CN101319306A - Industrial production system for producing high-silicon strip with magnetron sputtering continuous two-sided codeposition process - Google Patents
Industrial production system for producing high-silicon strip with magnetron sputtering continuous two-sided codeposition process Download PDFInfo
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- CN101319306A CN101319306A CNA200810116253XA CN200810116253A CN101319306A CN 101319306 A CN101319306 A CN 101319306A CN A200810116253X A CNA200810116253X A CN A200810116253XA CN 200810116253 A CN200810116253 A CN 200810116253A CN 101319306 A CN101319306 A CN 101319306A
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Abstract
The invention discloses an industrialized production system for making a high-silicon steel strip by a process of magnetron sputtering continuous double-sided codeposition. The industrialized production system of a high-silicon silicon plate comprises a welding machine (3), a preheating chamber (4), a magnetron sputtering chamber (1), a diffusion chamber (5), a cooling chamber (6), and a coiler (7), which are sequentially arranged on a production line starting from the deliverty of the low-silicon silicon plate to the production system by an unwinding coiler (2) to the finish of the production of high-silicon silicon plate. The industrialized production system for making the silicon material by the process of the continuous double-sided codeposition, driven by the unwinding coiler (2), is capable of performing deposition on a the low-silicon silicon plate with a thickness of less than 0.35mm with silicon content of between 5 and 8 weight percent to by means of symmetrically disposing a plurality of cathode targets in the magnetron sputtering chamber, thereby achieving the aim of continuous deposition of silicon material with low energy consumption and high production efficiency. The industrialized production system solves the defect that the silicon plate of the commercialized Fe-6.5 weight percentage Si can only be produced by adopting a method of chemical gas-phase deposition.
Description
Technical field
The present invention relates to a kind of technology of suitability for industrialized production high-silicon steel thin plate, more particularly say, be meant a kind ofly adopt magnetron sputtering continuous two-sided codeposition technology, silicon materials and diffusion make it to become the high-silicon steel thin plate in the upper and lower while sputter of low silicon silicon steel suitability for industrialized production system.
Background technology
The magnetron sputtering principle: the accelerated motion under anode and cathode two interpolar effect of electric field of charged ion and electronics obtains sufficiently high energy and bumps with argon molecules, and ionization goes out a large amount of argon ions and electronics.Argon ion quickens the bombarding cathode target under effect of electric field, sputter a large amount of target atom and be deposited on film forming on the substrate.Secondary electron is subjected to the influence of Lip river, magnetic field logical sequence magnetic force in flying to the process of substrate, be bound near in the plasma body zone of target surface, plasma density is very high in this zone, secondary electron is made circumferential motion around target surface under the effect in magnetic field, this electronic motion path is very long, in moving process constantly and the ar atmo ionization that bumps go out a large amount of argon ion bombardment targets, reduce gradually through the energy that repeatedly collides the back electronics, break away from the constraint of magnetic line of force, away from target, finally be deposited on the substrate.Magnetron sputtering is exactly with magnetic field constraint and prolongs the electronic motion path, changes the electronic motion direction, improves the specific ionization of working gas and effectively utilizes the energy of electronics.
Fe-6.5wt%Si silicon steel has excellent soft magnetic performance, as: the medium-high frequency iron loss is low, magnetic hysteresis flexible almost nil, coercive force is little, magnetic permeability and saturation induction density are high, it also has the advantage of good stability simultaneously, is a kind of outstanding soft magnetic materials.At present, the Fe-6.5wt%Si silicon plate adopts chemical gaseous phase depositing process and the preparation of hot rolling method basically.Chemical gaseous phase depositing process is to introduce silane gas in vacuum chamber, by heating silane gas is decomposed after, a certain amount of silicon of deposition on the silicon steel sheet that has carried out suitable pre-treatment, and then, obtain uniform Fe-6.5wt%Si silicon plate by thermal treatment.Rolling rule is that direct ingot casting to Fe-6.5wt%Si carries out heat, cold repeatedly rolling, obtains to wish the thin plate of thickness.Because the fragility of Fe-6.5wt%Si self and the restriction on the rolling technology, the Fe-6.5wt%Si silicon plate thickness of rolling preparation generally is difficult to be lower than 0.35mm, and cost is very high.
