CN103898300A - Method for controlling feature distribution of crystal boundary of high silicon steel through orientation recrystallization - Google Patents
Method for controlling feature distribution of crystal boundary of high silicon steel through orientation recrystallization Download PDFInfo
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- CN103898300A CN103898300A CN201410136097.9A CN201410136097A CN103898300A CN 103898300 A CN103898300 A CN 103898300A CN 201410136097 A CN201410136097 A CN 201410136097A CN 103898300 A CN103898300 A CN 103898300A
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Abstract
The invention provides a method for controlling feature distribution of a crystal boundary of high silicon steel through orientation recrystallization. The method comprises the following steps: refining boracic Fe-6.5wt% Si high silicon steel by using a vacuum sensing melting furnace, after the refining, casting the steel to obtain ingots, performing homogenization treatment on the ingots at 1050 DEG C, fogging into a plate which is 12mm in thickness at 900 DEG C, machining the high silicon steel in the fogged state into an orientation recrystallization test sample which is 2mm in thickness, 6mm in width and 80mm in length, mechanically polishing the orientation recrystallization test sample firstly, corroding the polished test sample in 5% dilute sulphuric acid for 20 minutes, subsequently washing in acetone, and performing orientation recrystallization in a vacuum chamber, wherein the thermal area temperature is 1050-1200 DEG C, the temperature gradient is 350 DEG C/cm, and the withdrawing rate is 0.4-12mu m/s. The method is reasonable in process design and simple to operate, and the mechanical processing and thermal processing property of the Fe-6.5wt% Si alloy can be improved.
Description
Technical field
What the present invention relates to is a kind of working method of metallic substance, particularly a kind of method of controlling the high silicon steel Grain Boundary Character distribution of boracic Fe-6.5wt%Si.
Background technology
Silicon steel (electrical steel), as iron core and other electrical component of various motors and transformer, is mainly the indispensable important non-retentive alloy in the field such as electric power, electronics.It is a kind of non-retentive alloy of usage quantity maximum, occupies critical role in soft magnetic materials field.The principal element that affects silicon steel magnetic property has silicone content, thickness of slab, grain-size, foreign matter content and crystallography texture etc.Before eighties of last century eighties, utilization improves the crystallography texture of silicon steel, the means such as grain-size, foreign matter content of controlling make magnetic property obtain very large improvement, but never larger raising of the magnetic property of silicon steel afterwards, therefore carries high Si content and the further thickness that reduces silicon steel has caused people's attention again.Along with the increase of silicone content, the resistivity of silicon steel increases, and eddy-current loss reduces, thereby shows good magnetic under upper frequency.In the time that silicone content reaches 6.5% left and right, magnetostriction coefficient levels off to zero, and magnetic permeability is increased to maximum, and iron loss drops to minimum.But Fe-6.5wt%Si alloy makes alloy become not only firmly but also is crisp because silicone content is high, mechanical workout and hot workability are obviously worsened.Because fragility problem is never resolved, very for a long period long, the progress of cold rolling high achieving no breakthrough property of silicon steel process.Research shows, distributes by controlling Grain Boundary Character, can effectively improve fragility, corrosion resistance nature and the creep-resistant property of metallic substance.Coherent reference file comprises:
[1]T.Watanabe.Metall?Trans?A14(1983):531；
[2]B.Alexandreanu,G.S.Was,Scripta?Mater.54(2009):1047；
[3]S.Bechtle,M.Jumar,B.P.Somerday,M.E.Launey,R.O.Ritchie,Acta?Mater,57(2009):4148；
[4]D.A.Molodo,P.J.Konijnenberg,Scripta?Mater,54(2006):977。
Summary of the invention
The object of the present invention is to provide a kind of control that can realize high silicon steel Grain Boundary Character distribution, improve the processing characteristics of high silicon steel, what controllability was good, simple to operate passes through the method that the high silicon steel Grain Boundary Character of Directional Recrystallization control distributes.
