CN104624642A - Method for rolling large unit-weight and wide molybdenum plates for sputtering target material - Google Patents
Method for rolling large unit-weight and wide molybdenum plates for sputtering target material Download PDFInfo
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- CN104624642A CN104624642A CN201510013786.5A CN201510013786A CN104624642A CN 104624642 A CN104624642 A CN 104624642A CN 201510013786 A CN201510013786 A CN 201510013786A CN 104624642 A CN104624642 A CN 104624642A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
- B21B1/30—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a non-continuous process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B15/00—Arrangements for performing additional metal-working operations specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/74—Temperature control, e.g. by cooling or heating the rolls or the product
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B9/00—Measures for carrying out rolling operations under special conditions, e.g. in vacuum or inert atmosphere to prevent oxidation of work; Special measures for removing fumes from rolling mills
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Abstract
The invention discloses a method for rolling large unit-weight and wide molybdenum plates for a sputtering target material. The method includes the steps that firstly, a powder metallurgy sintering molybdenum plate blank is taken and heated to the temperature of 1485 DEG C to 1495 DEG C, second-heating-number and six-pass hot rolling is conducted at the rolling speed of 48-52 m/min, and the molybdenum plate A is obtained; secondly, the molybdenum plate is taken, three-pass cold rolling is conducted at the rolling speed of 38-42 m/min, annealing is conducted, and the molybdenum plate B is obtained; thirdly, the molybdenum plate B is taken and heated to the temperature of 845-855 DEG C and is rolled at the rolling speed of 90-100 m/min, afterwards, flattening is conducted, and the molybdenum plate B is obtained. According to the method for rolling the large unit-weight and wide molybdenum plates for the sputtering target material, obtained finished molybdenum plate strip products are large in specification, high in purity and density, small in grain gap and uniform in density, the average grain size is small, aeolotropic small grains are even, the surface flatness is high, the good surface quality and the good use performance are achieved, the requirements for the specification and the use performance of the sputtering molybdenum target material for manufacturing large and high-elaboration LCD panels are met, and the method is suitable for application and popularization.
Description
Technical field
The invention belongs to molybdenum plate rolling technical field, be specifically related to the milling method of a kind of sputtering target material with large substance wide cut molybdenum plate band.
Background technology
In recent years, China's electronics and information industry developed rapidly, and one of greatest requirements area becoming thin film sputtering target in the world gradually, this great market also must receive the very big concern of Ge great sputtering target material manufacturing firm in the world.The development of flat-panel screens size, requires that deposit substrate is towards maximization future development.The greatest problem that target manufacturing firm faces how to guarantee the microstructure of large-size sputtering target material and the homogeneity of tissue and avoids producing defect.Particularly the uniformity of the microstructure of sputtering target material all has a great impact for rate of film build, the quality of deposition film and the thickness distribution etc. during sputtering.Under this huge market demand pulls, much be engaged in metallurgy, electronic material manufacturing enterprise, great attention is given to this, and drop into the research and development that a large amount of manpower financial capacity is engaged in the rolling of large gauge sputtering target material wide cut molybdenum ribbon, to the performance by improving sputtering target material molybdenum ribbon, reach the object obtaining optimum sputtered film material and large-scale flat-panel screens.
Large substance wide cut molybdenum plate generally refers to production board more than substance 100kg, and width is greater than the molybdenum plate of 1000mm.Its effect is mainly reflected in military project and civilian two aspects, and except national defense construction uses, the aspect such as flat-panel screens, solid state lighting, nuclear power, generating, computer circuits is all widely used.But the actual production of domestic molybdenum plate rolling processing enterprise is started late, and rolling technique is delayed, and production scale is little.For processing the molybdenum plate band of sputtering target material on market, specification is less than 80kg compared with little, short of width 800mm, substance, average grain size is large, density is low; And not through smooth, molybdenum plate surface quality and glacing flatness lower.Molybdenum plate bandwidth is not enough, density is uneven, microstructure is uneven, surface flatness is poor, has had a strong impact on the quality of the sputtering target material processed, specification and serviceability, governs the expansion in the extension product field of material based on molybdenum plate band; The molybdenum plate bandwidth rolled out, thickness, weight, purity, density, Microstructure Uniformity, average grain size size, specific die orientation etc., affect specification size, the serviceability of maximization and high-precision refinement LCD manufacture sputtering molybdenum target material, and then have influence on the specification size, picture quality, service life, cost price etc. of produced LCD display, govern the product quality of large-scale flat-panel screens.