Present commercial Fe-6.5wt%Si silicon plate adopts the chemical gaseous phase depositing process preparation basically.But owing to chemical gaseous phase depositing process exist surface quality poor, easily introduce that impurity reduces 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.
Summary of the invention
The objective of the invention is to propose a kind ofly to adopt magnetically controlled sputter method, prepare silicon materials, thereby make the suitability for industrialized production system of high-silicon steel thin plate at the upper and lower continuous two-sided codeposition of low silicon steel thin plate; This suitability for industrialized production system is by carrying out making the high-silicon steel thin plate behind preheating impurity elimination, magnetron sputtering double-surface depositing silicon material, silicon diffusion, the cooling and shaping to low silicon steel thin plate.The suitability for industrialized production system of continuous two-sided codeposition system silicon materials of the present invention under the drive of winder, realized the purpose of successive sedimentation silicon materials, and energy consumption is low, the production efficiency height by the mode of a plurality of negative electrode targets of symmetric arrangement in magnetron sputtering chamber.The suitability for industrialized production system of the continuous two-sided codeposition system silicon materials that the present invention proposes has solved the defective that existing commercial Fe-6.5wt%Si silicon plate adopts chemical gaseous phase depositing process to make basically.
The present invention is a kind of suitability for industrialized production system that adopts the high silicon strip of magnetron sputtering continuous two-sided codeposition technology system, this high-silicon steel thin plate suitability for industrialized production system is uncoiled machine (2) from low silicon steel thin plate and sends into production system and begin to end to making the high-silicon steel thin bundle that hardens, and the order of equipment is welding machine (3), preheating chamber (4), magnetron sputtering chamber (1), diffuser casing (5), cooling room (6), reeling machine (7) on the production line;
Preheating chamber (4) is used for low silicon steel thin plate (1a) is heated, and makes low silicon steel thin plate (1a) obtain uniform 200～300 ℃ and carries temperature; The Heating temperature that preheating chamber (4) provides is 200～300 ℃, effectively heated length 2～10m;
Magnetron sputtering chamber (1) is used at continuous codeposition silicon materials of the upper and lower while of fs thin plate (1A);
The fabrication process condition of magnetron sputtering chamber (1):
(A) number, the layout type of the negative electrode target in the magnetron sputtering chamber (1) are set; Described layout type is the staggered relatively or negative electrode target intersection placement of negative electrode target;
(B) to magnetron sputtering chamber (1) suction to 1.0 * 10
-3～8.0 * 10
-4Pa;
(C) charge into argon gas, the sputtering pressure that keeps magnetron sputtering chamber (1) is at 0.5～2.0Pa;
(D) sparking voltage 300～600V, current density 5～60mA, the sedimentation rate of single negative electrode target is 0.2～1.2 μ m/min in the adjusting magnetron sputtering chamber (1);
The target surface spacing h of two groups of negative electrode targets about in the magnetron sputtering chamber (1)
0=60～180mm, the spacing d of adjacent two negative electrode targets in the same side
0=300～500mm, the entire length L=5～30m of magnetron sputtering chamber (1);
Diffuser casing (5) is used for subordinate phase thin plate (1B) is heat-treated under 1000～1250 ℃ of hot environments, and the thermal treatment temp that diffuser casing (5) provides is 1000～1250 ℃, effectively heated length 5～20m;
Cooling room (6) is used for phase III thin plate (1C) is cooled off; The cooling temperature that cooling room (5) provides is 200～500 ℃, refrigerated area length 2～10m;
Continuous production speed v=1～50m/h that Abrollhaspel (2) provides;
Winder (7) is used for cooled high-silicon steel thin plate (1b) is carried out package one-tenth dish.
The negative electrode target includes cover plate (101), permanent magnet (102), magnetic boots (103), cathode sheath (104), cathode cap (106), outer cover (105) in the described magnetron sputtering chamber (1), permanent magnet (102) is positioned at the central position of magnetic boots (103), magnetic boots (103) are sleeved in the cathode sheath (104), cathode sheath (104) outer cover is equipped with outer cover (105), the bottom of outer cover (105) is connected with cathode cap (106), the inside of cathode cap (106) is provided with boss (161), is placed with target (110) on the boss (161); Gasket (107) is arranged between the upper end of cover plate (101) and cathode sheath (104), and cover plate (101) is provided with prosopyle (111), posticum (112), and prosopyle (111), posticum (112) are communicated with the water coolant of outside respectively by pipeline.
