Summary of the invention:
One of the object of the invention provides a kind of lightweight, cost is low, anti-oxidant, corrosion-resistant and the silvered aluminum powder of stable performance; Two of purpose provides and can at room temperature react, and technology is simple, the preparation method of easy to operate silvered aluminum powder; Three of purpose provides the application of this silvered aluminum powder.
One of the object of the invention can be realized through following technical measures:
Aluminium powder is made up of alumina particles, and alumina particles is connected with silver metal coating outward, and silver metal coating is connected with the organic material protective layer outward.
One of the object of the invention also can be realized through following technical measures:
The granularity of described aluminium powder is the 200-1500 order, and shape can be spherical a, sheet or polygon-shaped etc.
Described organic material protective layer is to soak certain hour with joining in the organic acid ester mixed liquor through silver-plated aluminium powder, the organic matter protective layer of the layer of protecting silver coating that outside silver coating, forms.
Two of the object of the invention can be realized through following technical measures:
This preparation method (one):
A. be the copper-bath of 5-50g/L according to concentration earlier: concentration is disodium edta solution=5-20 of 10-80g/L: 10-30 weight portion proportioning is mixed, and stirs 20-40 minute, makes its abundant complexing; Regulate pH=7.5-10 with ammoniacal liquor then; Again aluminium powder is inserted, then add or do not add the fluoride aqueous solution that concentration is 0.5-5g/L again, continue to stir; Treat that plating bath clarification after washing to neutral, gets the copper facing aluminium powder; Also can add sodium hydroxide solution auxiliary adjustment pH value in this step, like this, can reduce the addition of ammoniacal liquor, reduce the volatilization of ammoniacal liquor, be more conducive to operation; Through adding fluoride, fluorine ion helps accelerating the dissolving of aluminium oxide as aluminum ions complexing agent;
B. according to aluminium powder: silver nitrate=100: 5-45 weight portion proportioning, get silver nitrate and add 10-35 times of water gaging, get silver nitrate aqueous solution;
C. the copper facing aluminium powder of a step being placed concentration is the disodium edta aqueous solution of 0.005-0.1g/L, under 20-80 ℃, stirs 5-20 minute; And then in stirring the silver nitrate aqueous solution that slowly adds the b step down, continue to stir 30-80min, make silver displace copper ion; Let deposition of silver on the aluminium powder surface, add the reducing agent of aluminium powder 0.001-0.05 weight portion again, the silver ion of trace in the reducing solution; It also is deposited on the aluminium powder surface; Form the fine and close silver-colored protective layer of one deck, reaction finish after clean, centrifugal filtration, silvered aluminum powder;
D. in the silvered aluminum powder of c step, add organic acid ester mixed liquid dipping 0.5-2h, filtration drying gets product.
This preparation method (two)
A. earlier aluminium powder is inserted in the fluoride aqueous solution that concentration is 0.5-5g/L, stirring slow down adding concentration is the copper-bath of 5-50g/L, treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder;
B. according to aluminium powder: silver nitrate=100: 5-45 weight portion proportioning, get silver nitrate and add 10-35 times of water gaging, get silver nitrate aqueous solution;
C. the copper facing aluminium powder of a step being placed concentration is the disodium edta aqueous solution of 0.005-0.1g/L; Under 20-80 ℃, stirred 5-20 minute, and then in stirring the silver nitrate aqueous solution that slowly adds the b step down; Continue to stir 30-80min; The reducing agent that adds aluminium powder 0.001-0.05 weight portion again, reaction finish after clean, centrifugal filtration, silvered aluminum powder;
D. in the silvered aluminum powder of c step, add organic acid ester mixed liquid dipping 0.5-2h, filtration drying gets product.
This preparation method (three)
A. according to aluminium powder: silver nitrate=100: 5-45 weight portion proportioning, get silver nitrate and add 10-35 times of water gaging, get silver nitrate aqueous solution;
B. aluminium powder is inserted in the fluoride aqueous solution that concentration is 0.5-5g/L; Stir the silver nitrate aqueous solution that slowly adds a step down, continue to stir 30-80min, add the reducing agent of aluminium powder 0.001-0.05 weight portion then; Reaction finish after clean, centrifugal filtration, silvered aluminum powder;
C. in the silvered aluminum powder of b step, add organic acid ester mixed liquid dipping 0.5-2h, filtration drying gets product.
Two of the object of the invention also can be realized through following technical measures:
Described disodium edta is any one in Monosodium Edetate salt, disodium EDTA, sodium versenate salt, the tetrasodium salt of EDTA; Described reducing agent is glucose, tartaric acid, fructose, oxalic acid or formaldehyde; Described reducing agent is the mixed liquor that glucose and tartaric acid mix with arbitrary proportion; Described organic acid ester mixed liquor is by titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: (0.8-1.5): (0.2-0.8): (15-25): (55-70) the weight portion proportioning mixes; Described fluoride is sodium fluoride or ammonium fluoride.
