CN108341673A - A kind of high-strength composite conducting ceramic material and preparation method thereof - Google Patents
A kind of high-strength composite conducting ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high-strength composite conducting ceramic materials, are made of the component of following parts by weight：25 parts of Sr Sn Mo N B15,15 20 parts of silicon carbide, 10 15 parts of surface-modified fullerenes, 5 10 parts of lanthanum boride, 5 10 parts of zirconium carbide.The preparation method of the high-strength composite conducting ceramic material, includes the following steps：S1, Sr Sn Mo N B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and said components are ground with ball mill and are mixed to get mixture, then mixture is molded base；S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material.High-strength composite conducting ceramic material disclosed by the invention has the advantages that be not easy to reunite and the moisture absorption, anti-oxidant, anticorrosive, radioresistance, high temperature resistant, chemical stability are high, conductivity is high, service life is long, of low cost.
Description
Technical field
The present invention relates to technical field of ceramic material more particularly to a kind of high-strength composite conducting ceramic material and its preparations
Method.
Background technology
Ceramics are one of most common materials in daily life, and type is various, widely used, are related to industry, electric power, build
It builds, numerous industries such as instrument and meter.With the improvement of people ' s living standards and the further expansion of ceramic applications range, people couple
Ceramic material proposes new requirement, does not require nothing more than its beautiful, intensity and wear-resisting property is strong, also require it with excellent conduction
Property, heat resistance, corrosion resistance, inoxidizability, flexural strength and toughness.It is used under specified conditions with meeting, is further promoted
The development of ceramic material.
Conductivity ceramics is one kind in numerous ceramic materials, and it is novel to have ionic conduction, electronics, one kind of hole conduction
Functional material.Due to its chemical property stabilization, high temperature resistant, long lifespan, radioresistance, corrosion-resistant, anti-oxidant etc., it is widely used in
The fields such as electrode, gas sensor, ferroelectric material, superconductor.But the heat that existing conductivity ceramics generates while conduction
Amount is higher, and in the case where needing conduction not need higher heat for certain and is not suitable for, and constrains conductivity ceramics in bigger model
Enclose interior application.In addition to this, these conducting ceramic material physical and chemical properties are unstable, and conductivity is low, high temperature resistance
Difference, it is expensive, while wear-resisting property is poor, ceramic material in use can be due to conductivity decline after rubbing repeatedly.It is existing
There are these materials in technology to can no longer meet people to high-performance conductive ceramic material under the conditions of specific extreme environment
It uses.
A kind of conductivity ceramics is disclosed in Chinese invention patent 201510628153.5, the invention discloses a kind of conductive potteries
Ceramic material and preparation method thereof, above-mentioned conducting ceramic material are made of the component comprising following parts by weight：Alchlor 65-70
Part, 25-30 parts of spodumene, 5-8 parts of ferrite, 2-5 parts of titanium carbide, 2-3 parts of antimony oxide, 1-2 parts of Neon SiC powder,
0.02-0.8 parts of 1-2 parts of poly aluminium iron silicate, 0.5-1 parts of strontium carbonate, 0.5-1 parts of four fourth fat of metatitanic acid and ammonium persulfate.The present invention is also
Provide a kind of preparation method of conducting ceramic material.But that there is resistivity is uneven for the material, and conductivity is low, high temperature resistant and
Chemical stability is poor.
Therefore, it is necessary to seek more efficient way, prepares and be not easy to reunite and the moisture absorption, anti-oxidant, anticorrosive, anti-spoke
It penetrates, the conducting ceramic material that high temperature resistant, chemical stability are high, conductivity is high.
Invention content
In order to overcome the defects of the prior art, a kind of high-strength composite conducting ceramic material of present invention offer and its preparation
Method, preparation method is simple for this, and raw material is easy to get, cheap, of less demanding to equipment and reaction condition, is suitble to industrialization
Production；The high-strength composite conducting ceramic material being prepared by the preparation method overcomes existing conducting ceramic material
Physical and chemical properties it is unstable, conductivity is low, and high temperature resistance is poor, expensive, while wear-resisting property is poor, ceramic material
Can have due to the technical issues of conductivity declines after rubbing repeatedly and be not easy to reunite and the moisture absorption, anti-oxidant, anti-in use
Burn into radioresistance, high temperature resistant, chemical stability are high, conductivity is high, service life is long, advantage of low cost.