The employing magnetically controlled sputter method that the present invention proposes, at the upper and lower continuous two-sided codeposition system silicon materials of low silicon steel thin plate, obtain the suitability for industrialized production system of high-silicon steel thin plate, can improve and solve shortcomings such as existing manufacturing siliconized plate complex process, cost height.With Pure Silicon Metal (or ferro-silicon) is the negative electrode target, and with the low silicon silicon steel sheet (anode) of thickness in 0.1～0.35mm scope of continuous transmission, and two or more sets negative electrode targets are symmetrically distributed up and down at low silicon silicon steel sheet, and controlling magnetic field all is set behind the negative electrode target.Be evacuated down to vacuum tightness in advance in work system and reach 10
-2～10
-3Behind the Pa, system feeds argon gas, anode and cathode was connected power supply when pressure was raised to 0.5～2Pa, under electric field action, make the Ar atomic ionization, by Ar ion bombardment target, make the target surface atom simultaneously (or respectively) sputtering sedimentation on low silicon silicon steel sheet upper and lower surface, formation 10～30 μ m elementary silicon films (or high silicon content ferrosilicon film).Plated film pure iron strip transfers out sputtering zone and enters 1000～1250 ℃ of High temperature diffusion districts immediately, makes the surface silicon atom reach the rated process requirement to the silicon content of internal diffusion in steel band, and is evenly distributed, and obtains higher silicon silicon steel sheet.Method of the present invention can be adjusted coatings thickness and density by control utmost point discharge current density and low silicon silicon steel sheet transmission speed, determine to guarantee in desired indicator with the silicon content of adjusting in the low silicon silicon steel sheet diffusion time by control diffusion temperature and low silicon silicon steel sheet transmission speed, heating interval length, and Siliciumatom is evenly distributed in low silicon silicon steel sheet.Because method high efficiency of the present invention, the processing parameter of preparation process is controlled easily, and the quality of product is guaranteed easily, therefore extremely is fit to industrial applications.
Description of drawings
Fig. 1 is the upper and lower employing magnetically controlled sputter method of the present invention at low silicon steel thin plate, continuous two-sided codeposition system silicon materials, the suitability for industrialized production structure schematic diagram of acquisition high-silicon steel thin plate.
Fig. 2 is the layout diagrammatic sketch that magnetron sputtering chamber inner cathode target symmetry of the present invention is placed.
Fig. 3 is the layout diagrammatic sketch of the present invention's two negative electrode targets staggered relatively and low-silicon steel band.
Fig. 4 is the blast diagrammatic sketch of A negative electrode target of the present invention.
Fig. 4 A is the sectional view of A negative electrode target of the present invention.
Among the figure: 1. cathode target 101. cover plates 111. water inlet holes 112. apopores, 102. permanent magnets, 103. magnetic boots, 104. cathode sheaths, 105. shielding covers 106. cathode caps 161. boss 107. sealing gaskets 110. targets under cathode target 12. N under the cathode target 12b. B under the upper cathode target 12a. A of magnetron sputtering chamber 2. uncoilers 3. bonding machines 4. pre-hot cells 5. diffuser casings upper cathode target 11. N of the upper cathode target 11b. B of the low silicon silicon strip 1b. high silicon steel strap 1A. phase I thin plate 1B. second stage thin plate 1C. phase III thin plate 11a. A of 6. cooling chamber 7. winder 1a.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention is a kind of employing magnetically controlled sputter method, at the upper and lower continuous two-sided codeposition system silicon materials of low silicon steel thin plate, obtain the suitability for industrialized production system of high-silicon steel thin plate, (referring to shown in Figure 1) this high-silicon steel thin plate suitability for industrialized production system is uncoiled machine 2 from low silicon steel thin plate and sends into production system and begin to end to making the high-silicon steel thin bundle that hardens, and the order of equipment is welding machine 3, preheating chamber 4, magnetron sputtering chamber 1, diffuser casing 5, cooling room 6, reeling machine 7 on the production line.Described welding machine 3 is to be used for the low silicon steel thin plate of last time is welded from beginning to end mutually with this low silicon steel thin plate, realizes the continuous production of technology, has also solved the existing silicon steel thin plate that will hang down from beginning to end simultaneously and has increased as the tooling cost that waste material causes.In high-silicon steel thin plate suitability for industrialized production of the present invention system, also a cutting machine can be set before reeling machine 7, described cutting machine helps quantitatively to prepare the high-silicon steel thin plate according to the required silicon steel length requirement that the client proposes.Low silicon steel thin plate described in the present invention is meant that silicone content equals the silicon steel sheet less than 3wt%, and described high-silicon steel thin plate is meant the silicon steel sheet that makes behind production line of the present invention, and general silicone content is 5～8wt%.Production line of the present invention can carry out the deposition preparation of silicone content to thickness less than the silicon steel sheet of 0.35mm.
