CN106216883B - One kind is used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof - Google Patents
One kind is used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof Download PDFInfo
- Publication number
- CN106216883B CN106216883B CN201610570166.6A CN201610570166A CN106216883B CN 106216883 B CN106216883 B CN 106216883B CN 201610570166 A CN201610570166 A CN 201610570166A CN 106216883 B CN106216883 B CN 106216883B
- Authority
- CN
- China
- Prior art keywords
- parts
- stirred tank
- methyl
- retort
- tank retort
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/362—Selection of compositions of fluxes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses one kind to be used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof, is matched and formed in parts by weight by following components：Pure water, C8 aliphatic alcohol polyethenoxies (4) ether, Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate, N methyl (13C) N nitro-p-toluenesulfonamides, 3 nitrophthalimides, 1 hydroxyl 4 (p-totuidine base) anthraquinone, the anthraquinone of 1 amino 2 [4 [(base of 2 oxo 1H azatropylidenes of hexahydro 1) methyl] phenoxy group] 4 hydroxyl 9,10, meta-methoxy phenmethylol, mercury nanoparticle.The invention advantage is：This method can improve weld strength so that welding stress and welding deformation significantly reduce, and process stabilizing, are applicable that wide, cooling is fast, effect is good, the advantages of meeting different welding requirements.
Description
Technical field
It is especially a kind of to be used for that Cu-Mg-Sn-Fe is compound to be received the present invention relates to a kind of laser scaling powder and preparation method thereof
Rice material laser scaling powder and preparation method thereof, belongs to field of material technology.
Background technology
Cu-Mg-Sn-Fe composite nano materials are a kind of widely used engineering materials, are had compared with Other Engineering material
There are excellent mechanical performance and preferable hot property, such as high intensity, high-modulus, high rigidity；Of a relatively high heat distortion temperature, this
Body is uniform color, adds Cu-Mg-Sn-Fe fiber reinforcements, mechanical strength etc. and greatly improves, but rigidity can decline therewith, heat-resisting
Rank also significantly improves, and heat distortion temperature is up to 250 DEG C (1.8MPa)；Additionally show excellent self-lubricating abrasion-resistant, resist
Fatigue, creep resistant；Good oil resistant and solvent borne.But due to adding Cu-Mg-Sn-Fe fibers, cause its dimensional stability
Poor, hydraulic performance decline is obvious under high humidity environment.Its combination property can be greatly improved by filling method, improve deficiency, institute
One very common Cu-Mg-Sn-Fe composite nano materials method of modifying is turned into the filling of Cu-Mg-Sn-Fe fibers.With smelting
The continuous development of the industries such as gold, military equipment, household electrical appliance, the use to material also constantly propose new requirement, lightweight,
High-performance, environmental protection become new trend, and substantial amounts of metal material is substituted by nano material, Cu-Mg-Sn-Fe composite Nanos
Material accounts for critically important status as representative therein.The fiber-reinforced modified Cu-Mg-Sn-Fe of general Cu-Mg-Sn-Fe are answered
Close the nano material mode classical as one and use production for many producers, it is very big in the market sales volume at this stage, it is different
There is also different in performance and stability for the product of producer.Cu-Mg-Sn-Fe composite nano materials are as many functions
Part is widely used, and using more and more in particularly many military equipments, and assemble sequence proposes newly to post-production
Requirement, laser welding is exactly one of new technology wherein with fastest developing speed.Laser welding is the laser beam using high-energy-density
A kind of high-efficiency and precision welding method as thermal source.Laser welding is one of importance of Materialbearbeitung mit Laserlicht technology application.
It is mainly used in the 1970s welding thin-walled material and low speed welding, the heating of welding process category heat-conduction-type, i.e. laser emission
Workpiece surface, surface heat are internally spread by heat transfer, by control the width of laser pulse, energy, peak power and
The parameters such as repetition rate, melt workpiece, form specific molten bath.Due to its it is unique the advantages of, oneself is successfully applied to micro-, small-sized
In the precision welding of part.Compared with traditional material welding procedure, laser welding has weld strength height, heating and cooling velocity
It is exceedingly fast, heat affected area is small, welding stress and distortion very little；Noncontact processing, butt-welding fitting does not produce external force effect, solderable to be difficult to
The position of contact；Welding procedure is stable, and face of weld and inherent quality are good, and performance is high；Laser is in vacuum, air and certain gas
Energy welding in environment, many advantages, such as welding by Cu-Mg-Sn-Fe materials.Laser welding also proposes newly to material
Requirement, it is desirable to what material was capable of maximum allows laser beam to pass through, to ensure that welding position obtains enough energy, but
Existing Cu-Mg-Sn-Fe composite nano materials, it is impossible to meet the needs of laser welding.
The content of the invention
In order to solve the deficiencies in the prior art, the present invention provides one kind and is used for Cu-Mg-Sn-Fe composite nano materials laser
Scaling powder, it is characterised in that matched and formed in parts by weight by following components：230.613~455.439 parts of pure water, C8 fat
22.161~64.891 parts of fat alcohol polyoxyethylene (4) ether, Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate 25.578~
134.724 parts, 21.628~38.399 parts of N- methyl (13C)-N- nitro-p-toluenesulfonamides, 3- nitros phthalyl Asia
24.210~81.753 parts of amine, 27.873~88.944 parts of 1- hydroxyls -4- (p-totuidine base) anthraquinone, 1- amino -2- [4- [(six
Hydrogen -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] 24.130~47.586 parts of -4- hydroxyls -9,10- anthraquinone, a methoxy
21.398~66.925 parts of base phenmethylol, 29.47~84.965 parts of mercury nanoparticle, 3,4- diaminobenzene formonitrile HCNs 22.543~
64.738 parts, N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2- [(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl]-benzene
12.224~55.842 parts of acid amides, 13.970~49.564 parts of 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl ester, 2- amino trifluoros
24.742~64.271 parts of toluene, 5- thiophenyls benzimidazolyl-2 radicals -31.207~75.906 parts of methyl carbamate, mass concentration
For 21.882ppm~288.859ppm 54.815~108.75 parts of dodecenylsuccinic anhydride.