Three of the object of the invention can be realized through following technical measures:
The silvered aluminum powder that silvered aluminum powder of the present invention or the present invention are prepared from is applied to conduction, electromagnetic shielding, antistatic technique field.
Silvered aluminum powder is as a kind of functional properties conductivity filler; Can it be made an addition to and process goods such as conduction, electromagnetic shielding, antistatic in coating, adhesive, printing ink, plastics, the rubber, be widely used in conduction, electromagnetic shielding, the antistatic field of departments such as electronics, electromechanics, communication, printing, Aero-Space.
The same silver-plated copper powder of silvered aluminum powder of the present invention, silver-plated nickel powder are compared, and it has the following advantages: (1) light weight, and the density of aluminium powder is lower than copper powder, nickel powder, and therefore, the silvered aluminum powder quality of acquisition is light than silver-plated copper powder, silver-plated nickel powder; (2) cost is low, and the price of aluminium powder is lower than copper powder, nickel powder, and therefore, under the identical silver content, the cost of silvered aluminum powder is lower; (3) good corrosion resistance, silvered aluminum powder have anti electromagnet interference function preferably in the brine spray environment, can be widely used in the terminal electronic encapsulating products; (4) look shallow, because the color of silver-plated copper powder and silver-plated nickel powder is dark, can not select for use in some field.And silvered aluminum powder mainly is canescence and field gray, is a kind of light-colored conductive filler.Therefore, have and decorate and high reflection double effects, be widely used in the nonmetal product surface of electronics industry, aerospace industry and war industry etc.
The present invention be advantageous in that: need not complicated pre-treatment, reaction at room temperature, technology is simple, and is easy to operate, and need not add expensive reducing agent, stabilizing agent, and the coating impurity that obtains is few, the low and stable performance of cost.
The specific embodiment:
Following examples are that silvered aluminum powder is preferably filled a prescription; These non-limiting embodiments of filling a prescription; Just be used to specify the present invention, those skilled in the art can be protection scope of the present invention according to thinking of the present invention and the prescription that the proportioning of selecting materials filters out fully.
Embodiment 1:
A. be the copper-bath of 5g/L according to concentration earlier: concentration is Monosodium Edetate salting liquid=weight portion proportioning mixing in 5: 30 of 80g/L; Stirred 20 minutes, and made its abundant complexing, regulate pH=10 with ammoniacal liquor then; Again the aluminium powder of 200 order spherical aluminium particles is inserted; Continuation is stirred, and treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder;
B. according to aluminium powder: silver nitrate=100: 45 weight portion proportionings, get silver nitrate and add 10 times of water gagings, get silver nitrate aqueous solution;
C. the copper facing aluminium powder of a step being placed concentration is the Monosodium Edetate saline solution of 0.005g/L, under 80 ℃, stirred 5 minutes, and then in stirring down; Be controlled at the silver nitrate aqueous solution that slowly drips the b step in 60 minutes, continue again to stir 30min, make silver displace copper ion; Let deposition of silver on the aluminium powder surface, add the tartaric acid of aluminium powder 0.05 weight portion again, the silver ion of trace in the reducing solution; It also is deposited on the aluminium powder surface, forms the fine and close silver-colored protective layer of one deck, continue reaction 10 minutes; Reaction finishes the back to be cleaned reaction solution with distilled water and adds acetone again, filters the back and use oven for drying, gets silvered aluminum powder;
D. in the silvered aluminum powder of c step, add and use titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: 0.8: 0.8: the organic acid ester mixed liquor that 15: 55 weight portion proportionings mix; Soak 0.5h; Filtration drying; Promptly obtain the uniform aluminium powder 1 outer silvering 2 that is connected with of plating, the silvering 2 outer silvered aluminum powder products that are connected with organic material protective layer 3.
