CN108977638A - A kind of orientation silicon steel annealing separating agent and its application method - Google Patents
A kind of orientation silicon steel annealing separating agent and its application method Download PDFInfo
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- CN108977638A CN108977638A CN201810973007.XA CN201810973007A CN108977638A CN 108977638 A CN108977638 A CN 108977638A CN 201810973007 A CN201810973007 A CN 201810973007A CN 108977638 A CN108977638 A CN 108977638A
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 78
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 59
- 238000000137 annealing Methods 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 36
- 230000000694 effects Effects 0.000 claims abstract description 30
- 230000008569 process Effects 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- 239000002002 slurry Substances 0.000 claims description 18
- 229910021538 borax Inorganic materials 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 13
- 239000004328 sodium tetraborate Substances 0.000 claims description 13
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract description 104
- 239000000395 magnesium oxide Substances 0.000 abstract description 50
- 230000007547 defect Effects 0.000 abstract description 21
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000000391 magnesium silicate Substances 0.000 abstract description 9
- 229910052919 magnesium silicate Inorganic materials 0.000 abstract description 9
- 230000035699 permeability Effects 0.000 abstract description 8
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 abstract description 6
- 235000019792 magnesium silicate Nutrition 0.000 abstract description 6
- 230000008602 contraction Effects 0.000 abstract description 4
- 230000000877 morphologic effect Effects 0.000 abstract description 4
- 230000009257 reactivity Effects 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 229910000831 Steel Inorganic materials 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910052839 forsterite Inorganic materials 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a kind of orientation silicon steel annealing separating agent and its application methods.The present invention is not only defined the composition by weight percent of interleaving agent and bulk density, especially also different grain size ratio is limited, both it ensure that extra light calcined magnesia participated in bottom and generates reaction, in turn ensure between coil of strip there is certain gas permeability, allow high-temperature annealing process roll up in steam uniformly discharge, it is therefore prevented that because local steam release be obstructed due to lead to strip local deformation and moisture convergence and cause color difference the defects of generation.Furthermore, elementary particle in MgO interleaving agent is defined in the pattern of porous chips stratiform, when MgO microscopic appearance is in porous flake, its reactivity with higher and lower aquation rate feature, and the magnesia of the morphological types keeps higher activity in the key temperatures section that 900-1100 DEG C of magnesium silicate generates, and rise after 1100 DEG C with temperature and sinter bulky grain MgO into rapidly, volume contraction increases the gas permeability of coil of strip.
Description
Technical field
The present invention relates to orientation silicon steel manufacturing technology field more particularly to a kind of orientation silicon steel annealing separating agent and its uses
Method.
Background technique
Currently, the production for orientation silicon steel, needs in decarburizing annealing process, belt steel surface coating high annealing every
From agent, generally based on MgO, mainly there are two big effects: first is that coil of strip layers cementing in high-temperature annealing process is prevented, second is that
Chemical reaction occurs with the oxidation film of belt steel surface and generates Mg2SiO4Magnesium silicate bottom, to increase the surface insulation of orientation silicon steel
Property, promoted magnetic property.The characteristic of magnesia interleaving agent is to determine the key factor of belt steel surface magnesium silicate bottom layer quality, CAA
Activity value, aquation rate, specific surface area etc. are the key indexes for influencing bottom.
The control difficulty that low temperature process manufactures orientation silicon steel magnesium silicate bottom is bigger, and the requirement to magnesia interleaving agent is more
The defects of harshness, dew crystalline substance that wherein surface is also easy to produce, color difference, deformation is persistent ailment in the industry, is had with magnesia interleaving agent close
Relationship.This is because the steam release in magnesia is poor with Temperature Matching in high-temperature annealing process.Orientation silicon steel annealing
The volume weight of coil of strip is generally at 15 tons or more, in high-temperature annealing process, inevitably there is certain temperature difference in volume, real
The existing uniform bottom of coil of strip forming properties in high-temperature annealing process, then need to be oxidized the activity of magnesium interleaving agent, release of water etc.