To achieve the above object of the invention, the technical solution adopted by the present invention is a kind of high-strength composite conducting ceramic material,
It is made of the component of following parts by weight：Sr-Sn-Mo-N-B15-25 parts, 15-20 parts of silicon carbide, surface-modified fullerenes 10-15
Part, 5-10 parts of lanthanum boride, 5-10 parts of zirconium carbide.
Preferably, the preparation method of the Sr-Sn-Mo-N-B, includes the following steps：By metal molybdenum powder, strontium nitrate, chlorination
Tin, three normal-butyl Azide tin, six strontium borides are added mixing and are placed in stainless steel autoclave, and being put into after sealing being capable of program liter
In the electric furnace of temperature, with 5 DEG C/min of speed from room temperature temperature programming to 700-800 DEG C, then maintain 3-4 small at this temperature
When after naturally cool to room temperature.Afterwards deposit collection is got up to be washed with distilled water 3-5 times, then is washed 6-8 times with absolute ethyl alcohol,
Revolving obtains sample after removing solvent.
Preferably, the mass ratio of the metal molybdenum powder, strontium nitrate, stannic chloride, three normal-butyl Azide tin, six strontium borides is
(0.5-1):(1-2):0.5:(0.3-0.5):(0.3-0.5)。
Preferably, the preparation method of the surface-modified fullerenes, includes the following steps：Epoxy resin is dissolved in higher boiling
Solution is formed in solvent, after amino modified fullerene and epoxy silane coupling KH-560, base catalysis is added into solution again
Agent is stirred to react 10-14 hours at 50-60 DEG C, after settle out in water, ethyl alcohol washing crude product is used in combination 5-7 time, after done in vacuum
It is dried 15-24 hours at 80-90 DEG C of dry case, obtains surface-modified fullerenes.
Preferably, the epoxy resin, high boiling solvent, amino modified fullerene, epoxy silane coupling KH-560,
The mass ratio of base catalyst is 1:(5-10):(3-5):(0.3-0.5):(0.5-1).
Preferably, the high boiling solvent is in dimethyl sulfoxide, n,N-Dimethylformamide, N-Methyl pyrrolidone
It is one or more of.
Preferably, the base catalyst is selected from one or more of potassium hydroxide, sodium hydroxide, potassium carbonate, sodium carbonate.
Preferably, the preparation method of the high-strength composite conducting ceramic material, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and will be upper
It states component and is ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material.
Further, the high temperature sintering temperature is 750-850 DEG C, sintering time 5-7 hours.
It is using advantageous effect caused by above-mentioned technical proposal：
1) preparation method of high-strength composite conducting ceramic material provided by the invention, simple and practicable, raw material is easy to get, price
It is cheap, it is of less demanding to equipment and reaction condition, it is suitble to industrialized production.
2) high-strength composite conducting ceramic material provided by the invention, overcome existing conducting ceramic material physics and
Chemical property is unstable, and conductivity is low, and high temperature resistance is poor, expensive, while wear-resisting property is poor, and ceramic material was using
Cheng Zhonghui has due to the technical issues of conductivity declines after rubbing repeatedly and is not easy to reunite and the moisture absorption, anti-oxidant, anticorrosive, anti-
Radiation, high temperature resistant, chemical stability is high, conductivity is high, service life is long, advantage of low cost..
3) high-strength composite conducting ceramic material provided by the invention adds superconductor fullerene, with conductivity ceramics phase
Synergistic effect, substantially increases the conductivity of high-strength conductive ceramic material, by being modified to fullerene surface, is conducive to fowler
Alkene be uniformly dispersed and the compatibility with other components, with other components act synergistically so that high-strength composite conductivity ceramics
Materials chemistry performance is stablized, and uniform resistivity is not easy the moisture absorption and reunion, has excellent flexural strength, fracture toughness, heat resistanceheat resistant punching
Hitting property, and coefficient of thermal expansion is low.
Specific implementation mode
In order to make those skilled in the art more fully understand technical scheme of the present invention, and make the present invention features described above,
Purpose and advantage are more clear understandable, and with reference to embodiment, the present invention is described further.Embodiment is only used for
It is bright the present invention rather than limit the scope of the invention.
Amination fullerene used in the following embodiments of the present invention is purchased from the limited public affairs of Nanjing Xian Feng nano materials science and technology
Department, other raw materials are purchased from shellfish store of rubbing.
Embodiment 1
A kind of high-strength composite conducting ceramic material, is made of the component of following parts by weight：15 parts of Sr-Sn-Mo-N-B,
15 parts of silicon carbide, 10 parts of surface-modified fullerenes, 5 parts of lanthanum boride, 5 parts of zirconium carbide.
