CN109741852A - A kind of composite conducting material and preparation method thereof - Google Patents
A kind of composite conducting material and preparation method thereof Download PDFInfo
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- CN109741852A CN109741852A CN201811563388.0A CN201811563388A CN109741852A CN 109741852 A CN109741852 A CN 109741852A CN 201811563388 A CN201811563388 A CN 201811563388A CN 109741852 A CN109741852 A CN 109741852A
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Abstract
The present invention provides a kind of composite conducting materials and preparation method thereof, including following preparation step: vitreous copper being cleaned up, dries, mixes with ethanol solution, is crushed, is filtered, drying obtains vitreous copper powder；Obtained vitreous copper powder is further crushed using airslide disintegrating mill, is then mixed with modifier solution and carries out modified-reaction, dry after reaction, grinding obtains modified vitreous copper powder after crushing；Nano zine oxide is dissolved in acetone, titanate coupling agent is then added, is stirred, is filtered, drying obtains modified nano zinc oxide；Alpha-quartz, modified vitreous copper powder, modified nano zinc oxide, terbium sesquioxide, adhesive, dispersant is uniform, it is then press-formed, composite conducting material is obtained after sintering.Preparation method is simple by the present invention, is advantageously implemented large-scale production, the Electrical Conductivity of Composites being prepared can achieve 40.55-46.63Ms/m, and tensile strength can reach 522.37-603.73MPa, and hardness can achieve 80.5-88.5.
Description
Technical field
The present invention relates to Material Fields, more particularly to a kind of composite conducting material and preparation method thereof.
Background technique
In the process of processing and using, electrostatic phenomenon is extremely serious for material, in some cases, not only will affect material
Service performance, or even also will cause harm, make material spark due to caused by electrostatic and occurs to explode and burn.Conductive composite wood
The electrostatic capacity of material can be improved in material, to produce and process and using bringing great convenience, improving safety.In addition, aviation,
Requirement of the high-tech such as space flight, electromechanics, electronics to material property is increasingly harsh, index needed for developing according to microelectric technique, material
Material must have certain tensile strength and conductivity.Vitreous copper is largely original sulfides oxygenolysis again through reduction
Made of secondary mineral, it is high containing copper component, be a kind of more potential conductive material, conducting powder is made in vitreous copper by the present invention
End, and vitreous copper powder is modified with fatty alcohol ethylene oxide ether phosphate salt LBH400, its electric conductivity is improved, it is other
The synergistic effect of ingredient, making material integrally has good electric conductivity, higher intensity and hardness.
Summary of the invention
Technical problems to be solved:
It is an object of the present invention to solve the deficiency of the existing technology and provide a kind of composite conducting material and its preparation sides
Method.
Technical solution:
The present invention provides a kind of preparation methods of composite conducting material, including following preparation step:
Step 1: vitreous copper is cleaned up, 70 DEG C of drying are mixed with ethanol solution, then broken with Ultrasonic Pulverization instrument,
It takes out and filters, be placed in drying in drier and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
Then the vitreous copper powder of 800 mesh mixes with modifier solution and carries out modified-reaction, drying for 24 hours, is ground at 90 DEG C after reaction
Mill obtains modified vitreous copper powder after crushing；
Step 3: nano zine oxide is dissolved in acetone, then it is added and uses the diluted titanate coupling agent of acetone, 3000r/
Min stirs 20min, filters, drying obtains modified nano zinc oxide；
Step 4: by 60-80 parts of alpha-quartzs, 22-28 parts of modified vitreous copper powders, 10-14 parts of modified nano zinc oxides, 4-
8 parts of terbium sesquioxides, 6-12 parts of adhesives, 12-18 parts of dispersants are uniform, are then press-formed under 100MPa pressure,
In nitrogen atmosphere, composite conducting material is obtained after sintering.
Preferably, the solid-liquid ratio of vitreous copper and ethanol solution is 1:(300-500 in step 1), solid-liquid ratio unit is g/
mL。
Preferably, the temperature of modified-reaction is 60-80 DEG C in step 2, reaction time 30-50min.