Further, matched and formed in parts by weight by following components：231.613~454.439 parts of pure water, C8 fat
23.161~63.891 parts of alcohol polyoxyethylene (4) ether, Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate 26.578~133.724
Part, 22.628~37.399 parts of N- methyl (13C)-N- nitro-p-toluenesulfonamides, 3- nitrophthalimides
25.210~80.753 parts, 28.873~87.944 parts of 1- hydroxyls -4- (p-totuidine base) anthraquinone, 1- amino -2- [4- [(six
Hydrogen -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] 25.130~46.586 parts of -4- hydroxyls -9,10- anthraquinone, a methoxy
22.398~65.925 parts of base phenmethylol, 30.47~83.965 parts of mercury nanoparticle, 3,4- diaminobenzene formonitrile HCNs 23.543~
63.738 parts, N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2- [(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl]-benzene
13.224~54.842 parts of acid amides, 14.970~48.564 parts of 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl ester, 2- amino trifluoros
25.742~63.271 parts of toluene, 5- thiophenyls benzimidazolyl-2 radicals -32.207~74.906 parts of methyl carbamate, mass concentration
For 22.882ppm~287.859ppm 55.815~107.75 parts of dodecenylsuccinic anhydride.
Further, the invention also discloses a kind of system for Cu-Mg-Sn-Fe composite nano materials laser scaling powders
Preparation Method, by weight, comprise the following steps：
1st step：In stirred tank retort, pure water and C8 aliphatic alcohol polyethenoxies (4) ether are added, it is anti-to start stirred tank
The mixer in tank is answered, setting speed is 23.576rpm~69.272rpm, starts the double frequency heating dress in stirred tank retort
Put, temperature is risen to 38.941 DEG C~39.314 DEG C, add Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate and stir, enter
Row proenzyme self-catalyzed reaction 15.201~26.887 minutes, N- methyl (13C)-N- nitro-p-toluenesulfonamides are added, are passed through
Flow is 14.501m3/ min~55.665m3/ min xenon 0.23~0.88 hour；Added afterwards in stirred tank retort
3- nitrophthalimides, the double frequency heater being again started up in stirred tank retort, make temperature rise to 55.941 DEG C
~88.314 DEG C, 15.501~26.66 minutes are incubated, adds 1- hydroxyls -4- (p-totuidine base) anthraquinone, adjustment stirred tank reaction
The pH value of solution is 4.8695~8.9842 in tank, is incubated 15.501~255.66 minutes；
2nd step：Separately take mercury nanoparticle, by mercury nanoparticle power be 5.55399KW~10.9966KW under ultrasonic wave
Processing 0.21~0.88 hour, attrition grinding, and pass through 410.586~510.665 eye mesh screens；Mercury nanoparticle is added to separately
In one stirred tank retort, add 3, the 4- diaminobenzene formonitrile HCNs that mass concentration is 25.747ppm~255.671ppm and disperse
Mercury nanoparticle, start the double frequency heater in stirred tank retort, make solution temperature 4.8501 × 10 DEG C~8.9314
Between × 10 DEG C, start the mixer in stirred tank retort, and with 4.8941 × 102Rpm~8.9272 × 102Rpm speed
Stirring, adjustment pH value is between 4.8399~8.966, insulated and stirred 5.55 × 10-1~10.99 × 10-1Hour；Stop afterwards
Reaction stands 5.55 × 10~10.99 × 10 minutes, goes the removal of impurity；Suspension is added into 2- 5 amido benzotrifluorides, adjusts pH value
Between 1.501~2.665, the pure water elution of sediment is formed, by centrifuge in rotating speed 4.586 × 103Rpm~
9.665×103Solid content is obtained under rpm, 2.671 × 102DEG C~3.272 × 102Dried at a temperature of DEG C, 8.586 are crossed after grinding
×103~9.665 × 103Mesh sieve, it is standby；
3rd step：Separately take 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyls
Mercury nanoparticle after base -9,10- anthraquinone, meta-methoxy phenmethylol and the processing of the 2nd step, penetrated after well mixed using X near backwards to top
Penetrate irradiation, X penetrate closely backwards to top penetrate irradiation energy be 12.542MeV~40.318MeV, dosage be 60.717kGy~
100.11kGy, irradiation time are 24.405~49.274 minutes, obtain the 1- amino -2- [4- [(hexahydro -2- oxygen of character change
Generation -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy phenmethylol and mercury nanoparticle mix
Compound；By 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthracenes
Quinone, meta-methoxy phenmethylol and mercury nanoparticle mixture are placed in another stirred tank retort, are started in stirred tank retort
Double frequency heater, 23.695 DEG C~69.665 DEG C of design temperature, start the mixer in stirred tank retort, rotating speed is
15.501rpm~410.399rpm, pH are adjusted between 4.8542~8.9318, are dehydrated 24.272~38.201 minutes, standby；
4th step：1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidenes-the 1- that the character that 3rd step is obtained changes
Base) methyl] phenoxy group] -4- hydroxyls -9,10- anthraquinone, meta-methoxy phenmethylol and mercury nanoparticle be well mixed, add to quality
Concentration is that cocurrent adds to the stirred tank retort of the 1st step in 25.747ppm~255.671ppm 3,4- diaminobenzene formonitrile HCNs
In, flow acceleration is 160.300mL/min~888.979mL/min；Start stirred tank retort mixer, setting speed is
29.256rpm~69.81rpm；Stirring 4.8576~8.9318 minutes；Add N- [5- [double [2- (acetyl group oxygen) ethyl] ammonia
Base] -2- [(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl]-benzamide, start the double frequency heater in stirred tank retort,
59.879 DEG C~96.603 DEG C are warming up to, pH is adjusted between 4.8747~8.9671, and it is 14.576m to be passed through xenon throughput3/
Min~55.887m3/ min, insulation stand 49.662~79.663 minutes；It is again started up stirred tank retort mixer, rotating speed
For 24.970rpm~69.753rpm, 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl esters are added, make hydrophobic-parent of its reaction solution
Water plastic value is 5.55399~10.9966, and pH is adjusted between 4.8879~8.9603, insulation standing 48.158~
88.148 minutes；
5th step：Start the mixer in stirred tank retort, setting speed is 21.611rpm~88.98rpm, and side is stirred
While adding 2- 5 amido benzotrifluorides into stirred tank retort, start the double frequency heater in stirred tank retort, setting is stirred
It is 4.888 × 10 to mix the temperature in kettle retort2DEG C~9.810 × 102DEG C, after being incubated 48.158~88.148 minutes, add 5-
Thiophenyl benzimidazolyl-2 radicals-methyl carbamate, proenzyme self-catalyzed reaction 15.201~26.665 minutes；Laurylene is added afterwards
Base succinic anhydride, start the double frequency heater in stirred tank retort, set the temperature in stirred tank retort as 99.888
DEG C~155.810 DEG C, pH is adjusted between 4.8576~8.9887, and pressure is 0.21985MPa~0.22123MPa, during reaction
Between be 0.414~0.939 hour；0MPa is depressurized to afterwards, is cooled to 54.21879 DEG C~59.21671 DEG C dischargings, that is, is obtained one
Kind is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders.