Summary of the invention
The object of this invention is to provide the milling method of a kind of sputtering target material with large substance wide cut molybdenum plate band, solve the problem that molybdenum plate band specification is too little compared with little, short of width, substance, crystal grain gap is large, density is uneven, average grain size is too little, surface flatness is low prepared by prior art.
In order to realize above object, the technical solution adopted in the present invention is: a kind of sputtering target material milling method of large substance wide cut molybdenum plate band, comprises the following steps:
1) cogging: get powder metallurgy sintered molybdenum plate blank, is heated to 1485 ~ 1495 DEG C, and carry out two fire time six passage hot rollings with the mill speed of 48 ~ 52m/min, air cooling, alkali cleaning, obtains molybdenum plate A;
2) cold rolling: to get step 1) gained molybdenum plate A, carry out three passages with the mill speed of 38 ~ 42m/min cold rolling, annealing, obtains molybdenum plate B;
3) smooth: to get step 2) gained molybdenum plate B, be heated to 845 ~ 855 DEG C, be rolled with the mill speed of 90 ~ 100m/min, after carry out smooth, to obtain final product.
Step 1) in, described powder metallurgy sintered molybdenum plate blank comprises the component of following mass percent: Si 0.003%, Ca 0.002%, Mg 0.002%, P 0.001%, C 0.02%, O 0.003%, N 0.003%, surplus is Mo.
Step 1) in, described two fiery six passage hot rollings carry out three road rollings after often fire is heated to 1485 ~ 1495 DEG C, and wherein three passes of first fiery time are along parallel direction rolling, the three passes vertically tandem rolling of second fiery time.
Step 1) in, in described two fire time six passage hot rollings, the deformation rate of the first passage and four-pass rolling is 35% ~ 40%, second, third, the 5th, the deformation rate of the 6th passes is 25% ~ 30%.
Step 1) in, carry out preheating in a hydrogen atmosphere to molybdenum plate blank before described two fire time six passage hot rollings, described preheat temperature is 1485 ~ 1495 DEG C, and preheating time is 59 ~ 61min.
Step 1) in, carry out preheating to roll used before described two fire time six passage hot rollings, preheat temperature is 295 ~ 305 DEG C.
Step 1) before described two fire time six passage hot rollings, first by molybdenum plate blank grinder buffing, dispose the oxide skin on molybdenum plate blank surface.Polishing time controling is within 2min.After cleaning out, rapidly molybdenum plate blank is pushed roll.
In described two fire time six passage course of hot rolling, after the first fire time three passage hot rollings, before the second fire time three passage hot rollings, shear treatment is carried out to the head of molybdenum plate.This shear treatment effectively can control the layering of molybdenum plate peeling, obtains good surface quality.
Step 1) in, described alkali cleaning be by air cooling after molybdenum plate clean in molten state alkali.Wash after alkali cleaning, then use grinder buffing oxide skin and crackle.
The alkali that described alkali cleaning uses is NaOH.
Step 2) in, before described three passages are cold rolling, to step 1) gained molybdenum plate A carries out annealing in process; Described annealing in process is that after molybdenum plate A being heated to 895 ~ 905 DEG C of insulation 59 ~ 61min, air cooling is to room temperature.
Herein as being heated to 800 DEG C of annealing, molybdenum plate initial recrystallization, rolling stress starts to eliminate, but hardness, intensity are still very high, have larger resistance of deformation; Easily there is raw edges phenomenon in the molybdenum plate after cold rolling, trim losses is up to more than 35%.As being heated to more than 1000 DEG C annealing, all there is recrystallization in molybdenum plate, coarse grains, molybdenum plate embrittlement, and break serious, under less average pass reduction, lumber recovery is lower.According to production experience, molybdenum plate is heated to 895 ~ 905 DEG C of annealing, and recrystallization rate is about 30%, and crystal grain is still tiny does not grow up, and machining stress is effectively eliminated, smoothly cold rolling, and yield rate is high.
Step 2) in, in described cold-rolled process, the thickness of every time rolling pressure accounts for 18% ~ 22% of the front gross thickness of pressure.
Step 2) described cold rolling for tandem rolling.In tandem rolling process, require the reduction in pass that draught pressure keeps certain, to increase molybdenum plate band mechanical strength; Layering, cracking phenomena can not be there is in requirement.
Step 2) in, the annealing after cold rolling is in a hydrogen atmosphere, and after being heated to 895 ~ 905 DEG C of insulation 55 ~ 65min, air cooling is to room temperature.
Step 3) in, the deformation rate of described rolling is 1% ~ 2%.
Step 3) before described rolling, in a hydrogen atmosphere, by step 2) gained molybdenum plate B carries out preheating, preheat temperature is 845 ~ 855 DEG C, and preheating time is 39 ~ 41min.
