CN102260874A - Gradient iron silicon alloy with different silicon content distribution and preparation method of gradient iron silicon alloy - Google Patents
Gradient iron silicon alloy with different silicon content distribution and preparation method of gradient iron silicon alloy Download PDFInfo
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Abstract
The invention provides a gradient iron silicon alloy with different silicon (Si) content distribution and a preparation method of the gradient iron silicon alloy. The average silicon content of the alloy is 3.5 to 4.1 weight percent, the balance component is iron, the silicon content of the alloy is in gradient progressive reduction from the surface of the alloy to the heart of the alloy, and the progressive reduction gradient of the silicon content is 0.045 to 0.11 weight percent in each 10 microns of silicon. The preparation method of the gradient iron silicon alloy with different Si content distribution comprises four steps, namely preparation of a target, preparation of a low silicon steel substrate, magnetron sputtering and diffusion treatment. The gradient iron silicon alloy with different silicon content, prepared by adopting the magnetron sputtering method, has relative low iron loss under medium and high frequencies; compared with a chemical vapor deposition (CVD) method and a thermal dipping method, the gradient silicon steel prepared by the magnetron sputtering method has the advantages of high purity, component controllability, good surface quality, strong process controllability, good environment friendliness and the like; and the method applied to the preparation of the gradient silicon steel belongs to exploratory brand-new research with development value.
Description
Technical field
The present invention is specifically related to a kind of gradient iron silicon alloy with Different Silicon content distribution and preparation method thereof.
Background technology
Silicon steel is the silicon-iron soft magnetic alloy of a kind of carbon content very low (be generally less than≤0.02%), and silicon content is generally 1.5～4.5wt%.A kind of non-retentive alloy of its amount of being to use maximum occupies consequence in soft magnetic materials, be the base mateiral of development electric power and telecommunication industry, and high magnetic induction density is the very important technical indicator of silicon steel under low iron loss and the high-intensity magnetic field.
Silicone content in the siliconized plate is very big to the soft magnetic performance influence of its product, and along with the increase of silicone content, siliconized plate resistivity increases (eddy-current loss reduces), and magnetic permeability increases, and magnetocrystalline anisotropy constant reduces (magnetic hysteresis loss diminishes), and magnetostriction coefficient reduces.Therefore, high silicon steel is the ideal core material of making low noise, low iron loss, can be widely used in the process industry transformer, audio-frequency transformer, communication transformer and other medium-high frequency electronic transformers, lower noise electronic transformer, contravariant transformer, inducer, reactance coil, welding machine iron core etc.
Although high silicon steel has very excellent soft magnetic performance, all below 4wt%, this is to surpass after 5% because of increase, especially silicon content with Si content to the silicon content of siliconized plate commonly used, because B in producing at present
2(FeSi) or DO
3(Fe
3Si) appearance of ordered phase, alloy become not only firmly but also are crisp, make the machining property rapid deterioration, are difficult to adopt conventional rolling method to be processed into thin plate, thereby have hindered the widespread use of high silicon steel.
In the last few years, a kind of novel gradient silicon steel had caused people's extensive concern, compared with the high silicon steel of tradition, and it has under medium-high frequency in the low iron loss, simultaneously owing to the lower mechanical property of improving material of center silicone content.As reference 1:Recent development of non-oriented electrical steel sheet for automobile electrical devices[J] as described in Journal of Magnetism and Magnetic Materials 320 (2008) 2430-2435, it is 6.5wt% that NKK (NKK) adopts the chemical vapor deposition (CVD) method to prepare surperficial silicon content, the center silicone content is the gradient silicon steel of 3wt%, and dropped into and commercially produced, the Fe-6.5wt.%Si graded alloy is mainly used in high-frequency electronic equipment, as: high frequency convertor and high-speed engine in the automobile.But because the surface quality that exists of chemical meteorology deposition method is poor, easily introduce impurity and reduce that magnetic property, equipment life are low, problem that contaminate environment etc. can not be dealt carefully with, it can not be widely used in industrial production.Reference 2:Influence of the Si and Al gradient on the magnetic properties of high-Si electrical steel produced by hot dipping and diffusion annealing[J for another example] .Journal of Magnetism and Magnetic Materials 272-276 (2004) e521-e522 is described, T.Ros-Yanez etc. adopt hot dipping method in conjunction with twice diffusion annealing process (～850 ℃ and 1100 ℃～1250 ℃), having made surperficial silicon content is 5.9wt% silicon steel, and the center silicon content is the gradient silicon steel of 4.8wt%.Though hot dipping method has been improved the plasticity and toughness of material, enable in the final annealing cold rolling processing of interline of advancing, and realize to a certain extent sheet gauge, surface quality, microstructure and grain-oriented adjustment.But grain orientation is subjected to original Si in the base material, Al content, and middle cold-rolling process and final diffusion annealing process influence significantly are difficult to the good single texture of obtained performance.