The preparation method of the Sr-Sn-Mo-N-B, includes the following steps：By metal molybdenum powder 5g, strontium nitrate 10g, stannic chloride
5g, three normal-butyl Azide tin 3g, six strontium boride 3g are added mixing and are placed in stainless steel autoclave, and being put into after sealing being capable of journey
In the electric furnace of sequence heating, with 5 DEG C/min of speed from room temperature temperature programming to 700 DEG C, then maintain 3 hours at this temperature
After naturally cool to room temperature.Deposit collection is got up to be washed with distilled water 3 times afterwards, then washed 6 times with absolute ethyl alcohol, revolving is removed
Sample is obtained after removing solvent.
The preparation method of the surface-modified fullerenes, includes the following steps：Epoxy resin 10g is dissolved in dimethyl sulfoxide
Solution is formed in 50g, after amino modified fullerene 30g and epoxy silane coupling KH-5603g, hydrogen is added into solution again
Potassium oxide 5g is stirred to react 10 hours at 50 DEG C, after settle out in water, ethyl alcohol washing crude product is used in combination 5 times, after be dried in vacuo
It is dried 15 hours at 80 DEG C of case, obtains surface-modified fullerenes.
The preparation method of the high-strength composite conducting ceramic material, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and will be upper
It states component and is ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material；It is described
High temperature sintering temperature is 750 DEG C, sintering time 5 hours.
Embodiment 2
A kind of high-strength composite conducting ceramic material, is made of the component of following parts by weight：18 parts of Sr-Sn-Mo-N-B,
17 parts of silicon carbide, 12 parts of surface-modified fullerenes, 7 parts of lanthanum boride, 7 parts of zirconium carbide.
The preparation method of the Sr-Sn-Mo-N-B, includes the following steps：By metal molybdenum powder 7g, strontium nitrate 12g, stannic chloride
5g, three normal-butyl Azide tin 3.5g, six strontium boride 3.5g are added mixing and are placed in stainless steel autoclave, and energy is put into after sealing
In the electric furnace of enough temperature programmings, with 5 DEG C/min of speed from room temperature temperature programming to 720 DEG C, then maintain at this temperature
Room temperature is naturally cooled to after 3.2 hours.Deposit collection is got up to be washed with distilled water 4 times afterwards, then 7 are washed with absolute ethyl alcohol
Secondary, revolving obtains sample after removing solvent.
The preparation method of the surface-modified fullerenes, includes the following steps：Epoxy resin 10g is dissolved in N, N- dimethyl
Form solution in formamide 65g, after amino modified fullerene 40g and epoxy silane coupling KH- is added into solution again
5603.5g, sodium hydroxide 3.5g are stirred to react 12 hours at 53 DEG C, after settle out in water, ethyl alcohol washing crude product is used in combination 6 times,
It is dried 17 hours at 83 DEG C of vacuum drying chamber afterwards, obtains surface-modified fullerenes.
The preparation method of the high-strength composite conducting ceramic material, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and will be upper
It states component and is ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material；It is described
High temperature sintering temperature is 780 DEG C, sintering time 5.5 hours.
Embodiment 3
A kind of high-strength composite conducting ceramic material, is made of the component of following parts by weight：Sr-Sn-Mo-N-B20 parts, carbon
18 parts of SiClx, 13 parts of surface-modified fullerenes, 8 parts of lanthanum boride, 8 parts of zirconium carbide.
The preparation method of the Sr-Sn-Mo-N-B, includes the following steps：By metal molybdenum powder 8g, strontium nitrate 15g, stannic chloride
5g, three normal-butyl Azide tin 4g, six strontium boride 4g are added mixing and are placed in stainless steel autoclave, and being put into after sealing being capable of journey
In the electric furnace of sequence heating, with 5 DEG C/min of speed from room temperature temperature programming to 760 DEG C, then maintenance 3.5 is small at this temperature
When after naturally cool to room temperature.Deposit collection is got up to be washed with distilled water 5 times afterwards, then washed 7 times with absolute ethyl alcohol, rotated
Sample is obtained after removing solvent.
The preparation method of the surface-modified fullerenes, includes the following steps：Epoxy resin 10g is dissolved in N- methylpyrroles
Form solution in alkanone 80g, after amino modified fullerene 42g and epoxy silane coupling KH- is added into solution again
5604.3g, potassium carbonate 8g are stirred to react 13 hours at 57 DEG C, after settle out in water, ethyl alcohol washing crude product is used in combination 7 times, after
It is dried 20 hours at 87 DEG C of vacuum drying chamber, obtains surface-modified fullerenes.