In the present invention, an end of low silicon steel thin plate is fixed on the Abrollhaspel 2, and the other end of low silicon steel thin plate is wound into dish by reeling machine 7 after passing welding machine 3, preheating chamber 4, magnetron sputtering chamber 1, diffuser casing 5, cooling room 6 in turn.
In order to narrate conveniently, will to hang down the silicon steel thin plate and be referred to as fs thin plate 1A (i.e. low silicon steel thin plate after preheating chamber 4 is handled) before entering magnetron sputtering chamber 1;
Fs thin plate 1A is behind magnetron sputtering chamber 1, and the upper and lower surface of fs thin plate 1A has deposited a certain amount of silicon materials, is referred to as subordinate phase thin plate 1B this moment;
Subordinate phase thin plate 1B makes subordinate phase thin plate 1B go up sedimentary silicon materials by thermal treatment behind diffuser casing 5, is referred to as phase III thin plate 1C this moment.
In the present invention, the function of the various piece realization on the production line of industrialization magnetron sputtering double-surface codeposition production high-silicon steel plate is explained as follows:
One, the low silicon steel thin plate of heating
The Heating temperature that preheating chamber 4 provides is 200～300 ℃, effectively heated length 2～10m.
In the present invention, low silicon steel thin plate 1a is heated certain temperature help depositing silicon material in magnetron sputtering chamber 1, and the bond quality that improves silicon materials and fs thin plate 1A.
Two, the continuous codeposition silicon materials of magnetron sputtering double-surface
The fabrication process condition of magnetron sputtering chamber 1:
(A) number, the layout type of the negative electrode target in the magnetron sputtering chamber 1 are set; Described layout type is the staggered relatively or negative electrode target intersection placement of negative electrode target;
(B) to magnetron sputtering chamber 1 suction to 1.0 * 10
-3～8.0 * 10
-4Pa;
(C) charge into argon gas, the sputtering pressure that keeps magnetron sputtering chamber 1 is at 0.5～2.0Pa;
(D) sparking voltage 300～600V, current density 5～60mA, the sedimentation rate of single negative electrode target is 0.2～1.2 μ m/min in the adjusting magnetron sputtering chamber 1;
The sedimentation rate that magnetron sputtering chamber 1 provides is with sputtering pressure, sputtering power and target-substrate distance control, and thicknesses of layers is by single-sided cathodes target distribution number and the control of thin plate transmission speed.
The target surface spacing h of two groups of negative electrode targets about in the magnetron sputtering chamber 1
0=60～180mm, the spacing d of adjacent two negative electrode targets in the same side
0=300～500mm.The number of each side negative electrode target can be 3～30 and arrange.The layout type of two groups of negative electrode targets can be with fs thin plate 1A symmetry up and down, and it is staggered relatively with following negative electrode target to go up the negative electrode target, is called negative electrode target (referring to shown in Figure 2) staggered relatively; Also can be that up and down two groups of negative electrode targets intersect placement with fs thin plate 1A symmetry but go up negative electrode target and following negative electrode target, be called negative electrode target intersection placement (shown in Fig. 2 A).
Three, the diffusion of silicon materials
The thermal treatment temp that diffuser casing 5 provides is 1000～1250 ℃, effectively heated length 5～20m;
Four, cooling
The cooling temperature that cooling room 5 provides is 200～500 ℃, refrigerated area length 2～10m.
Five, controlled continuous production speed
Continuous production speed v=1～50m/h that Abrollhaspel 2 provides.
In the present invention, Abrollhaspel 2 is used to install low silicon steel thin plate on the one hand, on the other hand for continuous production provides continuous production speed v=1～50m/h, and this continuous production speed v and sedimentary silicone content G
Si, magnetron sputtering chamber 1 lateral length L, magnetron sputtering chamber 1 in that the number N of negative electrode target is set is relevant.