Summary of the invention
At problems of the prior art, the invention provides a kind of gradient iron silicon alloy and preparation method thereof with Different Silicon content distribution.Advantages such as this method has purity height, controllable component, surface quality is good, process controllability is strong, the feature of environmental protection is good, and the gradient iron silicon alloy of preparation has lower iron loss, and to a certain degree improves its mechanical property.
The present invention proposes a kind of gradient iron silicon alloy with Different Silicon content distribution, the average silicon content of this alloy is 3.53～4.05wt.%, all the other compositions are iron, the silicon content of this alloy entad satisfies from the surface, and portion's direction gradient successively decreases, the gradient of successively decreasing of silicon content is per 10 μ m silicon contents 0.045～0.11wt.% that successively decrease, the iron loss P of this gradient iron silicon alloy
10/1KBe 69.28～79.96W/kg, P
10/10KBe 3207～3476W/kg, the coercive force of this gradient iron silicon alloy is 23.79～27.43A/m, B
80=1.76～1.92T.
The present invention proposes a kind of preparation method with gradient iron silicon alloy of Different Silicon content distribution, specifically comprises following step:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target;
Step 2, the low silicon silicon steel sheet substrate of preparation:
After will hanging down silicon silicon steel sheet and removing insulation layer with sand paper, line cuts into print as substrate, cleans up in ultrasonic cleaner with acetone then, removes oil stain, obtains hanging down the silicon silicon steel sheet substrate;
Step 3, magnetron sputtering process:
The Fe that founding in the step 1 is good
5Si
3Target is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet substrate of step 2 preparation is installed on the positive plate of magnetic control sputtering device, and the gaseous tension of sputtering chamber that magnetic control sputtering device is set is smaller or equal to 1.0 * 10
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.8～1.0Pa during sputter.Sputtering power is 57.6～72W; Sputtering time is 60～80min, and making sputter thickness is 10 μ m～15 μ m, obtains the Silicon-rich film in low silicon silicon steel sheet substrate surface deposition.
Step 4, DIFFUSION TREATMENT:
The low silicon silicon steel sheet of deposition Silicon-rich film is put into 95 porcelain aluminum oxide end-blocking vitrified pipes, and the vitrified pipe opening is connected with the vacuum unit, makes vitrified pipe gas inside pressure 2 * 10
-3Below the Pa, carry out high vacuum DIFFUSION TREATMENT 20～40min, finally obtain having the gradient iron silicon alloy of different Si content distribution 1180～1200 ℃ of temperature ranges.
The invention has the advantages that:
(1) the present invention proposes a kind of gradient iron silicon alloy with Different Silicon content distribution and preparation method thereof, compare with CVD method and hot pickling process, magnetron sputtering method prepares advantages such as gradient silicon steel has purity height, controllable component, surface quality is good, process controllability is strong, the feature of environmental protection is good, and being applied to the preparation of gradient silicon steel is a kind of brand-new research that has the exploration of exploitation value.
(2) the present invention proposes a kind of gradient iron silicon alloy with Different Silicon content distribution and preparation method thereof, and gradient iron silicon alloy iron loss under medium-high frequency of the different Si content of employing magnetron sputtering method preparation is lower.