The preparation method of the high-strength composite conducting ceramic material, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and will be upper
It states component and is ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material；It is described
High temperature sintering temperature is 800 DEG C, sintering time 6 hours.
Embodiment 4
A kind of high-strength composite conducting ceramic material, is made of the component of following parts by weight：Sr-Sn-Mo-N-B23 parts, carbon
18 parts of SiClx, 14 parts of surface-modified fullerenes, 9 parts of lanthanum boride, 10 parts of zirconium carbide.
The preparation method of the Sr-Sn-Mo-N-B, includes the following steps：By metal molybdenum powder 9g, strontium nitrate 18g, stannic chloride
5g, three normal-butyl Azide tin 4.5g, six strontium boride 5g are added mixing and are placed in stainless steel autoclave, and being put into after sealing can
In the electric furnace of temperature programming, with 5 DEG C/min of speed from room temperature temperature programming to 790 DEG C, 3.8 are then maintained at this temperature
Room temperature is naturally cooled to after hour.Deposit collection is got up to be washed with distilled water 5 times afterwards, then washed 7 times with absolute ethyl alcohol, revolved
Sample is obtained after solvent is evaporated off.
The preparation method of the surface-modified fullerenes, includes the following steps：Epoxy resin 10g is dissolved in dimethyl sulfoxide
Solution is formed in 95g, after be added again into solution amino modified fullerene 45g and epoxy silane coupling KH-5604.5g,
Sodium hydroxide 9g is stirred to react 13.5 hours at 59 DEG C, after settle out in water, ethyl alcohol washing crude product is used in combination 7 times, after in vacuum
It is dried 22 hours at 88 DEG C of drying box, obtains surface-modified fullerenes.
The preparation method of the high-strength composite conducting ceramic material, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and will be upper
It states component and is ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material；It is described
High temperature sintering temperature is 830 DEG C, sintering time 6.5 hours.
Embodiment 5
A kind of high-strength composite conducting ceramic material, is made of the component of following parts by weight：Sr-Sn-Mo-N-B25 parts, carbon
20 parts of SiClx, 15 parts of surface-modified fullerenes, 10 parts of lanthanum boride, 10 parts of zirconium carbide.
The preparation method of the Sr-Sn-Mo-N-B, includes the following steps：By metal molybdenum powder 10g, strontium nitrate 20g, chlorination
Tin 5g, three normal-butyl Azide tin 5g, six strontium boride 5g are added mixing and are placed in stainless steel autoclave, and being put into after sealing can
In the electric furnace of temperature programming, with 5 DEG C/min of speed from room temperature temperature programming to 800 DEG C, then maintenance 4 is small at this temperature
When after naturally cool to room temperature.Deposit collection is got up to be washed with distilled water 5 times afterwards, then washed 8 times with absolute ethyl alcohol, rotated
Sample is obtained after removing solvent.
The preparation method of the surface-modified fullerenes, includes the following steps：Epoxy resin 10g is dissolved in N, N- dimethyl
Form solution in formamide 100g, after amino modified fullerene 50g and epoxy silane coupling KH- is added into solution again
5605g, sodium carbonate 10g are stirred to react 14 hours at 60 DEG C, after settle out in water, ethyl alcohol washing crude product is used in combination 7 times, after
It is dried 24 hours at 90 DEG C of vacuum drying chamber, obtains surface-modified fullerenes.
The preparation method of the high-strength composite conducting ceramic material, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and will be upper
It states component and is ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material；It is described
High temperature sintering temperature is 850 DEG C, sintering time 7 hours.
Comparative example 1
This example provides a kind of conducting ceramic material, according to the raw material of 201610469196.8 embodiment 1 of Chinese invention patent
It is prepared.
Comparative example 2
This example provides a kind of conducting ceramic material, raw material and the preparation method is the same as that of Example 1, unlike without addition Sr-
Sn-Mo-N-B。
Comparative example 3
This example provides a kind of conducting ceramic material, raw material and the preparation method is the same as that of Example 1, unlike without addition carbonization
Silicon.
Comparative example 4
This example provides a kind of conducting ceramic material, raw material and the preparation method is the same as that of Example 1, unlike without addition surface
Modified fullerenes.
Comparative example 5
This example provides a kind of conducting ceramic material, raw material and the preparation method is the same as that of Example 1, unlike without addition boronation
Lanthanum.
