CN105047247B - A kind of tin plating tin composition and its production and use of electric wire - Google Patents
A kind of tin plating tin composition and its production and use of electric wire Download PDFInfo
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Abstract
The invention provides a kind of tin plating tin composition and its production and use of electric wire, the tin composition is based on the mass percent shared by each component including following components:Metal Bi is 0.5~1.5%, metal In is 0.1~1.0%, metal Ag is 0.1~0.5%, Ni metal is 0.3~1.5%, carbon Nano sol is 0.5~1.5%, silane coupling agent is 0.5~1.5% and additive is 1~5%, and surplus is metal Sn.The present invention improves the performance of the tin composition by controlling metal Ag and Ni metal adding proportion and dosage, further improves the performance of the electric wire using the tin composition;And by adding carbon Nano sol and silane coupling agent, to improve the adaptation of coating and core, coating is set to be coupled with core closer, so as to improve the mechanical performance of electric wire.
Description
Technical field
The invention belongs to electric wire field, is related to a kind of tin plating tin composition and its production and use of electric wire.
Background technology
Electric wire product is widely used in national economy every field, is called " blood vessel " and " nerve " of national economy.
Electric wire manufacturing industry is that supporting its product of industry maximum in national economy must is fulfilled for each technical performance and price using field
Performance ratio requires, meets the requirement that living standards of the people improve constantly;It develops with the necessity for being ahead of application field development.
Now civilian, business and industrial electric wire and cable conductor, particularly civilian wiring, what is used mostly is all that copper is led
Body.In order to reduce the cost of electric wire, other electric properties of fine copper copper core electric wire are improved, it is necessary to traditional copper core electric wire
It is improved or replaces.Useful copper alloy substitutes fine copper in the prior art, and this copper alloy electric wire intensity is high, but electric conductivity
It can decline, the electric conductivity of this electric wire need further to improve.
Patent CN 103352138A disclose a kind of preparation method of copper alloy electric wire, the alloying element of the copper alloy
Mass percent is:Mn 0.2~0.6%, Al 0.4~1.5%, Ce 0.02~0.1%, Ni 0.02~0.15%, surplus
For Cu and inevitable impurity;By copper alloy casting ingot hot extrusion, 1~8mm wire rod is drawn into;In the protection of nitrogen atmosphere
Under, wire rod is put into heat-treatment furnace, heat treatment temperature is 1100 DEG C~1250 DEG C, and the time is 1.5~2.5 hours;Wire rod is empty
40~55 DEG C are cooled to, wraps up silver-plated carbon fiber shielding layer, extrudes one layer of protective jacket.The electric conductivity of electric wire is prepared in this method
Although can increase, mechanical performance and decay resistance are unsatisfactory.
In the prior art, have and take outside copper conductor the laminated gold of outsourcing one or coating to improve the skill of the performance of wire
Art scheme.Tin coating is a kind of good weldability and the coating with certain anti-corrosion capability, in electronic wire, printed substrate
It is widely used.Tin coating can use the method for plating, immersion plating and chemical plating to prepare.Immersion tin is easy to operate, and cost is low, but plates
Layer finite thickness, general only 0.5 μm, plating solution is easily poisoned, and can not meet industrial requirements.Electroless tin coating thickness is uniform, plating
Liquid dispersibility is good, and production efficiency is high, and easily-controlled operation, coating surface is bright and clean smooth, and compact crystallization, porosity is low, adhesion
It is a kind of preferably electroless plating technology of Small electronic component and electronic wire better than immersion tin and electrotinning.But because tin
Hydrogen-evolution overpotential is high, and catalytic activity is low, if individually can not all realize tin using reducing agents such as formaldehyde, sodium hypophosphite, boron hydrides
Continuously self-catalyzed deposition, thicker coating can not be obtained.
Patent CN 104332211A disclose a kind of tin plating phosphor-bronze wire, including core and coating, and the core material is phosphorus
Copper alloy, the coating are 100% pure stannum layer, and the pure stannum layer is evenly coated at the core outer layer, institute by hot dipping method
The straight through being 0.5mm~1.2mm of core is stated, and the tolerance of the diameter is ± 0.01, and the thickness of coating is 6 μm~9 μm,
The composition and mass percent of the phosphor copper be:Phosphorus 12%-18%, copper 80%-89%, remaining is impurity.In the patent
In mainly employ 100% pure stannum layer as coating, its tensile strength and conductance be not it is highly desirable, and tin coating with it is fine
The adaptation of core is also bad, easily peels off.