Promptly as lateral length L, negative electrode target number N one timing, siliceous deposits content G
SiFew, then the continuous production speed v is just fast.
Promptly as lateral length L, negative electrode target number N one timing, siliceous deposits content G
SiMany, then the continuous production speed v is just slow.
Promptly as lateral length L, siliceous deposits content G
SiOne regularly, and N is few for negative electrode target number, and then the continuous production speed v is just slow.
Promptly as lateral length L, siliceous deposits content G
SiOne regularly, and N is many for negative electrode target number, and then the continuous production speed v is just fast.
Promptly as negative electrode target number N, siliceous deposits content G
SiOne regularly, and lateral length L is short, and then the continuous production speed v is just slow.
Promptly as negative electrode target number N, siliceous deposits content G
SiOne regularly, and lateral length L is long, and then the continuous production speed v is just fast.
Six, package one-tenth dish
High-silicon steel thin plate suitability for industrialized production of the present invention system can produce the high-silicon steel thin plate 1b of 0.10～0.35mm thickness, and silicone content can reach 5～8wt% among the high-silicon steel thin plate 1b, and silicone content is evenly distributed.
In the present invention, be furnished with a plurality of negative electrode targets in the magnetron sputtering chamber 1, the negative electrode target is distributed in the upper and lower of fs thin plate 1A.The negative electrode target can be staggered relatively up and down, i.e. cathode cap (making target be right against the last lower belt surface of fs thin plate 1A) staggered relatively; The negative electrode target also can intersect dislocation and places up and down, and promptly the negative electrode target staggers mutually up and down, but cathode cap is still over against the last lower belt surface of fs thin plate 1A.The negative electrode target can be 3～30 in the number of each side negative electrode target of magnetron sputtering chamber 1 to be arranged (total up and down number is 6～60).Referring to Fig. 2, shown in Figure 3, fs thin plate 1A is between last negative electrode target and following negative electrode target, and upward the negative electrode target is that centrosymmetry is arranged with following negative electrode target with fs thin plate 1A, and last negative electrode target is staggered relatively with the cathode cap of following negative electrode target; Last negative electrode target is identical with the structure of following negative electrode target.Last negative electrode target can be meant that A goes up negative electrode target 11a, B and goes up negative electrode target 11b, N and go up negative electrode target 11, and following negative electrode target can be meant under the A under negative electrode target 12a, the B negative electrode target 12 under negative electrode target 12b, the N.Because target is to be placed on the boss of cathode cap of this anticathode target (go up the negative electrode target for and be called an anticathode target with a following negative electrode target), just can be implemented in fs thin plate 1A during sputter and goes up the purpose that lower belt surface prepares target simultaneously continuously.The entire length L=5 of magnetron sputtering chamber 1～30m, spacing d between vertical two negative electrode targets
0=300～500mm, the negative electrode target target surface spacing of symmetry placement is h up and down
0=60～180mm.
In the present invention, field of excitation in the negative electrode target adopts solenoid or permanent magnet excitation mode and homopolarity relative, promptly the direction of polarization of the permanent magnet of negative electrode target 12 (being positioned at fs thin plate 1A below) is relative under the last negative electrode target 11 of N (being arranged in fs thin plate 1A top), the N, be N extremely to the N utmost point, perhaps S is extremely to the S utmost point.Each negative electrode target be connected in parallel on one or separately separate connection on many direct currents or radio-frequency power supply, be anode with workpiece (as the low-silicon steel band), silicon target is a negative electrode.
Shown in Fig. 4, Fig. 4 A, N goes up negative electrode target 11 and includes cover plate 101, permanent magnet 102, magnetic boots 103, cathode sheath 104, cathode cap 106, outer cover 105, permanent magnet 102 is positioned at the central position of magnetic boots 103, magnetic boots 103 are sleeved in the cathode sheath 104, cathode sheath 104 outer cover are equipped with outer cover 105, the bottom of outer cover 105 is connected with cathode cap 106, and the inside of cathode cap 106 is provided with boss 161 (boss 161 is used to place target 110); Gasket 107 is arranged between the upper end of cover plate 101 and cathode sheath 104, cover plate 101 is provided with prosopyle 111, posticum 112, prosopyle 111, posticum 112 are communicated with the water coolant of outside respectively by pipeline, cooperate the upper end of realizing cover plate 101 is installed in cathode sheath 104 with screw (being located on the upper surface of cathode sheath 104) by screw.Target 110 is positioned on the boss 161 in the cathode cap 106.