With the comprehensive matching of atmosphere in steel roll temperature, cover, this is difficult.
And in order to solve the problems, such as that bottom is non-uniform, generally require magnesia to have while guaranteeing high reactivity
Low aquation rate, the purpose is to reduce the burst size of coil of strip steam in annealing process, but in fact, these two aspects is conflicting
, it is not easy to stability contorting, and it is relatively more limited to the adaptability of process window.
Summary of the invention
The present invention is solved and is orientated in the prior art by providing a kind of orientation silicon steel annealing separating agent and its application method
The technical issues of silicon steel high annealing coil of strip bottom color difference, deformation, realizes and obtains color and the uniform bottom layer quality of performance
Technical effect.
The present invention provides a kind of orientation silicon steel annealing separating agents, comprising: the composition by weight percent of the interleaving agent is:
MgO > 97%, Cl < 0.04%, CaO:0.02-0.06%, B:300-1000ppm, Fe2O3< 0.10%, other impurities element
< 0.10%；When using ethyl alcohol as dispersion solvent, detection granularity meets: particle D1 of the granularity less than 100 μm accounts for the 70- of total ingredient
100%, granularity is greater than 10 μm and the particle D2 less than the 100 μm 10-45% for accounting for D1, and particle D3 of the granularity less than 10 μm accounts for D1's
60-85%, particle D4 of the granularity less than 3 μm account for the 25-80% of D1, and particle D5 of the granularity less than or equal to 1 μm accounts for D1's
3%-25%；Elementary particle is greater than 10% in the quantitative proportion of porous chips stratiform in MgO interleaving agent；Bulk density V600 is less than
0.58g/ml。
Further, 200 DEG C of aquation rate Ig-Loss of the interleaving agent is less than 1.8%, through 950-1050 DEG C two hours
40% citric acid, 30 DEG C of activity degree CAA are between 50-100 seconds after sintering.
Further, 200 DEG C of aquation rate Ig-Loss of the interleaving agent is sintered less than 1.8% through 1000 DEG C for two hours
40% citric acid, 30 DEG C of activity degree CAA are between 50-100 seconds afterwards.
Further, in the interleaving agent sintering temperature of magnesia in the fabrication process less than 1090 DEG C.
The application method of orientation silicon steel annealing separating agent provided by the invention, comprising:
Above-mentioned orientation silicon steel annealing separating agent and water are mixed and made into slurries according to the weight percent of 1:7-10；
The slurries are coated uniformly on to the surface of strip, and dry, coated weight is controlled in 4-8g/m2；
High annealing is carried out to strip.
Further, described to mix above-mentioned orientation silicon steel annealing separating agent according to the weight percent of 1:7-10 with water
Slurries are made, comprising:
Above-mentioned orientation silicon steel annealing separating agent is mixed with water according to the weight percent of 1:7-10；
Borax and TiO are added into the solution after mixing2The slurries are made in additive.
Further, the weight percent of the borax is 0.2-1%；The TiO2The weight percent of additive is 2-
5%.
Further, the weight percent of the borax is 0.5%；The TiO2The weight percent of additive is 3%.
One or more technical solution provided in the present invention, has at least the following technical effects or advantages:
The present invention is not only defined the composition by weight percent of interleaving agent and bulk density, especially also to magnesia
Different grain size ratio is limited, and both ensure that extra light calcined magnesia participates in bottom and generates reaction, in turn ensuring between coil of strip has
Certain gas permeability allows high-temperature annealing process to roll up interior steam and uniformly discharges, it is therefore prevented that due to the release of local steam is obstructed
The generation for the defects of leading to strip local deformation and moisture convergence and causing color difference.In addition, to elementary particle in MgO interleaving agent
Be defined in the pattern of porous chips stratiform, when MgO microscopic appearance be in porous flake when, reactivity with higher and compared with
Low aquation rate feature, and the magnesia of the morphological types is kept in the key temperatures section that 900-1100 DEG C of magnesium silicate generates
Higher activity, and rise after 1100 DEG C with temperature and sinter bulky grain MgO into rapidly, volume contraction increases the ventilative of coil of strip
Property.Orientation silicon steel annealing separating agent provided by the invention can get the homogeneous bottom layer quality of uniform color, improve whole coil of strip bottom
The layer uniformity, and can inhibit the generation of strip annealing local deformation defect, it is produced especially suitable for low temperature process high magentic induction oriented
Silicon steel.
