CN108530099A - A kind of block carbon reinforcement/carbon composite and preparation method thereof - Google Patents
A kind of block carbon reinforcement/carbon composite and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of material, and in particular to a kind of block carbon reinforcement/carbon composite and preparation method thereof being sintered by solid phase reaction.Block carbon reinforcement/carbon composite; be by Nano diamond powder it is evenly dispersed in a solvent after; carbon cloth is allowed to impregnate by the slurry container containing Nano diamond powder; then the carbon cloth for soaking bridging slurry is dried to obtain to the precast body of the carbon cloth containing diamond powder; then it is cut out by required specification; it is laminated on together, applies pressure under protective atmosphere and obtain the carbon reinforcement/carbon composite after high temperature sintering.Block carbon reinforcement/carbon composite prepared by the present invention has high consistency and good mechanical property, can be used for wear-resistant material, electrode material, nuclear power industry etc..
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of block carbon reinforcement/carbon composite and its system
Preparation Method.
Background technology
Carbon material is always along with the process of development of human history, from zero dimension fullerene to one-dimensional carbon nanotube, then to two
Graphene is tieed up, common three-dimensional carbon material graphite, diamond is finally arrived, suffers from important application.Expect from single carbon materials
The carbon/carbon compound material of two-phase even multiphase is increasingly concerned, and application range is also increasingly wider.However, current carbon materials
It is not very high, synthetic method that the bottleneck of material especially its development of the composite material of carbon phase composition, which is product relative density obtained,
Mostly it is that liquid impregnation or vapour deposition process are made, the production cycle is longer, requires growing environment harsh.The present invention is by solid
Phase reaction is sintered to prepare block carbon reinforcement/carbon composite, compares, the preparation of traditional carbon/carbon compound material, production week
Phase property is shorter, and product consistency is opposite to be improved, and preparation method is simple, and operability is strong, expands the application of carbon/carbon compound material
Field.
Invention content
For overcome the deficiencies in the prior art, capture prepare the carbon/carbon compound material manufacturing cycle of high-density high-strength compared with
Long problem, the present invention provides a kind of block carbon reinforcement/carbon composite being sintered by solid phase reaction and its systems
Preparation Method.The present invention be by Nano diamond powder it is evenly dispersed in a solvent after, by carbon cloth by containing a nanometer Buddha's warrior attendant
It is allowed to impregnate in the slurry container of mountain flour body, then the carbon cloth for soaking bridging slurry is dried, cuts out, is stacked in by required specification
Together, apply pressure under protective atmosphere and obtain the carbon reinforcement/carbon composite after high temperature sintering.
The specific technical solution that the present invention uses is：
A kind of preparation method of block carbon reinforcement/carbon composite, is the presoma of first obtained composite material, using
Pressure sintering is converted into block carbon reinforcement/carbon composite.
Further, the presoma：Using diamond powder it is evenly dispersed in a solvent after, surface is coated with adhesive
Carbon cloth be allowed to impregnate by the slurry container containing Nano diamond powder, then will soak bridging slurry carbon cloth do
It is dry to be made.
Further, the preparation process of the presoma of the composite material includes the following steps：
(1) preparation of diamond dispersion liquid：It is 80~100nm and 0.24~0.26g to weigh 2.4~2.6g grain sizes respectively
Diameter is the diamond powder of the modified processing of 40~50nm, ground and mixed；50ml solvents are added in mixed powder after grinding,
20~30min of ultrasonic disperse；Obtain stable diamond dispersion liquid；
(2) preparation of block carbon reinforcement/carbon composite presoma：The carbon cloth that surface is coated with to adhesive passes through
It is allowed to impregnate in the diamond dispersion liquid configured, dry, solidification obtains the precast body of the carbon cloth containing diamond powder；
In the step (1), the solvent is absolute ethyl alcohol.
In the step (2), the adhesive is epoxyn.