The content of the invention
It is undesirable for the conductance, mechanical performance and acid-resistant corrosion of wire present in above-mentioned prior art, it is tin plating
The problems such as layer and the adaptation of fibre core are bad, the invention provides a kind of electric wire tin plating tin composition and preparation method thereof and use
On the way.The present invention improves the performance of the tin composition by controlling metal Ag and Ni metal adding proportion and dosage, enters one
Step improves the performance of the electric wire using the tin composition;And by adding carbon Nano sol and silane coupling agent, to improve coating
With the conjugation grade of core, coating is set to be coupled with core closer, so as to improve the mechanical performance of wire.
To use following technical scheme up to this purpose, the present invention:
In a first aspect, the invention provides a kind of tin plating tin composition of electric wire, it is characterised in that the tin composition is pressed
Mass percent meter shared by each component includes following components:
Ni metal and metal Ag mass ratio are 3 in the tin composition:1.
Wherein, metal Bi mass percent can be 0.5%, 0.7%, 0.9%, 1.0%, 1.3% or 1.5% etc.;Gold
Belong to In mass percent can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or
1.0% etc.;Metal Ag mass percent can be 0.1%, 0.2%, 0.3%, 0.4% or 0.5% etc.;The quality hundred of Ni metal
It can be 0.3%, 0.7%, 0.9%, 1.0%, 1.3% or 1.5% etc. to divide ratio;The mass percent of carbon Nano sol can be 0.5%,
0.7%th, 0.9%, 1.0%, 1.3% or 1.5% etc.;Silane coupling agent 0.5%, 0.7%, 0.9%, 1.0%, 1.3% or
1.5% etc.;The mass percent of additive can be 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5% etc..
Preferably, the tin composition based on the mass percent shared by each component including following components:
More preferably, the tin composition based on the mass percent shared by each component including following components:
The present invention improves the performance of the tin composition by controlling metal Ag and Ni metal adding proportion and dosage.
In the prior art, for Sn composition, when Ag addition is less than 3.5wt%, excessive Sn is had during tin plating
Formed with β-Sn, make to form trickle shrinkage cavity crack during solidification on Sn surfaces, influence properties of product.Meanwhile when Ag content is small
When 1.0wt%, the deteriorated weldability of material can be made.And the present invention by studying repeatedly, by control Ag and Cu ratio and
Content, the two is cooperateed with to adjust the performance of material.
Meanwhile the present invention improves the conjugation grade of tin composition and core by adding carbon Nano sol and silane coupling agent.
In the present invention, the silane coupling agent is 3- metacryloxies propyl trimethoxy silicane, 2- (3,4- epoxies
Hexyl) any one in ethyl trimethoxy silane or 3- glycidoxypropyltrime,hoxysilanes or at least two group
Close, the combination is typical but non-limiting examples have:3- metacryloxies propyl trimethoxy silicane and 2- (3,4- epoxies oneself
Base) ethyl trimethoxy silane combination, 2- (3,4- epoxyhexyl) ethyl trimethoxy silanes and 3- glycidoxypropyl groups
The combination of trimethoxy silane, 3- metacryloxies propyl trimethoxy silicane, 2- (3,4- epoxyhexyl) ethyl trimethoxy
Combination of base silane and 3- glycidoxypropyltrime,hoxysilanes etc..
In the present invention, the additive includes following components by mass percentage:
Reducing agent 30~40%
Nonionic surfactant 30~40%
Antioxidant 20~40%
The mass percent sum of each material is 100% in additive;
Wherein, reducing agent mass percent can be 30%, 32%, 34%, 36%, 38% or 40% etc.;Non-ionic surface
The mass percent of activating agent can be 30%, 32%, 34%, 36%, 38% or 40% etc.;The mass percent of antioxidant can
For 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38% or 40% etc..
Preferably, the additive includes following components by mass percentage:
Reducing agent 35%
Nonionic surfactant 35%
Antioxidant 30%
The mass percent sum of each material is 100% in additive.