Description of drawings
Fig. 1: the preparation method's of the present invention proposes a kind of gradient iron silicon alloy with Different Silicon content distribution schema;
Fig. 2: Si content distribution graphic representation is formed in a kind of gradient iron silicon alloy cross section behind 1180 ℃ of diffusion 20min with different Si content distribution that the present invention proposes;
Fig. 3: Si content distribution graphic representation is formed in a kind of gradient iron silicon alloy cross section behind 1190 ℃ of diffusion 30min with different Si content distribution that the present invention proposes;
Fig. 4: Si content distribution graphic representation is formed in a kind of gradient iron silicon alloy cross section behind 1200 ℃ of diffusion 40min with different Si content distribution that the present invention proposes;
The Si moiety and the cross section pattern thereof at sample in cross section 15.56 μ m degree of depth places among Fig. 5: the embodiment 3;
The Si moiety and the cross section pattern thereof at sample in cross section 125.3 μ m degree of depth places among Fig. 6: the embodiment 3;
The Si moiety and the cross section appearance thereof at sample in cross section 193.25 μ m degree of depth places among Fig. 7: the embodiment 3;
The Si moiety and the cross section appearance thereof at sample in cross section 325.3 μ m degree of depth places among Fig. 8: the embodiment 3.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention proposes a kind of gradient iron silicon alloy with Different Silicon content distribution, the average silicon content of this alloy is 3.53～4.05wt.%, all the other compositions are iron, the silicon content of this alloy entad satisfies from the surface, and portion's direction gradient successively decreases, the gradient of successively decreasing of silicon content is per 10 μ m silicon contents 0.045～0.11wt.% that successively decrease, the iron loss P of this gradient iron silicon alloy
10/1K(at amplitude magnetic induction density is under the condition of 1T, and frequency is the core loss value of 1kHz) is 69.28～79.96W/kg, P
10/10K(at amplitude magnetic induction density is under the condition of 1T, and frequency is the core loss value of 10kHz) is 3207～3476W/kg, and the coercive force of this gradient iron silicon alloy is 23.79～27.43A/m, is under the 800A/m condition in magnetic field, the magnetic induction density B of material
80Be B
80=1.76～1.92T.
The present invention proposes a kind of preparation method with gradient iron silicon alloy of Different Silicon content distribution, as shown in Figure 1, specifically comprises following step:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target.
Step 2, the low silicon silicon steel sheet substrate of preparation:
Will (silicon content be 3wt.% smaller or equal to the thick low silicon silicon steel sheet of 0.35mm, be preferably the 35WW250 trade mark) with behind the sand paper removal insulation layer, line cuts into print as substrate, for the JCK-500 magnetic control sputtering device, the print size satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm, and other model magnetic control sputtering devices can be selected according to the chip bench size.Oil stain is cleaned up stand-by with acetone (analytical pure) in ultrasonic cleaner, obtain low silicon silicon steel sheet substrate.
Step 3, magnetron sputtering process:
The target that founding in the step 1 is good is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet substrate after step 2 is handled is installed on the positive plate of magnetic control sputtering device.The gaseous tension of the sputtering chamber of magnetic control sputtering device is smaller or equal to 1.0 * 10 before the sputter
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.8～1.0Pa during sputter.Sputtering power is 57.6～72W; Sputtering time is 60～80min, and making sputter thickness is 10 μ m～15 μ m, obtains the Silicon-rich film in low silicon silicon steel sheet substrate surface deposition.
Step 4, DIFFUSION TREATMENT:
For fear of Silicon-rich film vapour loss, the low silicon silicon steel sheet that will deposit the Silicon-rich film is separately put into 95 porcelain aluminum oxide end-blocking vitrified pipes, and the vitrified pipe opening is connected with the vacuum unit, makes vitrified pipe gas inside pressure 2 * 10
-3Below the Pa, carry out high vacuum DIFFUSION TREATMENT 20～40min, obtain having the gradient iron silicon alloy of Different Silicon content distribution 1180～1200 ℃ of temperature ranges.