Further, the particle diameter of the mercury nanoparticle is 29.439 μm~39.891 μm.
Further, the invention also discloses a kind of answering for Cu-Mg-Sn-Fe composite nano materials laser scaling powders
With；It is mainly used in the application for Cu-Mg-Sn-Fe composite nano materials laser weldings.
Further, the Cu-Mg-Sn-Fe composite nano materials be Cu-Mg alloys, Cu-Sn alloys, Cu-Fe alloys,
At least one of Mg-Sn alloys, Mg-Fe alloys, Sn-Fe alloys.
Further, a kind of Cu-Mg-Sn-Fe composite nano materials laser scaling powders that are used for coordinate with retarder thinner
Use, it is 1 that one kind, which is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders with retarder thinner fit quality ratio,:450.724
~890.399；The retarder thinner is：1. bis- chloro- 2- of 4,5- [[4,5- dihydro -3- methyl -5- oxos -1- (3- sulfonyloxies
Phenyl) -1H- pyrazoles -4- bases] azo] benzene sulfonic acid disodium, 2. 4- [4,5- dihydro -3- methyl -4- [[4- methyl -3- [[(4- first
Base phenyl) amino] sulfonyl] phenyl] azo] -5- oxygen -1H- pyrazol-1-yls] benzene sulfonic acid, the 3. chloro- 2- of 5- [[1- (2- chlorobenzenes
Base) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] one kind in three kinds of benzene sulfonic acid, the retarder thinner
For common commercial goods.
It is a kind of disclosed in patent of the present invention to be used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders and its preparation side
Method, it the advantage is that：
(1) when being used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders using one kind of the present invention, this method
Weld strength can be improved so that welding stress and welding deformation significantly reduce；
(2) a kind of Cu-Mg-Sn-Fe composite nano materials laser scaling powder that is used for of the present invention being capable of petition of surrender face significantly
Tension force, process stabilizing, it is applicable that wide, cooling is fast, effect is good, meets different welding requirements；
(3) a kind of Cu-Mg-Sn-Fe composite nano materials laser scaling powders that are used for of the present invention have chemical property steady
It is fixed, be applicable wide, pH value range is wide, adhesion-tight rate is high, metal surface cleaning than it is high the advantages of；
(4) one kind of the present invention will not be to surrounding enviroment for Cu-Mg-Sn-Fe composite nano materials laser scaling powders
Pollute；It is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders, equipment requirement letter using one kind of the present invention
List, operation cost are low.
Brief description of the drawings
Fig. 1 is a kind of to be used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders in testing experiment during differential responses
Between under the conditions of embodiment and reference examples deformation coefficient of stabilization variation diagram.
Fig. 2 is a kind of to be used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders in testing experiment during differential responses
Between under the conditions of embodiment and reference examples scaling powder coefficient of stabilization variation diagram.
Fig. 3 is a kind of to be used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders in testing experiment during differential responses
Between under the conditions of embodiment and reference examples weld strength enhancing rate variation diagram.
Embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing substantially from
In the case of spirit and essence of the invention, the modification and replacement made to the inventive method, step or condition, the present invention is belonged to
Scope.Unless otherwise specified, the conventional meanses that technological means used in embodiment is well known to those skilled in the art.
Embodiment 1
One kind of the present invention, which is prepared, according to following steps is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders,
And by weight：
1st step：In stirred tank retort, 230.613 parts of pure water, C8 aliphatic alcohol polyethenoxies (4) ether are added
22.161 parts, start the mixer in stirred tank retort, setting speed 23.576rpm, start in stirred tank retort
Double frequency heater, temperature is risen to 38.941 DEG C, add 25.578 parts of Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate and stir
Mix uniformly, carry out proenzyme self-catalyzed reaction 15.201 minutes, add N- methyl (13C)-N- nitro-p-toluenesulfonamides
21.628 parts, it is 14.501m to be passed through flow3/ min xenon 0.23 hour；3- nitros are added in stirred tank retort afterwards
24.210 parts of phthalimide, the double frequency heater being again started up in stirred tank retort, makes temperature rise to 55.941
DEG C, 15.501 minutes are incubated, adds 27.873 parts of 1- hydroxyls -4- (p-totuidine base) anthraquinone, is adjusted molten in stirred tank retort
The pH value of liquid is 4.8695, is incubated 15.501 minutes；
2nd step：Separately take 29.47 parts of mercury nanoparticle, by mercury nanoparticle power be 5.55399KW under ultrasonication
0.21 hour, attrition grinding, and pass through 410.586 eye mesh screens；Mercury nanoparticle is added in another stirred tank retort,
22.543 parts of 3, the 4- diaminobenzenes formonitrile HCN that mass concentration is 25.747ppm is added, disperses mercury nanoparticle, it is anti-to start stirred tank
The double frequency heater in tank is answered, makes solution temperature between 4.8501 × 10 DEG C, starts the mixer in stirred tank retort,
And with 4.8941 × 102Rpm speed stirring, adjustment pH value is between 4.8399, insulated and stirred 5.55 × 10-1Hour；Afterwards
Stop reaction and stand 5.55 × 10 minutes, go the removal of impurity；Suspension is added into 24.742 parts of 2- 5 amido benzotrifluorides, adjusts pH value
Between 1.501, the pure water elution of sediment is formed, by centrifuge in rotating speed 4.586 × 103Solid content is obtained under rpm,
2.671 × 102Dried at a temperature of DEG C, 8.586 × 10 are crossed after grinding3Mesh sieve, it is standby；
3rd step：Separately take 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyls
29.47 parts of mercury nanoparticle after 24.130 parts of base -9,10- anthraquinone, 21.398 parts of meta-methoxy phenmethylol and the processing of the 2nd step, is mixed
Penetrated after closing uniformly using X and closely penetrate irradiation backwards to top, X penetrate closely backwards to push up the energy of penetrating irradiation be 12.542MeV, dosage be
60.717kGy, irradiation time are 24.405 minutes, obtain the 1- amino -2- [4- [(hexahydro -2- oxo -1H- nitrogen of character change
Miscellaneous Zhuo -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy phenmethylol and mercury nanoparticle mixture；By 1-
Amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy
Phenmethylol and mercury nanoparticle mixture are placed in another stirred tank retort, start the double frequency heating dress in stirred tank retort
Put, 23.695 DEG C of design temperature, start the mixer in stirred tank retort, rotating speed 15.501rpm, pH are adjusted to 4.8542
Between, it is dehydrated 24.272 minutes, it is standby；4th step：1- amino -2- [4- [(hexahydro -2- the oxygen that the character that 3rd step is obtained changes
Generation -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy phenmethylol and mercury nanoparticle mix
Close and uniformly, add in 22.543 parts of 3, the 4- diaminobenzenes formonitrile HCN that mass concentration is 25.747ppm, cocurrent adds to stirring for the 1st step
Mix in kettle retort, flow acceleration 160.300mL/min；Start stirred tank retort mixer, setting speed is
29.256rpm；Stirring 4.8576 minutes；Add N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2- [(chloro- 2- benzene of 6-
