CN106119848B - The preparation method and its hot rolling treatment of the sintering enamelled coating of the compound slurry of the nanometer enamel of surface of low-carbon steel - Google Patents
The preparation method and its hot rolling treatment of the sintering enamelled coating of the compound slurry of the nanometer enamel of surface of low-carbon steel Download PDFInfo
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- CN106119848B CN106119848B CN201610536428.7A CN201610536428A CN106119848B CN 106119848 B CN106119848 B CN 106119848B CN 201610536428 A CN201610536428 A CN 201610536428A CN 106119848 B CN106119848 B CN 106119848B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D5/00—Coating with enamels or vitreous layers
- C23D5/02—Coating with enamels or vitreous layers by wet methods
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D13/00—After-treatment of the enamelled articles
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D7/00—Treating the coatings, e.g. drying before burning
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- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
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- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The preparation method and its hot rolling treatment of the sintering enamelled coating of the compound slurry of the nanometer enamel of surface of low-carbon steel.The present invention relates to a kind of preparation method of the nano combined fused slurry enamel coating of surface of low-carbon steel and its hot rolling treatment coating for metal surfaces processing technology fields, the present invention passes through the preparation and hot rolling treatment of nanometer enamel fused slurry coating, it prepares hole and outstanding milkiness is good, the corrosion-resistant finishes of compact and uniform structure.In the preparation of coating and course of hot rolling, the present invention controls nanotechnology, Glaze Composition, the effectively orderly combination of material hot rolling technique, the characteristic small using the particle size of nano-powder, energy is high effectively reduces the hole and crackle of nanometer slurry sinter coating, improve the compactness and uniformity of coating, using Composition Control technique, coating structure is made to have the characteristics that fine and close less porous hole, and then effectively prevents Cl‑Deng the infiltration of other ions.
Description
Technical field
The present invention relates to a kind of preparations applied to quiet steel nano enamel slurry corrosion-resistant finishes and corresponding hot rolling to add
Work technology belongs to nanometer slurry sinter coating technology and hot rolling treatment technical field.
Background technique
The sintering enamelled coating of nanometer slurry be nanotechnology with plasma spray technology effectively in conjunction with and generate one is more new
The technology of grain husk is further extension and expansion after micron powder spraying technology, but due to the skin effect of nano-powder, small ruler
Very little effect, high energy efficiency should wait properties, have more excellent and unique performance compared with micron particles, so nanometer slurry is sintered
It is that new new technology is started in completely new having that enamel coating technology, which can also be said, at home and abroad has a large amount of scientific research at present
Personnel and scientific research institution start that the preparation of the sintering enamelled coating of nanometer slurry and post-processing technology are explored and studied, at present
In the mainly Thermal Barrier Coating Technologies that this facilitates research more, and in anti-corrosion nano enamel coating especially metal alloy corrosion resistant
Research is still less in terms of losing nanometer enamel coating.
Hole, crackle and structure it is loose uneven the defects of be plasma-coated at present existing one and biggish ask
Topic, there is presently no good methods can solve this problem, and the nanometer slurry from current thermal barrier coating field is sintering enamelled
From the point of view of the case where coating, hole, crackle and the non-uniform situation of short texture have apparent improvement compared with micron powder coating,
But this problem still has in the sintering enamelled coating of nanometer slurry, and in the reality of nanometer enamel fused slurry enamel coating
Obviously revealed in application process, this to the sintering enamelled coating of nanometer slurry industrialized production popularization practical by very big
Limitation, especially enamel coating is more obvious in corrosion resistant application aspect, and the presence of hole and crackle can be such that corrosive deposit wears
Open-work hole and crackle and directly contacted with matrix, so that protective coating be made to fail.So effectively reducing the hole in coating and splitting
Line is nanometer slurry sintering paint-on technique field urgent problem to be solved.
Summary of the invention
The present invention prepares hole and the porosity by preparation and hot rolling treatment to nanometer enamel fused slurry coating
It is few, the corrosion resistant enamel coating of compact and uniform structure.In the preparation of coating and coating procedure, the present invention carries out enamel composition
Depth profiling can effectively solve glaze and matrix during the application of slip and combine untight ask by the way that 1 ~ 3% binder is added
Topic.The good diopside phase of corrosion resistance is obtained by the proportion between control raw mineral materials simultaneously, furthermore passes through control Na2O
And B2O3Amount be sintered boron oxygen triangle body close packed structure and reduce the intrinsic porous amorphous structure of enamel layer.Meanwhile the present invention
Nanosizing is carried out to enamel particle by long-time ball milling.The characteristic small using the particle size of nano-powder, energy is high is effective
The hole and crackle of fused slurry coating are reduced, the compactness and uniformity for improving coating make coating using material hot rolling technology
Structure more dense uniform, hole under the crunch effect of roll-force is further reduced.