Detailed description of the invention
Fig. 1 is the pattern schematic diagram of orientation silicon steel annealing separating agent provided in an embodiment of the present invention；
Fig. 2 is the flow chart of the application method of orientation silicon steel annealing separating agent provided in an embodiment of the present invention.
Specific embodiment
The embodiment of the present invention solves the prior art by providing a kind of orientation silicon steel annealing separating agent and its application method
The technical issues of middle orientation silicon steel high annealing coil of strip bottom color difference, deformation, realizes and obtains color and the uniform bottom of performance
The technical effect of quality.
Technical solution in the embodiment of the present invention is to solve the above problems, general thought is as follows:
The embodiment of the present invention is not only defined the composition by weight percent of interleaving agent and bulk density, especially also right
Magnesia different grain size ratio is limited, and both ensure that extra light calcined magnesia participates in bottom and generates reaction, has been in turn ensured steel
There is certain gas permeability between volume, allows high-temperature annealing process to roll up interior steam and uniformly discharge, it is therefore prevented that because local steam discharges
The generation for the defects of being obstructed and leading to strip local deformation and moisture convergence and cause color difference.In addition, to base in MgO interleaving agent
This particle is defined in the pattern of porous chips stratiform, and when MgO microscopic appearance is in porous flake, reaction with higher is lived
Property and lower aquation rate feature, and the magnesia of the morphological types is in the key temperatures area that 900-1100 DEG C of magnesium silicate generates
Between keep higher activity, and rise after 1100 DEG C with temperature and sinter bulky grain MgO into rapidly, volume contraction increases coil of strip
Gas permeability.Orientation silicon steel annealing separating agent provided in an embodiment of the present invention can get the homogeneous bottom layer quality of uniform color, improve
The whole coil of strip bottom uniformity, and can inhibit the generation of strip annealing local deformation defect, it is produced especially suitable for low temperature process
High magnetic induction grain-oriented silicon steel.
Above-mentioned technical proposal in order to better understand, in conjunction with appended figures and specific embodiments to upper
Technical solution is stated to be described in detail.
Referring to Fig. 1, orientation silicon steel annealing separating agent provided in an embodiment of the present invention, comprising: the Ingredients Weight hundred of interleaving agent
Ratio is divided to be: MgO > 97%, Cl < 0.04%, CaO:0.02-0.06%, B:300-1000ppm, Fe2O3< 0.10%, other are miscellaneous
Prime element < 0.10%；When using ethyl alcohol as dispersion solvent, detection granularity meets: particle D1 of the granularity less than 100 μm accounts for total ingredient
70-100%, granularity is greater than 10 μm and the particle D2 less than the 100 μm 10-45%, particle D3 of the granularity less than 10 μm for accounting for D1
The 60-85% of D1 is accounted for, particle D4 of the granularity less than 3 μm accounts for the 25-80% of D1, and particle D5 of the granularity less than or equal to 1 μm is accounted for
The 3%-25% of D1；Elementary particle is greater than 10% (Electronic Speculum × 20000 systems in the quantitative proportion of porous chips stratiform in MgO interleaving agent
Meter)；Bulk density (V600) is less than 0.58g/ml.
Further, the aquation rate Ig-Loss (200 DEG C) of interleaving agent is sintered less than 1.8% through 950-1050 DEG C for two hours
40% citric acid, 30 DEG C of activity degree CAA are between 50-100 seconds afterwards, to guarantee that MgO is also equipped with certain reaction at high operating temperatures
Activity degree, without being scorched to death.
Further, the aquation rate Ig-Loss (200 DEG C) of interleaving agent is less than 1.8%, after 1000 DEG C of sintering in two hours
40% 30 DEG C of citric acid activity degree CAA is between 50-100 seconds.