Step 3) in, described smooth speed is less than 90m/min.
The backing roll of described smooth planisher is plain-barreled roll, and cylindricity is 0.01mm; The cylindricity of working roll is 0.005mm, and roughness is 0.4; In top roll, height is 0.004mm, and lower roll is plain-barreled roll, and two roller diameter deviations are 0.01mm.
The purging system of described planisher inlet location, adopts instrument supply gas.Water content and the impurity of instrument supply gas are few, reduce the dirt of molybdenum plate belt surface.
In formation process, by production and processing monitoring, control the roll change cycle.Roll rolling time is long, the serious uneven wear of roll surface, and roll crown reduces too many, may cause flatness defect.
The sputtering target material of the present invention milling method of large substance wide cut molybdenum plate band, with powder metallurgy sintered molybdenum plate blank for raw material, carries out cogging, cold rolling and smooth successively, by many fire time multi-pass tandem rollings, gained sputtering target material is comparatively large with large substance wide cut molybdenum plate band trimmed size, and width is greater than 1000mm, more than substance 100kg, purity is high, and density is large, and crystal grain gap is little, density is even, average grain size is little, and the little crystal grain of anisotropy is even, and surface flatness is high; Gained molybdenum plate belt surface is smooth, and smooth rate improves more than 70% than common molybdenum plate, and surface cleanness improves more than 90%; Gained molybdenum plate band has excellent surface quality and serviceability, meet and to maximize and high-precision refinement LCD manufacture sputters the requirement of molybdenum target material to specification and serviceability, with the sputtering target material that this molybdenum plate band processes, target service efficiency improves more than 40%, rate of film build during sputtering improves more than 10%, the comprehensive quality of deposition film improves 30%, thickness distribution evening ratio improves more than 20%, improve the specification of produced LCD display, image quality and service life, reduce production cost, be applicable to applying.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further illustrated.
In detailed description of the invention, powder metallurgy sintered molybdenum plate blank used is commercial goods, purchased from Luanchuanmolybdenum company.
Embodiment 1
The sputtering target material milling method of large substance wide cut molybdenum plate band of the present embodiment, comprises the following steps:
1) cogging:
Get powder metallurgy sintered molybdenum plate blank, specification 87mm × 550mm × 450mm, density 9.6g/cm
3, substance is about 206kg; Described powder metallurgy sintered molybdenum plate blank comprises the component of following mass percent: Si 0.003%, Ca 0.002%, Mg 0.002%, P 0.001%, C 0.02%, O 0.003%, N 0.003%, and surplus is Mo;
Molybdenum plate blank is put into 450kw Medium Frequency Induction Heating Furnace, under hydrogen shield atmosphere, be heated to 1490 DEG C and carry out preheating, preheating time is 60min;
Molybdenum plate blank after preheating is placed on ф 800mm × 1200mm bis-roller unidirectional type hot-rolling mill, carries out two fire time six passage hot rollings with the mill speed of 50m/min; Carry out online preheating before roll rolling used, preheat temperature is 300 DEG C;
Before molybdenum plate blank enters roll, first by molybdenum plate blank grinder buffing, dispose the oxide skin on molybdenum plate blank surface; Molybdenum plate blank, within 2min, after cleaning out, is pushed roll rapidly by polishing time controling;
Described two fiery six passage hot rollings carry out three road rollings after often fire is heated to 1490 DEG C, and wherein three passes of first fiery time are along parallel direction rolling, the three passes vertically tandem rolling of second fiery time;
In described two fire time six passage course of hot rolling, the first passage after time heating of every fire, i.e. the deformation rate of the first passage and four-pass rolling is 35% ~ 40%; Second, third, the 5th, the deformation rate of the 6th passes is 25% ~ 30%; The thickness of the present embodiment is the molybdenum plate blank of 87 ± 0.2mm, and drafts is as shown in table 1 below:
Every time pressure scale of split rolling method in table 1 embodiment 1
| Passage | 1 | 2 | 3 | 4 | 5 | 6 |
| Supplied materials thickness (mm) | 87.00 | 56.55 | 42.41 | 31.81 | 19.09 | 13.36 |
| Finished product thickness (mm) | 56.55 | 42.41 | 31.81 | 19.09 | 13.36 | 10.00 |
| Absolute draft amount (%) | 30.45 | 14.14 | 10.60 | 12.72 | 5.73 | 3.36 |
| Relative reduction (%) | 35.00 | 25.00 | 25.00 | 40.00 | 30.00 | 25.15 |
| General working rate (%) before final pass | 0.00 | 35.00 | 51.25 | 63.44 | 78.06 | 84.64 |
| General working rate (%) after final pass | 35.00 | 51.25 | 63.44 | 78.06 | 84.64 | 88.51 |
In described two fire time six passage course of hot rolling, maintenance mill speed is 50m/min;
After the first fire time three passage hot rollings, before the second fire time three passage hot rollings, shear treatment is carried out to the head of molybdenum plate, effectively control the layering of molybdenum plate peeling, obtain good surface quality;
6th passes terminates rear air cooling, after cleaning molybdenum plate, rinses, with grinder buffing oxide skin and crackle, after trimming shaping, obtain the molybdenum plate A of long 1800mm × wide 1000mm × thick 10mm with water in molten state alkali pond;
2) cold rolling:
Getting step 1) gained molybdenum plate A carries out annealing in process, puts into 450kw Medium Frequency Induction Heating Furnace by molybdenum plate A, and under hydrogen shield atmosphere, after being heated to 900 DEG C of insulation 60min, air cooling is to room temperature;
Molybdenum plate after annealing in process is placed in 1200mm 4-roller reversible cold rolling mill group, carries out three passages with the mill speed of 40m/min and intersect cold rolling;
In cold-rolled process, the thickness of every time rolling pressure accounts for 18% ~ 22% of the front gross thickness of pressure; In tandem rolling process, require the reduction in pass that draught pressure keeps certain, to increase molybdenum plate band mechanical strength, occur without layering, cracking phenomena; The thickness of the present embodiment is the molybdenum plate material that 10 ± 0.1mm is thick, and drafts is as shown in table 2:
Every time pressure scale in cold-rolled process in table 2 embodiment 1
| Passage | 1 | 2 | 3 |
| Supplied materials thickness (mm) | 10.00 | 7.90 | 6.32 |
| Finished product thickness (mm) | 7.90 | 6.32 | 5.00 |
| Absolute draft amount (%) | 2.10 | 1.58 | 1.32 |
| Relative reduction (%) | 21.00 | 20.00 | 20.89 |
| General working rate (%) before final pass | 0.00 | 21.00 | 36.80 |
| General working rate (%) after final pass | 21.00 | 36.80 | 50.00 |
In cold-rolled process, maintenance mill speed is 40m/min;
After 3rd passes terminates, through annealing process process, obtain the molybdenum plate B of long 3200mm × wide 1000mm × thick 4.5mm; Described annealing in process is in a hydrogen atmosphere, and after being heated to 900 DEG C of insulation 60min, air cooling is to room temperature;
3) smooth:
Get step 2) gained molybdenum plate B, put into 450kw Medium Frequency Induction Heating Furnace, under hydrogen shield atmosphere, be heated to 850 DEG C and carry out preheating, preheating time is 40min;
Be rolled with the mill speed of 90m/min by molybdenum plate after preheating, rolling deformation rate controls 2%;
Molybdenum plate after rolling is placed in the reversible planisher of 1200mm tetra-roller carries out smooth; The backing roll of planisher used is plain-barreled roll, and cylindricity is 0.01mm; The cylindricity of working roll is 0.005mm, and roughness is 0.4; In top roll, height is 0.004mm, and lower roll is plain-barreled roll, and two roller diameter deviations are 0.01mm; Improve the purging system of planisher inlet location, increase by row's nozzle, the angle between nozzle blowing direction and molybdenum plate is 145 °, adopts water content and the few instrument supply gas of impurity, reduces the dirt of molybdenum plate belt surface;
In formation process, the smooth speed controlling planisher is 85m/min, reduces the appearance of vibration line;
In formation process, by production and processing monitoring, control the roll change cycle; Roll rolling time is long, the serious uneven wear of roll surface, and roll crown reduces too many, may cause flatness defect.
Smooth complete after, obtain the large substance wide cut molybdenum plate band finished product of sputtering target material.