Comparative example 6
This example provides a kind of conducting ceramic material, raw material and the preparation method is the same as that of Example 1, unlike without addition carbonization
Zirconium.
Conducting ceramic material sample described in embodiment 1-5 and comparative example 1-6 is tested for the property, test result is shown in Table 1,
Test method is as follows：
1) hardness：With the load of 49.03-980.7N, the square pyramidal diamond that opposite face angle is 136 ° is pressed into ceramics
Material surface measures impression catercorner length after being kept for the defined time, then the size of hardness is calculated by formula.
2) conductivity：Four-point probe acquires the test data under integrated mode twice, collected data warp in real time
Computer is analyzed, to obtain required test result.
3) bending strength：It is tested according to GB/T6569-86 test methods.
4) fracture toughness：It is tested according to ASTMC1421-2001 test methods.
5) coefficient of thermal expansion：It is tested according to GB/T16535-1996 test methods.
1 conducting ceramic material performance parameter of table
As seen from Table 1, high-strength composite conducting ceramic material disclosed by the embodiments of the present invention, with conduction in the prior art
Ceramic material is compared, and has higher conductivity, superior mechanical property, and coefficient of thermal expansion is lower.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. a kind of high-strength composite conducting ceramic material, which is characterized in that be made of the component of following parts by weight：Sr-Sn-Mo-
N-B15-25 parts, 15-20 parts of silicon carbide, 10-15 parts of surface-modified fullerenes, 5-10 parts of lanthanum boride, 5-10 parts of zirconium carbide.
2. high-strength composite conducting ceramic material according to claim 1, which is characterized in that the Sr-Sn-Mo-N-B's
Preparation method includes the following steps：Metal molybdenum powder, strontium nitrate, stannic chloride, three normal-butyl Azide tin, six strontium borides are added
Mixing is placed in stainless steel autoclave, is put into after sealing in the electric furnace for capableing of temperature programming, with 5 DEG C/min of speed from room
Warm temperature programming naturally cools to room temperature to 700-800 DEG C after then maintaining 3-4 hours at this temperature.Deposit is received afterwards
Collection gets up to be washed with distilled water 3-5 times, then is washed 6-8 times with absolute ethyl alcohol, and revolving obtains sample after removing solvent.
3. high-strength composite conducting ceramic material according to claim 2, which is characterized in that the metal molybdenum powder, nitric acid
Strontium, stannic chloride, three normal-butyl Azide tin, six strontium borides mass ratio be (0.5-1):(1-2):0.5:(0.3-0.5):
(0.3-0.5)。
4. high-strength composite conducting ceramic material according to claim 1, which is characterized in that the surface-modified fullerenes
Preparation method, include the following steps：Epoxy resin is dissolved in high boiling solvent and forms solution, after ammonia is added into solution again
Base modified fullerenes and epoxy silane coupling KH-560, base catalyst are stirred to react 10-14 hours at 50-60 DEG C, after
Settle out in water, ethyl alcohol washing crude product 5-7 times be used in combination, after dried 15-24 hours at 80-90 DEG C of vacuum drying chamber, obtain surface
Modified fullerenes.
5. high-strength composite conducting ceramic material according to claim 4, which is characterized in that the epoxy resin, height boiling
Select solvent, amino modified fullerene, epoxy silane coupling KH-560, base catalyst mass ratio be 1:(5-10):(3-
5):(0.3-0.5):(0.5-1)。
6. high-strength composite conducting ceramic material according to claim 4, which is characterized in that the high boiling solvent is selected from
One or more of dimethyl sulfoxide, N,N-dimethylformamide, N-Methyl pyrrolidone.
7. high-strength composite conducting ceramic material according to claim 4, which is characterized in that the base catalyst is selected from hydrogen
One or more of potassium oxide, sodium hydroxide, potassium carbonate, sodium carbonate.
8. a kind of preparation method according to claim 1-7 any one of them high-strength composite conducting ceramic materials, feature
It is, includes the following steps：
S1, Sr-Sn-Mo-N-B, silicon carbide, surface-modified fullerenes, lanthanum boride, zirconium carbide are weighed in proportion, and by above-mentioned group
Divide to be ground with ball mill and be mixed to get mixture, then mixture is molded base；
S2, by the mixture high temperature sintering after step S1 bases, obtain high-strength composite conducting ceramic material.
9. the preparation method of high-strength composite conducting ceramic material according to claim 8, which is characterized in that the high temperature
Sintering temperature is 750-850 DEG C, sintering time 5-7 hours.
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