CN109020594A - A kind of preparation method of carbon nanotube-aluminium nitride ceramics - Google Patents

A kind of preparation method of carbon nanotube-aluminium nitride ceramics Download PDF

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Publication number
CN109020594A
CN109020594A CN201811056877.7A CN201811056877A CN109020594A CN 109020594 A CN109020594 A CN 109020594A CN 201811056877 A CN201811056877 A CN 201811056877A CN 109020594 A CN109020594 A CN 109020594A
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aluminium nitride
nitride ceramics
carbon nanotube
cobalt
plating
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陈伟
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Zhangjiagang City Fook New Mstar Technology Ltd
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Zhangjiagang City Fook New Mstar Technology Ltd
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    • C04B35/806
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844Coating fibres
    • C04B35/62876Coating fibres with metals
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62886Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention discloses a kind of preparation methods of carbon nanotube-aluminium nitride ceramics, it include: that (1) carbon nanotube that partial size is 20~40nm is added in deionized water, 30~40min of ultrasonic disperse obtains the carbon nano tube suspension that mass concentration is 5~15g/L;(2) it is added in the plating solution containing 20~40g/L cobalt salt solution into above-mentioned carbon nano tube suspension, it is 8~9 that lye, which is added, and adjusts the pH of plating solution, and magnetic agitation reacts 3~5h under 30~40 DEG C of water bath conditions, centrifuge separation, washing, it is dry, obtain cobalt-plating carbon nano-tube pipe;It (3) is that 1:50~150 mix according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, add the binder that weight percent is 1~3%, it stirs evenly, it is suppressed under the pressure condition of 50~100MPa after the drying of gained mixed slurry, in 1000~1200 DEG C of 1~2h of roasting, 50min is kept the temperature, carbon nanotube-aluminium nitride ceramics is obtained.In carbon nanotube-aluminium nitride ceramics in the present invention, by adding cobalt-plating carbon nano-tube pipe, not only hardness with higher, but also there is good fracture toughness.

