CN109852110A - A kind of preparation method improving chromium-free environment-friendly coating orientation silicon steel surface quality - Google Patents
A kind of preparation method improving chromium-free environment-friendly coating orientation silicon steel surface quality Download PDFInfo
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- CN109852110A CN109852110A CN201910006739.6A CN201910006739A CN109852110A CN 109852110 A CN109852110 A CN 109852110A CN 201910006739 A CN201910006739 A CN 201910006739A CN 109852110 A CN109852110 A CN 109852110A
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Abstract
The present invention provides a kind of preparation methods for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step includes: S1, to carrying out decarburizing annealing after orientation silicon steel hot rolled plate cold rolling, high annealing is carried out after coating annealing separation agent, is coated the phosphate-based environmentally friendly insulating coating solution of Chrome-free；Heat up drying after S2, coating, and plate temperature is 200-400 DEG C, and the heating rate is 60~85 DEG C/s；Sintering curing obtains product under the mixed-gas atmosphere of hydrogen and nitrogen after S3, drying, and the sintering curing time is 45-90s；Wherein, tension is applied to directional silicon steel during the coating, drying and sintering curing.The surface coverings class defects such as using environment-friendly coating orientation silicon steel produced by the present invention with excellent surface quality, coating adhesion is good, and uncoated piebald, coating powder, coating are bad.
Description
Technical field
The invention belongs to orientation silicon steel technical fields, and in particular to a kind of raising chromium-free environment-friendly coating orientation silicon steel surface matter
The preparation method of amount.
Background technique
Orientation silicon steel is largely used to as magnetive cord material, in order to reduce energy loss, it is desirable that iron loss is small.In order to reduce
Iron loss, assigning tension to steel plate is an effective method.Therefore, smaller than steel plate by thermal expansion coefficient by being formed at high temperature
Material constitute epithelium come to steel plate assign tension, achieve the purpose that reduce iron loss.
The manufacturing method of directional silicon steel is at present, after generating forsterite system epithelium in making finished products process, then
Form the insulating coating based on phosphate.This insulating coating main component based on phosphate is gluey SiO2,
Aluminium dihydrogen phosphate and chromic anhydride.Wherein chromic anhydride is harmful substance, is banned from use by ROHS instruction.Instruction requires, and 2006
The index of harmful element has to comply with regulation in the electric equipment products sold on EU market from July 1, in, that is, to be limited
Harmful substance has；Cadmium, lead, mercury, Cr VI, polybrominated biphenyls, polymerization bromination diphenyl ether etc..It has taken the lead in requiring to enter its area
Chromium cannot be contained in the electric steel plate in domain, there will be more and more countries and regions to propose similar requirement from now on.In order to
The shortcomings that overcoming the coating of nocuousness containing chromium, the substances of domestic and international silicon steel manufacturer consideration other forms substitute chromic anhybride.
Patent No. KR20010082119 describes the development situation of a kind of Chrome-free oriented electrical steel and its insulating coating, is situated between
Continued the chemical component and production technology of the steel grade, and last insulating coating includes: trbasic zinc phosphate；Magnesium phosphate；0.5-12% boric acid
Or one of borate containing Na, Al, Ca, Li, Mg.Coating the result shows that coating corrosion resistance is poor, appearance of coat
It is bad.Patent No. JP19790150688 describes a kind of insulating coating for Chrome-free orientation silicon steel, and content includes: 7-60
Part magnesium phosphate；8-40 part one or two kind of sulfate；20 parts of silica gel.Coating the result shows that coating adhesion is general, appearance of coat
It is bad, while the corrosion resistance of coating becomes unsatisfactory.Patent No. ZL200610030717.6 proposes a kind of orientation
Silicon steel chromium-free environment-friendly insulating coating.Its chemical component mass percent are as follows: 0.01%~3% block polyether non-ionic surface
Activating agent, 0.2%~3% boric acid, 9%~30% aluminium dihydrogen phosphate, 8%~20% colloidal silicon dioxide.Coating the result shows that
Coating non-refractory, causes poor corrosion resistance.Application number CN20098111435 provides a kind of with the covering of chromium-free tension
The grain-oriented magnetic steel sheet of film contains in the tension cover film using phosphate and silica as constituent in the present invention
There are manganese compound and potassium compound.It is excellent that application number JP20070176395 provides a kind of having for grain-oriented magnetic steel plate
Hygroscopicity and the Chrome-free stress film masking liquid for reducing iron loss effect.Masking liquid component are as follows: the silica gel of 20 mass parts mixes 10~80 weights
Measure part it is one or more be selected from Mg, Al, Ca, the phosphate of Fe and Mn, 3~30 parts by weight be selected from magnesium, aluminium, iron, manganese, cobalt, bismuth,
Zinc, calcium, barium, strontium or nickel chloride, 1~10 mass parts it is one or more selected from Li, Na, K, Mg, Mn, Ca, Ba, Sr, Fe,
Co, Sn, Ni, Cu, Zn, Al and Bi borate and sulfate.But the heat resistance of the film is poor.Application number 201610593984.8
Disclose a kind of chromium-free environmental-protection insulating paint for orientation silicon steel.Have in coating: 25-50% biphosphate saline solution, 25-
50% silica solution, 1-7% tungstates, 1-5% titanyl sulfate and 10-45% deionized water.And propose that coating is coated on oriented silicon
It need to be in N after steel2Or baking and sintering curing are carried out under the protective atmospheres such as Ar, wherein baking temperature is 400-520 DEG C, baking time
For 30-70s, sintering curing temperature is 780-850 DEG C, and the sintering curing time is 35-75s.The coating has good corrosion-resistant
Property, resistance to hygroscopicity and adhesion.Patent No. ZL201310673461.0 discloses a kind of orientation silicon steel surface tension of capable of improving
Chrome-free stress coat and preparation method help coating to provide steel plate tension from masking liquid ingredient.