Benzothiazolyl) azo] phenyl] 12.224 parts of-benzamide, start the double frequency heater in stirred tank retort, be warming up to
59.879 DEG C, pH is adjusted between 4.8747, and it is 14.576m to be passed through xenon throughput3/ min, insulation stand 49.662 minutes；
Stirred tank retort mixer is again started up, rotating speed 24.970rpm, adds 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl esters
13.970 parts, the hydrophobe-hydrophile plastic value for making its reaction solution is 5.55399, and pH is adjusted between 4.8879, and insulation is quiet
Put 48.158 minutes；
5th step：Start the mixer in stirred tank retort, setting speed 21.611rpm, while stirring to stirred tank
24.742 parts of 2- 5 amido benzotrifluorides are added in retort, start the double frequency heater in stirred tank retort, setting stirring
Temperature in kettle retort is 4.888 × 102DEG C, after being incubated 48.158 minutes, add 5- thiophenyls benzimidazolyl-2 radicals-amino first
Sour 31.207 parts of methyl esters, carry out proenzyme self-catalyzed reaction 15.201 minutes；21.882ppm dodecenyl-succinic acid is added afterwards
54.815 parts of acid anhydride, start the double frequency heater in stirred tank retort, set the temperature in stirred tank retort as 99.888
DEG C, pH is adjusted between 4.8576, pressure 0.21985MPa, and the reaction time is 0.414 hour；0MPa is depressurized to afterwards, is dropped
Temperature obtains one kind and is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders to 54.21879 DEG C of dischargings.
The particle diameter of wherein described mercury nanoparticle is 29.439 μm.
In the application, it is described a kind of for Cu-Mg-Sn-Fe composite nano materials laser scaling powder needs and retarder thinner
It is used cooperatively, it is 1 that one kind, which is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders with retarder thinner fit quality ratio,:
450.724；The retarder thinner is：Bis- chloro- 2- of 4,5- [[4,5- dihydro -3- methyl -5- oxos -1- (3- sulfonyloxy benzene
Base) -1H- pyrazoles -4- bases] azo] benzene sulfonic acid disodium, the retarder thinner 4, bis- chloro- 2- of 5- [[4,5- dihydro -3- methyl -5-
Oxo -1- (3- oxyphenyls) -1H- pyrazoles -4- bases] azo] benzene sulfonic acid disodium is common commercial goods.
Embodiment 2
One kind of the present invention, which is prepared, according to following steps is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders,
And by weight：
1st step：In stirred tank retort, 455.439 parts of pure water, C8 aliphatic alcohol polyethenoxies (4) ether are added
64.891 parts, start the mixer in stirred tank retort, setting speed 69.272rpm, start in stirred tank retort
Double frequency heater, temperature is risen to 39.314 DEG C, add 134.724 parts of Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate and stir
Mix uniformly, carry out proenzyme self-catalyzed reaction .26.887 minutes, add N- methyl (13C)-N- nitro-p-toluenesulfonamides
38.399 parts, it is 55.665m to be passed through flow3/ min xenon 0.88 hour；3- nitros are added in stirred tank retort afterwards
81.753 parts of phthalimide, the double frequency heater being again started up in stirred tank retort, makes temperature rise to 88.314
DEG C, 26.66 minutes are incubated, adds 88.944 parts of 1- hydroxyls -4- (p-totuidine base) anthraquinone, adjusts solution in stirred tank retort
PH value be 8.9842, be incubated 255.66 minutes；
2nd step：84.965 parts of mercury nanoparticle separately is taken, by mercury nanoparticle at power is ultrasonic wave under 10.9966KW
Reason 0.88 hour, attrition grinding, and pass through 510.665 eye mesh screens；Mercury nanoparticle is added to another stirred tank retort
In, 64.738 parts of 3, the 4- diaminobenzenes formonitrile HCN that mass concentration is 255.671ppm is added, disperses mercury nanoparticle, starts stirring
Double frequency heater in kettle retort, make solution temperature between 8.9314 × 10 DEG C, start stirring in stirred tank retort
Machine is mixed, and with 8.9272 × 102Rpm speed stirring, adjustment pH value is between 8.966, insulated and stirred 10.99 × 10-1Hour；
Stop reaction afterwards and stand 10.99 × 10 minutes, go the removal of impurity；Suspension is added into 64.271 parts of 2- 5 amido benzotrifluorides, adjusted
Whole pH value forms the pure water elution of sediment, by centrifuge in rotating speed 9.665 × 10 between 2.6653Obtained under rpm
Solid content, 3.272 × 102Dried at a temperature of DEG C, 9.665 × 10 are crossed after grinding3Mesh sieve, it is standby；
3rd step：Separately take 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyls
84.965 parts of mercury nanoparticle after 47.586 parts of base -9,10- anthraquinone, 66.925 parts of meta-methoxy phenmethylol and the processing of the 2nd step, is mixed
Penetrated after closing uniformly using X and closely penetrate irradiation backwards to top, X penetrate closely backwards to push up the energy of penetrating irradiation be 40.318MeV, dosage be
100.11kGy, irradiation time are 49.274 minutes, obtain the 1- amino -2- [4- [(hexahydro -2- oxo -1H- nitrogen of character change
Miscellaneous Zhuo -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy phenmethylol and mercury nanoparticle mixture；By 1-
Amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy
Phenmethylol and mercury nanoparticle mixture are placed in another stirred tank retort, start the double frequency heating dress in stirred tank retort
Put, 69.665 DEG C of design temperature, start the mixer in stirred tank retort, rotating speed 410.399rpm, pH are adjusted to
Between 8.9318, it is dehydrated 38.201 minutes, it is standby；
4th step：1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidenes-the 1- that the character that 3rd step is obtained changes
Base) methyl] phenoxy group] -4- hydroxyls -9,10- anthraquinone, meta-methoxy phenmethylol and mercury nanoparticle be well mixed, add to quality
Concentration is that cocurrent is added in the stirred tank retort of the 1st step in 255.671ppm 64.738 parts of 3,4- diaminobenzenes formonitrile HCN, stream
Acceleration is 888.979mL/min；Start stirred tank retort mixer, setting speed 69.81rpm；8.9318 points of stirring
Clock；Add N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2- [(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl]-benzene
55.842 parts of acid amides, start the double frequency heater in stirred tank retort, be warming up to 96.603 DEG C, pH be adjusted to 8.9671 it
Between, it is 55.887m to be passed through xenon throughput3/ min, insulation stand 79.663 minutes；It is again started up the stirring of stirred tank retort
Machine, rotating speed 69.753rpm, 49.564 parts of 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl ester is added, make dredging for its reaction solution
Water-hydrophilic plastic value is 10.9966, and pH is adjusted between 8.9603, and insulation stands 88.148 minutes；
5th step：Start the mixer in stirred tank retort, setting speed 88.98rpm, while stirring to stirred tank
64.271 parts of 2- 5 amido benzotrifluorides are added in retort, start the double frequency heater in stirred tank retort, setting stirring
Temperature in kettle retort is 9.810 × 102DEG C, after being incubated 88.148 minutes, add 5- thiophenyls benzimidazolyl-2 radicals-amino first
Sour 75.906 parts of methyl esters, carry out proenzyme self-catalyzed reaction 26.665 minutes；288.859ppm dodecenyl succinate is added afterwards
108.75 parts of acid anhydrides, start the double frequency heater in stirred tank retort, set temperature in stirred tank retort as
155.810 DEG C, pH is adjusted between 8.9887, pressure 0.22123MPa, and the reaction time is 0.939 hour；It is depressurized to afterwards
0MPa, 59.21671 DEG C of dischargings are cooled to, that is, obtain one kind and be used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders.