Description

A kind of preparation method of carbon nanotube-aluminium nitride ceramics
Technical field
The present invention relates to technical field of ceramic material, more particularly to a kind of preparation side of carbon nanotube-aluminium nitride ceramics Method.
Background technique
Aluminium nitride ceramics is big with mechanical strength, insulation resistance is big, and hardness is high, the excellent performance such as wear resistant corrosion resistant.It In petro chemical industry, national defence, both mechanically and electrically by favor in the fields such as industry, but since the height of ceramic material is hard crisp The difference of property and the two coefficient of expansion, so that it is poor with the bond strength of metallic matrix.
Carbon nanotube is the carbonaceous material of nano-scale, and due to its great surface area, good electrical and thermal conductivity performance is excellent Mechanical property more has very big application prospect in recent years.Ceramic physical and chemical performance by adding carbon nanotube can It is significantly improved, but its hardness and fracture toughness need to improve.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of carbon nanotube-aluminium nitride ceramics, it can Solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of carbon nanotube-aluminium nitride ceramics, to overcome the prior art In deficiency.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of carbon nanotube-aluminium nitride ceramics, comprising:
(1) carbon nanotube that partial size is 20~40nm is added in deionized water, 30~40min of ultrasonic disperse obtains matter Measure the carbon nano tube suspension that concentration is 5~15g/L;
(2) it is added in the plating solution containing 20~40g/L cobalt salt solution into above-mentioned carbon nano tube suspension, lye tune is added The pH for saving plating solution is 8~9, and magnetic agitation reacts 3~5h under 30~40 DEG C of water bath conditions, is centrifugated, and washs, dry, is obtained To cobalt-plating carbon nano-tube pipe;
(3) it is that 1:50~150 mix according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, adds The binder that weight percent is 1~3%, stirs evenly, in the pressure condition of 50~100MPa after the drying of gained mixed slurry Under suppressed, in 1000~1200 DEG C of 1~2h of roasting, keep the temperature 50min, obtain carbon nanotube-aluminium nitride ceramics.
Preferably, in step (1), the mass concentration of the carbon nano tube suspension is 10g/L.
Preferably, in step (1), ultrasonic power is 400~600W.
Preferably, in step (2), the cobalt salt solution is cobalt nitrate solution or cobalt chloride solution.
Preferably, in step (2), the plating solution further includes 30~40g/L sodium citrate solution, 15~25g/L times phosphorous Acid sodium solution and 40~60g/L ammonium nitrate solution.
Preferably, in step (2), the lye is sodium hydroxide solution or ammonia spirit.
Preferably, in step (3), the cobalt-plating carbon nano-tube pipe and the aluminium nitride ceramics weight ratio are 1:100.
Preferably, in step (3), drying temperature is 110 DEG C.
Compared with the prior art, the advantages of the present invention are as follows: in carbon nanotube-aluminium nitride ceramics in the present invention, pass through Cobalt-plating carbon nano-tube pipe is added, not only hardness with higher, but also there is good fracture toughness.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of carbon nanotube-aluminium nitride ceramics, comprising:
(1) carbon nanotube that partial size is 20~40nm is added in deionized water, 30~40min of ultrasonic disperse obtains matter Measure the carbon nano tube suspension that concentration is 5~15g/L;
(2) it is added in the plating solution containing 20~40g/L cobalt salt solution into above-mentioned carbon nano tube suspension, lye tune is added The pH for saving plating solution is 8~9, and magnetic agitation reacts 3~5h under 30~40 DEG C of water bath conditions, is centrifugated, and washs, dry, is obtained To cobalt-plating carbon nano-tube pipe;
(3) it is that 1:50~150 mix according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, adds The binder that weight percent is 1~3%, stirs evenly, in the pressure condition of 50~100MPa after the drying of gained mixed slurry Under suppressed, in 1000~1200 DEG C of 1~2h of roasting, keep the temperature 50min, obtain carbon nanotube-aluminium nitride ceramics.
Wherein, in step (1), the mass concentration of the carbon nano tube suspension is 10g/L;Ultrasonic power be 400~ 600W, it is preferred that ultrasonic power 500W.
Wherein, in step (2), the cobalt salt solution is cobalt nitrate solution or cobalt chloride solution;The plating solution further includes 30 ~40g/L sodium citrate solution, 15~25g/L ortho phosphorous acid sodium solution and 40~60g/L ammonium nitrate solution, it is preferred that described Plating solution further includes 35g/L sodium citrate solution, 20g/L ortho phosphorous acid sodium solution and 50g/L ammonium nitrate solution;The lye is hydrogen Sodium hydroxide solution or ammonia spirit.
Wherein, in step (3), the cobalt-plating carbon nano-tube pipe and the aluminium nitride ceramics weight ratio are 1:100;Drying temperature It is 110 DEG C.
Carbon nanotube-aluminium nitride ceramics preparation method is illustrated with specific embodiment below.
Embodiment 1
(1) carbon nanotube that partial size is 20nm is added in deionized water, ultrasonic disperse 30min, obtaining mass concentration is The carbon nano tube suspension of 5g/L;
(2) it is added in the plating solution containing 20g/L cobalt salt solution into above-mentioned carbon nano tube suspension, lye is added and adjusts plating The pH of liquid is 8, and magnetic agitation reacts 3h under 30 DEG C of water bath conditions, is centrifugated, and is washed, dry, obtains cobalt-plating carbon nano-tube pipe;
(3) it is that 1:50 is mixed according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, adds weight The binder that percentage is 1%, stirs evenly, and is suppressed under the pressure condition of 50MPa after the drying of gained mixed slurry, in 1000 DEG C of roasting 1h keep the temperature 50min, obtain carbon nanotube-aluminium nitride ceramics.
Embodiment 2
(1) carbon nanotube that partial size is 30nm is added in deionized water, ultrasonic disperse 35min, obtaining mass concentration is The carbon nano tube suspension of 10g/L;
(2) it is added in the plating solution containing 30g/L cobalt salt solution into above-mentioned carbon nano tube suspension, lye is added and adjusts plating The pH of liquid is 8.5, and magnetic agitation reacts 4h under 35 DEG C of water bath conditions, is centrifugated, and is washed, dry, obtains cobalt-plating carbon nano-tube Pipe;
(3) it is that 1:100 is mixed according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, adds weight The binder that percentage is 2%, stirs evenly, and is suppressed under the pressure condition of 75MPa after the drying of gained mixed slurry, in 1100 DEG C of roasting 1.5h keep the temperature 50min, obtain carbon nanotube-aluminium nitride ceramics.
Embodiment 3
(1) carbon nanotube that partial size is 40nm is added in deionized water, ultrasonic disperse 40min, obtaining mass concentration is The carbon nano tube suspension of 15g/L;
(2) it is added in the plating solution containing 40g/L cobalt salt solution into above-mentioned carbon nano tube suspension, lye is added and adjusts plating The pH of liquid is 9, and magnetic agitation reacts 5h under 40 DEG C of water bath conditions, is centrifugated, and is washed, dry, obtains cobalt-plating carbon nano-tube pipe;
(3) it is that 1:150 is mixed according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, adds weight The binder that percentage is 3%, stirs evenly, and is suppressed under the pressure condition of 100MPa after the drying of gained mixed slurry, In 1200 DEG C of roasting 2h, 50min is kept the temperature, carbon nanotube-aluminium nitride ceramics is obtained.
It is not only with higher hard by adding cobalt-plating carbon nano-tube pipe in carbon nanotube-aluminium nitride ceramics in the present invention Degree, and there is good fracture toughness.Carbon nanotube-aluminium nitride ceramics fracture toughness and hardness are tested, tied Fruit shows carbon nanotube-aluminium nitride ceramics fracture toughness up to 3.92MPam1/2, hardness is up to 9.68GPa.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (8)