The object of the present invention is achieved like this:
With the high silicon steel of vacuum induction melting stove refining boracic Fe-6.5wt%Si, after refining, pour into a mould, obtain ingot casting; The weight ratio chemical composition of described ingot casting is that 0.05%C, 6.31%Si, 0.11%Mn, 0.008%P, 0.006%S, 0.005%Al, 0.043%B, residue are Fe; Ingot casting, 1050 ℃ of homogenizing processing, is then forged into the sheet material that 12mm is thick, and forging temperature is 900 ℃; The high silicon steel that forges state is processed into and is of a size of the Directional Recrystallization sample that 2mm is thick, 6mm is wide, 80mm is long; First Directional Recrystallization sample carries out mechanical polishing, and the sample after polishing corrodes 20min in 5% dilute sulphuric acid, then cleans with acetone;
In vacuum chamber, carry out Directional Recrystallization, hot-zone temperature is 1050～1200 ℃, and thermograde is 350 ℃/cm, and withdrawing rate is 0.4～12 μ m/s, and Directional Recrystallization process is to realize by orientation anneal.
The detailed process of described Directional Recrystallization is:
(1) the good sample of pre-treatment is arranged on the pumping rod that connects servomotor in orientation anneal stove, adjusts induction coil with metal cools liquid level distance, guarantee that in the front end sample of hot-zone, thermograde is 350 ℃/cm in the time that hot-zone temperature is 1150 ℃;
(2) close orientation anneal bell be evacuated to～10
-3pa;
(3) start induction power supply heating, when specimen temperature in hot-zone reaches after 1050～1200 ℃, start servomotor, sample is moved from bottom to top, rate travel is 0.4～12 μ m/s.
When specimen temperature in hot-zone reaches after 1150 ℃, start servomotor.
Rate travel is 3 μ m/s.
Tool of the present invention has the following advantages and positively effect:
(1) the present invention, by orientation anneal process implementation Directional Recrystallization, can control the quantity of low-angle boundary and low ∑ coincidence site lattice (CSL) crystal boundary, makes it to form the characteristic distribution with special grain boundary.Realize the control that high silicon steel Grain Boundary Character is distributed.
(2) adopt the present invention, can make high silicon steel forming frequency value after Directional Recrystallization be 4～4.8 times of random orientation distribution statistics values low-angle boundary and low ∑ coincidence site lattice (CSL) crystal boundary (3≤Σ≤29), thereby effectively improve the processing characteristics of high silicon steel.
(3) controllability of the present invention is good, simple to operate, is applicable to commercial scale production.
Accompanying drawing explanation
Fig. 1 is the microstructure after high silicon steel Directional Recrystallization.
Fig. 2 a-Fig. 2 b is misorientation distribution plan and the Grain Boundary Character distribution plan after high silicon steel Directional Recrystallization.
Embodiment
Below in conjunction with example, the present invention is further described.
With the high silicon steel of vacuum induction melting stove refining boracic Fe-6.5wt%Si, after cast, obtain ingot casting.By ingot casting cool to room temperature after 1050 ℃ of homogenizing are processed, be then forged into the sheet material that 12mm is thick, forging temperature is 900 ℃.The high silicon steel sample that forges state is processed into and is of a size of long 80mm, wide 6mm, the Directional Recrystallization sample of thick 2mm.The Directional Recrystallization sample making is carried out to mechanical polishing processing, and the sample after polishing corrodes 20min in 5% dilute sulphuric acid, finally cleans with acetone.Directional Recrystallization completes in vacuum chamber, and vacuum tightness is 10
-3pa, hot-zone temperature is 1150 ℃, withdrawing rate is 3 μ m/s.Obtain the high silicon steel of Fe-6.5wt%Si that feature crystal boundary distributes that has of the present invention.
Concrete Directional Recrystallization process is as follows:
1. the good sample of pre-treatment is arranged on the pumping rod that connects servomotor in orientation anneal stove, adjusts induction coil with metal cools liquid level distance, guarantee that in the front end sample of hot-zone, thermograde is about 350 ℃/cm in the time that hot-zone temperature is 1150 ℃.
2. close orientation anneal bell be evacuated to～10
-3pa.
3. start induction power supply heating, when specimen temperature in hot-zone reaches after 1150 ℃, start servomotor, sample is moved from bottom to top, rate travel is 3 μ m/s.