Sample after step 4 is handled is taken out, test its cross section moiety through EDS, the average silicon content of this alloy is 3.5～4.1wt.%, all the other compositions are iron, the silicon content of this alloy entad satisfies from the surface that portion's direction gradient successively decreases, and the gradient of successively decreasing of silicon content is per 10 μ m silicon contents 0.045～0.11wt.% that successively decrease.Dc magnetic energy through soft magnetism direct current test apparatus specimen; Soft magnetism through silicon steel tester test material exchanges performance.The iron loss P of this iron silicon alloy
10/1KBe 69～80W/kg, P
10/10KBe 3200～3500W/kg;
Embodiment 1:
The preparation method of the gradient iron silicon alloy with Different Silicon content distribution of preparation specifically comprises following step in this enforcement:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target.
Step 2, the low silicon silicon steel sheet substrate of preparation:
Be that line cut into print, for the JCK-500 magnetic control sputtering device after the low silicon silicon steel sheet of 35WW250 was removed insulation layer with sand paper with the trade mark, the print size satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm, in ultrasonic cleaner cleans up stand-by with acetone (analytical pure) oil stain.
Step 3, magnetron sputtering process:
The target that founding in the step 1 is good is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet substrate after step 2 is handled is installed on the positive plate of magnetic control sputtering device.The gaseous tension of the sputtering chamber of magnetic control sputtering device equals 1.0 * 10 before the sputter
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.8Pa during sputter.Sputtering power is 72W; Sputtering time is 80min, and making sputter thickness is 15 μ m, and deposition obtains the Silicon-rich film.
Step 4, DIFFUSION TREATMENT:
For fear of Silicon-rich film vapour loss, will deposit Silicon-rich film sample separately and put into 95 porcelain aluminum oxide end-blocking vitrified pipes, the vitrified pipe opening is connected with the vacuum unit, makes vitrified pipe gas inside pressure 2 * 10
-3Pa carries out high vacuum DIFFUSION TREATMENT 20min under 1180 ℃ of temperature, obtain having the gradient iron silicon alloy of Different Silicon content distribution.
Gradient iron silicon alloy after step 4 is handled is tested through EDS, a kind of gradient iron silicon alloy for preparing in the present embodiment with Different Silicon content distribution, its cross section different positions degree of depth has different silicon contents, as shown in Figure 2, it is 5.28wt.% that the surface silicon content has maximum value, it is 3.44wt.% that heart portion silicon content has minimum value, and its gradient is reduced to 0.11wt.% for average per 10 μ m Si content, and average Si content is 4.05wt.%; Through the dc magnetic energy of soft magnetism direct current test apparatus specimen, obtaining the sample coercive force is 26.83A/m, B
80=1.76T; Soft magnetism through silicon steel tester test material exchanges performance, P
10/1K=69.28W/kg, P
10/10K=3207W/kg.
Embodiment 2:
The preparation method of the gradient iron silicon alloy with Different Silicon content distribution of preparation specifically comprises following step in this enforcement:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target.
Step 2, the specimen preparation of low-silicon steel tape base sheet:
After the low silicon silicon steel sheet of 35WW250 removed insulation layer with sand paper, line cut into print, for the JCK-500 magnetic control sputtering device, the print size satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm, in ultrasonic cleaner cleans up stand-by with acetone (analytical pure) oil stain.
Step 3, magnetron sputtering process:
The target that founding in the step 1 is good is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet after step 2 is handled is installed on the positive plate of magnetic control sputtering device.The gaseous tension of the sputtering chamber of magnetic control sputtering device equals 0.5 * 10 before the sputter
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 1.0Pa during sputter.Sputtering power is 60W; Sputtering time is 60min, and making sputter thickness is 12 μ m, and deposition obtains the Silicon-rich film.
Step 4, DIFFUSION TREATMENT:
For fear of Silicon-rich film vapour loss, will deposit Silicon-rich film sample separately and put into 95 porcelain aluminum oxide end-blocking vitrified pipes, the vitrified pipe opening is connected with the vacuum unit, makes vitrified pipe gas inside pressure 1 * 10
-3Under the Pa, carry out high vacuum DIFFUSION TREATMENT 30min, obtain having the gradient iron silicon alloy of Different Silicon content distribution 1190 ℃ of temperature ranges.