In the present invention, the reducing agent is any one in sodium hypophosphite, potassium hypophosphite, hypophosphorous acid amine or organo-borane
Or at least two combination, it is described combination typical case but non-limiting examples have:The combination of sodium hypophosphite and potassium hypophosphite, hypophosphorous acid
The combination of potassium and hypophosphorous acid amine, the combination of hypophosphorous acid amine and organo-borane, sodium hypophosphite, potassium hypophosphite, hypophosphorous acid amine and organic
Combination of borine etc..
Preferably, the nonionic surfactant is polyoxyethylene alkylaryl ether, polyoxyethylene nonyl phenolic ether, polyoxy second
Any one in allylic alkylation amine, polyoxyethylene sorbitol ester or polyethyleneimine or at least two combination, the combination allusion quotation
Type but non-limiting examples have:The combination of polyoxyethylene alkylaryl ether and polyoxyethylene nonyl phenolic ether, polyoxyethylene nonyl phenolic ether and
The combination of the combination of polyoxyethylene alkyl amine, polyoxyethylene sorbitol ester and polyethyleneimine, polyoxyethylene alkylaryl ether,
The combination of polyoxyethylene nonyl phenolic ether and polyoxyethylene alkyl amine, polyoxyethylene alkylaryl ether, polyoxyethylene nonyl phenolic ether, polyoxy second
The combination of allylic alkylation amine and polyoxyethylene sorbitol ester, polyoxyethylene alkylaryl ether, polyoxyethylene nonyl phenolic ether, polyoxyethylene
Combination of alkylamine, polyoxyethylene sorbitol ester and polyethyleneimine etc..
Preferably, the antioxidant is in ascorbic acid, catechol, resorcinol, hydroquinones or trimesic acid
Any one or at least two combination, the typical but non-limiting example of the combination has:Ascorbic acid and catechol
Combination, the combination of catechol and resorcinol, the combination of resorcinol, hydroquinones and trimesic acid, ascorbic acid, adjacent benzene
The combination of diphenol, resorcinol and hydroquinones, ascorbic acid, catechol, resorcinol, hydroquinones and trimesic acid
Combination etc..
In the present invention, the dosage of reducing agent, nonionic surfactant and antioxidant is not arbitrarily to use, and it is
It can make the optimal scheme of material property by what substantial amounts of experiment repeatedly obtained.
Second aspect, the invention provides the preparation method of above-mentioned tin composition, it the described method comprises the following steps:
Under protective atmosphere, the metal Sn of formula ratio is melted and is warming up to 400~450 DEG C, then put into formula ratio
Metal Bi, metal In, carbon Nano sol and silane coupling agent, 300~350 DEG C are cooled to after 15~30min of magnetic agitation, then added
Enter the additive of formula ratio, after 15~30min of magnetic agitation, be warming up to metal Ag that formula ratio is added after 1100~1200 DEG C and
Ni metal, 30~40min is stood after 10~20min of magnetic agitation, then carry out ingot casting and air cooling is stripped to obtain required product.
Wherein, by metal Sn melt and be warming up to 400~450 DEG C can be 400 DEG C, 405 DEG C, 410 DEG C, 415 DEG C, 420 DEG C,
425 DEG C, 430 DEG C, 435 DEG C, 440 DEG C, 445 DEG C or 450 DEG C etc.;
Be cooled to 300~350 DEG C after 15~30min of magnetic agitation, wherein the magnetic agitation time can be 15min, 20min,
25min or 30min etc., cooling temperature can be 300 DEG C, 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C or 350 DEG C etc.;
The additive of formula ratio is added, after 15~30min of magnetic agitation, is warming up to 1100~1200 DEG C, magnetic force stirs herein
It can be 15min, 20min, 25min or 30min etc. to mix the time, warming temperature can be 1100 DEG C, 1110 DEG C, 1120 DEG C, 1130 DEG C,
1140 DEG C, 1150 DEG C, 1160 DEG C, 1170 DEG C, 1180 DEG C, 1190 DEG C or 1200 DEG C etc.;
The metal Ag and Ni metal of formula ratio are added, stands 30~40min after 10~20min of magnetic agitation, herein magnetic force
Mixing time is 10min, 12min, 14min, 16min, 18min or 20min, time of repose can be 30min, 32min, 34min,
36min, 38min or 40min etc..
