with
Tri-butyl aluminum is added dropwise into container by 0.1mL/s, and dripping quantity is the 3% of above-mentioned isopropanol volume, then container is placed in into ultrasonic wave shake
Swing in device, setpoint frequency is 1.8MHz, shake 30min, use quality fraction is 70% salpeter solution regulation pH to 3.0, will
Container is placed in reflux, and design temperature is 60 DEG C, and flow back 23h；After above-mentioned backflow terminates, to the residue in reflux
Thing is filtered, and is collected filtrate, is counted by weight, take 70 parts of absolute ethyl alcohols, 30 parts of ferric nitrates, 20 parts of filtrates, 12 parts
Expoxy propane, 3 parts of ammonium citrates, 1 part of sucrose fatty ester and 0.9 part of platinum nitrate, first by absolute ethyl alcohol, ferric nitrate, lemon
Sour ammonium, sucrose fatty ester and platinum nitrate are put into glass container, and 10min is stirred with 160r/min；After above-mentioned stirring terminates,
Filtrate and expoxy propane in above-mentioned parts by weight is put into glass container, then glass container is placed in ultrasonic oscillation device
In, at 26 DEG C, after 2.1MHz vibrations 30min, glass container is placed in 10 DEG C of refrigerating chambers and stands 2h, then glass is held
Mixture in device is put into vacuum freeze drier, and -50 DEG C of design temperature, vacuum is 11Pa, is freeze-dried 2h；Will be above-mentioned
Dried object is put into electric smelting furnace, and design temperature is 900 DEG C, melts 3min, collects fused mass, you can obtain high-activity nano aluminothermy
Agent.
The application process of the present invention：When carrying out electric resistance welding, setting electric current is 1.4 × 104A, then add preparation of the present invention
High-activity nano thermite, material is welded, weld interval is 0.12s, welding material tests is obtained, solder joint, which is drawn, cuts strong
The solder joint tensile-sbear strength of the more traditional thermite of degree improves 2 times, and firing temperature is 369K, and the thermal efficiency improves 1 times.
Example 2
In mass ratio 1:3, take aluminium chloride and aluminium powder to be put into ball mill, a diameter of 20mm agate ball is added into ball mill,
Protected using nitrogen, with 300r/min ball milling 50min, collect ball milling thing, 9 times of isopropanol of ball milling thing and ball milling amount of substance is put
Enter in container and stir, container is heated, be heated to 70 DEG C, be incubated 25min；After above-mentioned insulation terminates, with
Tri-butyl aluminum is added dropwise into container by 0.1mL/s, and dripping quantity is the 5% of above-mentioned isopropanol volume, then container is placed in into ultrasonic wave shake
Swing in device, setpoint frequency is 2.2MHz, shake 40min, use quality fraction is 70% salpeter solution regulation pH to 3.5, will
Container is placed in reflux, and design temperature is 65 DEG C, and flow back 25h；After above-mentioned backflow terminates, to the residue in reflux
Thing is filtered, and is collected filtrate, is counted by weight, take 80 parts of absolute ethyl alcohols, 35 parts of ferric nitrates, 25 parts of filtrates, 16 parts
Expoxy propane, 5 parts of ammonium citrates, 3 parts of sucrose fatty esters and 1.2 parts of platinum nitrates, first by absolute ethyl alcohol, ferric nitrate, lemon
Sour ammonium, sucrose fatty ester and platinum nitrate are put into glass container, and 15min is stirred with 160r/min；After above-mentioned stirring terminates,
Filtrate and expoxy propane in above-mentioned parts by weight is put into glass container, then glass container is placed in ultrasonic oscillation device
In, at 29 DEG C, after 2.4MHz vibrations 35min, glass container is placed in 15 DEG C of refrigerating chambers and stands 3h, then glass is held
Mixture in device is put into vacuum freeze drier, and -45 DEG C of design temperature, vacuum is 12Pa, is freeze-dried 3h；Will be above-mentioned
Dried object is put into electric smelting furnace, and design temperature is 1100 DEG C, melts 5min, collects fused mass, you can obtain high-activity nano aluminium
Thermit powder.
The application process of the present invention：When carrying out electric resistance welding, setting electric current is 2.1 × 104A, then add preparation of the present invention
High-activity nano thermite, material is welded, weld interval is 0.15s, welding material tests is obtained, solder joint, which is drawn, cuts strong
The solder joint tensile-sbear strength of the more traditional thermite of degree improves 3 times, and firing temperature is 392K, and the thermal efficiency improves 3 times.
Example 3
In mass ratio 1:3, take aluminium chloride and aluminium powder to be put into ball mill, a diameter of 20mm agate ball is added into ball mill,
Protected using nitrogen, with 300r/min ball milling 45min, collect ball milling thing, 8 times of isopropanol of ball milling thing and ball milling amount of substance is put
Enter in container and stir, container is heated, be heated to 65 DEG C, be incubated 23min；After above-mentioned insulation terminates, with
Tri-butyl aluminum is added dropwise into container by 0.1mL/s, and dripping quantity is the 4% of above-mentioned isopropanol volume, then container is placed in into ultrasonic wave shake
Swing in device, setpoint frequency is 3.0MHz, shake 35min, use quality fraction is 70% salpeter solution regulation pH to 3.3, will
Container is placed in reflux, and design temperature is 63 DEG C, and flow back 24h；After above-mentioned backflow terminates, to the residue in reflux
Thing is filtered, and is collected filtrate, is counted by weight, take 75 parts of absolute ethyl alcohols, 33 parts of ferric nitrates, 23 parts of filtrates, 15 parts
Expoxy propane, 4 parts of ammonium citrates, 2 parts of sucrose fatty esters and 1.1 parts of platinum nitrates, first by absolute ethyl alcohol, ferric nitrate, lemon
Sour ammonium, sucrose fatty ester and platinum nitrate are put into glass container, and 13min is stirred with 160r/min；After above-mentioned stirring terminates,
Filtrate and expoxy propane in above-mentioned parts by weight is put into glass container, then glass container is placed in ultrasonic oscillation device
In, at 27 DEG C, after 2.3MHz vibrations 33min, glass container is placed in 13 DEG C of refrigerating chambers and stands 2h, then glass is held
Mixture in device is put into vacuum freeze drier, and -48 DEG C of design temperature, vacuum is 11Pa, is freeze-dried 2h；Will be above-mentioned
Dried object is put into electric smelting furnace, and design temperature is 1000 DEG C, melts 4min, collects fused mass, you can obtain high-activity nano aluminium
Thermit powder.