The present invention proposes a kind of preparation method of nano combined fused slurry enamel coating of surface of low-carbon steel, it is characterised in that
With following process and step:
A. use the compositing formula of enamel powder for (wt.%): 55.26SiO2, 6.59Al2O3, 8.56ZnO,
8.12B2O3, 4.96Na2O, 10.77CaO, 2.24MgO and 1 ~ 3CeO.
B. powder ball milling: the dry ball milling of 80 ~ 200h is passed through to the enamel powder that preparation is completed celestial body grinding machine of being expert at, is connect
Get off to add the wet ball grinding process that the grinding aids such as ethyl alcohol carry out 200h, next ball and material is separated, finally as drying
Machine drying;
C. prepare coating slurry: by the nano-scale particle of above-mentioned milled, (i.e. the diameter of these particles is tens to several hundred
Between nanometer), there is certain glue wherein adding a certain amount of cobalt oxide and preparing there are also the ethyl alcohol of nickel oxide and addition 10%
The slurry of degree, so as to directly as sintering coating material;Specific method is 1 ~ 1.5% will to be added in nanometer enamel powder to stick
Soil and ethyl alcohol and 0.5%NiO+1.5%CoO binder, make it be mixed into jelly, the volume of solid matter point in jelly
Number is 75 ~ 95%;10 ~ 35min is stirred to jelly using mechanical mixing method under conditions of 50 ~ 70 DEG C;It can be prepared by slurry;
D. surface coating and green body production: the surface that slurry is uniformly coated in mild steel is taken out after stirring, is connect
It is put into drying box and dries 20 ~ 50min;One layer of uniform coating has just been obtained in specimen surface in this way, has obtained so-called green body;
E. sample is sintered: and then the idiosome prepared is placed in Muffle furnace and is sintered, temperature is 750 ~ 900 DEG C, sintering
Time is that 15 ~ 60min obtains uniform enamel coating;
F. hot rolling treatment: setting start rolling temperature are as follows: 300 ~ 980 DEG C, total rolling is than being 10 ~ 30%, using 3 ~ 5 passages reality
Now sample is kept the temperature 30min under start rolling temperature first, keeps sample temperature uniform by whole drafts before rolling starts;Rolling
After sample be placed in high temperature process furnances under hydrogen atmosphere make annealing treatment, annealing temperature is 500 ~ 900 DEG C, annealing knot
Sample furnace cooling after beam.
The present invention has a characteristic that
1, of the invention by the way that by nanotechnology, Glaze Composition control and material hot rolling technique effectively orderly combine, and
Its respective advantage is made full use of, there is small-size effect, skin effect and high energy efficiency should wait special performances, warding off for nano-powder
It in porcelain coating procedure, combines more closely, more uniformly spreads between particle, to effectively reduce the hole in coating and split
Line, the proportion of Glaze Composition are capable of the phase composition of Effective Regulation sintered product, until with excellent corrosion resistance object mutually simultaneously
And generate the phase structure of even compact.In course of hot rolling, since by the crunch rolled, coat inside structure is slightly variable
Shape keeps coating structure more fine and close, is heat-treated under hydrogen state to sample after rolling, carries out sufficiently to sample
Interpenetrated atom in coating in the case where reduction, to keep coating structure more uniform.
2, the present invention can produce hole and crackle is few by a series of coherent techniques, and outstanding milkiness is excellent, compact structure
The uniform nanometer enamel coating of ingredient.The invention also can be suitable for receiving using other metal materials as matrix by the adjustment of parameter
The preparation of riceization coating.
3, present invention process is coherent, effect is obvious, no pollution to the environment, but because current nano-powder technology of preparing into
Step, nano-powder cost reduces, so the present invention is suitable for very much industrializing expanding production.