Preferably, the solid-liquid ratio of vitreous copper powder and modifier solution is 1:(20-40 in step 2), solid-liquid ratio unit is
g/mL。
Preferably, modifier solution is fatty alcohol ethylene oxide ether phosphate salt and ethyl alcohol according to volume ratio 1:2 in step 2
It mixes.
Preferably, the mass ratio of titanate coupling agent and zinc oxide is (0.05-0.08) in step 3: 1.
Preferably, sintering temperature is 1100 DEG C -1500 DEG C in step 4, sintering time 3h.
The utility model has the advantages that
Preparation method is simple by the present invention, is advantageously implemented large-scale production, the composite conducting material tool being prepared
There are good electric conductivity, higher intensity and hardness, the Electrical Conductivity of Composites being prepared can achieve 40.55-
46.63Ms/m, tensile strength can reach 522.37-603.73MPa, and hardness can achieve 80.5-88.5；
The present invention is modified vitreous copper powder with fatty alcohol ethylene oxide ether phosphate salt LBH400, fatty alcohol ethylene oxide
Ether phosphate salt LBH400 can preferably be adsorbed in vitreous copper powder surface, improve its electric conductivity；
As conductive compositions after being modified in the present invention using vitreous copper, while it being added to terbium sesquioxide, vitreous copper
In contain a large amount of copper, terbium sesquioxide is present in material with compound form, is distributed in granular form transgranular, can be improved
The conductivity of copper；
Nano zine oxide is added in the present invention, zinc plays the role of solution strengthening and refined crystalline strengthening to copper, can significantly mention
The integral strength and hardness of high material, the addition of terbium sesquioxide play the role of deoxidation, purification and refinement crystal grain, improve material
Electric conductivity.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit this in any way
Invention.
Embodiment 1
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh, then mixes with modifier solution, and modifier solution is fatty alcohol ethylene oxide ether phosphate salt
LBH400 and ethyl alcohol are mixed according to volume ratio 1:2, and the solid-liquid ratio of vitreous copper powder and modifier solution is 1:30 (g/mL),
The modified-reaction 40min at 70 DEG C, it is then dry at 90 DEG C to grind for 24 hours, modified vitreous copper powder is obtained after crushing；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 80 parts of alpha-quartzs, 22 parts of modified vitreous copper powders, 14 parts of modified nano zinc oxides, 4 part of three oxidation two
Terbium, 12 parts of polytetrafluoroethylene (PTFE), 12 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed, in nitrogen under 100MPa pressure
During atmosphere is enclosed, 3h is sintered at 1500 DEG C and obtains composite conducting material.
Embodiment 2
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh, then mixes with modifier solution, and modifier solution is fatty alcohol ethylene oxide ether phosphate salt
LBH400 and ethyl alcohol are mixed according to volume ratio 1:2, and the solid-liquid ratio of vitreous copper powder and modifier solution is 1:30 (g/mL),
The modified-reaction 40min at 70 DEG C, it is then dry at 90 DEG C to grind for 24 hours, modified vitreous copper powder is obtained after crushing；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 60 parts of alpha-quartzs, 28 parts of modified vitreous copper powders, 10 parts of modified nano zinc oxides, 8 part of three oxidation two
Terbium, 6 parts of polytetrafluoroethylene (PTFE), 18 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed, in nitrogen under 100MPa pressure
During atmosphere is enclosed, 3h is sintered at 1100 DEG C DEG C and obtains composite conducting material.
Embodiment 3
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh, then mixes with modifier solution, and modifier solution is fatty alcohol ethylene oxide ether phosphate salt
LBH400 and ethyl alcohol are mixed according to volume ratio 1:2, and the solid-liquid ratio of vitreous copper powder and modifier solution is 1:30 (g/mL),
The modified-reaction 40min at 70 DEG C, it is then dry at 90 DEG C to grind for 24 hours, modified vitreous copper powder is obtained after crushing；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 75 parts of alpha-quartzs, 24 parts of modified vitreous copper powders, 13 parts of modified nano zinc oxides, 5 part of three oxidation two
Terbium, 10 parts of polytetrafluoroethylene (PTFE), 14 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed, in nitrogen under 100MPa pressure
During atmosphere is enclosed, 3h is sintered at 1400 DEG C and obtains composite conducting material.