Embodiment 2
The sputtering target material milling method of large substance wide cut molybdenum plate band of the present embodiment, comprises the following steps:
1) cogging:
Get powder metallurgy sintered molybdenum plate blank, specification 87mm × 550mm × 450mm, density 9.6g/cm
3, substance is about 206kg; Described powder metallurgy sintered molybdenum plate blank comprises the component of following mass percent: Si 0.003%, Ca 0.002%, Mg 0.002%, P 0.001%, C 0.02%, O 0.003%, N 0.003%, and surplus is Mo;
Molybdenum plate blank is put into 450kw Medium Frequency Induction Heating Furnace, under hydrogen shield atmosphere, be heated to 1485 DEG C and carry out preheating, preheating time is 61min;
Molybdenum plate blank after preheating is placed on ф 800mm × 1200mm bis-roller unidirectional type hot-rolling mill, carries out two fire time six passage hot rollings with the mill speed of 48m/min; Carry out online preheating before roll rolling used, preheat temperature is 295 DEG C;
Before molybdenum plate blank enters roll, first by molybdenum plate blank grinder buffing, dispose the oxide skin on molybdenum plate blank surface; Molybdenum plate blank, within 2min, after cleaning out, is pushed roll rapidly by polishing time controling;
Described two fiery six passage hot rollings carry out three road rollings after often fire is heated to 1485 DEG C, and wherein three passes of first fiery time are along parallel direction rolling, the three passes vertically tandem rolling of second fiery time;
In described two fire time six passage course of hot rolling, the first passage after time heating of every fire, i.e. the deformation rate of the first passage and four-pass rolling is 35% ~ 40%; Second, third, the 5th, the deformation rate of the 6th passes is 25% ~ 30%; The thickness of the present embodiment is the molybdenum plate blank of 87 ± 0.2mm, and drafts is as shown in table 3 below:
Every time pressure scale of split rolling method in table 3 embodiment 2
| Passage | 1 | 2 | 3 | 4 | 5 | 6 |
| Supplied materials thickness (mm) | 87.00 | 52.20 | 39.15 | 29.36 | 19.08 | 13.36 |
| Finished product thickness (mm) | 52.20 | 39.15 | 29.36 | 19.08 | 13.36 | 10.00 |
| Absolute draft amount (%) | 34.80 | 13.05 | 9.79 | 10.28 | 5.72 | 3.36 |
| Relative reduction (%) | 40.00 | 25.00 | 25.00 | 35.00 | 30.00 | 25.15 |
| General working rate (%) before final pass | 0.00 | 40.00 | 55.52 | 66.25 | 78.07 | 84.64 |
| General working rate (%) after final pass | 40.00 | 55.52 | 66.25 | 78.07 | 84.64 | 88.51 |
In described two fire time six passage course of hot rolling, maintenance mill speed is 48m/min;
After the first fire time three passage hot rollings, before the second fire time three passage hot rollings, shear treatment is carried out to the head of molybdenum plate, effectively control the layering of molybdenum plate peeling, obtain good surface quality;
6th passes terminates rear air cooling, after cleaning molybdenum plate, rinses, with grinder buffing oxide skin and crackle, after trimming shaping, obtain the molybdenum plate A of long 1800mm × wide 1000mm × thick 10mm with water in molten state alkali pond;
2) cold rolling:
Getting step 1) gained molybdenum plate A carries out annealing in process, puts into 450kw Medium Frequency Induction Heating Furnace by molybdenum plate A, and under hydrogen shield atmosphere, after being heated to 905 DEG C of insulation 59min, air cooling is to room temperature;
Molybdenum plate after annealing in process is placed in 1200mm 4-roller reversible cold rolling mill group, carries out three passages with the mill speed of 40m/min and intersect cold rolling;
In cold-rolled process, the thickness of every time rolling pressure accounts for 18% ~ 22% of the front gross thickness of pressure; In tandem rolling process, require the reduction in pass that draught pressure keeps certain, to increase molybdenum plate band mechanical strength, occur without layering, cracking phenomena; The thickness of the present embodiment is the molybdenum plate material that 10 ± 0.1mm is thick, and drafts is as shown in table 4:
Every time pressure scale in cold-rolled process in table 4 embodiment 2
| Passage | 1 | 2 | 3 |
| Supplied materials thickness (mm) | 10.00 | 8.00 | 6.40 |
| Finished product thickness (mm) | 8.00 | 6.40 | 5.00 |
| Absolute draft amount (%) | 2.00 | 1.60 | 1.40 |
| Relative reduction (%) | 20.00 | 20.00 | 21.88 |
| General working rate (%) before final pass | 0.00 | 21.00 | 36.00 |
| General working rate (%) after final pass | 20.00 | 36.00 | 50.00 |
In cold-rolled process, maintenance mill speed is 42m/min;
After 3rd passes terminates, through annealing process process, obtain the molybdenum plate B of long 3200mm × wide 1000mm × thick 4.5mm; Described annealing in process is in a hydrogen atmosphere, and after being heated to 895 DEG C of insulation 65min, air cooling is to room temperature;
3) smooth:
Get step 2) gained molybdenum plate B, put into 450kw Medium Frequency Induction Heating Furnace, under hydrogen shield atmosphere, be heated to 845 DEG C and carry out preheating, preheating time is 41min;
Be rolled with the mill speed of 95m/min by molybdenum plate after preheating, rolling deformation rate controls 1.5%;
Molybdenum plate after rolling is placed in the reversible planisher of 1200mm tetra-roller carries out smooth; The backing roll of planisher used is plain-barreled roll, and cylindricity is 0.01mm; The cylindricity of working roll is 0.005mm, and roughness is 0.4; In top roll, height is 0.004mm, and lower roll is plain-barreled roll, and two roller diameter deviations are 0.01mm; Improve the purging system of planisher inlet location, increase by row's nozzle, the angle between nozzle blowing direction and molybdenum plate is 145 °, adopts water content and the few instrument supply gas of impurity, reduces the dirt of molybdenum plate belt surface;
In formation process, the smooth speed controlling planisher is 80m/min, reduces the appearance of vibration line;
In formation process, by production and processing monitoring, control the roll change cycle; Roll rolling time is long, the serious uneven wear of roll surface, and roll crown reduces too many, may cause flatness defect.