Specific embodiment
Embodiment 1
10% ethyl alcohol and clay is added in the enamel powder prepared and 0.5%NiO+1%CoO binder becomes glue
Object, the volume fraction of solid matter is 70% in jelly, stirs 10min to jelly using mechanical mixing method.After stirring
Coated in Q235 surface of low-carbon steel, placing into baking oven makes its skin drying form idiosome, and obtained idiosome is put into Muffle furnace
It is sintered 30 minutes under conditions of 810 DEG C.Sample is subjected to hot rolling treatment after firing, start rolling temperature is 300 DEG C, in sample
It is rolled after keeping the temperature 30min at 300 DEG C, sample is placed in pipe after rolling than being 10% by totally 3 passage, total rolling for rolling
It is made annealing treatment in a hydrogen atmosphere in formula furnace, annealing temperature is 500 DEG C, keeps the temperature sample furnace cooling after 30min.
Embodiment 2
10% ethyl alcohol and clay is added in the enamel powder prepared and 0.5%NiO+1%CoO binder becomes glue
Object, the volume fraction of solid matter is 75% in jelly, stirs 10min to jelly using mechanical mixing method.After stirring
Coated in Q235 surface of low-carbon steel, placing into baking oven makes its skin drying form idiosome, and obtained idiosome is put into Muffle furnace
It is sintered 30 minutes under conditions of 830 DEG C.Sample is subjected to hot rolling treatment after firing, start rolling temperature is 450 DEG C, in sample
It is rolled after keeping the temperature 30min at 450 DEG C, sample is placed in pipe after rolling than being 15% by totally 4 passage, total rolling for rolling
It is made annealing treatment in a hydrogen atmosphere in formula furnace, annealing temperature is 600 DEG C, keeps the temperature sample furnace cooling after 30min.
Embodiment 3
10% ethyl alcohol and clay is added in the enamel powder prepared and 0.5%NiO+1%CoO binder becomes glue
Object, the volume fraction of solid matter is 80% in jelly, stirs 10min to jelly using mechanical mixing method.After stirring
Coated in Q235 surface of low-carbon steel, placing into baking oven makes its skin drying form idiosome, and obtained idiosome is put into Muffle furnace
It is sintered 30 minutes under conditions of 850 DEG C.Sample is subjected to hot rolling treatment after firing, start rolling temperature is 780 DEG C, in sample
It is rolled after keeping the temperature 30min at 780 DEG C, sample is placed in pipe after rolling than being 20% by totally 5 passage, total rolling for rolling
It is made annealing treatment in a hydrogen atmosphere in formula furnace, annealing temperature is 700 DEG C, keeps the temperature sample furnace cooling after 30min.
Embodiment 4
10% ethyl alcohol and clay is added in the enamel powder prepared and 0.5%NiO+1%CoO binder becomes glue
Object, the volume fraction of solid matter is 85% in jelly, stirs 10min to jelly using mechanical mixing method.After stirring
Coated in Q235 surface of low-carbon steel, placing into baking oven makes its skin drying form idiosome, and obtained idiosome is put into Muffle furnace
It is sintered 30 minutes under conditions of 850 DEG C.Sample is subjected to hot rolling treatment after firing, start rolling temperature is 850 DEG C, in sample
It is rolled after keeping the temperature 30min at 850 DEG C, sample is placed in pipe after rolling than being 25% by totally 5 passage, total rolling for rolling
It is made annealing treatment in a hydrogen atmosphere in formula furnace, annealing temperature is 800 DEG C, keeps the temperature sample furnace cooling after 30min.
Embodiment 5
10% ethyl alcohol and clay is added in the enamel powder prepared and 0.5%NiO+1%CoO binder becomes glue
Object, the volume fraction of solid matter is 90% in jelly, stirs 10min to jelly using mechanical mixing method.After stirring
Coated in Q235 surface of low-carbon steel, placing into baking oven makes its skin drying form idiosome, and obtained idiosome is put into Muffle furnace
It is sintered 30 minutes under conditions of 870 DEG C.Sample is subjected to hot rolling treatment after firing, start rolling temperature is 900 DEG C, in sample
It is rolled after keeping the temperature 30min at 980 DEG C, sample is placed in pipe after rolling than being 30% by totally 5 passage, total rolling for rolling
It is made annealing treatment in a hydrogen atmosphere in formula furnace, annealing temperature is 850 DEG C, keeps the temperature sample furnace cooling after 30min.