The particle diameter of wherein described mercury nanoparticle is 39.891 μm.
In the application, it is described a kind of for Cu-Mg-Sn-Fe composite nano materials laser scaling powder needs and retarder thinner
It is used cooperatively, it is 1 that one kind, which is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders with retarder thinner fit quality ratio,:
890.399；The retarder thinner is：The chloro- 2- of 5- [[1- (2- chlorphenyls) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -
4- yls] azo] benzene sulfonic acid, the chloro- 2- of retarder thinner the 5- [[1- (2- chlorphenyls) -4,5- dihydro -3- methyl -5- oxos -1H-
Pyrazoles -4- bases] azo] benzene sulfonic acid is common commercial goods.
Embodiment 3
One kind of the present invention, which is prepared, according to following steps is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders,
And by weight：
1st step：In stirred tank retort, 230.9613 parts of pure water, C8 aliphatic alcohol polyethenoxies (4) ether are added
22.9161 parts, start the mixer in stirred tank retort, setting speed 23.9576rpm, start in stirred tank retort
Double frequency heater, temperature is risen to 38.9941 DEG C, add Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate 25.9578
Part stirs, and carries out proenzyme self-catalyzed reaction 15.9201 minutes, adds N- methyl (13C)-N- nitro-p-toluenesulfonamides
21.9628 parts, it is 14.9501m to be passed through flow3/ min xenon 0.923 hour；3- nitre is added in stirred tank retort afterwards
24.9210 parts of base phthalimide, the double frequency heater being again started up in stirred tank retort, rises to temperature
55.9941 DEG C, 15.9501 minutes are incubated, adds 27.9873 parts of 1- hydroxyls -4- (p-totuidine base) anthraquinone, adjustment stirred tank is anti-
The pH value for answering solution in tank is 4.89695, is incubated 15.9501 minutes；
2nd step：29.947 parts of mercury nanoparticle separately is taken, by mercury nanoparticle at power is ultrasonic wave under 5.559399KW
Reason 0.921 hour, attrition grinding, and pass through 410.9586 eye mesh screens；Mercury nanoparticle is added to the reaction of another stirred tank
In tank, 22.9543 parts of 3, the 4- diaminobenzenes formonitrile HCN that mass concentration is 25.9747ppm is added, disperses mercury nanoparticle, is started
Double frequency heater in stirred tank retort, make solution temperature between 4.89501 × 10 DEG C, start in stirred tank retort
Mixer, and with 4.89941 × 102Rpm speed stirring, adjusts pH value between 4.89399, and insulated and stirred 5.559 ×
10-1Hour；Stop reaction afterwards and stand 5.559 × 10 minutes, go the removal of impurity；Suspension is added into 2- 5 amido benzotrifluorides
24.9742 parts, adjustment pH value forms the pure water elution of sediment, by centrifuge in rotating speed 4.9586 between 1.9501
×103Solid content is obtained under rpm, 2.9671 × 102Dried at a temperature of DEG C, 8.9586 × 10 are crossed after grinding3Mesh sieve, it is standby；
3rd step：Separately take 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyls
29.947 parts of mercury nanoparticle after 24.9130 parts of base -9,10- anthraquinone, 21.9398 parts of meta-methoxy phenmethylol and the processing of the 2nd step,
Penetrated after well mixed using X and closely penetrate irradiation backwards to top, X penetrate closely backwards to push up the energy of penetrating irradiation be 12.9542MeV, dosage be
60.9717kGy, irradiation time are 24.9405 minutes, obtain the 1- amino -2- [4- [(hexahydro -2- oxos -1H- of character change
Azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy phenmethylol and mercury nanoparticle mixture；Will
1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, a methoxy
Base phenmethylol and mercury nanoparticle mixture are placed in another stirred tank retort, start the double frequency heating in stirred tank retort
Device, 23.9695 DEG C of design temperature start the mixer in stirred tank retort, and rotating speed 15.9501rpm, pH are adjusted to
Between 4.89542, it is dehydrated 24.9272 minutes, it is standby；
4th step：1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidenes-the 1- that the character that 3rd step is obtained changes
Base) methyl] phenoxy group] -4- hydroxyls -9,10- anthraquinone, meta-methoxy phenmethylol and mercury nanoparticle be well mixed, add to quality
Concentration is that cocurrent is added in the stirred tank retort of the 1st step in 25.9747ppm 22.9543 parts of 3,4- diaminobenzenes formonitrile HCN,
Flow acceleration is 160.9300mL/min；Start stirred tank retort mixer, setting speed 29.9256rpm；Stirring
4.89576 minute；Add N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2- [(the chloro- 2-[4-morpholinodithio bases of 6-) azo]
Phenyl] 12.9224 parts of-benzamide, start the double frequency heater in stirred tank retort, be warming up to 59.9879 DEG C, pH adjustment
To between 4.89747, it is 14.9576m to be passed through xenon throughput3/ min, insulation stand 49.9662 minutes；It is again started up stirring
Kettle retort mixer, rotating speed 24.9970rpm, 13.9970 parts of 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl ester is added, is made
The hydrophobe-hydrophile plastic value of its reaction solution is 5.559399, and pH is adjusted between 4.89879, and insulation stands 48.9158
Minute；
5th step：Start the mixer in stirred tank retort, setting speed 21.9611rpm, while stirring to stirring
24.9742 parts of 2- 5 amido benzotrifluorides are added in kettle retort, start the double frequency heater in stirred tank retort, setting is stirred
It is 4.9888 × 10 to mix the temperature in kettle retort2DEG C, after being incubated 48.9158 minutes, add 5- thiophenyls benzimidazolyl-2 radicals-ammonia
31.9207 parts of base methyl formate, carry out proenzyme self-catalyzed reaction 15.9201 minutes；21.9882ppm laurylene is added afterwards
54.9815 parts of base succinic anhydride, start the double frequency heater in stirred tank retort, set the temperature in stirred tank retort
For 99.9888 DEG C, pH is adjusted between 4.89576, pressure 0.219985MPa, and the reaction time is 0.4914 hour；Drop afterwards
0MPa is depressed into, is cooled to 54.219879 DEG C of dischargings, that is, obtains one kind and helps weldering for Cu-Mg-Sn-Fe composite nano materials laser
Agent.
