CN104593708A - Preparation method of planar niobium target - Google Patents
Preparation method of planar niobium target Download PDFInfo
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- CN104593708A CN104593708A CN201510020338.8A CN201510020338A CN104593708A CN 104593708 A CN104593708 A CN 104593708A CN 201510020338 A CN201510020338 A CN 201510020338A CN 104593708 A CN104593708 A CN 104593708A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
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Abstract
The invention provides a preparation method of a planar niobium target. The method comprises the following steps: (A) forging a niobium ingot, wherein the forging mode is radial squaring and axial drawing; carrying out acid pickling on the forged niobium ingot, and carrying out thermal treatment on the pickled niobium ingot; (B) forging the niobium ingot obtained in the step (A), wherein the forging mode is flattening forging; carrying out acid pickling on the forged niobium ingot, and carrying out thermal treatment on the pickled niobium ingot; and (C) rolling the niobium ingot obtained in the step (B), and carrying out thermal treatment on the rolled niobium plate to obtain the planar niobium target. Through adoption of forging and rolling modes, a columnar zone and a central isometric crystal zone in the cast ingot and a fine crystal zone near the edge of the niobium ingot are effectively crushed; and meanwhile, the niobium target tissue is relatively uniform through middle thermal treatment and product thermal treatment, so as to obtain a uniform and fine isometric crystal structure.
Description
Technical field
The present invention relates to the preparation method of sputtering target material, particularly relate to a kind of preparation method of plane niobium target.
Background technology
Plane niobium target is mainly used in plated film industry, by energetic particle hits, there is highly purified target material solid plate, clash into atom by physical process, pass into gas to sputtering chamber simultaneously, clash into sputtering the target atom to react, form Coating Materials, and be finally deposited on substrate material, form the film with certain characteristic.
Sputtering target material requires uniform component, suitable particle size and concrete crystallographic orientation, and the high request of above-mentioned sputtering target material is all to obtain uniform film deposition rate over the entire substrate.Niobium target is mainly used in Surface Engineering material, as plated film industries such as boats and ships, chemical industry, liquid-crystal display and heat-resisting, corrosion-resistant high connductivity.Plane niobium target is the niobium target that diameter is more than or equal to 150mm, and it is commonly referred to naked target, and first its back of the body target with copper or aluminium welds by user in use, then sputters, is deposited on by niobium atom on substrate material, realizes sputter coating.In order to realize the homogeneity of plated film, it is brilliant that plane niobium target needs broken niobium ingot to cast, and ensure the perfect recrystallization of plane niobium target interior tissue, grain-size is less than 100 μm, and uniformity.And the method preparing niobium target in prior art still can not meet above-mentioned requirements, this application provides a kind of preparation method of plane niobium target thus.
Summary of the invention
The technical problem that the present invention solves is the preparation method providing a kind of plane niobium target, and plane niobium target prepared by the application has homogeneous microstructure, grain fineness number is less than 100 μm of equiaxed grain structures.
In view of this, this application provides a kind of preparation method of plane niobium target, comprise the following steps:
A), forged by niobium ingot, the mode of described forging is that radial direction beats square shaft to pulling; Niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated;
B), by steps A) the niobium ingot that obtains forges, and the mode of described forging is for flattening forging; Niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated;
C), by step B) the niobium ingot that obtains is rolled, heat-treated by the niobium plate after rolling, obtain plane niobium target.
Preferably, steps A) described in forging working modulus be greater than 50%.
Preferably, step B) described in forging working modulus be greater than 30%.
Preferably, step C) described in the working modulus of rolling be greater than 50%.
Preferably, steps A) described in the feed of forging be 100 ~ 150mm, draught is 40 ~ 60mm.
Preferably, step B) described in the feed of forging be 80 ~ 120mm, draught is 30 ~ 50mm.
Preferably, steps A) with step B) described in the mixing solutions of the hydrofluoric acid of the solution of pickling to be volume ratio be 1:2:3, hydrochloric acid and nitric acid, the concentration of described hydrofluoric acid is 40wt%, and the concentration of described hydrochloric acid is 37wt%, and the concentration of described nitric acid is 65wt%.
Preferably, steps A) described in heat treated temperature be 1000 DEG C ~ 1300 DEG C, described heat treated soaking time is 60 ~ 120min; Step B) described in heat treated temperature be 1000 ~ 1300 DEG C, described heat treated soaking time is 60 ~ 120min; Step C) described in heat treated temperature be 1100 DEG C ~ 1300 DEG C, described heat treated soaking time is 90 ~ 120min.