Further, the sintering process is that the presoma lamination of composite material is positioned in mold, in protection gas
It is sintered under atmosphere；40~100MPa pressure is applied to mold when sintering；When reaching maximum sintering temperature, 2~8min is kept the temperature, pressure release is cold
But to room temperature.When high temperature, diamond particles are graphite-phase through phase transition, are filled in the gap between carbon cloth, are caused
Close block carbon reinforcement/carbon composite.
The mold is graphite jig.
The protective atmosphere is argon gas.
When the sintering processing is that discharge plasma is sintered；Heating rate is 100~150 DEG C/min.
The pressurization initial temperature is 900 DEG C.
Possessed advantageous effect is the present invention compared with prior art：
The present invention is to prepare carbon/carbon compound material by the way of solid-phase sintering, big using diamond density, in high temperature
When diamond atom liveness it is big, be converted into the smaller graphite-phase of density through phase transition volume expansion, come between filling carbon fiber
Gap to improve the consistency of product.Compare, traditional carbon/carbon compound material be mostly using the method for liquid phase or gas phase come
It prepares, growing environment requires harshness, and periodically longer, product consistency is not very high.The present invention is sintered by solid phase reaction
Obtained block carbon reinforcement/carbon composite, consistency are up to 90%, and the production cycle is shorter, simple for process, operability
By force, the application field of carbon/carbon compound material is expanded, the higher occasion of performance ratio is more especially required, such as aerospace, army
Work production etc..
Description of the drawings
Fig. 1 is that the present invention prepares a kind of outline flowchart of block carbon reinforcement/carbon composite.
Specific implementation mode
Below by way of the description to embodiment, the specific implementation mode of the present invention is described in further detail.
Embodiment 1：
Flow as shown in Fig. 1, the preparation method of block carbon reinforcement/carbon composite, including composite material forerunner
The preparation of body, the sintering of block carbon reinforcement/carbon composite, are as follows：
(1) preparation of composite material precursor：
1. the preparation of diamond dispersion liquid：It is 50nm through surface that weigh 2.5g grain sizes respectively, which be 100nm and 0.25g grain sizes,
Modified bortz powder is put into mortar mixing, grinds 10min, the powder after grinding is put into the beaker of 100ml, Xiang Qi
50ml absolute ethyl alcohols are added dropwise in beaker, beaker is put into and is cleaned by ultrasonic in instrument, 30min is disperseed using 120w power ultrasonics, is obtained
Stable diamond dispersion liquid；
2. the preparation of block carbon reinforcement/carbon composite presoma powder：Surface is coated with epoxyn
Carbon cloth is dry by being allowed to impregnate in the diamond dispersion liquid that has configured, cures the carbon cloth containing diamond powder
Precast body.(2) sintering of composite material：
It is positioned over internal diameter after the precast body of carbon cloth containing diamond powder is cut lamination by definite shape and is
In the graphite jig of 10mm, under protection of argon gas, be sintered using discharge plasma, when sintering heating rate be 150 DEG C/
Min, sintering temperature is 1600 DEG C, axial compressive force 40MPa, and when high temperature, diamond particles are graphite-phase through phase transition, are filled in
In gap between carbon cloth, the fine and close block carbon reinforcement/carbon composite for being 72% is obtained.
Embodiment 2：
Flow as shown in Fig. 1, the preparation method of block carbon reinforcement/carbon composite, including composite material forerunner
The preparation of body, the sintering of block carbon reinforcement/carbon composite, are as follows：
(1) preparation of composite material precursor：
1. the preparation of diamond dispersion liquid：It is 50nm through surface that weigh 2.5g grain sizes respectively, which be 100nm and 0.25g grain sizes,
Modified bortz powder is put into mortar mixing, grinds 10min, the powder after grinding is put into the beaker of 100ml, Xiang Qi
50ml absolute ethyl alcohols are added dropwise in beaker, beaker is put into and is cleaned by ultrasonic in instrument, 30min is disperseed using 120w power ultrasonics, is obtained
Stable diamond dispersion liquid；
2. the preparation of block carbon reinforcement/carbon composite presoma powder：Surface is coated with epoxyn
Carbon cloth is dry by being allowed to impregnate in the diamond dispersion liquid that has configured, cures the carbon cloth containing diamond powder
Precast body.(2) sintering of composite material：
It is positioned over internal diameter after the precast body of carbon cloth containing diamond powder is cut lamination by definite shape and is
In the graphite jig of 10mm, under protection of argon gas, be sintered using discharge plasma, when sintering heating rate be 150 DEG C/
Min, sintering temperature are 1700 DEG C, axial compressive force 40MPa, soaking time 5min；When high temperature, diamond particles are through phase transition
Graphite-phase is filled in the gap between carbon cloth, obtains the fine and close block carbon reinforcement/carbon composite for being 74.3%.
Embodiment 3：
Flow as shown in Fig. 1, the preparation method of block carbon reinforcement/carbon composite, including composite material forerunner
The preparation of body, the sintering of block carbon reinforcement/carbon composite, are as follows：
(1) preparation of composite material precursor：
1. the preparation of diamond dispersion liquid：It is 50nm through surface that weigh 2.5g grain sizes respectively, which be 100nm and 0.25g grain sizes,
Modified bortz powder is put into mortar mixing, grinds 10min, the powder after grinding is put into the beaker of 100ml, Xiang Qi
50ml absolute ethyl alcohols are added dropwise in beaker, beaker is put into and is cleaned by ultrasonic in instrument, 30min is disperseed using 120w power ultrasonics, is obtained
Stable diamond dispersion liquid；
2. the preparation of block carbon reinforcement/carbon composite presoma powder：Surface is coated with epoxyn
Carbon cloth is dry by being allowed to impregnate in the diamond dispersion liquid that has configured, cures the carbon cloth containing diamond powder
Precast body.(2) sintering of composite material：
It is positioned over internal diameter after the precast body of carbon cloth containing diamond powder is cut lamination by definite shape and is
In the graphite jig of 10mm, under protection of argon gas, be sintered using discharge plasma, when sintering heating rate be 150 DEG C/
Min, sintering temperature are 1700 DEG C, axial compressive force 70MPa, soaking time 5min；When high temperature, diamond particles are through phase transition
Graphite-phase is filled in the gap between carbon cloth, obtains densification up to 82.5% block carbon reinforcement/carbon composite.
Embodiment 4：
Flow as shown in Fig. 1, the preparation method of block carbon reinforcement/carbon composite, including composite material forerunner
The preparation of body, the sintering of block carbon reinforcement/carbon composite, are as follows：
(1) preparation of composite material precursor：
1. the preparation of diamond dispersion liquid：It is 50nm through surface that weigh 2.5g grain sizes respectively, which be 100nm and 0.25g grain sizes,
Modified bortz powder is put into mortar mixing, grinds 10min, the powder after grinding is put into the beaker of 100ml, Xiang Qi
50ml absolute ethyl alcohols are added dropwise in beaker, beaker is put into and is cleaned by ultrasonic in instrument, 30min is disperseed using 120w power ultrasonics, is obtained
Stable diamond dispersion liquid；
2. the preparation of block carbon reinforcement/carbon composite presoma powder：Surface is coated with epoxyn
Carbon cloth is dry by being allowed to impregnate in the diamond dispersion liquid that has configured, cures the carbon cloth containing diamond powder
Precast body.(2) sintering of composite material：
It is positioned over internal diameter after the precast body of carbon cloth containing diamond powder is cut lamination by definite shape and is
In the graphite jig of 10mm, under protection of argon gas, be sintered using discharge plasma, when sintering heating rate be 100 DEG C/
Min, sintering temperature are 1600 DEG C, axial compressive force 100MPa, soaking time 5min；When high temperature, diamond particles are through phase transition
It for graphite-phase, is filled in the gap between carbon cloth, obtains densification up to 90.8% block carbon reinforcement/carbon composite wood
Material.
Above description is the specific implementation mode of the present invention, and each substantive content illustrated not to the present invention constitutes limit
System, person of ordinary skill in the field make an amendment or deform to specific implementation mode above-mentioned, without departing substantially from the essence of the present invention.
Claims (7)
1. a kind of preparation method of block carbon reinforcement/carbon composite, it is characterised in that：In a solvent using diamond powder
After evenly dispersed, by carbon cloth by being allowed to impregnate in the slurry container containing Nano diamond powder, bridging then will be soaked
The carbon cloth of slurry is dried, and is cut out, is laminated on together by required specification, is applied pressure under protective atmosphere and is obtained after high temperature sintering
To the carbon reinforcement/carbon composite.
2. the preparation method of block carbon reinforcement/carbon composite according to claim 1, it is characterised in that：The gold
Hard rock powder is compounded using the diamond of at least two different-grain diameters.
3. the preparation method of block carbon reinforcement/carbon composite according to claim 1, it is characterised in that：Including with
Lower step：
(1) preparation of diamond dispersion liquid：Weigh that 2.4~2.6g grain sizes are 80~100nm and 0.24~0.26g grain sizes are respectively
The diamond powder of the modified processing of 40~50nm, ground and mixed；50ml solvents, ultrasound is added in mixed powder after grinding
Disperse 20~30min；Obtain stable diamond dispersion liquid；
(2) preparation of block carbon reinforcement/carbon composite presoma：The carbon cloth that surface is coated with to adhesive passes through and configures
It is allowed to impregnate in good diamond dispersion liquid, dry, solidification obtains the precast body of the carbon cloth containing diamond powder；
(3) preparation of block carbon reinforcement/carbon composite：The precast body of the carbon cloth containing diamond powder will be prepared
It cuts out, is laminated on together by required specification, apply pressure under protective atmosphere and obtain the carbon reinforcement/carbon after high temperature sintering
Composite material.
4. the preparation method of block carbon reinforcement/carbon composite according to claim 3, it is characterised in that：The step
Suddenly in (1), the solvent is absolute ethyl alcohol.
5. the preparation method of block carbon reinforcement/carbon composite according to claim 3, it is characterised in that：The step
Suddenly in (2), the adhesive is epoxyn.
6. the preparation method of block carbon reinforcement/carbon composite according to claim 3, it is characterised in that：The step
Suddenly in (3), it is characterised in that：The detailed process of the sintering is：The presoma lamination for weighing the composite material is positioned over mould
In tool, the mold is graphite jig；It is sintered under protective atmosphere, the protective atmosphere is argon gas；Start to mould at 900 DEG C
The pressure of tool pressurization, application is 40~70MPa；When reaching maximum sintering temperature, the maximum temperature is 1600~1700
℃；Held for some time, the soaking time are 2~8min；Then pressure release is cooled to room temperature.
7. the preparation method of block carbon reinforcement/carbon composite according to claim 3, it is characterised in that：The burning
When becoming discharge plasma sintering, heating rate is 100~150 DEG C/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315358A (en) * | 2021-12-27 | 2022-04-12 | 海南大学 | Fully-compact binderless tungsten carbide ceramic and preparation method thereof |
| CN115385704A (en) * | 2022-08-23 | 2022-11-25 | 广西三元华鑫特种陶瓷有限公司 | Method for reducing drying stress deformation of micro-nano fiber reinforced silicon carbide material semi-finished product |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315358A (en) * | 2021-12-27 | 2022-04-12 | 海南大学 | Fully-compact binderless tungsten carbide ceramic and preparation method thereof |
| CN114315358B (en) * | 2021-12-27 | 2023-01-24 | 海南大学 | Fully-compact binderless tungsten carbide ceramic and preparation method thereof |
| CN115385704A (en) * | 2022-08-23 | 2022-11-25 | 广西三元华鑫特种陶瓷有限公司 | Method for reducing drying stress deformation of micro-nano fiber reinforced silicon carbide material semi-finished product |
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| CN108530099B (en) | 2021-09-07 |
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