Embodiment 1:
On the Fe-3.0wt%Si of thick 0.20mm low-silicon steel band, make the high silicon strip of Fe-6.5wt%Si
At upper and lower double-sided deposition purity 99.9% silicon materials of the Fe-3.0wt%Si of thick 0.20mm low-silicon steel band, the depositing silicon material thickness is 15 μ m.
The condition such as the following table of the high silicon strip of magnetron sputtering double-surface codeposition suitability for industrialized production:
The procedure of processing of the high silicon strip of magnetron sputtering double-surface codeposition suitability for industrialized production includes:
The first step: prepared silicon target
Target is a polysilicon, thickness 6mm * length 300mm * width 300mm, and boss 161 sizes that are provided with in target size and the cathode cap 106 are suitable;
Second step: silicon strip is installed
One end of the Fe-3.0wt%Si low-silicon steel band of thick 0.20mm is installed on the Abrollhaspel 2, and the other end is installed in reeling machine 7 in turn behind welding machine 3, preheating chamber 4, magnetron sputtering chamber 1, diffuser casing 5, cooling room 6;
The 3rd step: adjust magnetron sputtering chamber
Fe-3.0wt%Si silicon strip with thick 0.20mm in magnetron sputtering chamber 1 is a centrosymmetry, respectively puts 12 negative electrode targets up and down; More than the given condition of table is controlled;
The 4th step: table is adjusted the processing conditions of preheating chamber 4, diffuser casing 5, cooling room 6 on the foundation;
The 5th step: adjust Abrollhaspel 2 and transmit the high silicon strip of system with speed 10m/h at the uniform velocity;
The 6th step: through reeling machine 7 package one-tenth dishes.
The high silicon strip that the 5th step is made detects through EDS energy spectrometer and electron probe micro-analysis, and high silicon strip section reaches 6.55wt% at the Si of upper layer content, and high silicon strip center Si content reaches 6.48wt%, and Si content presents uniform distribution substantially in zone face.Its soft magnetic performance B after testing
s=1.78T, P
10/50=0.50W/Kg, P
10/400=7.86W/Kg.
Embodiment 2:
On 35WW270 low-silicon steel band, make the high silicon strip of Fe-6.5wt%Si
At upper and lower double-sided deposition purity 99.9% silicon materials of 35WW270 low-silicon steel band, the depositing silicon material thickness is 20 μ m.
The condition such as the following table of the high silicon strip of magnetron sputtering double-surface codeposition suitability for industrialized production:
The procedure of processing of the high silicon strip of magnetron sputtering double-surface codeposition suitability for industrialized production includes:
The first step: prepared silicon target
Target is a polysilicon, thickness 6mm * length 300mm * width 300mm, and boss 161 sizes that are provided with in target size and the cathode cap 106 are suitable;
Second step: silicon strip is installed
One end of 35WW270 low-silicon steel band is installed on the Abrollhaspel 2, and the other end is installed in reeling machine 7 in turn behind welding machine 3, preheating chamber 4, magnetron sputtering chamber 1, diffuser casing 5, cooling room 6;
The 3rd step: adjust magnetron sputtering chamber
In magnetron sputtering chamber 1, be centrosymmetry, respectively put 18 negative electrode targets up and down with the 35WW270 silicon strip; More than the given condition of table is controlled;
The 4th step: table is adjusted the processing conditions of preheating chamber 4, diffuser casing 5, cooling room 6 on the foundation;
The 5th step: adjust Abrollhaspel 2 and transmit the high silicon strip of system with speed 8m/h at the uniform velocity;
The 6th step: through reeling machine 7 package one-tenth dishes.
The high silicon strip that the 5th step is made detects through EDS energy spectrometer and electron probe micro-analysis, and high silicon strip section reaches 6.65wt% at the Si of upper layer content, and high silicon strip center Si content reaches 6.42wt%, and Si content presents uniform distribution substantially in zone face.Its soft magnetic performance B after testing
s=1.80T, P
10/50=0.48W/Kg, P
10/400=9.85W/Kg.