In the present embodiment, the sintering temperature of magnesia in the fabrication process is less than 1090 DEG C in interleaving agent, to guarantee to give birth to
At magnesia particle shape and activity meet the requirements.
What needs to be explained here is that the magnesia in orientation silicon steel annealing separating agent provided in an embodiment of the present invention can be
The mixture of one kind or two or more difference magnesia.In this case, at least one of interleaving agent magnesia was manufacturing
Sintering temperature in journey is less than 1090 DEG C.
Referring to fig. 2, the application method of orientation silicon steel annealing separating agent provided in an embodiment of the present invention, comprising:
Step S110: above-mentioned orientation silicon steel annealing separating agent and water are mixed according to the weight percent of 1:7-10
Slurries；
This step is specifically described:
Above-mentioned orientation silicon steel annealing separating agent is mixed with water according to the weight percent of 1:7-10；
Borax and TiO are added into the solution after mixing2Slurries are made in additive, so as to reduce slurries and band
The reaction temperature point of the silica of steel surface, and then guarantee to react in belt steel surface and generate Mg2SiO4Magnesium silicate bottom.
In the present embodiment, the weight percent of borax is 0.2-1%；TiO2The weight percent of additive is 2-5%.
Further, the weight percent of borax is 0.5%；TiO2The weight percent of additive is 3%.
Step S120: slurries are coated uniformly on to the surface of strip, and dry, coated weight is controlled in 4-8g/m2, to guarantee
Bottom, which generates, reacts required MgO amount, while guaranteeing that interlayer has certain air gap amount.
Step S130: high annealing is carried out to strip.
Case study on implementation 1
0.30mm orientation silicon steel is produced using low temperature process.When using ethyl alcohol as dispersion solvent, detection granularity meets: granularity is big
Particle D2 in 10 μm and less than 100 μm accounts for the 15-35% of D1, and particle D4 of the granularity less than 3 μm accounts for the 50% of D1, and granularity is less than
Or the particle D5 equal to 1 μm accounts for elementary particle in 17%, the MgO interleaving agent of D1 and is greater than in the quantitative proportion of porous chips stratiform
10% (Electronic Speculum × 20000 statistics)；Bulk density (V600) is less than 0.45g/ml, and aquation rate Ig-Loss (200 DEG C) is less than
1.0%, 40% citric acid, 30 DEG C of activity degree CAA are between 60-75 seconds after 1000 DEG C of sintering in two hours.
The composition by weight percent of interleaving agent is: MgO=98%, Cl < 0.03%, CaO=0.052%, B:600ppm,
Fe2O3=0.04%, other impurities element < 0.10%.
It is mixed according to interleaving agent with the weight percent of water 1:9, and 0.5% borax is added into the solution after mixing
TiO2 additive with 3%, is coated uniformly on the surface of strip after slurries are made, and dry, coated weight is controlled in 6g/m2, so
After carry out high annealing.
Case study on implementation 1 is primarily referred to as in 0.3mm specification orientation silicon steel application, wherein including 6 kinds of MgO in the scope of the invention
Specific embodiment (specific embodiment 1-6) and 3 kinds are not included in the comparative example (comparative example 1-3) of the scope of the invention.
The effect of case study on implementation 1 is shown in Table 1.
1 present invention of table is in 0.3mm specification orientation silicon steel implementation result and comparative example
Note 1: in table 1, "●" indicates moderate underlayer thickness, highly uniform, no color differnece, without the brilliant defect of dew；" ◎ " is indicated
Underlayer thickness is thinner, uniform, no color differnece, has the brilliant defect of slight dew；"○" indicate underlayer thickness it is thicker, it is uniform, have color difference, have it is light
The brilliant defect of micro- dew；" ※ " indicates that bottom is uneven, has serious color difference and large area to reveal brilliant defect.
It can be seen that from the result in table 1 and 0.30mm orientation silicon steel produced using low temperature process, mentioned in the embodiment of the present invention
Under the application of the orientation silicon steel annealing separating agent of confession, bottom layer quality is formed uniformly, and electromagnetic performance is excellent.