These formulas can only preferably meet certain performance of steel plate after masking liquid coating, but not consider the coating of masking liquid
Energy.Due to being free of chromium compound in environmentally friendly insulating coating solution, coating is poor, and masking liquid diffusivity is bad after coating, is easy to produce
Surface covering defect, coating and sintering process of this patent by adjusting masking liquid provide a kind of with excellent surface quality
Chromium-free environment-friendly coating orientation silicon steel.
Summary of the invention
In view of this, largely only considered the insulating properties of steel plate after coating, resistance to without chrome coating for what is developed both at home and abroad
High temperature, corrosion-resistant, adhesion, but the Painting effect of masking liquid is not considered the problems of, the present invention is mainly adjusted by the coating of masking liquid
And sintering process, a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality is provided, is solved due to applying
Surface of steel plate caused by liquid Painting effect is bad leads to the problem of coating class defect, and such as coating piebald, coating is bad, and coating plays powder
Deng.
The present invention provides a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step includes:
S1, to decarburizing annealing is carried out after orientation silicon steel hot rolled plate cold rolling, carry out high annealing after being coated with annealing separation agent, then
It is coated with the phosphate-based environmentally friendly insulating coating solution of Chrome-free；
Heat up drying after S2, coating, and the steel billet temperature is 200~400 DEG C, and heating rate is 60~85 DEG C/s；
Sintering curing obtains product under the mixed-gas atmosphere of hydrogen and nitrogen after S3, drying；
Wherein, tension is applied to directional silicon steel during the coating, drying and sintering curing.
Be coated with rear control plate temperature, guarantee coating be fully cured and uniformity, avoid coating from crossing solidification, effectively prevent coating
Play powder defect.Control panel temperature simultaneously cooperates specific heating rate heating drying, and heating rate is too fast, and the moisture in coating evaporated
Fastly, the bubble of generation causes coating surface coarse in skin breakage, and in addition heating rate is too fast, and masking liquid has little time to spread, and easily produces
Raw surface covering piebald defect；Heating rate is excessively slow, and the phosphate contained in the phosphate-based coating of Chrome-free is easy crystallization, surface
It is also easy to produce micro-crack, influences the insulating properties and corrosion resistance of coating.After coated and dried under specific gas atmosphere sintering curing, effectively
The bad defect of coating surface caused by peroxidating is avoided, whole process applies tension to steel plate, with stoving process and sintering curing
Technique, which cooperates, to be influenced, and is promoted the extension of masking liquid while being improved the magnetic property of steel plate.
Preferably, in step S1, the phosphate-based environmentally friendly insulating coating solution component of the Chrome-free includes phosphate and silica solution, with
Account for masking liquid mass percent meter, phosphate accounting 30%~60%, silica solution accounting 20%~45%；The phosphate be Mg,
One or more of phosphate of Al, Ca, Zn, Ni or Co；The silica solution partial size is 8-15nm.By regulating and controlling silica solution grain
Diameter reaches suitable gel time, improves masking liquid coating, and can effectively avoid particle agglomeration and influence masking liquid brightness.
More preferred, in step S1, the coating thickness of the phosphate-based environmentally friendly insulating coating solution of the Chrome-free is 1~4 μm.It applies
Layer is excessively thin, is unfavorable for the insulation performance of steel plate；Overweight coating, coating is bad, and coating easily plays powder.In coating process, to improve
The coating performance of masking liquid, control masking liquid temperature are 30-40 DEG C, guarantee to promote masking liquid scalability while masking liquid service performance, make
Coating is more evenly.