In the present invention, the protective atmosphere is any one in nitrogen, helium, neon or argon gas or at least two group
Close, the combination is typical but non-limiting examples have:The combination of the combination of nitrogen and helium, neon and argon gas, nitrogen, helium and
The combination of neon, the combination etc. of nitrogen, helium, neon and argon gas.
In the present invention, the speed of magnetic agitation is 1500~2000r/min, such as 1500r/min, 1600r/min,
1700r/min, 1800r/min, 1900r/min or 2000r/min etc..
The third aspect, the invention provides a kind of electric wire being prepared using above-mentioned tin composition, the electric wire includes
Cored wire and surrounding layer, wherein surrounding layer are made by above-mentioned tin composition, and its specific preparation method is as follows:
The tin composition being prepared is melted first, then cored wire is placed in the melt of tin, during energization long enough
Between, until cored wire surface forms certain tin layers i.e. surrounding layer, normal temperature is cooled to after then cored wire is taken out.
Compared with prior art, the invention has the advantages that:
The present invention improves the performance of the tin composition by controlling metal Ag and Ni metal adding proportion and dosage,
Further improve the performance of the electric wire using the tin composition;And by adding carbon Nano sol and silane coupling agent, to improve
The adaptation of coating and core, coating is set to be coupled with core closer, so as to improve the mechanical performance of electric wire.Using the present invention
Electric wire its tensile strength that middle tin composition is prepared reaches more than 200MPa, and electrical conductivity is 110~130%IACS, thermal conductivity
Rate is 580~630wm-1k-1。
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for help and understands the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1:
The preparation of tin composition:
In a nitrogen atmosphere, 92.3kg metal Sn is melted and is warming up to 425 DEG C, then put into 1kg metal Bi,
The 3- metacryloxy propyl trimethoxy silicanes of 0.5kg metals In, 1kg carbon Nano sol and 1kg, with 1700r/min magnetic
Power stirring 22min after be cooled to 325 DEG C, add formula ratio 3kg additives (wherein, the dosage of sodium hypophosphite is 35wt%,
The dosage of polyoxyethylene alkylaryl ether is 35wt%, and the dosage of ascorbic acid is 30wt%), with 1700r/min magnetic agitations
After 25min, 0.3kg metal Ag and 0.9kg Ni metals are added after being warming up to 1150 DEG C, after 1700r/min magnetic agitations 15min
35min is stood, then ingot casting is carried out and air cooling is stripped to obtain required product.
Then, the tin composition being prepared is melted, cored wire is placed in the melt of tin, be powered enough for a long time,
Until cored wire surface forms certain tin layers i.e. surrounding layer, normal temperature is cooled to after then cored wire is taken out, obtains tinned wire.
Performance test is carried out to tinned wire, tensile strength is measured and reaches more than 230MPa, electrical conductivity 129%IACS,
Thermal conductivity is 627wm-1k-1。
Embodiment 2:
The preparation of tin composition:
In a nitrogen atmosphere, 90.1kg metal Sn is melted and is warming up to 400 DEG C, then put into 1.2kg metal Bi,
The combination of 0.7kg metals In, 1.2kg carbon Nano sol and 1.2kg 2- (3,4- epoxyhexyl) ethyl trimethoxy silane, with
350 DEG C are cooled to after 1500r/min magnetic agitations 30min, adds 4kg additives (wherein, the use of hypophosphorous acid amine of formula ratio
Measure as 40wt%, the dosage of polyoxyethylene alkyl amine is 40wt%, and the dosage of catechol is 20wt%), with 1500r/min magnetic
After power stirring 30min, 0.4kg metal Ag and 1.2kg Ni metals are added after being warming up to 1200 DEG C, with 1500r/min magnetic agitations
40min is stood after 20min, then ingot casting is carried out and air cooling is stripped to obtain required product.
Then, the tin composition being prepared is melted, cored wire is placed in the melt of tin, be powered enough for a long time,
Until cored wire surface forms certain tin layers i.e. surrounding layer, normal temperature is cooled to after then cored wire is taken out, obtains tinned wire.