Preferably, the diameter of described niobium ingot is 150mm ~ 350mm.
This application provides a kind of preparation method of plane niobium target, comprise the following steps: niobium ingot is carried out radial square shaft of beating to the forging pulled out, the niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated; Again niobium ingot is carried out flattening forging, the niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated; Finally niobium ingot is rolled, obtains plane niobium target.The application is in the process of preparation plane niobium target, forging process is the radial side of beating, the mode that axially pulling and flattening are forged combines, make the columnar zone in niobium ingot, effective fragmentation is implemented near Center Equiaxial Crystal district and niobium ingot edge, the metal flow of blank centre portions increases, the degree of irregularity of central tissue obtains remarkable improvement, when multi-direction stressed, its original as cast condition open grain structure is made to obtain multi-faceted abundant fragmentation, thus impel niobium ingot to obtain the relatively uniform tissue of crystal grain, avoiding central part is not implemented into effectively broken and to the follow-up existence leaving over down " crystal zone " adverse tissue such as tissue and open grain structure, niobium ingot is out of shape at rolling sequence evenly, and coordinate middle thermal treatment process after processing, what make niobium target organizes more and more homogenizing, refinement, finally obtains homogeneous microstructure, equiaxed grain structure plane niobium target that grain fineness number is less than 100 μm.
Accompanying drawing explanation
Fig. 1 is the metallograph of niobium target prepared by embodiment 1;
Fig. 2 is the metallograph of niobium target prepared by embodiment 2;
Fig. 3 is the metallograph of niobium target prepared by embodiment 3.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of preparation method of plane niobium target, comprise the following steps:
A), forged by niobium ingot, the mode of described forging is that radial direction beats square shaft to pulling; Niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated;
B), by steps A) the niobium ingot that obtains forges, and the mode of described forging is for flattening forging; Niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated;
C), by step B) the niobium ingot that obtains is rolled, heat-treated by the niobium plate after rolling, obtain plane niobium target.
This application provides a kind of preparation method of plane niobium target.In the process preparing niobium target, the application adopts the mode of forging and combining with rolling, niobium ingot is cast brilliant fully broken, obtains evenly, the microtexture of refinement, finally obtain homogeneous microstructure, equiaxed grain structure plane niobium target that grain fineness number is less than 100 μm.
According to the present invention, described in the application, plane niobium target ingot casting has larger diameter, and diameter is more than or equal to 150mm, is preferably 150mm ~ 350mm, therefore obtains homogeneous microstructure by the preparation method of the application, equiaxed grain structure that grain fineness number is less than 100 μm.First niobium ingot forges by the application.Above-mentioned niobium ingot the application has no particular limits, and prepares according to side well known to those skilled in the art.In forging process, described niobium ingot is carried out the forging mode that radial beat side and axis pull out by the application, and to make the columnar zone of niobium ingot, the fine grained region of Center Equiaxial Crystal district and niobium ingot adjacent edges obtains effective fragmentation.The working modulus of the process forging of this time forging is greater than 50%, is enough to ensure that niobium ingot casting crystalline substance is able to abundant fragmentation, and the metal fluidity of centre portions increases, and degree of irregularity significantly improves.The working modulus of described forging is preferably 55% ~ 75%.Obtain to make niobium ingot and be out of shape comparatively uniformly, when pulling operates, the feed entrance point before and after should making during each time compression staggers mutually.Described in the application, the number of times of the radial side of beating, axially pulling is preferably 1 ~ 2 time.The feed of described forging is preferably 100 ~ 150mm, and draught is preferably 40 ~ 60mm.In order to eliminate the impurity that in forging process, surface produces, niobium ingot after forging is carried out pickling by the application, the solution of described pickling is preferably the mixing solutions of hydrofluoric acid, hydrochloric acid and the nitric acid that volume ratio is 1:2:3, wherein the concentration of hydrofluoric acid is 40wt%, the concentration of hydrochloric acid is 37wt%, and the concentration of nitric acid is 65wt%.In order to eliminate the unrelieved stress in forging process, niobium ingot after pickling is heat-treated by the application, and described heat treated temperature is preferably 1000 DEG C ~ 1300 DEG C, is more preferably 1100 DEG C ~ 1200 DEG C, described heat treated soaking time is preferably 60 ~ 120min, is more preferably 75min ~ 90min.