Preferably, in step S1, the chemical component of the orientation silicon steel hot rolled plate are as follows: by percentage to the quality, C:0.04
~0.08%, Si:3.14~3.4%, Mn:0.06~0.12%, S:0.02~0.03%, Als:0.02~0.03%, N:
0.006~0.01%, surplus is Fe and inevitable impurity.
Preferably, in step S3, the percent by volume that the hydrogen accounts for mixed gas is 0~30%.
More preferred, in step S3, the percent by volume that the hydrogen accounts for mixed gas is 15~25%.
More preferred, in step S3, the sintering curing temperature is 750~950 DEG C.Temperature is too low, and curing of coatings is not
Completely, cause coating hardness inadequate, generate the bad defect of coating；Temperature is excessively high, is unfavorable for production energy-saving, while coating is excessively solid
Change, generates coating and play powder defect.
It is further preferred that the sintering curing time is 45~90s in step S3.Curing time is too short, coating diffusion
Unevenly, it is also easy to produce coating piebald defect；Sintering time is too long, and coating has been easy to produce powder defect.
Preferably, described to apply the tension that tension is 6~8.5MPa.The tension of application is too small, and coating is not achieved to steel plate
Magnetic improvement, the overtension of application are unfavorable for the control of steel plate template.
Compared with prior art, the beneficial effects of the present invention are: not contained in oriented silicon steel manufactured by the present invention
Chromium harmful to environment and human body, product belong to environmentally friendly machine.And it is orientated using environment-friendly coating produced by the present invention
The surface coverings such as silicon steel has excellent surface quality, and coating adhesion is good, and uncoated piebald, coating powder, coating are bad
Class defect, it is practical.
Specific embodiment
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with embodiment, but this hair
Bright protection scope is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention, can pass through
Market is commercially available or can be prepared by existing method.
The present invention provides a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step includes:
S1, to carrying out decarburizing annealing, the chemical component of the orientation silicon steel hot rolled plate after orientation silicon steel hot rolled plate cold rolling are as follows:
By percentage to the quality, C:0.04~0.08%, Si:3.14~3.4%, Mn:0.06~0.12%, S:0.02~0.03%,
Als:0.02~0.03%, N:0.006~0.01%, surplus are Fe and inevitable impurity；It is laggard to be coated with annealing separation agent
Row high annealing is coated the phosphate-based environmentally friendly insulating coating solution of Chrome-free with a thickness of 1~4 μm, controls masking liquid temperature in coating process
Degree is 30-40 DEG C；The phosphate-based environmentally friendly insulating coating solution component of the Chrome-free includes phosphate and silica solution, to account for masking liquid quality hundred
Divide than meter, phosphate accounting 30%~60%, silica solution accounting 20%~45%；The phosphate be Mg, Al, Ca, Zn, Ni or
One or more of phosphate of Co；The silica solution partial size is 8-15nm.In several embodiments of the invention, environmental protection is exhausted
Edge masking liquid Main Components are phosphate and silica solution, and surplus is water, but the masking liquid component that this technique is applicable in is not limited thereto, and are increased
Add the phosphate-based environmentally friendly insulating coating solution of the Chrome-free of certain auxiliary agents that can also achieve the effect that improve surface quality using this technique.
Steel billet temperature is warming up to 200~400 DEG C of drying after S2, coating, and the heating rate is 60~85 DEG C/s；
After S3, drying under the mixed-gas atmosphere of hydrogen and nitrogen, 750~950 DEG C of 45~90s of sintering curing of temperature are obtained
Product；The percent by volume that the hydrogen accounts for mixed gas is 0~30%, it is preferred that hydrogen accounts for the volume basis of mixed gas
Than being 15~25%；
Wherein, 6~8.5MPa tension is applied to directional silicon steel during the coating, drying and sintering curing.
Below in conjunction with ten specific embodiments to a kind of raising chromium-free environment-friendly coating orientation silicon steel surface matter of the application
The preparation method of amount is described in detail.