The application process of the present invention：When carrying out electric resistance welding, setting electric current is 1.8 × 104A, then add preparation of the present invention
High-activity nano thermite, material is welded, weld interval is 0.14s, welding material tests is obtained, solder joint, which is drawn, cuts strong
The solder joint tensile-sbear strength of the more traditional thermite of degree improves 3 times, and firing temperature is 373K, and the thermal efficiency improves 2 times.
Claims (1)
1. a kind of preparation method of high-activity nano thermite, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:3, take aluminium chloride and aluminium powder to be put into ball mill, a diameter of 20mm agate is added into ball mill
Ball, is protected using nitrogen, with 300r/min 40~50min of ball milling, ball milling thing is collected, by 7~9 times of ball milling thing and ball milling amount of substance
Isopropanol be put into container and stir, container is heated, 60~70 DEG C are heated to, 20~25min is incubated；
（2）After above-mentioned insulation terminates, tri-butyl aluminum is added dropwise into container with 0.1mL/s, dripping quantity is above-mentioned isopropanol volume
3~5%, then container is placed in ultrasonic oscillation device, setpoint frequency is 1.8~2.2MHz, shakes 30~40min, uses
Mass fraction for 70% salpeter solution regulation pH to 3.0~3.5, container is placed in reflux, design temperature be 60~
65 DEG C, flow back 23~25h；
（3）After above-mentioned backflow terminates, the residue in reflux is filtered, filtrate is collected, counts by weight,
Take 70~80 parts of absolute ethyl alcohols, 30~35 portions of ferric nitrates, 20~25 portions of filtrates, 12~16 portions of expoxy propane, 3~5 portions of lemons
Sour ammonium, 1~3 part of sucrose fatty ester and 0.9~1.2 part of platinum nitrate, first by absolute ethyl alcohol, ferric nitrate, ammonium citrate, sucrose
Fatty acid ester and platinum nitrate are put into glass container, and 10~15min is stirred with 160r/min；
（4）After above-mentioned stirring terminates, the filtrate and expoxy propane in above-mentioned parts by weight are put into glass container, then will
Glass container is placed in ultrasonic oscillation device, at 26~29 DEG C, is vibrated with 2.1~2.4MHz after 30~35min, glass is held
Device is placed in 2~3h of standing in 10~15 DEG C of refrigerating chambers, and then the mixture in glass container is put into vacuum freeze drier,
Design temperature -50~-45 DEG C, vacuum is 11~12Pa, is freeze-dried 2~3h；
（5）Above-mentioned dried object is put into electric smelting furnace, design temperature is 900~1100 DEG C, melts 3~5min, collects melting
Thing, you can obtain high-activity nano thermite.
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| CN201710132841.1A CN107052569B (en) | 2017-03-08 | 2017-03-08 | A kind of preparation method of high-activity nano thermite |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3890168A (en) * | 1970-09-21 | 1975-06-17 | Harold A Shumway | Exothermic welding composition |
| CN102248280A (en) * | 2011-06-24 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | Thermit reaction foil, manufacturing method thereof and application thereof to welding process |
| CN102848101A (en) * | 2012-10-16 | 2013-01-02 | 重庆理工大学 | Bi-component powder thermit for resistance welding of aluminum alloy |
| CN104923982A (en) * | 2015-06-23 | 2015-09-23 | 青岛克立克信息技术有限公司 | Novel hot-melting welding material |
| CN106141499A (en) * | 2016-08-05 | 2016-11-23 | 雷春生 | A kind of grounding grid heat release welding preparation method of ultra-fine welding powder |
-
2017
- 2017-03-08 CN CN201710132841.1A patent/CN107052569B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3890168A (en) * | 1970-09-21 | 1975-06-17 | Harold A Shumway | Exothermic welding composition |
| CN102248280A (en) * | 2011-06-24 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | Thermit reaction foil, manufacturing method thereof and application thereof to welding process |
| CN102848101A (en) * | 2012-10-16 | 2013-01-02 | 重庆理工大学 | Bi-component powder thermit for resistance welding of aluminum alloy |
| CN104923982A (en) * | 2015-06-23 | 2015-09-23 | 青岛克立克信息技术有限公司 | Novel hot-melting welding material |
| CN106141499A (en) * | 2016-08-05 | 2016-11-23 | 雷春生 | A kind of grounding grid heat release welding preparation method of ultra-fine welding powder |
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Effective date of registration: 20201229 Address after: No.168, Changjiang Road, Donghu street, Pizhou City, Xuzhou City, Jiangsu Province Patentee after: Liu Ronghua Address before: Room 7088-7, 7 / F, 1558 Jiangnan Road, Ningbo hi tech Zone, Ningbo City, Zhejiang Province Patentee before: Ningbo Hi-tech Zone Yuanchuang Technology Co.,Ltd. |