The particle diameter of wherein described mercury nanoparticle is 29.9439 μm.
In the application, it is described a kind of for Cu-Mg-Sn-Fe composite nano materials laser scaling powder needs and retarder thinner
It is used cooperatively, it is 1 that one kind, which is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders with retarder thinner fit quality ratio,:
450.9724；The retarder thinner is：4- [4,5- dihydro -3- methyl -4- [[4- methyl -3- [[(4- aminomethyl phenyls) amino] sulphurs
Acyl group] phenyl] azo] -5- oxygen -1H- pyrazol-1-yls] benzene sulfonic acid, retarder thinner 4- [4, the 5- dihydro -3- methyl -4-
[[4- methyl -3- [[(4- aminomethyl phenyls) amino] sulfonyl] phenyl] azo] -5- oxygen -1H- pyrazol-1-yls] benzene sulfonic acid is normal
See commercial goods.
Reference examples
Reference examples carry out welding examination using certain commercially available brand for Cu-Mg-Sn-Fe composite nano materials laser scaling powders
Test.
Embodiment 4
The Cu-Mg-Sn-Fe composite nano materials laser scaling powder that is used for that embodiment 1~3 and reference examples are obtained is carried out
Soldering test, wherein being used cooperatively for Cu-Mg-Sn-Fe composite nano materials laser scaling powders with retarder thinner, for Cu-
The mass ratio of Mg-Sn-Fe composite nano materials laser scaling powders and retarder thinner is 1:450.724 the retarder thinner is in reality
Apply in example 1 is bis- chloro- 2- of 4,5- [[4,5- dihydro -3- methyl -5- oxos -1- (3- oxyphenyls) -1H- pyrazoles -4- bases]
Azo] benzene sulfonic acid disodium, it is 4- [4,5- dihydro -3- methyl -4- [[4- methyl -3- [[(4- aminomethyl phenyls) ammonia in example 2
Base] sulfonyl] phenyl] azo] -5- oxygen -1H- pyrazol-1-yls] benzene sulfonic acid, it is the chloro- 2- of 5- [[1- (2- chlorobenzenes in embodiment 3
Base) -4,5- dihydro -3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] benzene sulfonic acid.
Above-described embodiment welding performance test result is as shown in table 1 below.
As seen from Table 1, one kind of the present invention is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders, and it draws
It is high to stretch intensity, bending strength, notch impact strength, unnotched impact strength, 1.98MPa heat distortion temperatures, rigidity enhancing rate
In the product of prior art production.
In addition, it is that one kind of the present invention helps for Cu-Mg-Sn-Fe composite nano materials laser as shown in Figures 1 to 3
What solder flux was carried out with reference examples, with usage time change test data statistics.Find out in figure, embodiment 1~3 is stable in deformation
The technical indicators such as rate, scaling powder coefficient of stabilization, weld strength enhancing rate, significantly better than the product of prior art production.
Claims (5)
1. one kind is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders, it is characterised in that by following components by weight
Number proportioning composition：
230.613~455.439 parts of pure water, 22.161~64.891 parts of C8 aliphatic alcohol polyethenoxies (4) ether, fatty alcohol polyoxy
25.578~134.724 parts of ethene polyethenoxy ether shuttle hydrochlorate, N- methyl (13C)-N- nitro-p-toluenesulfonamides 21.628
~38.399 parts, 24.210~81.753 parts of 3- nitrophthalimides, 1- hydroxyls -4- (p-totuidine base) anthraquinone
27.873~88.944 parts, 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyls
24.130~47.586 parts of base -9,10- anthraquinone, 21.398~66.925 parts of meta-methoxy phenmethylol, mercury nanoparticle 29.47~
84.965 parts, 3,4- 22.543~64.738 parts of diaminobenzene formonitrile HCNs, N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2-
[(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl] 12.224~55.842 parts of-benzamide, 2- cyano group -3,3- diphenylacrylates
Different 13.970~49.564 parts of monooctyl ester, 24.742~64.271 parts of 2- 5 amido benzotrifluorides, 5- thiophenyls benzimidazolyl-2 radicals-amino
31.207~75.906 parts of methyl formate, mass concentration are 21.882ppm~288.859ppm dodecenylsuccinic anhydride
54.815~108.75 parts.
2. one kind according to claim 1 is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders, its feature exists
In being matched and formed in parts by weight by following components：
231.613~454.439 parts of pure water, 23.161~63.891 parts of C8 aliphatic alcohol polyethenoxies (4) ether, fatty alcohol polyoxy
26.578~133.724 parts of ethene polyethenoxy ether shuttle hydrochlorate, N- methyl (13C)-N- nitro-p-toluenesulfonamides 22.628
~37.399 parts, 25.210~80.753 parts of 3- nitrophthalimides, 1- hydroxyls -4- (p-totuidine base) anthraquinone
28.873~87.944 parts, 1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyls
25.130~46.586 parts of base -9,10- anthraquinone, 22.398~65.925 parts of meta-methoxy phenmethylol, mercury nanoparticle 30.47~
83.965 parts, 3,4- 23.543~63.738 parts of diaminobenzene formonitrile HCNs, N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2-
[(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl] 13.224~54.842 parts of-benzamide, 2- cyano group -3,3- diphenylacrylates
Different 14.970~48.564 parts of monooctyl ester, 25.742~63.271 parts of 2- 5 amido benzotrifluorides, 5- thiophenyls benzimidazolyl-2 radicals-amino
32.207~74.906 parts of methyl formate, mass concentration are 22.882ppm~287.859ppm dodecenylsuccinic anhydride
55.815~107.75 parts.