Gradient iron silicon alloy after step 4 is handled is tested through EDS, its cross section different positions degree of depth has different silicon contents, as shown in Figure 3, the silicon content maximum value is 4.53wt.%, minimum value is 3.14wt.%, its gradient is reduced to 0.097wt.% for average per 10 μ m Si content, and average Si content is 3.72wt.%; Through the dc magnetic energy of soft magnetism direct current test apparatus specimen, obtaining the sample coercive force is 27.43A/m, B
80=1.85T; Soft magnetism through silicon steel tester test material exchanges performance, P
10/1K=70.76W/kg, P
10/10K=3209W/kg.
Embodiment 3:
The preparation method of the gradient iron silicon alloy with Different Silicon content distribution of preparation specifically comprises following step in this enforcement:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target.
Step 2, the specimen preparation of low-silicon steel tape base sheet:
After the low silicon silicon steel sheet of 35WW250 removed insulation layer with sand paper, line cut into print, for the JCK-500 magnetic control sputtering device, the print size satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm, in ultrasonic cleaner cleans up stand-by with acetone (analytical pure) oil stain.
Step 3, magnetron sputtering process:
The target that founding in the step 1 is good is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet after step 2 is handled is installed on the positive plate of magnetic control sputtering device.The gaseous tension of the sputtering chamber of magnetic control sputtering device is smaller or equal to 1.0 * 10 before the sputter
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.8Pa during sputter.Sputtering power is 57.6W; Sputtering time is 70min, and making sputter thickness is 10 μ m, and deposition obtains rich Si film.
Step 4, DIFFUSION TREATMENT:
For fear of rich Si film vapour loss, will deposit rich Si film sample separately and put into 95 porcelain aluminum oxide end-blocking vitrified pipes, the vitrified pipe opening is connected with the vacuum unit, makes vitrified pipe gas inside pressure 2 * 10
-3Below the Pa, carry out high vacuum DIFFUSION TREATMENT 40min, obtain having the gradient iron silicon alloy of different Si content distribution 1200 ℃ of temperature ranges.
To the conjunction of gradient iron silicon go out after step 4 is handled, through the EDS test, its cross section different positions degree of depth has different silicon contents, as shown in Figure 4.The silicone content maximum value is 3.98wt.%, and minimum value is 3.16wt.%.Fig. 5 is the cross section shape appearance figure at sample in cross section 15.56 μ m degree of depth places, to the silicone content of should the A of degree of depth place ordering is 3.92wt.%, Fig. 6 is the cross section pattern at sample in cross section 125.3 μ m degree of depth places, to the silicone content of should the B of degree of depth place ordering is 3.21wt.%, Fig. 7 is the cross section shape appearance figure at sample in cross section 193.25 μ m degree of depth places, to the silicone content of should the C of degree of depth place ordering is 3.11wt.%, Fig. 8 is the cross section shape appearance figure at sample in cross section 325.3 μ m degree of depth places, to the silicone content of should the D of degree of depth place ordering is 3.66wt.%, the gradient of successively decreasing that calculates the silicon content of this gradient iron silicon alloy is reduced to 0.045wt.% for average per 10 μ m Si content, and average Si content is 3.53wt.%; Through the dc magnetic energy of soft magnetism direct current test apparatus specimen, obtaining the sample coercive force is 23.79A/m, B
80=1.92T; Soft magnetism through silicon steel tester test material exchanges performance, P
10/1K=79.96W/kg, P
10/10K=3476W/kg.
Embodiment 4:
Present embodiment proposes a kind of preparation method with gradient iron silicon alloy of Different Silicon content distribution, specifically comprises following step:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target.
Step 2, the low silicon silicon steel sheet substrate of preparation:
(silicon content is 3wt.% will to equal the thick low silicon silicon steel sheet of 0.30mm, the 35WW250 trade mark) with behind the sand paper removal insulation layer, line cuts into print as substrate, for the JCK-500 magnetic control sputtering device, the print size satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm, in ultrasonic cleaner cleans up stand-by with acetone (analytical pure) oil stain.