Embodiment 4
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh, then mixes with modifier solution, and modifier solution is fatty alcohol ethylene oxide ether phosphate salt
LBH400 and ethyl alcohol are mixed according to volume ratio 1:2, and the solid-liquid ratio of vitreous copper powder and modifier solution is 1:30 (g/mL),
The modified-reaction 40min at 70 DEG C, it is then dry at 90 DEG C to grind for 24 hours, modified vitreous copper powder is obtained after crushing；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 65 parts of alpha-quartzs, 26 parts of modified vitreous copper powders, 11 parts of modified nano zinc oxides, 7 part of three oxidation two
Terbium, 8 parts of polytetrafluoroethylene (PTFE), 16 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed, in nitrogen under 100MPa pressure
During atmosphere is enclosed, 3h is sintered at 1200 DEG C DEG C and obtains composite conducting material.
Embodiment 5
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh, then mixes with modifier solution, and modifier solution is fatty alcohol ethylene oxide ether phosphate salt
LBH400 and ethyl alcohol are mixed according to volume ratio 1:2, and the solid-liquid ratio of vitreous copper powder and modifier solution is 1:30 (g/mL),
The modified-reaction 40min at 70 DEG C, it is then dry at 90 DEG C to grind for 24 hours, modified vitreous copper powder is obtained after crushing；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 70 parts of alpha-quartzs, 25 parts of modified vitreous copper powders, 12 parts of modified nano zinc oxides, 6 part of three oxidation two
Terbium, 9 parts of polytetrafluoroethylene (PTFE), 15 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed, in nitrogen under 100MPa pressure
During atmosphere is enclosed, 3h is sintered at 1300 DEG C and obtains composite conducting material.
Comparative example 1
This comparative example is not the difference from embodiment 1 is that be modified vitreous copper powder.Specifically:
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 80 parts of alpha-quartzs, 22 parts of vitreous copper powders, 14 parts of modified nano zinc oxides, 4 parts of terbium sesquioxides,
12 parts of polytetrafluoroethylene (PTFE), 12 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed, in nitrogen under 100MPa pressure
In atmosphere, 3h is sintered at 1500 DEG C and obtains composite conducting material.
Comparative example 2
This comparative example is not the difference from embodiment 1 is that add terbium sesquioxide.Specifically:
Step 1: vitreous copper is cleaned up, 70 DEG C of drying, with 65wt% ethanol solution according to solid-liquid ratio 1:400 (g/
ML it) mixes, is then crushed 55h with Ultrasonic Pulverization instrument, take out and filter, be placed in drying in 60 DEG C of driers and obtain vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200- is filtered out
The vitreous copper powder of 800 mesh, then mixes with modifier solution, and modifier solution is fatty alcohol ethylene oxide ether phosphate salt
LBH400 and ethyl alcohol are mixed according to volume ratio 1:2, and the solid-liquid ratio of vitreous copper powder and modifier solution is 1:30 (g/mL),
The modified-reaction 40min at 70 DEG C, it is then dry at 90 DEG C to grind for 24 hours, modified vitreous copper powder is obtained after crushing；
Step 3: nano zine oxide is dissolved in acetone, solid-liquid ratio is 1:10 (g/mL), and then addition dilutes 2 with acetone
The mass ratio of titanate coupling agent NTC401 again, titanate coupling agent NTC401 and zinc oxide is 0.065:1,3000r/min
20min is stirred, is then filtered, drying obtains modified nano zinc oxide；
Step 4: by 80 parts of alpha-quartzs, 22 parts of modified vitreous copper powders, 14 parts of modified nano zinc oxides, 12 parts of polytetrafluoros
Ethylene, 12 parts of dehydrated alcohols are uniformly mixed, then ball milling 3h is press-formed under 100MPa pressure, in nitrogen atmosphere, in
It is sintered 3h at 1500 DEG C and obtains composite conducting material.