3. one kind according to claim 1 is used for Cu-Mg-Sn-Fe composite nano materials laser scaling powders, its feature exists
In described one kind is used cooperatively for Cu-Mg-Sn-Fe composite nano materials laser scaling powders with retarder thinner, and one kind is used for
Cu-Mg-Sn-Fe composite nano materials laser scaling powders are 1 with retarder thinner fit quality ratio:450.724~890.399；Institute
Stating retarder thinner is：1. bis- chloro- 2- of 4,5- [[4,5- dihydros -3- methyl -5- oxos -1- (3- oxyphenyls) -1H- pyrroles
Azoles -4- bases] azo] benzene sulfonic acid disodium, 2. 4- [4,5- dihydro -3- methyl -4- [[4- methyl -3- [[(4- aminomethyl phenyls) amino]
Sulfonyl] phenyl] azo] -5- oxygen -1H- pyrazol-1-yls] benzene sulfonic acid, 3. the chloro- 2- of 5- [[1- (2- chlorphenyls) -4,5- dihydros -
3- methyl -5- oxo -1H- pyrazoles -4- bases] azo] one kind in three kinds of benzene sulfonic acid, the retarder thinner is common commercially available business
Product.
A kind of 4. preparation side for Cu-Mg-Sn-Fe composite nano materials laser scaling powders according to claim 1 or 2
Method, it is characterised in that by weight, comprise the following steps：
1st step：In stirred tank retort, pure water and C8 aliphatic alcohol polyethenoxies (4) ether are added, starts stirred tank retort
In mixer, setting speed is 23.576rpm~69.272rpm, start stirred tank retort in double frequency heater, make
Temperature rises to 38.941 DEG C~39.314 DEG C, adds Fatty alcohol polyoxyethylene polyoxypropylene ether shuttle hydrochlorate and stirs, carries out enzyme
Former self-catalyzed reaction 15.201~26.887 minutes, N- methyl (13C)-N- nitro-p-toluenesulfonamides are added, are passed through flow
For 14.501m3/ min~55.665m3/ min xenon 0.23~0.88 hour；3- nitre is added in stirred tank retort afterwards
Base phthalimide, the double frequency heater being again started up in stirred tank retort, make temperature rise to 55.941 DEG C~
88.314 DEG C, 15.501~26.66 minutes are incubated, adds 1- hydroxyls -4- (p-totuidine base) anthraquinone, adjusts stirred tank retort
The pH value of middle solution is 4.8695~8.9842, is incubated 15.501~255.66 minutes；
2nd step：Separately take mercury nanoparticle, by mercury nanoparticle power be 5.55399KW~10.9966KW under ultrasonication
0.21~0.88 hour, attrition grinding, and pass through 410.586~510.665 eye mesh screens；Mercury nanoparticle is added to another
In stirred tank retort, add the scattered mercury of 3,4- diaminobenzenes formonitrile HCN that mass concentration is 25.747ppm~255.671ppm and receive
Rice particulate, starts the double frequency heater in stirred tank retort, makes solution temperature 4.8501 × 10 DEG C~8.9314 × 10
Between DEG C, start the mixer in stirred tank retort, and with 4.8941 × 102Rpm~8.9272 × 102Rpm speed is stirred
Mix, adjustment pH value is between 4.8399~8.966, insulated and stirred 5.55 × 10-1~10.99 × 10-1Hour；Stop afterwards anti-
5.55 × 10~10.99 × 10 minutes should be stood, goes the removal of impurity；Suspension is added into 2- 5 amido benzotrifluorides, adjustment pH value exists
Between 1.501~2.665, the pure water elution of sediment is formed, by centrifuge in rotating speed 4.586 × 103Rpm~9.665
×103Solid content is obtained under rpm, 2.671 × 102DEG C~3.272 × 102Dried at a temperature of DEG C, 8.586 × 10 are crossed after grinding3
~9.665 × 103Mesh sieve, it is standby；
3rd step：1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9 separately are taken,
Mercury nanoparticle after 10- anthraquinones, meta-methoxy phenmethylol and the processing of the 2nd step, is penetrated using X after well mixed and closely penetrates spoke backwards to top
According to, X penetrate closely backwards to top penetrate irradiation energy be 12.542MeV~40.318MeV, dosage be 60.717kGy~100.11kGy,
Irradiation time is 24.405~49.274 minutes, obtains the 1- amino -2- [4- [(hexahydro -2- oxo -1H- azepines of character change
Zhuo -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy phenmethylol and mercury nanoparticle mixture；By 1- ammonia
Base -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) methyl] phenoxy group] -4- hydroxyl -9,10- anthraquinones, meta-methoxy benzene
Methanol and mercury nanoparticle mixture are placed in another stirred tank retort, start the double frequency heating dress in stirred tank retort
Put, 23.695 DEG C~69.665 DEG C of design temperature, start stirred tank retort in mixer, rotating speed be 15.501rpm~
410.399rpm, pH are adjusted between 4.8542~8.9318, are dehydrated 24.272~38.201 minutes, standby；
4th step：1- amino -2- [4- [(hexahydro -2- oxo -1H- azatropylidene -1- bases) first that the character that 3rd step is obtained changes
Base] phenoxy group] -4- hydroxyls -9,10- anthraquinone, meta-methoxy phenmethylol and mercury nanoparticle be well mixed, and adding to mass concentration is
In 25.747ppm~255.671ppm 3,4- diaminobenzene formonitrile HCNs, cocurrent is added in the stirred tank retort of the 1st step, and stream adds
Speed is 160.300mL/min~888.979mL/min；Start stirred tank retort mixer, setting speed 29.256rpm
~69.81rpm；Stirring 4.8576~8.9318 minutes；Add N- [5- [double [2- (acetyl group oxygen) ethyl] amino] -2-
[(the chloro- 2-[4-morpholinodithio bases of 6-) azo] phenyl]-benzamide, start the double frequency heater in stirred tank retort, be warming up to
59.879 DEG C~96.603 DEG C, pH is adjusted between 4.8747~8.9671, and it is 14.576m to be passed through xenon throughput3/ min~
55.887m3/ min, insulation stand 49.662~79.663 minutes；Stirred tank retort mixer is again started up, rotating speed is
24.970rpm~69.753rpm, 2- cyano group -3,3- diphenyl 2-Propenoic acid-2-ethylhexyl esters are added, make the hydrophobe-hydrophile of its reaction solution
Plastic value is 5.55399~10.9966, and pH is adjusted between 4.8879~8.9603, insulation standing 48.158~
88.148 minutes；
5th step：Start stirred tank retort in mixer, setting speed is 21.611rpm~88.98rpm, while stirring to
2- 5 amido benzotrifluorides are added in stirred tank retort, start the double frequency heater in stirred tank retort, set stirred tank
Temperature in retort is 4.888 × 102DEG C~9.810 × 102DEG C, after being incubated 48.158~88.148 minutes, add 5- benzene sulphur
Base benzimidazolyl-2 radicals-methyl carbamate, proenzyme self-catalyzed reaction 15.201~26.665 minutes；Laurylene base amber is added afterwards
Amber acid anhydrides, start the double frequency heater in stirred tank retort, set temperature in stirred tank retort as 99.888 DEG C~
155.810 DEG C, pH is adjusted between 4.8576~8.9887, and pressure is 0.21985MPa~0.22123MPa, and the reaction time is
0.414~0.939 hour；0MPa is depressurized to afterwards, is cooled to 54.21879 DEG C~59.21671 DEG C dischargings, that is, is obtained a kind of use
In Cu-Mg-Sn-Fe composite nano materials laser scaling powders.