1. a kind of preparation method of carbon nanotube-aluminium nitride ceramics characterized by comprising
(1) carbon nanotube that partial size is 20~40nm is added in deionized water, it is dense to obtain quality by 30~40min of ultrasonic disperse Degree is the carbon nano tube suspension of 5~15g/L;
(2) it is added in the plating solution containing 20~40g/L cobalt salt solution into above-mentioned carbon nano tube suspension, lye is added and adjusts plating The pH of liquid is 8~9, and magnetic agitation reacts 3~5h under 30~40 DEG C of water bath conditions, is centrifugated, and is washed, dry, is plated Cobalt carbon nanotube;
(3) it is that 1:50~150 mix according to weight ratio with aluminium nitride ceramics by above-mentioned cobalt-plating carbon nano-tube pipe, adds weight Percentage be 1~3% binder, stir evenly, gained mixed slurry drying after under the pressure condition of 50~100MPa into Row compacting keeps the temperature 50min, obtains carbon nanotube-aluminium nitride ceramics in 1000~1200 DEG C of 1~2h of roasting.
2. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (1), The mass concentration of the carbon nano tube suspension is 10g/L.
3. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (1), Ultrasonic power is 400~600W.
4. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (2), The cobalt salt solution is cobalt nitrate solution or cobalt chloride solution.
5. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (2), The plating solution further includes 30~40g/L sodium citrate solution, 15~25g/L ortho phosphorous acid sodium solution and 40~60g/L ammonium nitrate Solution.
6. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (2), The lye is sodium hydroxide solution or ammonia spirit.
7. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (3), The cobalt-plating carbon nano-tube pipe and the aluminium nitride ceramics weight ratio are 1:100.
8. the preparation method of carbon nanotube-aluminium nitride ceramics according to claim 1, which is characterized in that in step (3), Drying temperature is 110 DEG C.
CN201811056877.7A 2018-09-11 2018-09-11 A kind of preparation method of carbon nanotube-aluminium nitride ceramics Withdrawn CN109020594A (en)

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Publication number Priority date Publication date Assignee Title
CN114378291A (en) * 2022-01-11 2022-04-22 金华职业技术学院 Multi-cladding cobalt-coated carbon nanotube composite powder and preparation method thereof

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Application publication date: 20181218