Embodiment 6
10% ethyl alcohol and clay is added in the enamel powder prepared and 0.5%NiO+1%CoO binder becomes glue
Object, the volume fraction of solid matter is 95% in jelly, stirs 10min to jelly using mechanical mixing method.After stirring
Coated in Q235 surface of low-carbon steel, placing into baking oven makes its skin drying form idiosome, and obtained idiosome is put into Muffle furnace
It is sintered 30 minutes under conditions of 900 DEG C.Sample is subjected to hot rolling treatment after firing, start rolling temperature is 980 DEG C, in sample
It is rolled after keeping the temperature 30min at 980 DEG C, sample is placed in pipe after rolling than being 30% by totally 5 passage, total rolling for rolling
It is made annealing treatment in a hydrogen atmosphere in formula furnace, annealing temperature is 900 DEG C, keeps the temperature sample furnace cooling after 30min.To each reality
Apply that example sample after processing carries out surface macroscopic view and corrosion resisting property is tested, the results are shown in Table 1.
From the point of view of example test case, prepared nanometer enamel coating has the microcosmic knot of dense uniform through the invention
Structure and very strong corrosion resisting property.
Claims (1)
1. a kind of preparation method of the nano combined fused slurry enamel coating of surface of low-carbon steel, it is characterised in that have following mistake
Journey and step:
A. use the compositing formula of enamel powder for (wt.%): 55.26SiO2, 6.59Al2O3, 8.56ZnO, 8.12B2O3,
4.96Na2O, 10.77CaO, 2.24MgO and 1~3CeO;
B. powder ball milling: the dry ball milling of 80~200h is passed through to the enamel powder that preparation is completed celestial body grinding machine of being expert at, next
The wet ball grinding process that ethyl alcohol grinding aid carries out 200h is added, next ball and material is separated, is finally placed in drying machine drying
?;
C. prepare coating slurry: by the nano-scale particle of milled, i.e., the diameter of these particles tens between several hundred nanometers,
Wherein adding a certain amount of cobalt oxide, there are also the ethyl alcohol of nickel oxide and addition 10% to prepare the slurry with certain viscosity, from
And it can be directly as sintering coating material;Specific method be will be added in nanometer enamel powder 1~1.5% clay and ethyl alcohol with
And 0.5%NiO+1.5%CoO binder, so that it is mixed into jelly, in jelly the volume fraction of solid matter be 75~
95%;10~35min is stirred to jelly using mechanical mixing method under conditions of 50~70 DEG C;It can be prepared by required certain viscous
The slurry of degree;
D. surface coating and green body production: the surface that slurry is uniformly coated on mild steel is taken out after stirring, is subsequently placed into
Drying box dries 20~50min;One layer of uniform coating has just been obtained in specimen surface in this way, has obtained so-called green body;
E. sample is sintered: and then the idiosome prepared is placed in Muffle furnace and is sintered, temperature is 750~900 DEG C, and sintering time is
15~60min obtains uniform enamel coating;
F. hot rolling treatment: setting start rolling temperature are as follows: 300~980 DEG C, total rolling is realized than being 10~30% using 3~5 passages
Sample is kept the temperature 30min under start rolling temperature first, keeps sample temperature uniform by whole drafts before rolling starts;Rolling knot
Sample is placed in high temperature process furnances under hydrogen atmosphere after beam and is made annealing treatment, annealing temperature is 500~900 DEG C, annealing knot
Sample furnace cooling after beam.
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CN103590032A (en) * | 2013-11-11 | 2014-02-19 | 上海大学 | Method for preparing Ni-Cr-Al coating on surface of low-carbon steel based on nanotechnology |
CN103590033A (en) * | 2013-11-11 | 2014-02-19 | 上海大学 | Method for preparing Ni-Cr-Mo plating on surface of low-carbon steel based on nanotechnology |
CN105271750A (en) * | 2014-07-10 | 2016-01-27 | 北京航空航天大学 | Preparation of enamel coating modified by rare earth doping and nanometer effect |
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CN104451655B (en) * | 2013-09-13 | 2018-02-16 | 中国科学院金属研究所 | High temperature resistance material surface alloy coating composite material, coating and preparation method thereof |
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US3453849A (en) * | 1965-10-13 | 1969-07-08 | Texas Instruments Inc | Manufacture of clad metals |
CN103590032A (en) * | 2013-11-11 | 2014-02-19 | 上海大学 | Method for preparing Ni-Cr-Al coating on surface of low-carbon steel based on nanotechnology |
CN103590033A (en) * | 2013-11-11 | 2014-02-19 | 上海大学 | Method for preparing Ni-Cr-Mo plating on surface of low-carbon steel based on nanotechnology |
CN105271750A (en) * | 2014-07-10 | 2016-01-27 | 北京航空航天大学 | Preparation of enamel coating modified by rare earth doping and nanometer effect |
Non-Patent Citations (1)
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