Embodiment 3:
On 35WW440 low-silicon steel band, make high silicon strip
At upper and lower double-sided deposition purity 99.9% silicon materials of 35WW440 low-silicon steel band, the depositing silicon material thickness is 20 μ m.
The condition such as the following table of the high silicon strip of magnetron sputtering double-surface codeposition suitability for industrialized production:
The procedure of processing of the high silicon strip of magnetron sputtering double-surface codeposition suitability for industrialized production includes:
The first step: prepared silicon target
Target is a polysilicon, thickness 6mm * length 300mm * width 300mm, and boss 161 sizes that are provided with in target size and the cathode cap 106 are suitable;
Second step: silicon strip is installed
One end of 35WW440 low-silicon steel band is installed on the Abrollhaspel 2, and the other end is installed in reeling machine 7 in turn behind welding machine 3, preheating chamber 4, magnetron sputtering chamber 1, diffuser casing 5, cooling room 6;
The 3rd step: adjust magnetron sputtering chamber
In magnetron sputtering chamber 1, be centrosymmetry, respectively put 18 negative electrode targets up and down with the 35WW440 silicon strip; More than the given condition of table is controlled;
The 4th step: table is adjusted the processing conditions of preheating chamber 4, diffuser casing 5, cooling room 6 on the foundation;
The 5th step: adjust Abrollhaspel 2 and transmit the high silicon strip of system with speed 8m/h at the uniform velocity;
The 6th step: through reeling machine 7 package one-tenth dishes.
The high silicon strip that the 5th step is made detects through EDS energy spectrometer and electron probe micro-analysis, and high silicon strip section reaches 5.2wt% at the Si of upper layer content, and high silicon strip center Si content reaches 5.15wt%, and Si content presents uniform distribution substantially in zone face.Its soft magnetic performance B after testing
s=1.88T, P
10/50=0.80W/Kg, P
10/400=13.05W/Kg.
Claims (5)
1, a kind of suitability for industrialized production system that adopts the high silicon strip of magnetron sputtering continuous two-sided codeposition technology system, it is characterized in that: this high-silicon steel thin plate suitability for industrialized production system is uncoiled machine (2) from low silicon steel thin plate and sends into production system and begin to end to making the high-silicon steel thin bundle that hardens, and the order of equipment is welding machine (3), preheating chamber (4), magnetron sputtering chamber (1), diffuser casing (5), cooling room (6), reeling machine (7) on the production line;
Preheating chamber (4) is used for low silicon steel thin plate (1a) is heated, and makes low silicon steel thin plate (1a) obtain uniform 200～300 ℃ and carries temperature; The Heating temperature that preheating chamber (4) provides is 200～300 ℃, effectively heated length 2～10m;
Magnetron sputtering chamber (1) is used at continuous codeposition silicon materials of the upper and lower while of fs thin plate (1A);
The fabrication process condition of magnetron sputtering chamber (1):
(A) number, the layout type of the negative electrode target in the magnetron sputtering chamber (1) are set; Described layout type is the staggered relatively or negative electrode target intersection placement of negative electrode target;
(B) to magnetron sputtering chamber (1) suction to 1.0 * 10
-3～8.0 * 10
-4Pa;
(C) charge into argon gas, the sputtering pressure that keeps magnetron sputtering chamber (1) is at 0.5～2.0Pa;
(D) sparking voltage 300～600V, current density 5～60mA, the sedimentation rate of single negative electrode target is 0.2～1.2 μ m/min in the adjusting magnetron sputtering chamber (1);
The target surface spacing h of two groups of negative electrode targets about in the magnetron sputtering chamber (1)
0=60～180mm, the spacing d of adjacent two negative electrode targets in the same side
0=300～500mm, the entire length L=5～30m of magnetron sputtering chamber (1);
Diffuser casing (5) is used for subordinate phase thin plate (1B) is heat-treated under 1000～1250 ℃ of hot environments, and the thermal treatment temp that diffuser casing (5) provides is 1000～1250 ℃, effectively heated length 5～20m;
Cooling room (6) is used for phase III thin plate (1C) is cooled off; The cooling temperature that cooling room (5) provides is 200～500 ℃, refrigerated area length 2～10m;
Continuous production speed v=1～50m/h that Abrollhaspel (2) provides;
Winder (7) is used for cooled high-silicon steel thin plate (1b) is carried out package one-tenth dish.