Embodiment 1
Present embodiments provide a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step packet
It includes:
S1, to carrying out decarburizing annealing, the chemical component of the orientation silicon steel hot rolled plate after orientation silicon steel hot rolled plate cold rolling are as follows:
By percentage to the quality, C:0.06%, Si:3.3%, Mn:0.09%, S:0.025%, Als:0.025%, N:0.008%, it is remaining
Amount is Fe and inevitable impurity；High annealing is carried out after coating annealing separation agent, it is phosphate-based to be coated 30 DEG C of Chrome-free
Environmentally friendly insulating coating solution, coating layer thickness are 1 μm；The phosphoric acid that the phosphate-based environmentally friendly insulating coating solution of the Chrome-free is 40% containing mass fraction
Salt and 30% silica solution, the phosphate are magnesium phosphate and calcium phosphate；
Heating drying is carried out to steel plate after S2, coating, the heating rate is 60 DEG C/s, and drying plate temperature is 250 DEG C；
After S3, drying under the mixed-gas atmosphere of hydrogen and nitrogen, 750 DEG C of sintering curing 45s of temperature obtain product；It is described
The percent by volume that hydrogen accounts for mixed gas is 15%；
Wherein, 6.0MPa tension is applied to directional silicon steel during the coating, drying and sintering curing.
Embodiment 2-8
Embodiment 2-8 is each provided with a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step
Suddenly almost the same with embodiment 1, difference is: coating layer thickness, drying and warning speed, drying plate temperature, sintering temperature, curing time
And apply the technological parameter of tension, specifically, the above-mentioned technological parameter of embodiment 2-8 is as shown in table 1, remaining do not refer to part with
The preparation process of embodiment 1 is identical.Coating performance obtained by embodiment 1-8 and case of surface defects are as shown in table 2.
Comparative example 9-10
In order to which the preparation method of the raising chromium-free environment-friendly coating orientation silicon steel surface quality provided with embodiment 1-8 is formed pair
According to, it is further provided comparative example 9 and comparative example 10, step and embodiment 1 are almost the same, and difference is: coating layer thickness, baking
Dry heating rate, drying plate temperature, sintering temperature, curing time and the technological parameter for applying tension, specifically, comparative example 9-10
Above-mentioned technological parameter is as shown in table 1, remaining does not refer to that part is identical as the preparation process of embodiment 1.It is applied obtained by comparative example 9-10
Layer performance and case of surface defects are as shown in table 2.
The process parameter table of table 1 embodiment 1-8 and comparative example 9-10
Coating performance and case of surface defects obtained by 2 embodiment 1-8 of table and comparative example 9-10
As can be seen from Table 1 and Table 2, in Examples 1 to 8, according to the manufacturing method proposed in the present invention, the environmental protection
Coating orientation silicon steel surface is without surface covering class defect, excellent surface quality, and adhesion is good.In comparative example 9, drying rate mistake
Fastly, curing time is too long, causes coating adhesion poor, surface covering is bad.In comparative example 10, overweight coating, when drying, heats up
Excessive velocities lead to surface covering piebald, and it is serious to play powder.
Embodiment 9
Present embodiments provide a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step packet
It includes:
S1, to carrying out decarburizing annealing, the chemical component of the orientation silicon steel hot rolled plate after orientation silicon steel hot rolled plate cold rolling are as follows:
By percentage to the quality, C:0.05%, Si:3.20%, Mn:0.12%, S:0.03%, Als:0.02%, N:0.009%, it is remaining
Amount is Fe and inevitable impurity；High annealing is carried out after coating annealing separation agent, is coated the Chrome-free phosphoric acid with a thickness of 3 μm
Salt system environmental protection insulating coating solution；The Chrome-free phosphate-based environmentally friendly insulating coating solution contains 50% phosphate of mass percent and 25%
Silica solution, surplus are water, and the phosphate is the phosphate of Al, Ca, Co；
Heating drying after S2, coating, 300 DEG C of control panel temperature, heating rate is 71 DEG C/s；
After S3, drying under the mixed-gas atmosphere of hydrogen and nitrogen, 880 DEG C of sintering curing 75s of temperature obtain product；It is described
The percent by volume that hydrogen accounts for mixed gas is 10%；
Wherein, 8.2MPa tension is applied to directional silicon steel during the coating, drying and sintering curing.
Coating performance obtained by the present embodiment and case of surface defects and embodiment 1-8 are almost the same, and coating adhesion is good,
The defects of appearance is outstanding, and uncoated piebald, coating play powder, coating is bad.