Smooth complete after, obtain the large substance wide cut molybdenum plate band finished product of sputtering target material.
Embodiment 3
The sputtering target material milling method of large substance wide cut molybdenum plate band of the present embodiment, comprises the following steps:
1) cogging:
Get powder metallurgy sintered molybdenum plate blank, specification 87mm × 550mm × 450mm, density 9.6g/cm
3, substance is about 206kg; Described powder metallurgy sintered molybdenum plate blank comprises the component of following mass percent: Si 0.003%, Ca 0.002%, Mg 0.002%, P 0.001%, C 0.02%, O 0.003%, N 0.003%, and surplus is Mo;
Molybdenum plate blank is put into 450kw Medium Frequency Induction Heating Furnace, under hydrogen shield atmosphere, be heated to 1495 DEG C and carry out preheating, preheating time is 59min;
Molybdenum plate blank after preheating is placed on ф 800mm × 1200mm bis-roller unidirectional type hot-rolling mill, carries out two fire time six passage hot rollings with the mill speed of 52m/min; Carry out online preheating before roll rolling used, preheat temperature is 305 DEG C;
Before molybdenum plate blank enters roll, first by molybdenum plate blank grinder buffing, dispose the oxide skin on molybdenum plate blank surface; Molybdenum plate blank, within 2min, after cleaning out, is pushed roll rapidly by polishing time controling;
Described two fiery six passage hot rollings carry out three road rollings after often fire is heated to 1495 DEG C, and wherein three passes of first fiery time are along parallel direction rolling, the three passes vertically tandem rolling of second fiery time;
In described two fire time six passage course of hot rolling, the first passage after time heating of every fire, i.e. the deformation rate of the first passage and four-pass rolling is 35% ~ 40%; Second, third, the 5th, the deformation rate of the 6th passes is 25% ~ 30%; The thickness of the present embodiment is the molybdenum plate blank of 87 ± 0.2mm, and drafts is as shown in table 5 below:
Every time pressure scale of split rolling method in table 5 embodiment 3
| Passage | 1 | 2 | 3 | 4 | 5 | 6 |
| Supplied materials thickness (mm) | 87.00 | 54.81 | 40.56 | 30.01 | 18.61 | 13.77 |
| Finished product thickness (mm) | 54.81 | 40.56 | 30.01 | 18.61 | 13.77 | 10.00 |
| Absolute draft amount (%) | 32.19 | 14.25 | 10.55 | 11.40 | 4.84 | 3.77 |
| Relative reduction (%) | 37.00 | 26.00 | 26.00 | 38.00 | 26.00 | 27.38 |
| General working rate (%) before final pass | 0.00 | 37.00 | 53.38 | 65.51 | 78.61 | 84.17 |
| General working rate (%) after final pass | 37.00 | 53.38 | 65.51 | 78.61 | 84.17 | 88.51 |
In described two fire time six passage course of hot rolling, maintenance mill speed is 52m/min;
After the first fire time three passage hot rollings, before the second fire time three passage hot rollings, shear treatment is carried out to the head of molybdenum plate, effectively control the layering of molybdenum plate peeling, obtain good surface quality;
6th passes terminates rear air cooling, after cleaning molybdenum plate, rinses, with grinder buffing oxide skin and crackle, after trimming shaping, obtain the molybdenum plate A of long 1800mm × wide 1000mm × thick 10mm with water in molten state alkali pond;
2) cold rolling:
Getting step 1) gained molybdenum plate A carries out annealing in process, puts into 450kw Medium Frequency Induction Heating Furnace by molybdenum plate A, and under hydrogen shield atmosphere, after being heated to 895 DEG C of insulation 61min, air cooling is to room temperature;
Molybdenum plate after annealing in process is placed in 1200mm 4-roller reversible cold rolling mill group, carries out three passages with the mill speed of 40m/min and intersect cold rolling;
In cold-rolled process, the thickness of every time rolling pressure accounts for 18% ~ 22% of the front gross thickness of pressure; In tandem rolling process, require the reduction in pass that draught pressure keeps certain, to increase molybdenum plate band mechanical strength, occur without layering, cracking phenomena; The thickness of the present embodiment is the molybdenum plate material that 10 ± 0.1mm is thick, and drafts is as shown in table 6:
Every time pressure scale in cold-rolled process in table 6 embodiment 3