Case study on implementation 2
0.23mm orientation silicon steel is produced using low temperature process.When using ethyl alcohol as dispersion solvent, detection granularity meets: granularity is big
Particle D2 in 10 μm and less than 100 μm accounts for the 10-40% of D1, and particle D4 of the granularity less than 3 μm accounts for the 50% of D1, and granularity is less than
Or the particle D5 equal to 1 μm accounts for the 3-25% of D1, elementary particle is greater than in the quantitative proportion of porous chips stratiform in MgO interleaving agent
15% (Electronic Speculum × 20000 statistics)；Bulk density (V600) is less than 0.50g/ml, and aquation rate Ig-Loss (200 DEG C) is less than
1.0%, 40% citric acid, 30 DEG C of activity degree CAA are between 60-80 seconds after 1000 DEG C of sintering in two hours.
The composition by weight percent of interleaving agent is: MgO=98%, Cl < 0.03%, CaO=0.052%, B:600ppm,
Fe2O3=0.04%, other impurities element < 0.10%.
It is mixed according to interleaving agent with the weight percent of water 1:9, and 0.5% borax is added into the solution after mixing
With 3% TiO2Additive is coated uniformly on the surface of strip after slurries are made, and dries, and coated weight is controlled in 7g/m2, then
Carry out high annealing.
Case study on implementation 2 is primarily referred to as in 0.23mm specification orientation silicon steel application, wherein including 6 kinds in the scope of the invention
MgO specific embodiment (specific embodiment 7-12) and 3 kinds are not included in the comparative example (comparative example 4-6) of the scope of the invention.
The effect of case study on implementation 2 is shown in Table 2.
2 present invention of table is in 0.23mm specification orientation silicon steel implementation result and comparative example
Note 2: in table 2, "●" indicates moderate underlayer thickness, highly uniform, no color differnece, without the brilliant defect of dew；" ◎ " is indicated
Underlayer thickness is thinner, uniform, no color differnece, has the brilliant defect of slight dew；"○" indicate underlayer thickness it is thicker, it is uniform, have color difference, have it is light
The brilliant defect of micro- dew；" ※ " indicates that bottom is uneven, has serious color difference and large area to reveal brilliant defect.
It can be seen that from the result in table 2 and 0.23mm orientation silicon steel produced using low temperature process, mentioned in the embodiment of the present invention
Under the application of the orientation silicon steel annealing separating agent of confession, bottom layer quality is formed uniformly, and electromagnetic performance is excellent.
Case study on implementation 3
0.18mm orientation silicon steel is produced using low temperature process.When using ethyl alcohol as dispersion solvent, detection granularity meets: granularity is big
Particle D2 in 10 μm and less than 100 μm accounts for the 10-40% of D1, and particle D4 of the granularity less than 3 μm accounts for the 50% of D1, and granularity is less than
Or the particle D5 equal to 1 μm accounts for the 3-25% of D1, elementary particle is greater than in the quantitative proportion of porous chips stratiform in MgO interleaving agent
15% (Electronic Speculum × 20000 statistics)；Bulk density (V600) is less than 0.50g/ml, and aquation rate Ig-Loss (200 DEG C) is less than
1.0%, 40% citric acid, 30 DEG C of activity degree CAA are between 60-80 seconds after 1000 DEG C of sintering in two hours.
The composition by weight percent of interleaving agent is: MgO=98%, Cl=0.02%, CaO=0.032%, B:600ppm,
Fe2O3=0.04%, other impurities element < 0.10%.
It is mixed according to interleaving agent with the weight percent of water 1:9, and 0.5% borax is added into the solution after mixing
With 3% TiO2Additive is coated uniformly on the surface of strip after slurries are made, and dries, and coated weight is controlled in 6g/m2, then
Carry out high annealing.
Case study on implementation 3 is primarily referred to as in 0.18mm specification orientation silicon steel application, wherein including 6 kinds in the scope of the invention
MgO specific embodiment (specific embodiment 13-18) and 3 kinds are not included in the comparative example (comparative example 7-9) of the scope of the invention.