Performance test is carried out to tinned wire, tensile strength is measured and reaches more than 220MPa, electrical conductivity 121%IACS,
Thermal conductivity is 621wm-1k-1。
Embodiment 3:
The preparation of tin composition:
In a nitrogen atmosphere, 94.8kg metal Sn is melted and is warming up to 450 DEG C, then put into 0.7kg metal Bi,
0.3kg metals In, 0.7kg carbon Nano sol and 0.7kg 2- (3,4- epoxyhexyl) ethyl trimethoxy silane, with 2000r/
300 DEG C are cooled to after min magnetic agitations 15min, adding the 2kg additives of formula ratio, (wherein, the dosage of organo-borane is
30wt%, the dosage of polyoxyethylene sorbitol ester is 30wt%, and the dosage of hydroquinones is 40wt%), with 2000r/min magnetic
After power stirring 15min, 0.2kg metal Ag and 0.6kg Ni metals are added after being warming up to 1100 DEG C, with 2000r/min magnetic agitations
30min is stood after 10min, then ingot casting is carried out and air cooling is stripped to obtain required product.
Then, the tin composition being prepared is melted, cored wire is placed in the melt of tin, be powered enough for a long time,
Until cored wire surface forms certain tin layers i.e. surrounding layer, normal temperature is cooled to after then cored wire is taken out, obtains tinned wire.
Performance test is carried out to tinned wire, tensile strength is measured and reaches more than 211MPa, electrical conductivity 118%IACS,
Thermal conductivity is 589wm-1k-1。
Embodiment 4:
Except each component dosage is component:Metal Bi is 1.5kg, metal In is 1.0kg, metal Ag is 0.5kg, Ni metal is
1.5kg, carbon Nano sol are 1.5kg, silane coupling agent 1.5kg, additive are 5kg and metal Sn is outside 87.5kg, its
His step is in the same manner as in Example 1, to obtained tinned wire carry out performance test, measure tensile strength reach 208MPa with
On, electrical conductivity 116%IACS, thermal conductivity 588wm-1k-1。
Embodiment 5:
Except each component dosage is:Metal Bi is 0.5kg, metal In is 0.1kg, metal Ag is 0.1kg, Ni metal is
0.3kg, carbon Nano sol are 0.5kg, silane coupling agent 0.5kg, additive are 1kg and metal Sn is outside 97kg, other
Step is in the same manner as in Example 1, to obtained tinned wire carry out performance test, measure tensile strength reach 209MPa with
On, electrical conductivity 119%IACS, thermal conductivity 585wm-1k-1。
Comparative example 1:
In addition to not adding metal Ag, other steps are in the same manner as in Example 1, and performance is carried out to obtained tinned wire
Test, measures tensile strength and reaches more than 179MPa, electrical conductivity 99%IACS, thermal conductivity 501wm-1k-1。
Comparative example 2:
In addition to not adding Ni metal, other steps are in the same manner as in Example 1, and performance is carried out to obtained tinned wire
Test, measures tensile strength and reaches more than 179MPa, electrical conductivity 99%IACS, thermal conductivity 501wm-1k-1。
Comparative example 3:
In addition to metal Ag mass percent is 4%, other steps are in the same manner as in Example 1, to obtained tin plating
Electric wire carries out performance test, measures tensile strength and reaches more than 180MPa, electrical conductivity 101%IACS, thermal conductivity 512wm-1k-1。
Comparative example 4:
In addition to the mass percent of Ni metal is 4%, other steps are in the same manner as in Example 1, to obtained tin plating
Electric wire carries out performance test, measures tensile strength and reaches more than 179MPa, electrical conductivity 103%IACS, thermal conductivity 509wm-1k-1。
Comparative example 5:
Except Ni metal and metal Ag mass ratio are 5:Outside 1, other steps are in the same manner as in Example 1, to obtained
Tinned wire carries out performance test, measures tensile strength and reaches more than 184MPa, electrical conductivity 94%IACS, thermal conductivity is
531wm-1k-1。
Both Ag and Cu are can be seen that with reference to comparative example 1-5 and embodiment 1-5 result to be combined and follow certain
Proportioning can have a significant impact to the combination property of product.