Embodiment 2:
A. be the copper-bath of 50g/L according to concentration earlier: concentration is Monosodium Edetate salting liquid=weight portion proportioning mixing in 20: 10 of 10g/L; Stirred 40 minutes, and made its abundant complexing, regulate pH=7.5 with ammoniacal liquor then; Again the aluminium powder of 1500 order spherical aluminium particles is inserted; Continuation is stirred, and treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder;
B. according to aluminium powder: silver nitrate=100: 5 weight portion proportionings, get silver nitrate and add 25 times of water gagings, get silver nitrate aqueous solution;
C. the copper facing aluminium powder of a step being placed concentration is the Monosodium Edetate saline solution of 0.1g/L, under 20 ℃, stirred 20 minutes, and then in stirring down; Be controlled at the silver nitrate aqueous solution that slowly drips the b step in 20 minutes, continue again to stir 80min, make silver displace copper ion; Let deposition of silver on the aluminium powder surface, add the tartaric acid of aluminium powder 0.001 weight portion again, the silver ion of trace in the reducing solution; It also is deposited on the aluminium powder surface, forms the fine and close silver-colored protective layer of one deck, continue reaction 20 minutes; Reaction finishes the back to be cleaned reaction solution with distilled water and adds acetone again, filters the back and use oven for drying, gets silvered aluminum powder;
D. in the silvered aluminum powder of c step, add and use titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: 1.5: 0.2: the organic acid ester mixed liquor that 25: 70 weight portion proportionings mix; Soak 2h; Filtration drying; Promptly obtain the uniform aluminium powder 1 outer silvering 2 that is connected with of plating, the silvering 2 outer silvered aluminum powder products that are connected with organic material protective layer 3.
Embodiment 3:
A. be the copper-bath of 25g/L according to concentration earlier: concentration is Monosodium Edetate salting liquid=weight portion proportioning mixing in 12: 20 of 50g/L; Stirred 30 minutes, and made its abundant complexing, regulate pH=9.0 with ammoniacal liquor then; Again the aluminium powder of 800 order spherical aluminium particles is inserted; Continuation is stirred, and treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder;
B. according to aluminium powder: silver nitrate=100: 25 weight portion proportionings, get silver nitrate and add 20 times of water gagings, get silver nitrate aqueous solution;
C. the copper facing aluminium powder of a step being placed concentration is the Monosodium Edetate saline solution of 0.05g/L, under 50 ℃, stirred 12 minutes, and then in stirring down; Be controlled at the silver nitrate aqueous solution that slowly drips the b step in 40 minutes, continue again to stir 50min, make silver displace copper ion; Let deposition of silver on the aluminium powder surface, add the tartaric acid of aluminium powder 0.01 weight portion again, the silver ion of trace in the reducing solution; It also is deposited on the aluminium powder surface, forms the fine and close silver-colored protective layer of one deck, continue reaction 15 minutes; Reaction finishes the back to be cleaned reaction solution with distilled water and adds acetone again, filters the back and use oven for drying, gets silvered aluminum powder;
D. in the silvered aluminum powder of c step, add and use titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: 1.2: 0.5: the organic acid ester mixed liquor that 20: 60 weight portion proportionings mix; Soak 1.0h; Filtration drying; Promptly obtain the uniform aluminium powder 1 outer silvering 2 that is connected with of plating, the silvering 2 outer silvered aluminum powder products that are connected with organic material protective layer 3.
Embodiment 4:
Different is in a step, to add the Fluorinse quickening alumina dissolution that concentration is 0.5-5g/L, and all the other are respectively with embodiment 1-3.
Embodiment 5:
Different is in a step, to add sodium hydroxide solution auxiliary adjustment pH value, and all the other are respectively with embodiment 1-4.
Embodiment 6:
Different is that step a. puts into pure water stirring 20 minutes with the aluminium powder of 200 order spherical aluminium particles earlier; Insert then in the Fluorinse that concentration is 0.5g/L; Stirring slow down adding concentration is the copper-bath of 50g/L, treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder; All the other are respectively with embodiment 1-3.
Embodiment 7:
Different is that step a. puts into pure water stirring 20 minutes with the aluminium powder of 1500 order spherical aluminium particles earlier; Insert then in the Fluorinse that concentration is 5g/L; Stirring slow down adding concentration is the copper-bath of 5g/L, treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder; All the other are respectively with embodiment 1-3.
Embodiment 8:
Different is that step a. puts into pure water stirring 20 minutes with the aluminium powder of 800 order spherical aluminium particles earlier; Insert then in the Fluorinse that concentration is 3g/L; Stirring slow down adding concentration is the copper-bath of 25g/L, treats that plating bath clarification after washing to neutral, gets the copper facing aluminium powder; All the other are respectively with embodiment 1-3.
Embodiment 9:
A. according to aluminium powder: silver nitrate=100: 5 weight portion proportionings, get silver nitrate and add 10 times of water gagings, get silver nitrate aqueous solution;
B. earlier the aluminium powder of 200 order spherical aluminium particles is put into pure water and stirred 20 minutes, stir then and be controlled at the silver nitrate aqueous solution that slowly adds a step in 20 minutes down, continue to stir 80min; Make silver displace copper ion, let deposition of silver on the aluminium powder surface, add the tartaric acid of aluminium powder 0.001 weight portion again; The silver ion of trace also is deposited on the aluminium powder surface it in the reducing solution, forms the fine and close silver-colored protective layer of one deck; Continue reaction 10 minutes; Reaction finishes the back to be cleaned reaction solution with distilled water and adds acetone again, filters the back and use oven for drying, gets silvered aluminum powder;
C. in the silvered aluminum powder of b step, add and use titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: 0.8: 0.8: the organic acid ester mixed liquor that 15: 55 weight portion proportionings mix; Soak 0.5h; Filtration drying; Promptly obtain the uniform aluminium powder 1 outer silvering 2 that is connected with of plating, the silvering 2 outer silvered aluminum powder products that are connected with organic material protective layer 3.