The effect of case study on implementation 3 is shown in Table 3.
3 present invention of table is in 0.18mm specification orientation silicon steel implementation result and comparative example
Note 3: in table 3, "●" indicates moderate underlayer thickness, highly uniform, no color differnece, without the brilliant defect of dew；" ◎ " is indicated
Underlayer thickness is thinner, uniform, no color differnece, has the brilliant defect of slight dew；"○" indicate underlayer thickness it is thicker, it is uniform, have color difference, have it is light
The brilliant defect of micro- dew；" ※ " indicates that bottom is uneven, has serious color difference and large area to reveal brilliant defect.
It can be seen that from the result in table 3 and 0.18mm orientation silicon steel produced using low temperature process, mentioned in the embodiment of the present invention
Under the application of the orientation silicon steel annealing separating agent of confession, bottom layer quality is formed uniformly, and electromagnetic performance is excellent.
By above-mentioned case study on implementation it is found that orientation silicon steel annealing separating agent provided in an embodiment of the present invention passes through in 0.18mm-
The defects of using effect is good on 0.30mm specification low temperature high magnetic induction grain-oriented silicon steel, efficiently solves " surface chromatic aberration ", " deformation ",
Obtain uniform bottom and excellent electromagnetic performance.
[technical effect]
1, the embodiment of the present invention is not only defined the composition by weight percent of interleaving agent and bulk density, especially also
Magnesia different grain size ratio is limited, both ensure that extra light calcined magnesia participates in bottom and generates reaction, in turn ensured
There is certain gas permeability between coil of strip, allows high-temperature annealing process to roll up interior steam and uniformly discharge, it is therefore prevented that because local steam is released
Put the generation for the defects of being obstructed and leading to strip local deformation and moisture convergence and cause color difference.In addition, in MgO interleaving agent
Elementary particle is defined in the pattern of porous chips stratiform, when MgO microscopic appearance is in porous flake, reaction with higher
Active and lower aquation rate feature, and the key temperatures that the magnesia of the morphological types is generated in 900-1100 DEG C of magnesium silicate
Section keeps higher activity, and rises after 1100 DEG C with temperature and sinter bulky grain MgO into rapidly, and volume contraction increases coil of strip
Gas permeability.Orientation silicon steel annealing separating agent provided in an embodiment of the present invention can get the homogeneous bottom layer quality of uniform color, mention
The high whole coil of strip bottom uniformity, and can inhibit the generation of strip annealing local deformation defect, it is raw especially suitable for low temperature process
Produce high magnetic induction grain-oriented silicon steel.
2, the aquation rate Ig-Loss (200 DEG C) of interleaving agent is less than 1.8%, 40% after 950-1050 DEG C of sintering in two hours
30 DEG C of activity degree CAA of citric acid are between 50-100 seconds, to ensure that MgO at high operating temperatures and can also have and is certain anti-
Activity degree is answered, without being scorched to death.
3, the sintering temperature of magnesia in the fabrication process is less than 1090 DEG C in interleaving agent, to ensure that the oxidation of generation
Magnesium particle shape and activity are met the requirements.
4, in the application method of orientation silicon steel annealing separating agent, the coated weight of slurries is controlled in 4-8g/m2, to protect
It has demonstrate,proved bottom and has generated and reacted required MgO amount, while having guaranteed that interlayer has certain air gap amount.
5, in the application method of orientation silicon steel annealing separating agent, borax and TiO are added into the solution after mixing2Add
Add agent, slurries are made, reduces the reaction temperature point of the silica of slurries and belt steel surface, and then ensure that can be in strip
Surface reaction generates Mg2SiO4Magnesium silicate bottom.
Orientation silicon steel annealing separating agent provided in an embodiment of the present invention taken into account the activity of magnesia interleaving agent, aquation rate,
The factor indexs such as gas permeability, adaptability is stronger, has widened rear procedure technology window, has improved surface lumber recovery.