Comparative example 6:
In addition to not adding carbon Nano sol, other steps are in the same manner as in Example 1, and obtained tinned wire is carried out
Performance test, measure tensile strength and reach more than 181MPa, electrical conductivity 102%IACS, thermal conductivity 529wm-1k-1。
Comparative example 7:
In addition to not adding silane coupling agent, other steps are in the same manner as in Example 1, and obtained tinned wire is carried out
Performance test, measure tensile strength and reach more than 177MPa, electrical conductivity 99%IACS, thermal conductivity 521wm-1k-1。
Comparative example 8:
In addition to not adding carbon Nano sol and silane coupling agent, other steps are in the same manner as in Example 1, to obtained
Tinned wire carries out performance test, measures tensile strength and reaches more than 170MPa, electrical conductivity 91%IACS, thermal conductivity is
501wm-1k-1。
Integrated embodiment 1-5 and comparative example 7-8 result can be seen that addition carbon Nano sol and silane coupling agent, come
Improve the adaptation of coating and core, coating is coupled with core closer, so as to improve the mechanical performance of electric wire.
In summary, the present invention improves the tin combination by controlling metal Ag and Ni metal adding proportion and dosage
The performance of thing, further improve the performance of the electric wire using the tin composition;And coupled by adding carbon Nano sol and silane
Agent, to improve the adaptation of coating and core, coating is set to be coupled with core closer, so as to improve the mechanical performance of wire.
Using the electric wire that tin composition is prepared in the present invention, its tensile strength reaches more than 200MPa, and electrical conductivity is 110~130%
IACS, thermal conductivity are 580~630wm-1k-1。
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (9)
1. the tin plating preparation method with tin composition of a kind of electric wire, it is characterised in that the tin composition is as shared by each component
Mass percent meter includes following components:
Ni metal and metal Ag mass ratio are 3 in the tin composition:1;
The silane coupling agent is 3- metacryloxies propyl trimethoxy silicane, 2- (3,4- epoxyhexyls) ethyl trimethoxy
Any one in base silane or 3- glycidoxypropyltrime,hoxysilanes or at least two combination;
The additive includes following components by mass percentage:
Reducing agent 30~40%
Nonionic surfactant 30~40%
Antioxidant 20~40%
The mass percent sum of each material is 100% in additive;
It the described method comprises the following steps:
Under protective atmosphere, the metal Sn of formula ratio is melted and is warming up to 400~450 DEG C, then put into the metal of formula ratio
Bi, metal In, carbon Nano sol and silane coupling agent, 300~350 DEG C are cooled to after 15~30min of magnetic agitation, adds and matches somebody with somebody
The additive just measured, after 15~30min of magnetic agitation, it is warming up to the metal Ag and metal that formula ratio is added after 1100~1200 DEG C
30~40min is stood after Cu, 10~20min of magnetic agitation, then ingot casting is carried out and air cooling is stripped to obtain required product.
2. preparation method according to claim 1, it is characterised in that quality percentage of the composition as shared by each component
Include following components than meter:
3. preparation method according to claim 1 or 2, it is characterised in that quality of the composition as shared by each component
Percentages include following components:
4. preparation method according to claim 1, it is characterised in that the additive includes following by mass percentage
Component:
Reducing agent 35%
Nonionic surfactant 35%
Antioxidant 30%
The mass percent sum of each material is 100% in additive.
5. preparation method according to claim 1, it is characterised in that the reducing agent is sodium hypophosphite, potassium hypophosphite, secondary
Any one in phosphamide or organo-borane or at least two combination.
6. preparation method according to claim 1, it is characterised in that the nonionic surfactant is polyoxyethylene alkane
It is any one in base aryl ether, polyoxyethylene nonyl phenolic ether, polyoxyethylene alkyl amine, polyoxyethylene sorbitol ester or polyethyleneimine
Kind or at least two combination.
7. preparation method according to claim 1, it is characterised in that the antioxidant be ascorbic acid, catechol,
Any one in resorcinol, hydroquinones or trimesic acid or at least two combination.
8. preparation method according to claim 1, it is characterised in that the protective atmosphere is nitrogen, helium, neon or argon
Any one in gas or at least two combination.
9. preparation method according to claim 1, it is characterised in that the speed of magnetic agitation is 1500~2000r/min.
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