| Passage | 1 | 2 | 3 |
| Supplied materials thickness (mm) | 10.00 | 8.20 | 6.40 |
| Finished product thickness (mm) | 8.20 | 6.40 | 5.00 |
| Absolute draft amount (%) | 1.80 | 1.80 | 1.40 |
| Relative reduction (%) | 18.00 | 22.00 | 21.88 |
| General working rate (%) before final pass | 0.00 | 18.00 | 36.00 |
| General working rate (%) after final pass | 18.00 | 36.00 | 50.00 |
In cold-rolled process, maintenance mill speed is 38m/min;
After 3rd passes terminates, through annealing process process, obtain the molybdenum plate B of long 3200mm × wide 1000mm × thick 4.5mm; Described annealing in process is in a hydrogen atmosphere, and after being heated to 905 DEG C of insulation 55min, air cooling is to room temperature;
3) smooth:
Get step 2) gained molybdenum plate B, put into 450kw Medium Frequency Induction Heating Furnace, under hydrogen shield atmosphere, be heated to 855 DEG C and carry out preheating, preheating time is 39min;
Be rolled with the mill speed of 100m/min by molybdenum plate after preheating, rolling deformation rate controls 1%;
Molybdenum plate after rolling is placed in the reversible planisher of 1200mm tetra-roller carries out smooth; The backing roll of planisher used is plain-barreled roll, and cylindricity is 0.01mm; The cylindricity of working roll is 0.005mm, and roughness is 0.4; In top roll, height is 0.004mm, and lower roll is plain-barreled roll, and two roller diameter deviations are 0.01mm; Improve the purging system of planisher inlet location, increase by row's nozzle, the angle between nozzle blowing direction and molybdenum plate is 145 °, adopts water content and the few instrument supply gas of impurity, reduces the dirt of molybdenum plate belt surface;
In formation process, the smooth speed controlling planisher is 87m/min, reduces the appearance of vibration line;
In formation process, by production and processing monitoring, control the roll change cycle; Roll rolling time is long, the serious uneven wear of roll surface, and roll crown reduces too many, may cause flatness defect.
Smooth complete after, obtain the large substance wide cut molybdenum plate band finished product of sputtering target material.
Experimental example
The large substance wide cut molybdenum plate carry sample of Example 1 ~ 3 gained sputtering target material carries out Performance Detection, and result is as shown in table 7.
Wherein, comparative example is commercial goods (the hot rolled thin molybdenum plate that Jinduicheng Molybdenum Co., Ltd produces, operative norm: ASTM B386-03, thick 2-5mm, wide 700mm, long 20000mm).
The large substance wide cut molybdenum plate band performance test results of table 7 embodiment 1 ~ 3 gained sputtering target material
Performance test results shows: the large substance wide cut molybdenum plate band of embodiment 1 ~ 3 gained sputtering target material, and structure cell shows subcircular, and the little crystal grain of anisotropy is even, and gap is little; Average crystal grain length 20 μm, reduce 25%, and total amount is less than 10% more than 40 μm of number of die than common molybdenum plate (comparative example); Density is even, improves more than 60% than common molybdenum plate; With the sputtering target material that this molybdenum plate band processes, target service efficiency improves more than 40%; Rate of film build during sputtering improves more than 10%, and the comprehensive quality of deposition film improves 30%, and thickness distribution evening ratio improves more than 20%, molybdenum plate surfacing, and smooth rate improves more than 70% than common molybdenum plate, and surface cleanness improves more than 90%.Result of the test shows: the sputtering target material of the present invention milling method of large substance wide cut molybdenum plate band, gained sputtering target material is larger with large substance wide cut molybdenum plate band trimmed size, purity is high, density is large, crystal grain gap is little, and density is even, and average grain size is little, the little crystal grain of anisotropy is even, and surface flatness is high; There is excellent surface quality and serviceability, meet and to maximize and high-precision refinement LCD manufacture sputters the requirement of molybdenum target material to specification and serviceability.