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 (8)
1. a kind of orientation silicon steel annealing separating agent characterized by comprising the composition by weight percent of the interleaving agent is: MgO
> 97%, Cl < 0.04%, CaO:0.02-0.06%, B:300-1000ppm, Fe2O3< 0.10%, other impurities element <
0.10%；When using ethyl alcohol as dispersion solvent, detection granularity meets: particle D1 of the granularity less than 100 μm accounts for the 70- of total ingredient
100%, granularity is greater than 10 μm and the particle D2 less than the 100 μm 10-45% for accounting for D1, and particle D3 of the granularity less than 10 μm accounts for D1's
60-85%, particle D4 of the granularity less than 3 μm account for the 25-80% of D1, and particle D5 of the granularity less than or equal to 1 μm accounts for D1's
3%-25%；Elementary particle is greater than 10% in the quantitative proportion of porous chips stratiform in MgO interleaving agent；Bulk density V600 is less than
0.58g/ml。
2. orientation silicon steel annealing separating agent as described in claim 1, which is characterized in that 200 DEG C of aquation of the interleaving agent
Rate Ig-Loss is less than 1.8%, and 40% citric acid, 30 DEG C of activity degree CAA were at 50-100 seconds after 950-1050 DEG C of sintering in two hours
Between.
3. orientation silicon steel annealing separating agent as claimed in claim 2, which is characterized in that 200 DEG C of aquation of the interleaving agent
Rate Ig-Loss is less than 1.8%, and 40% citric acid, 30 DEG C of activity degree CAA are between 50-100 seconds after 1000 DEG C of sintering in two hours.
4. orientation silicon steel annealing separating agent as claimed in any one of claims 1-3, which is characterized in that oxygen in the interleaving agent
Change the sintering temperature of magnesium in the fabrication process less than 1090 DEG C.
5. a kind of application method of orientation silicon steel annealing separating agent characterized by comprising
By orientation silicon steel annealing separating agent such as of any of claims 1-4 and water according to the weight percent of 1:7-10
It is mixed and made into slurries；
The slurries are coated uniformly on to the surface of strip, and dry, coated weight is controlled in 4-8g/ ㎡；
High annealing is carried out to strip.
6. application method as claimed in claim 5, which is characterized in that it is described will be as of any of claims 1-4
Orientation silicon steel annealing separating agent and water are mixed and made into slurries according to the weight percent of 1:7-10, comprising:
By orientation silicon steel annealing separating agent such as of any of claims 1-4 and water according to the weight percent of 1:7-10
Mixing；
Borax and TiO are added into the solution after mixing2The slurries are made in additive.
7. application method as claimed in claim 6, which is characterized in that the weight percent of the borax is 0.2-1%；It is described
TiO2The weight percent of additive is 2-5%.
8. application method as claimed in claim 7, which is characterized in that the weight percent of the borax is 0.5%；It is described
TiO2The weight percent of additive is 3%.
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| CN111186850A (en) * | 2019-12-27 | 2020-05-22 | 南京宝淳新材料科技有限公司 | Magnesium oxide for oriented silicon steel annealing separant and preparation method thereof |
| CN111302366A (en) * | 2020-02-26 | 2020-06-19 | 南京宝淳新材料科技有限公司 | Magnesium oxide for annealing separant of grain-oriented electromagnetic steel plate |
| CN111996354A (en) * | 2020-08-27 | 2020-11-27 | 上海实业振泰化工有限公司 | Preparation method of liquid additive for oriented silicon steel |
| CN114854960A (en) * | 2022-03-30 | 2022-08-05 | 武汉钢铁有限公司 | Annealing separant for reducing surface defects of oriented silicon steel and using method thereof |
| WO2022262144A1 (en) * | 2021-06-18 | 2022-12-22 | 协和化学工业株式会社 | Preparation method for annealing separating agent, annealing separating agent, and directional electromagnetic steel plate |
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| CN116133989A (en) * | 2020-08-28 | 2023-05-16 | 杰富意钢铁株式会社 | Powder for annealing separating agent, method for producing the same, and method for producing oriented electromagnetic steel sheet |
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