Fig. 1 is the microstructure after high silicon steel Directional Recrystallization.As can be seen from Fig., after Directional Recrystallization, obtained having the column crystal microstructure of big L/D ratio.Fig. 2 a-Fig. 2 b is misorientation distribution plan and the Grain Boundary Character distribution plan after high silicon steel Directional Recrystallization.Can find out from figure Fig. 2 a, the misorientation after Directional Recrystallization is distributed as Gaussian distribution, and the misorientation of Fe-6.5wt%Si silicon steel after Directional Recrystallization distributes and be similar to stochastic distribution.Can find out from figure Fig. 2 b, after Directional Recrystallization, sample has formed coincidence site lattice (CSL) crystal boundary (special grain boundary) (3≤Σ≤29) of high frequency (11%) low-angle boundary and the low ∑ value of high frequency (44%).Low-angle boundary value is about 4.8 times of random grains orientation statistical value (2.3%), and special grain boundary value is about 4 times of statistical value (11.3%).This Grain Boundary Character that has shown that sample after Directional Recrystallization has formed coincidence site lattice (CSL) crystal boundary with high frequency low-angle boundary and low ∑ value distributes.
Claims (4)
1. the method distributing by the high silicon steel Grain Boundary Character of Directional Recrystallization control, is characterized in that: with the high silicon steel of vacuum induction melting stove refining boracic Fe-6.5wt%Si, after refining, pour into a mould, obtain ingot casting; Ingot casting, 1050 ℃ of homogenizing processing, is then forged into the sheet material that 12mm is thick, and forging temperature is 900 ℃; The high silicon steel that forges state is processed into and is of a size of the Directional Recrystallization sample that 2mm is thick, 6mm is wide, 80mm is long; First Directional Recrystallization sample carries out mechanical polishing, and the sample after polishing corrodes 20min in 5% dilute sulphuric acid, then cleans with acetone;
In vacuum chamber, carry out Directional Recrystallization, hot-zone temperature is 1050～1200 ℃, and thermograde is 350 ℃/cm, and withdrawing rate is 0.4～12 μ m/s, and Directional Recrystallization process is to realize by orientation anneal.
2. the method distributing by the high silicon steel Grain Boundary Character of Directional Recrystallization control according to claim 1, is characterized in that the detailed process of described Directional Recrystallization is:
(1) the good sample of pre-treatment is arranged on the pumping rod that connects servomotor in orientation anneal stove, adjusts induction coil with metal cools liquid level distance, guarantee that in the front end sample of hot-zone, thermograde is 350 ℃/cm in the time that hot-zone temperature is 1150 ℃;
(2) close orientation anneal bell be evacuated to～10
-3pa;
(3) start induction power supply heating, when specimen temperature in hot-zone reaches after 1050～1200 ℃, start servomotor, sample is moved from bottom to top, rate travel is 0.4～12 μ m/s.
3. the method distributing by the high silicon steel Grain Boundary Character of Directional Recrystallization control according to claim 2, is characterized in that reaching after 1150 ℃ when specimen temperature in hot-zone, starts servomotor.
4. according to the method that the high silicon steel Grain Boundary Character of Directional Recrystallization control distributes of passing through described in claim 2 or 3, it is characterized in that rate travel is 3 μ m/s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112048605A (en) * | 2020-08-03 | 2020-12-08 | 西北工业大学 | Directional annealing device and method for preparing metal columnar crystals |
| CN115233082A (en) * | 2022-07-28 | 2022-10-25 | 东北大学 | Method for preparing electrical steel thin strip with strong {100} surface texture through directional recrystallization |
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|---|---|---|---|---|
| CN112048605A (en) * | 2020-08-03 | 2020-12-08 | 西北工业大学 | Directional annealing device and method for preparing metal columnar crystals |
| CN115233082A (en) * | 2022-07-28 | 2022-10-25 | 东北大学 | Method for preparing electrical steel thin strip with strong {100} surface texture through directional recrystallization |
| CN115233082B (en) * | 2022-07-28 | 2023-02-24 | 东北大学 | Method for preparing electrical steel thin strip with strong {100} surface texture through directional recrystallization |
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Application publication date: 20140702 |