Step 3, magnetron sputtering process:
The target that founding in the step 1 is good is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet substrate after step 2 is handled is installed on the positive plate of magnetic control sputtering device.The gaseous tension of the sputtering chamber of magnetic control sputtering device equals 1.0 * 10 before the sputter
-4Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.9Pa during sputter.Sputtering power is 65W; Sputtering time is 70min, and making sputter thickness is 13 μ m, obtains the Silicon-rich film in low silicon silicon steel sheet substrate surface deposition.
Step 4, DIFFUSION TREATMENT:
For fear of Silicon-rich film vapour loss, the low silicon silicon steel sheet that will deposit the Silicon-rich film is separately put into 95 porcelain aluminum oxide end-blocking vitrified pipes, and the vitrified pipe opening is connected with the vacuum unit, and making vitrified pipe gas inside pressure is 2 * 10
-4Pa carries out high vacuum DIFFUSION TREATMENT 20min 1185 ℃ of temperature ranges, obtains having the gradient iron silicon alloy of Different Silicon content distribution.
A kind of gradient iron silicon alloy that obtains in the present embodiment with Different Silicon content distribution, the average silicon content of this alloy is 3.87wt.%, all the other compositions are iron, the silicon content of this alloy entad satisfies from the surface, and portion's direction gradient successively decreases, the gradient of successively decreasing of silicon content is per 10 μ m silicon contents 0.103wt.% that successively decrease, the iron loss P of this gradient iron silicon alloy
10/1KBe 70W/kg, P
10/10KBe 3300W/kg, the coercive force of this gradient iron silicon alloy is 25.03A/m, B
80=1.80T.
Embodiment 5:
Present embodiment proposes a kind of preparation method with gradient iron silicon alloy of Different Silicon content distribution, specifically comprises following step:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target.
Step 2, the low silicon silicon steel sheet substrate of preparation:
(silicon content is 3wt.% will to equal the thick low silicon silicon steel sheet of 0.35mm, the 35WW250 trade mark) with behind the sand paper removal insulation layer, line cuts into print as substrate, for the JCK-500 magnetic control sputtering device, the print size satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm, in ultrasonic cleaner cleans up stand-by with acetone (analytical pure) oil stain.
Step 3, magnetron sputtering process:
The target that founding in the step 1 is good is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet substrate after step 2 is handled is installed on the positive plate of magnetic control sputtering device.The gaseous tension of the sputtering chamber of magnetic control sputtering device equals 0.8 * 10 before the sputter
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.85Pa during sputter.Sputtering power is 64W; Sputtering time is 63min, and making sputter thickness is 11 μ m, obtains the Silicon-rich film in low silicon silicon steel sheet substrate surface deposition.
Step 4, DIFFUSION TREATMENT:
For fear of Silicon-rich film vapour loss, the low silicon silicon steel sheet that will deposit the Silicon-rich film is separately put into 95 porcelain aluminum oxide end-blocking vitrified pipes, and the vitrified pipe opening is connected with the vacuum unit, and making vitrified pipe gas inside pressure is 1 * 10
-4Pa carries out high vacuum DIFFUSION TREATMENT 30min 1195 ℃ of temperature ranges, obtains having the gradient iron silicon alloy of Different Silicon content distribution.
The average silicon content of the gradient iron silicon alloy with Different Silicon content distribution that this enforcement prepares is 3.65wt.%, all the other compositions are iron, the silicon content of this alloy entad satisfies from the surface, and portion's direction gradient successively decreases, the gradient of successively decreasing of silicon content is per 10 μ m silicon contents 0.06wt.% that successively decrease, the iron loss P of this gradient iron silicon alloy
10/1KBe 73.12W/kg, P
10/10KBe 3400W/kg, the coercive force of this gradient iron silicon alloy is 26.78A/m, B
80=1.87T.
Claims (7)
1. gradient iron silicon alloy with Different Silicon content distribution, it is characterized in that: the average silicon content of the gradient iron silicon alloy of described Different Silicon content distribution is 3.53～4.05wt.%, all the other compositions are iron; The silicon content of this alloy successively decreases to alloy heart portion direction gradient from alloy surface, and the gradient of successively decreasing of silicon content is per 10 μ m silicon contents 0.045～0.11wt.% that successively decrease.