The composite conducting material being prepared in embodiment 1-5 and comparative example 1-2 is tested for the property:
With the electric conductivity of double bridge method measurement sample, hardness is measured on HB-300 Brinell hardness tester, in WE-30 type ten thousand
Aircraft measurements tensile strength can be tested, test result see the table below 1:
Table 1
By test result it is found that the present invention preparation method is simple, be advantageously implemented large-scale production, be prepared
Composite conducting material has good electric conductivity, higher intensity and hardness.Scheme in embodiment 5 is of the invention best
Preparation method.The Electrical Conductivity of Composites that the present invention is prepared can achieve 40.55-46.63Ms/m, and tensile strength can reach
522.37-603.73MPa hardness can achieve 80.5-88.5；
The present invention is modified vitreous copper powder with fatty alcohol ethylene oxide ether phosphate salt LBH400, fatty alcohol ethylene oxide
Ether phosphate salt LBH400 can preferably be adsorbed in vitreous copper powder surface, improve its electric conductivity；
As conductive compositions after being modified in the present invention using vitreous copper, while it being added to terbium sesquioxide, vitreous copper
In contain a large amount of copper, terbium sesquioxide is present in material with compound form, is distributed in granular form transgranular, can be improved
The conductivity of copper；
Nano zine oxide is added in the present invention, zinc plays the role of solution strengthening and refined crystalline strengthening to copper, can significantly mention
The integral strength and hardness of high material, the addition of terbium sesquioxide play the role of deoxidation, purification and refinement crystal grain, improve material
Electric conductivity.
Claims (7)
1. a kind of preparation method of composite conducting material, which is characterized in that including following preparation step:
Step 1: vitreous copper is cleaned up, 70 DEG C of drying are mixed with ethanol solution, then broken with Ultrasonic Pulverization instrument, are taken out
It filters, is placed in drying in drier and obtains vitreous copper powder；
Step 2: vitreous copper powder obtained in step 1 is further crushed using airslide disintegrating mill, 200-800 mesh is filtered out
Vitreous copper powder, then mixed with modifier solution and carry out modified-reaction, it is dry at 90 DEG C after reaction to grind for 24 hours, crush
After obtain modified vitreous copper powder；
Step 3: nano zine oxide is dissolved in acetone, then it is added and uses the diluted titanate coupling agent of acetone, 3000r/min
20min is stirred, is filtered, drying obtains modified nano zinc oxide；
Step 4: by 60-80 parts of alpha-quartzs, 22-28 parts of modified vitreous copper powders, 10-14 parts of modified nano zinc oxides, 4-8 parts
Terbium sesquioxide, 6-12 part adhesive, 12-18 parts of dispersants are uniform, are then press-formed under 100MPa pressure, in nitrogen
During atmosphere is enclosed, composite conducting material is obtained after sintering.
2. a kind of preparation method of composite conducting material according to claim 1, which is characterized in that vitreous copper in step 1
Solid-liquid ratio with ethanol solution is 1:(300-500), solid-liquid ratio unit is g/mL.
3. a kind of preparation method of composite conducting material according to claim 1, which is characterized in that modified anti-in step 2
The temperature answered is 60-80 DEG C, reaction time 30-50min.
4. a kind of preparation method of composite conducting material according to claim 1, which is characterized in that vitreous copper in step 2
The solid-liquid ratio of powder and modifier solution is 1:(20-40), solid-liquid ratio unit is g/mL.
5. a kind of preparation method of composite conducting material according to claim 1, which is characterized in that modifying agent in step 2
Solution is that fatty alcohol ethylene oxide ether phosphate salt and ethyl alcohol are mixed according to volume ratio 1:2.
6. a kind of preparation method of composite conducting material according to claim 1, which is characterized in that titanate esters in step 3
The mass ratio of coupling agent and zinc oxide is (0.05-0.08): 1.
7. a kind of preparation method of composite conducting material according to claim 1, which is characterized in that be sintered temperature in step 4
Degree is 1100 DEG C -1500 DEG C, sintering time 3h.
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| CN101279984A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Alkyl phenol sulfonic polyoxyethylene ether phosphate salt and preparation thereof |
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