Claims (10)
1. a sputtering target material milling method for large substance wide cut molybdenum plate band, is characterized in that: comprise the following steps:
1) cogging: get powder metallurgy sintered molybdenum plate blank, is heated to 1485 ~ 1495 DEG C, and carry out two fire time six passage hot rollings with the mill speed of 48 ~ 52m/min, air cooling, alkali cleaning, obtains molybdenum plate A;
2) cold rolling: to get step 1) gained molybdenum plate A, carry out three passages with the mill speed of 38 ~ 42m/min cold rolling, annealing, obtains molybdenum plate B;
3) smooth: to get step 2) gained molybdenum plate B, be heated to 845 ~ 855 DEG C, be rolled with the mill speed of 90 ~ 100m/min, after carry out smooth, to obtain final product.
2. the sputtering target material according to claim 1 milling method of large substance wide cut molybdenum plate band, it is characterized in that: step 1) in, described two fire time six passage hot rollings carry out three road rollings after every fire is heated to 1485 ~ 1495 DEG C, wherein three passes of first fiery time are along parallel direction rolling, the three passes vertically tandem rolling that the second fire is secondary.
3. the sputtering target material according to claim 1 and 2 milling method of large substance wide cut molybdenum plate band, it is characterized in that: step 1) in, in described two fire time six passage hot rollings, the deformation rate of the first passage and four-pass rolling is 35% ~ 40%, second, third, the 5th, the deformation rate of the 6th passes is 25% ~ 30%.
4. the sputtering target material according to claim 1 milling method of large substance wide cut molybdenum plate band, it is characterized in that: step 1) in, before described two fire time six passage hot rollings, in a hydrogen atmosphere preheating is carried out to molybdenum plate blank, described preheat temperature is 1485 ~ 1495 DEG C, and preheating time is 59 ~ 61min.
5. the milling method of large substance wide cut molybdenum plate band of the sputtering target material according to claim 1 or 4, is characterized in that: step 1) in, carry out preheating to roll used before described two fire time six passage hot rollings, preheat temperature is 295 ~ 305 DEG C.
6. the sputtering target material according to claim 1 milling method of large substance wide cut molybdenum plate band, is characterized in that: step 2) in, before described three passages are cold rolling, to step 1) gained molybdenum plate A carries out annealing in process; Described annealing in process is that after molybdenum plate A being heated to 895 ~ 905 DEG C of insulation 55 ~ 65min, air cooling is to room temperature.
7. the milling method of large substance wide cut molybdenum plate band of the sputtering target material according to claim 1 or 6, is characterized in that: step 2) in, in described cold-rolled process, the thickness of every time rolling pressure accounts for 18% ~ 22% of the front gross thickness of pressure.
8. the sputtering target material according to claim 1 milling method of large substance wide cut molybdenum plate band, is characterized in that: step 2) in, the annealing after cold rolling is in a hydrogen atmosphere, and after being heated to 895 ~ 905 DEG C of insulation 55 ~ 65min, air cooling is to room temperature.
9. the sputtering target material according to claim 1 milling method of large substance wide cut molybdenum plate band, is characterized in that: step 3) in, the deformation rate of described rolling is 1% ~ 2%.
10. the sputtering target material according to claim 1 milling method of large substance wide cut molybdenum plate band, is characterized in that: step 3) in, described smooth speed is less than 90m/min.
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| CN106964650A (en) * | 2017-03-24 | 2017-07-21 | 洛阳高新四丰电子材料有限公司 | A kind of rolling mill practice of TFT LCD/AMOLED flat-panel screens wide cut molybdenum target material |
| CN108687158A (en) * | 2018-05-11 | 2018-10-23 | 成都联虹钼业有限公司 | A kind of preparation method of isotropism molybdenum plate |
| CN109848424A (en) * | 2018-12-03 | 2019-06-07 | 有研工程技术研究院有限公司 | A kind of grid pulse travelling-wave tubes aperture plate molybdenum foil and preparation method thereof |
| CN112609162A (en) * | 2020-12-10 | 2021-04-06 | 宁波江丰钨钼材料有限公司 | LCD molybdenum target material and rolling method and application thereof |
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| CN109848424B (en) * | 2018-12-03 | 2021-08-10 | 有研工程技术研究院有限公司 | Molybdenum foil for grid control pulse traveling wave tube grid mesh and preparation method thereof |
| CN112609162A (en) * | 2020-12-10 | 2021-04-06 | 宁波江丰钨钼材料有限公司 | LCD molybdenum target material and rolling method and application thereof |
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