2, the suitability for industrialized production system of the high silicon strip of employing according to claim 1 magnetron sputtering continuous two-sided codeposition technology system, it is characterized in that: the negative electrode target includes cover plate (101) in the magnetron sputtering chamber (1), permanent magnet (102), magnetic boots (103), cathode sheath (104), cathode cap (106), outer cover (105), permanent magnet (102) is positioned at the central position of magnetic boots (103), magnetic boots (103) are sleeved in the cathode sheath (104), cathode sheath (104) outer cover is equipped with outer cover (105), the bottom of outer cover (105) is connected with cathode cap (106), the inside of cathode cap (106) is provided with boss (161), is placed with target (110) on the boss (161); Gasket (107) is arranged between the upper end of cover plate (101) and cathode sheath (104), and cover plate (101) is provided with prosopyle (111), posticum (112), and prosopyle (111), posticum (112) are communicated with the water coolant of outside respectively by pipeline.
3, the suitability for industrialized production system of the high silicon strip of employing according to claim 1 magnetron sputtering continuous two-sided codeposition technology system is characterized in that: the negative electrode target is arranged as staggered relatively or intersection dislocation placement in the magnetron sputtering chamber (1).
4, the suitability for industrialized production system of the high silicon strip of employing according to claim 1 magnetron sputtering continuous two-sided codeposition technology system is characterized in that: total number of negative electrode target is 6～60 in the magnetron sputtering chamber (1).
5, the suitability for industrialized production system of the high silicon strip of employing according to claim 1 magnetron sputtering continuous two-sided codeposition technology system, it is characterized in that: production line can carry out the deposition diffusion of silicone content less than the low silicon silicon steel sheet of 0.35mm to thickness, and diffusion back silicone content is 5～8wt%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102485955A (en) * | 2010-12-02 | 2012-06-06 | 兰州大成科技股份有限公司 | Method for preparing thin silicon steel strip through vacuum film plating |
| CN102978569A (en) * | 2012-12-18 | 2013-03-20 | 兰州大成科技股份有限公司 | Method for preparing alloy thin plate with Fe, 5.5-6.5% by weight of Si and 0.3-1.0% by weight of Al by adopting continuous multi-arc ion plating physical vapor deposition |
| CN106319468A (en) * | 2016-11-03 | 2017-01-11 | 安徽富芯微电子有限公司 | Method for increasing quality of magnetron sputtering coating |
| CN107282928A (en) * | 2017-07-17 | 2017-10-24 | 贵州理工学院 | Powder Diffusion prepares the method and device of high-silicon steel thin strip under magnetic field |
| CN110004419A (en) * | 2019-02-28 | 2019-07-12 | 武汉理工大学 | A method of Fe-Si film is prepared using non-balance magnetically controlled sputter technology |
| CN110592552A (en) * | 2019-09-03 | 2019-12-20 | 肇庆宏旺金属实业有限公司 | Steel coil titanizing process |
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2008
- 2008-07-08 CN CN200810116253XA patent/CN101319306B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102485955A (en) * | 2010-12-02 | 2012-06-06 | 兰州大成科技股份有限公司 | Method for preparing thin silicon steel strip through vacuum film plating |
| CN102978569A (en) * | 2012-12-18 | 2013-03-20 | 兰州大成科技股份有限公司 | Method for preparing alloy thin plate with Fe, 5.5-6.5% by weight of Si and 0.3-1.0% by weight of Al by adopting continuous multi-arc ion plating physical vapor deposition |
| CN106319468A (en) * | 2016-11-03 | 2017-01-11 | 安徽富芯微电子有限公司 | Method for increasing quality of magnetron sputtering coating |
| CN107282928A (en) * | 2017-07-17 | 2017-10-24 | 贵州理工学院 | Powder Diffusion prepares the method and device of high-silicon steel thin strip under magnetic field |
| CN107282928B (en) * | 2017-07-17 | 2023-05-09 | 贵州理工学院 | Method and device for preparing high-silicon steel thin strip by powder diffusion method under magnetic field |
| CN110004419A (en) * | 2019-02-28 | 2019-07-12 | 武汉理工大学 | A method of Fe-Si film is prepared using non-balance magnetically controlled sputter technology |
| CN110592552A (en) * | 2019-09-03 | 2019-12-20 | 肇庆宏旺金属实业有限公司 | Steel coil titanizing process |
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