Embodiment 10
The present invention provides a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step includes:
S1, to carrying out decarburizing annealing, the chemical component of the orientation silicon steel hot rolled plate after orientation silicon steel hot rolled plate cold rolling are as follows:
By percentage to the quality, C:0.08%, Si:3.19%, Mn:0.11%, S:0.02%, Als:0.03%, N:0.01%, surplus
For Fe and inevitable impurity；High annealing is carried out after coating annealing separation agent, is coated the Chrome-free phosphate with a thickness of 2 μm
It is environmentally friendly insulating coating solution；The phosphate-based environmentally friendly insulating coating solution of the Chrome-free contains 30% phosphate, 30% silica solution, and surplus is
Water, the phosphate are trbasic zinc phosphate；
Heating drying after S2, coating, 230 DEG C of control panel temperature, heating rate is 62 DEG C/s；
After S3, drying under the mixed-gas atmosphere of hydrogen and nitrogen, 800 DEG C of sintering curing 50s of temperature obtain product；It is described
The percent by volume that hydrogen accounts for mixed gas is 5%；
Wherein, 6.8MPa tension is applied to directional silicon steel during the coating, drying and sintering curing.
Coating performance obtained by the present embodiment and case of surface defects and embodiment 1-8 are almost the same, and coating adhesion is good,
The defects of appearance is outstanding, and uncoated piebald, coating play powder, coating is bad.
Although preferred embodiments of the present invention have been described, it is created once a person skilled in the art knows basic
Property concept, then additional changes and modifications may be made to these embodiments.So it includes excellent that the following claims are intended to be interpreted as
It selects embodiment and falls into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (9)
1. a kind of preparation method for improving chromium-free environment-friendly coating orientation silicon steel surface quality, step include:
S1, to decarburizing annealing is carried out after orientation silicon steel hot rolled plate cold rolling, carry out high annealing after being coated with annealing separation agent, be coated
The phosphate-based environmentally friendly insulating coating solution of Chrome-free；
Heat up drying after S2, coating, and plate temperature is 200~400 DEG C, and heating rate is 60~85 DEG C/s；
Sintering curing obtains product under the mixed-gas atmosphere of hydrogen and nitrogen after S3, drying；
Wherein, tension is applied to directional silicon steel during the coating, drying and sintering curing.
2. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as described in claim 1, it is characterised in that:
In step S1, the phosphate-based environmentally friendly insulating coating solution component of the Chrome-free includes phosphate and silica solution, to account for masking liquid quality percentage
Than meter, phosphate accounting 30%~60%, silica solution accounting 20%~45%；The phosphate is Mg, Al, Ca, Zn, Ni or Co
One or more of phosphate；The silica solution partial size is 8~15nm.
3. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as claimed in claim 2, it is characterised in that:
In step S1, the coating thickness of the phosphate-based environmentally friendly insulating coating solution of the Chrome-free is 1~4 μm；It controls and applies in the coating process
Liquid temperature is 30~40 DEG C.
4. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as described in claim 1, it is characterised in that:
In step S1, the chemical component of the orientation silicon steel hot rolled plate are as follows: by percentage to the quality, C:0.04~0.08%, Si:3.14
~3.4%, Mn:0.06~0.12%, S:0.02~0.03%, Als:0.02~0.03%, N:0.006~0.01%, surplus
For Fe and inevitable impurity.
5. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as described in claim 1, it is characterised in that:
In step S3, the percent by volume that the hydrogen accounts for mixed gas is 0~30%.
6. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as claimed in claim 5, it is characterised in that:
In step S3, the percent by volume that the hydrogen accounts for mixed gas is 15~25%.
7. such as the preparation method described in claim 5 or 6 for improving chromium-free environment-friendly coating orientation silicon steel surface quality, feature exists
In: in step S3, the sintering curing temperature is 750~950 DEG C.
8. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as claimed in claim 7, it is characterised in that:
In step S3, the sintering curing time is 45~90s.
9. improving the preparation method of chromium-free environment-friendly coating orientation silicon steel surface quality as described in claim 1, it is characterised in that:
It is described to apply the tension that tension is 6~8.5MPa.
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| CN110376237A (en) * | 2019-07-08 | 2019-10-25 | 武汉钢铁有限公司 | The silicon steel monolithic coating sample sintering experiment devices and methods therefor of controllable tension |
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| CN111748248A (en) * | 2020-06-15 | 2020-10-09 | 武汉钢铁有限公司 | Chromium-free semi-organic insulating paint suitable for Bi-containing ultrahigh magnetic induction oriented silicon steel without bottom layer |
| CN113248947A (en) * | 2021-05-21 | 2021-08-13 | 武汉科技大学 | Chromium-free inorganic insulating paint capable of modifying surface of oriented silicon steel and preparation method thereof |
| CN113278311A (en) * | 2021-05-28 | 2021-08-20 | 武汉科技大学 | Chromium-free inorganic insulating coating for oriented silicon steel and preparation method thereof |
| CN115109440A (en) * | 2022-06-21 | 2022-09-27 | 湖北武洲新材料科技有限公司 | Oriented silicon steel with excellent moisture resistance and manufacturing method thereof |
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