5. a kind of preparation method for Cu-Mg-Sn-Fe composite nano materials laser scaling powders according to claim 4,
Characterized in that, the particle diameter of the mercury nanoparticle is 29.439 μm~39.891 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610570166.6A CN106216883B (en) | 2016-07-19 | 2016-07-19 | One kind is used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610570166.6A CN106216883B (en) | 2016-07-19 | 2016-07-19 | One kind is used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106216883A CN106216883A (en) | 2016-12-14 |
| CN106216883B true CN106216883B (en) | 2018-02-13 |
Family
ID=57531110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610570166.6A Expired - Fee Related CN106216883B (en) | 2016-07-19 | 2016-07-19 | One kind is used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106216883B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111390428B (en) * | 2020-05-12 | 2021-09-28 | 江苏满江红金属新材料科技有限公司 | Solder paste assistant for laser welding and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398698A (en) * | 2001-07-25 | 2003-02-26 | 邓和升 | Clean-free liquid flux |
| CN1562554A (en) * | 2004-03-30 | 2005-01-12 | 深圳市唯特偶化工开发实业有限公司 | Welding flux agent of solder with no lead and free from cleaning |
| CN102821908A (en) * | 2010-03-11 | 2012-12-12 | 苏威氟有限公司 | Fine particulate flux |
| CN104032323A (en) * | 2014-03-10 | 2014-09-10 | 深圳市贝加电子材料有限公司 | Cleaning agent suitable for components after high-temperature welding |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4042418B2 (en) * | 2002-01-30 | 2008-02-06 | 昭和電工株式会社 | Soldering flux |
| JP3797990B2 (en) * | 2003-08-08 | 2006-07-19 | 株式会社東芝 | Thermosetting flux and solder paste |
-
2016
- 2016-07-19 CN CN201610570166.6A patent/CN106216883B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398698A (en) * | 2001-07-25 | 2003-02-26 | 邓和升 | Clean-free liquid flux |
| CN1562554A (en) * | 2004-03-30 | 2005-01-12 | 深圳市唯特偶化工开发实业有限公司 | Welding flux agent of solder with no lead and free from cleaning |
| CN102821908A (en) * | 2010-03-11 | 2012-12-12 | 苏威氟有限公司 | Fine particulate flux |
| CN104032323A (en) * | 2014-03-10 | 2014-09-10 | 深圳市贝加电子材料有限公司 | Cleaning agent suitable for components after high-temperature welding |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106216883A (en) | 2016-12-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhang et al. | Effects of Ga addition on microstructure and properties of Sn–Ag–Cu/Cu solder joints | |
| CN106216883B (en) | One kind is used for Cu Mg Sn Fe composite nano materials laser scaling powders and preparation method thereof | |
| CN105458274A (en) | Ball milling preparation method for nickel-based high-temperature graphene alloy powder | |
| CN107433402B (en) | A kind of preparation method and applications of graphene-nano mattisolda | |
| CN101745763A (en) | High-efficiency preparation method of precise welded ball | |
| Fanselow et al. | Production of micron-sized polymer particles for additive manufacturing by melt emulsification | |
| CN108247082A (en) | A kind of nano silver concentrate and preparation method | |
| CN103920984A (en) | Combined type stirring, rubbing and welding head manufactured by using double materials and manufacturing process thereof | |
| CN103157389A (en) | Method for preparing asymmetric porous metal film | |
| CN108941585A (en) | The preparation method of 3D printing and soft magnetism patch integrated component submicron metal | |
| Chen et al. | Interfacial microstructure and mechanical reliability of Sn-58Bi/ENEPIG solder joints | |
| CN108842096A (en) | A kind of self-lubricating composite and preparation method thereof of argentiferous copper and indium alloy | |
| CN108032043A (en) | The preparation method of materials with high melting point agitating friction weldering composite stirring head | |
| Jamadon et al. | Utilization of a porous Cu interlayer for the enhancement of Pb-Free Sn-3.0 Ag-0.5 Cu Solder joint | |
| CN106216640A (en) | A kind of chrome additive for high-magnesium aluminum alloy founding and preparation method thereof | |
| Itagaki et al. | Spherical particles with and without attached nanoparticles formed by DC-arc spheroidization of irregularly shaped stainless-steel powder | |
| CN103611996B (en) | A kind of welding method of mother-daughter board connector long needle | |
| CN104707626A (en) | Raney nickel catalyst and preparation method thereof | |
| Lin et al. | Microstructural development in a rapidly cooled eutectic Sn–3.5% Ag solder reinforced with copper powder | |
| Xue et al. | Wettability and interfacial whiskers of Sn–9Zn–0.5 Ga–0.08 Nd solder with Sn, SnBi and Au/Ni coatings | |
| Zhai et al. | Research on interlayer alloys for transient liquid phase diffusion bonding of single crystal nickel base superalloy DD6 | |
| CN107160053B (en) | It is a kind of for aluminium and the solder stick of aluminum alloy soft soldering and preparation method thereof | |
| Feng et al. | Oxidation during the production of FGH4095 superalloy powders by electrode induction-melt inert gas atomization | |
| CN105108328B (en) | A kind of Continuous Drive Friction Welding of booster main shaft connects method | |
| Jha et al. | Development processes of cost effective aluminium metal matrix composite-A review |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180213 Termination date: 20180719 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |