CN106946551A - A kind of graphene/carbon nano-tube strengthens the preparation method of alumina ceramic coating - Google Patents
A kind of graphene/carbon nano-tube strengthens the preparation method of alumina ceramic coating Download PDFInfo
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Abstract
The present invention, which provides a kind of graphene/carbon nano-tube, strengthens the preparation method of alumina ceramic coating.Its feature is to be added to a small amount of graphene in aluminum oxide with the CNT after treating, and prepares composite ceramic coat and brushes on matrix.The slurry is by AL2O3Powder, graphene powder, treated CNT and adhesive composition, will grind after the CNT drying after processing, with graphene, AL2O3The 8h of ball milling 6 in proportion, the wherein mass percent of nano material are no more than 0.4%, and mixed aggregate is sufficiently stirred for adhesive by 1: 0.8 mass ratio, dried in the shade naturally in ventilation after 2h in 50 300 DEG C by gradient-heated 5h, that is, prepare alumina composite ceramic coating.The invention is compared with ceramic coating processing common method, and simpler with equipment and technology, operational suitability is strong, and coating good dispersion, and bond strength is good, the advantage such as wear resistant corrosion resistant.
Description
Technical field：
The present invention relates to the preparation method that a kind of graphene/carbon nano-tube strengthens alumina ceramic coating.
Background technology：
Aluminium oxide ceramics has that mechanical strength is big, insulaion resistance big, and hardness is high, the excellent performance such as wear resistant corrosion resistant.It
In petro chemical industry, national defence, favor is both mechanically and electrically enjoyed in the field such as industry, but be due to the high hard crisp of ceramic material
Property, and both coefficients of expansion difference so that its bond strength with metallic matrix is poor.
CNT and graphene are all the carbonaceous materials of nano-scale, due to its great surface area, good conduction
Heat conductivility, superior mechanical property has very big application prospect in recent years, and a kind of collaboration can be also produced between them
Effect, the composite physical and chemical performance added with graphene carbon pipe can be significantly improved, but be due to Van der Waals
The effect of power, graphene and CNT are easily reunited, and the CNT for mixing functionalization can not only improve the scattered of itself
Property, the interfacial interaction between reinforcement and matrix can also be improved, therefore strengthen pottery by adding carbon pipe and graphene
The performance of porcelain coating has actual meaning.
Ceramic coating is widely used, and preparation technology is numerous, and conventional have a spraying process, vapour deposition process, self-propagating high-temperature method,
Sol-gal process, laser cladding, wherein slurry process etc., slurry process are simple due to technique, easy to operate, strong adaptability, and not
Limited by space enrironment than larger development prospect.
The content of the invention：
The invention aims to overcome the shortcomings of existing ceramic coating presence, there is provided a kind of graphene/carbon nano-tube
Strengthen the preparation method of alumina ceramic coating, this method security is good, and low cost is simple to operate, stable preparation process, production
Efficiency high, good product performance.
To achieve the above object, the present invention uses following technical proposals：
(1) by MWNT, the MWNT of carboxylation is made in heating water bath in the concentrated sulfuric acid and concentrated nitric acid；
(2) it will be dried after the MWNT of carboxylation and a certain amount of SDBS ultrasonic disperses under the conditions of vacuum drying and grind preparation
Obtain MWNT-COOH-SDBS；
(3) above-mentioned material, graphene, Al are weighed respectively with balance2O3, wherein treated carbon pipe and graphene accounts for three
The 0~0.4% of gross mass；
(4) ceramic aggregate weighed is loaded into planetary type ball-milling tank, abrading-ball is agate ball, and ratio of grinding media to material uses 2: 1, at room temperature
Required mixed powder is made in 250~300r/min mixing and ball millings 6-8h；
(5) well mixed aggregate and adhesive in mass ratio 1: 0.8 are sufficiently stirred for；
(6) obtained slurry undercoat is brushed and overlayed on Q235 matrixes, dry in the shade 2~3h naturally；
(7) exemplar is put into air dry oven and heats 5h at 50~300 DEG C, obtain its natural cooling 24h in case
Required finished product.
It is preferred that, step (1) described MWNT ID is in 2~5nm, OD ＜ 8nm, and length is at 10~30 μm；Stone described in step 2
Black alkene thickness is in 4~20nm, and flit size is at 5~10 μm, and alumina powder granularity is at 20~40 μm.
It is preferred that, the volume ratio of the concentrated sulfuric acid (98wt%) and concentrated nitric acid (70wt%) described in step (1) is set to 3: 1,
Stood after 20~30min of ultrasound, water bath heating temperature is set to 110~120 DEG C, 20~30min is heated using stirrer, with oil
Bath natural cooling 1h, the CNT mixed liquor after cooling pours into distilled water diluting, and CNT is precipitated using centrifuge
After outwell upper strata acid solution, with 0.22 μm of cellulose mixture adipose membrane vacuum filtration, and with distilled water cyclic washing to neutrality, finally will
The product filtered is dried in vacuo at 50 DEG C, and the MWNT (MWNT-COOH) of carboxylation is obtained after grinding.
It is preferred that, the product and SDBS of the step of taking equivalent in step (2) (1) in absolute ethyl alcohol after ultrasound 2h, will be produced
Thing is dried in vacuo at 50 DEG C, obtains mixing the MWNT-COOH-SDBS of functionalization after grinding.
It is preferred that, step (3) the graphene thickness is in 4~20nm, and flit size is in 5~10 μm, alumina powder grain
Degree is at 20~40 μm.
It is preferred that, step (4) ball milling is run using forward and reverse two way alternate, forward and reverse every 2h alternate runs, ball mill
The rotating speed of rotating disk is about the 1/2 of ball grinder rotating speed, after ball milling terminates, and spherical tank needs to place one day, and the powder allowed after ball milling has
In one relaxation time, sample again afterwards.
It is preferred that, coating is prepared on matrix using the mode uniformly coated in step (6), the thickness of the coating exists
0.3~0.6mm.
It is preferred that, it is staged heating technique described in step (7)：Uniform heating temperature is to being incubated 1h after 50 DEG C, then
It is even to be heated to 100 DEG C and be incubated 2h in this stage, continue to be heated to 250 DEG C, be incubated 1h, be heated to 300 DEG C of insulation 1h.
The invention has the advantages that：Graphene and the special two-dimensional structure of carbon pipe and mechanical property can reduce pottery
The extension of porcelain crackle improves the toughness of alumina ceramic material simultaneously, while anchoring strength of coating is high, compactness is good, and antifriction is resistance to
Grind performance high, and solidification temperature requires low；Whole preparation technology strong adaptability, and preparation technology is easy, low cost, with extensive
Application prospect.
Specific embodiment：
Embodiment one：According to graphene 0.2%, aluminum oxide 99.8% weighs powder, with planetary ball mill in 300r/
Ball milling 8h under min, mixing aggregate in mass ratio 1: 0.8 is sufficiently stirred for adhesive, is brushed and is overlayed on Q235 exemplars with undercoat, from
50 DEG C of insulation 1h are uniformly heated to after the right 2h that dries in the shade in air dry oven, 100 DEG C is then heated to, is incubated 2h, continue to heat
To 250 DEG C, 1h is incubated, 300 DEG C of insulation 1h is heated to, its natural cooling 24h in case is obtained required finished product.Fracture toughness
4.2MPa*m1/2 is reached, bending strength reaches 358MPa, (pure alumina 3.5MPa*m1/2,350MPa), coefficient of friction is
0.47 (pure alumina 0.48).
Embodiment two：According to graphene 0.2%, the aluminum oxide 99.6% of MWNT-COOH-SDBS 0.2% weighs powder,
With planetary ball mill under 300r/min ball milling 8h, mixing aggregate in mass ratio 1: 0.8 be sufficiently stirred for adhesive, use undercoat brush
It is coated on Q235 exemplars, is uniformly heated to 50 DEG C of insulation 1h after the 2h that dries in the shade naturally in air dry oven, is then heated to 100
DEG C, 2h is incubated, continues to be heated to 250 DEG C, is incubated 1h, 300 DEG C of insulation 1h is heated to, obtains its natural cooling 24h in case
Required finished product.Fracture toughness reaches 4.8MPa*ml/2, bending strength reach 371MPa (pure alumina 3.5MPa*ml/2,
350MPa), coefficient of friction is 0.43 (pure alumina 0.48).
Embodiment three：Powder is weighed according to the aluminum oxide 99.8% of MWNT-COOH-SDBS 0.2%, planetary ball mill is used
The ball milling 8h under 300r/min, mixing aggregate in mass ratio 1: 0.8 is sufficiently stirred for adhesive, is brushed with undercoat and is overlayed on Q235 samples
On part, 50 DEG C of insulation 1h are uniformly heated to after the 2h that dries in the shade naturally in air dry oven, 100 DEG C is then heated to, is incubated 2h, after
It is continuous to be heated to 250 DEG C, 1h is incubated, 300 DEG C are heated to, 1h is incubated, its natural cooling 24h in case is obtained required finished product.
Fracture toughness reaches 4.3MPa*m1/2, and bending strength reaches 354MPa, (pure alumina 3.5MPa*m1/2,350MPa), friction
Coefficient is 0.45 (pure alumina 0.48).
Embodiment four：Powder is weighed according to the aluminum oxide 99.8% of MWNT-COOH 0.2%, is existed with planetary ball mill
Ball milling 8h under 300r/min, mixing aggregate in mass ratio 1: 0.8 is sufficiently stirred for adhesive, is brushed with undercoat and is overlayed on Q235 exemplars
On, 50 DEG C of insulation 1h are uniformly heated to after the 2h that dries in the shade naturally in air dry oven, 100 DEG C is then heated to, is incubated 2h, continue
250 DEG C are heated to, 1h is incubated, 300 DEG C of insulation 1h is heated to, its natural cooling 24h in case is obtained required finished product.Fracture
Toughness reaches 4.3MPa*m1/2, and bending strength reaches 356MPa (pure alumina 3.5MPa*m1/2,350MPa), and coefficient of friction is
0.41 (pure alumina 0.48).
The porosity of coating is made between 5~17%, due to SDBS property, the compactness of sample in scheme one
It is higher.
Coating abrasion rate reduces 50~70% compared to pure alumina.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, nothing
By from the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by institute
Attached claim rather than described above are limited, it is intended that will fall in the implication and scope of the equivalency of claim
All changes include in the present invention.Any mark in claim should not be considered as to the claim involved by limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It may be appreciated other embodiment.
Claims (9)
1. a kind of graphene/carbon nano-tube strengthens the preparation method of alumina ceramic coating, it is with graphene and treated carbon
Nanotube is enhancing phase, using aluminum oxide as matrix, it is characterised in that the preparation method comprises the following steps：
(1) by MWNT, the MWNT of carboxylation is made in heating water bath in the concentrated sulfuric acid and concentrated nitric acid；(2) by the MWNT of carboxylation with it is a certain amount of
SDBS ultrasonic disperses after dry and grind under the conditions of vacuum drying and be prepared into MWNT-COOH-SDBS；(3) distinguished with balance
Weigh above-mentioned material, graphene, Al2O3, wherein treated carbon pipe and graphene accounts for the 0~0.4% of three's gross mass；(4) will
The ceramic aggregate weighed loads planetary type ball-milling tank, and abrading-ball is agate ball, and ratio of grinding media to material uses 2: 1, at room temperature 250~300r/min
Required mixed powder is made in mixing and ball milling 6-8h；(5) well mixed aggregate and adhesive in mass ratio 1: 0.8 are fully stirred
Mix；(6) obtained slurry undercoat is brushed and overlayed on Q235 matrixes, dry in the shade 2~3h naturally；(7) exemplar is put into air blast to do
In 50~250 DEG C of scope internal heating curing 5h in dry case, its natural cooling 24h in case is set to obtain required finished product.
2. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：The ID of MWNT described in step 1 is in 2~5nm, OD ＜ 8nm, and length is at 10~30 μm.
3. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：The volume ratio of the concentrated sulfuric acid (98wt%) and concentrated nitric acid (70wt%) described in step 1 is set to after 3: 1,20~30min of ultrasound
Stand, water bath heating temperature is set to 110~120 DEG C, 20~30min is heated using stirrer, with oil bath pan natural cooling 1h,
CNT mixed liquor after cooling pours into distilled water diluting, CNT is outwelled upper strata acid solution after precipitating using centrifuge,
With 0.22 μm of cellulose mixture adipose membrane vacuum filtration, and with distilled water cyclic washing to neutrality, finally by the product filtered 50
It is dried in vacuo at DEG C, the MWNT (MWNT-COOH) of carboxylation is obtained after grinding.
4. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：The product and SDBS of the step 1 of equivalent are taken in step 2, in absolute ethyl alcohol after ultrasound 2h, vacuum is done at 50 DEG C by product
It is dry, obtain mixing the MWNT-COOH-SDBS of functionalization after grinding.
5. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：Graphene thickness described in step 3 is in 4~20nm, and flit size is at 5~10 μm, and alumina powder granularity is at 20~40 μm.
6. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：Step 4 ball milling is run using forward and reverse two way alternate, and forward and reverse every 2h alternate runs, the rotating speed of ball mill rotating disk is about
For the 1/2 of ball grinder rotating speed, after ball milling terminates, spherical tank needs to place one day, and the powder allowed after ball milling has a relaxation time, it
Sample again afterwards.
7. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：Coating is prepared on matrix using the mode uniformly coated in step 6, the thickness of the coating is in 0.3~0.6mm.
8. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：It is staged heating technique described in step 7：Uniform heating temperature is to being incubated 1h after 50 DEG C, then is uniformly heated to 100 DEG C simultaneously
2h is incubated in this stage, continues to be heated to 250 DEG C, is incubated 1h, 300 DEG C of insulation 1h are heated to.
9. graphene/carbon nano-tube according to claim 1 strengthens the preparation method of alumina ceramic coating, its feature exists
In：Anchoring strength of coating is high, and compactness is good, and properties of antifriction and wear resistance is high, and solidification temperature requires low.
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| CN108046745A (en) * | 2018-01-03 | 2018-05-18 | 景德镇陶瓷大学 | A kind of preparation method of the magnesia household china of graphene enhancing |
| CN108299016A (en) * | 2017-12-28 | 2018-07-20 | 佛山市因诺维生物科技有限公司 | A kind of new ceramic material |
| CN108359971A (en) * | 2018-01-04 | 2018-08-03 | 江西领航宇宙陶瓷材料有限公司 | A kind of preparation method of the quantum ceramic coating based on carbon nanotube |
| CN108455588A (en) * | 2017-12-28 | 2018-08-28 | 佛山市因诺维生物科技有限公司 | A kind of high abrasion ceramic material |
| CN108546157A (en) * | 2018-05-31 | 2018-09-18 | 西北工业大学 | A kind of surface modifying method of carbon/carbon composite |
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