2. a kind of gradient iron silicon alloy with Different Silicon content distribution according to claim 1 is characterized in that: the iron loss P of the gradient iron silicon alloy of described Different Silicon content distribution
10/1KBe 69.28～79.96W/kg, P
10/10KBe 3207～3476W/kg.
3. a kind of gradient iron silicon alloy with Different Silicon content distribution according to claim 1, it is characterized in that: the coercive force of the gradient iron silicon alloy of described Different Silicon content distribution is 23.79～27.43A/m, B
80=1.76～1.92T.
4. preparation method with gradient iron silicon alloy of Different Silicon content distribution is characterized in that: specifically comprise following step:
Step 1, preparation target:
Adopt fusion casting preparation Fe
5Si
3Target;
Step 2, the low silicon silicon steel sheet substrate of preparation:
After will hanging down silicon silicon steel sheet and removing insulation layer with sand paper, line cuts into print as substrate, cleans up in ultrasonic cleaner with acetone then, obtains hanging down the silicon silicon steel sheet substrate;
Step 3, magnetron sputtering process:
The Fe that founding in the step 1 is good
5Si
3Target is put into magnetic control sputtering device as the negative electrode target, and the low silicon silicon steel sheet substrate of step 2 preparation is installed on the positive plate of magnetic control sputtering device, and the gaseous tension of sputtering chamber that magnetic control sputtering device is set is smaller or equal to 1.0 * 10
-3Pa, the sputtering atmosphere of magnetic control sputtering device is a pure argon, the gaseous tension of sputtering chamber satisfies 0.8～1.0Pa during sputter; Sputtering power is 57.6～72W; Sputtering time is 60～80min, and sputter thickness is 10 μ m～15 μ m, obtains the Silicon-rich film in low silicon silicon steel sheet substrate surface deposition;
Step 4, DIFFUSION TREATMENT:
The low silicon silicon steel sheet of deposition Silicon-rich film is put into 95 porcelain aluminum oxide end-blocking vitrified pipes, and the vitrified pipe opening is connected with the vacuum unit, makes vitrified pipe gas inside pressure 2 * 10
-3Below the Pa, carry out high vacuum DIFFUSION TREATMENT 20～40min, finally obtain having the gradient iron silicon alloy of different Si content distribution 1180～1200 ℃ of temperature ranges.
5. a kind of preparation method with gradient iron silicon alloy of Different Silicon content distribution according to claim 4 is characterized in that: the low silicon silicon steel sheet thickness in the described step 2 is smaller or equal to 0.35mm, and silicon content is 3wt.%.
6. according to claim 4 or 5 described a kind of preparation methods with gradient iron silicon alloy of Different Silicon content distribution, it is characterized in that: the trade mark of described low silicon silicon steel sheet is 35WW250.
7. a kind of preparation method with gradient iron silicon alloy of Different Silicon content distribution according to claim 4 is characterized in that: the print size in the described step 2 satisfies the long 40mm that is, wide is 8mm, and thickness is 0.35mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002302744A (en) * | 2001-04-06 | 2002-10-18 | Nkk Corp | High-silicon electromagnetic steel sheet |
| CN1807687A (en) * | 2006-01-26 | 2006-07-26 | 北京航空航天大学 | Process for preparing high silicon stalloy by pack siliconizing process |
| CN1944706A (en) * | 2006-10-30 | 2007-04-11 | 北京航空航天大学 | Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002302744A (en) * | 2001-04-06 | 2002-10-18 | Nkk Corp | High-silicon electromagnetic steel sheet |
| CN1807687A (en) * | 2006-01-26 | 2006-07-26 | 北京航空航天大学 | Process for preparing high silicon stalloy by pack siliconizing process |
| CN1944706A (en) * | 2006-10-30 | 2007-04-11 | 北京航空航天大学 | Method for preparing Fe-6.5 wt% Si thin plate using continuous magnetic control sputtering physical gas phase depositing |
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