Embodiment 10:
A. according to aluminium powder: silver nitrate=100: 45 weight portion proportionings, get silver nitrate and add 35 times of water gagings, get silver nitrate aqueous solution;
B. earlier the aluminium powder of 1500 order spherical aluminium particles is put into pure water and stirred 5 minutes, stir then and be controlled at the silver nitrate aqueous solution that slowly adds a step in 60 minutes down, continue to stir 30min; Make silver displace copper ion, let deposition of silver on the aluminium powder surface, add the tartaric acid of aluminium powder 0.05 weight portion again; The silver ion of trace also is deposited on the aluminium powder surface it in the reducing solution, forms the fine and close silver-colored protective layer of one deck; Continue reaction 20 minutes; Reaction finishes the back to be cleaned reaction solution with distilled water and adds acetone again, filters the back and use oven for drying, gets silvered aluminum powder;
C. in the silvered aluminum powder of b step, add and use titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: 1.5: 0.2: the organic acid ester mixed liquor that 25: 70 weight portion proportionings mix; Soak 2.0h; Filtration drying; Promptly obtain the uniform aluminium powder 1 outer silvering 2 that is connected with of plating, the silvering 2 outer silvered aluminum powder products that are connected with organic material protective layer 3.
Embodiment 11:
A. according to aluminium powder: silver nitrate=100: 25 weight portion proportionings, get silver nitrate and add 20 times of water gagings, get silver nitrate aqueous solution;
B. earlier the aluminium powder of 800 order spherical aluminium particles is put into pure water and stirred 10 minutes, insert then in the Fluorinse that concentration is 3.0g/L, stir and be controlled at the silver nitrate aqueous solution that slowly adds a step in 40 minutes down; Continue to stir 50min, make silver displace copper ion, let deposition of silver on the aluminium powder surface; The tartaric acid that adds aluminium powder 0.01 weight portion again, the silver ion of trace also is deposited on the aluminium powder surface it in the reducing solution; The fine and close silver-colored protective layer of formation one deck continues reaction 15 minutes, and reaction end back is cleaned reaction solution with distilled water and added acetone again; Filter the back and use oven for drying, get silvered aluminum powder;
C. in the silvered aluminum powder of b step, add and use titanate esters: fatty acid ester: n-propyl gallate: xylenes: acetone=1: 1.2: 0.5: the organic acid ester mixed liquor that 20: 60 weight portion proportionings mix; Soak 1.0h; Filtration drying; Promptly obtain the uniform aluminium powder 1 outer silvering 2 that is connected with of plating, the silvering 2 outer silvered aluminum powder products that are connected with organic material protective layer 3.
Embodiment 12:
Different is to replace sodium fluoride with ammonium fluoride, and all the other are respectively with embodiment 4,6-11.
Embodiment 13:
With embodiment 1-8, different is in a and c step, to replace Monosodium Edetate salt with disodium EDTA.
Embodiment 14:
With embodiment 1-8, different is in a and c step, to replace Monosodium Edetate salt with sodium versenate salt.
Embodiment 15:
With embodiment 1-8, different is in a and c step, to replace Monosodium Edetate salt with tetrasodium salt of EDTA.
Embodiment 16:
With embodiment 1-15 different be in a step, to replace spherical aluminium powder with sheet shape aluminium powder.
Embodiment 17:
With embodiment 1-15, different is in a step, to replace spherical aluminium powder with polygon-shaped aluminium powder.
Embodiment 18:
Different is in the c step, to replace tartaric acid with glucose, and all the other are respectively with embodiment 1-17.
Embodiment 19
Different is in the c step, to replace tartaric acid with fructose, and all the other are respectively with embodiment 1-17.
Embodiment 20:
Different is in the c step, to replace tartaric acid with oxalic acid, and all the other are respectively with embodiment 1-17.
Embodiment 21:
Different is in the c step, to replace tartaric acid with formaldehyde, and all the other are respectively with embodiment 1-17.
Embodiment 22:
Different is in the c step, to replace tartaric acid with glucose and tartaric acid with the mixed liquor that arbitrary proportion mixes, and all the other are respectively with embodiment 1-17.