Niobium ingot then forges by the application, described in be forged to flatten forging.Niobium ingot described in the application through radial beat side, axially pulling and flattening forge, make niobium ingot when multi-direction stressed, niobium ingot original as cast condition open grain structure obtains multi-faceted fragmentation, thus is conducive to niobium ingot and obtains uniform grain structure.Described working modulus of flattening forging is preferably greater than 30%, is more preferably 35% ~ 55%.The number of times of the flat forging of described bat is preferably 1 ~ 2 time.The feed of described forging is preferably 80 ~ 120mm, and draught is preferably 30 ~ 50mm.In order to eliminate the impurity that in forging process, surface produces, niobium ingot after forging is carried out pickling by the application, the solution of described pickling is preferably the mixing solutions of hydrofluoric acid, hydrochloric acid and the nitric acid that volume ratio is 1:2:3, wherein the concentration of hydrofluoric acid is 40wt%, the concentration of hydrochloric acid is 37wt%, and the concentration of nitric acid is 65wt%.In order to eliminate the unrelieved stress in forging process, niobium ingot after pickling is heat-treated by the application, and described heat treated temperature is preferably 1000 DEG C ~ 1300 DEG C, is more preferably 1100 DEG C ~ 1200 DEG C, described heat treated soaking time is preferably 60 ~ 120min, is more preferably 75min ~ 90min.In the process of forging, the thermal treatment related to therebetween, what also can make niobium ingot organizes more and more homogenizing, refinement.
More even in order to make niobium ingot be out of shape, the niobium ingot after forging is rolled by the application.The working modulus of described rolling is greater than 50%, is preferably 55% ~ 75%.The mode of the application to described rolling has no particular limits, and is rolling mode well known to those skilled in the art.
The niobium plate obtained after rolling is finally heat-treated by the application, to eliminate the unrelieved stress in the operation of rolling, described heat treated temperature is preferably 1100 DEG C ~ 1300 DEG C, be more preferably 1150 DEG C ~ 1250 DEG C, described heat treated soaking time is preferably 90min ~ 120min, is more preferably 100min ~ 110min.The thermal treatment carried out after rolling, is conducive to making niobium ingot after a series of forging and rolling, obtain homogeneous microstructure, equiaxed grain structure that grain fineness number is little.
Niobium target is generally welded together by polylith target in use, in order to reduce weld seam, more and more higher to the requirement of single flat niobium target.Preferably, niobium target is finally carried out mechanical workout by the application again, and to make the planeness of target be less than 0.2mm, surfaceness is less than 0.8 μm.The application adopts levelling machine to smooth target, makes its planeness be less than 0.2mm, adopts polishing and burnishing machine rubbing down to ensure that the surfaceness of target is less than 0.8 μm.
The application is in the process of preparation plane niobium target, forging process is the radial side of beating, the mode that axially pulling and flattening are forged combines, adopt rational distorted area geometrical factor, make the columnar zone in niobium ingot, effective fragmentation is implemented near Center Equiaxial Crystal district and niobium ingot edge, the metal flow of blank centre portions increases, the degree of irregularity of central tissue obtains remarkable improvement, when multi-direction stressed, its original as cast condition open grain structure is made to obtain multi-faceted abundant fragmentation, thus impel niobium ingot to obtain the relatively uniform tissue of crystal grain, avoiding central part is not implemented into effectively broken and to the follow-up existence leaving over down " crystal zone " adverse tissue such as tissue and open grain structure, at rolling sequence, adopt rational reduction in pass, controlled rolling distorted area geometrical factor, make niobium ingot be out of shape evenly, and coordinate middle thermal treatment process after processing, what make niobium target organizes more and more homogenizing, refinement, finally obtains homogeneous microstructure, equiaxed grain structure plane niobium target that grain fineness number is less than 100 μm.In addition, the application, on the basis that above-mentioned niobium ingot is processed, by the smoothing in later stage, mechanical workout and surface treatment, has prepared the plane niobium target meeting sputter coating requirement.
In order to understand the present invention further, below in conjunction with embodiment, the preparation method to plane niobium target provided by the invention is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
The niobium ingot of Φ 190mm × L is carried out the radial direction side of beating successively, axially pulling, obtain the niobium ingot of 100mm × 100mm × Lmm, feed L=100 ~ the 150mm of forging, draught Δ h=40 ~ 60mm, be out of shape comparatively uniformly for obtaining, when pulling operates, feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopts standard gauge block as cushion block; By niobium ingot saw material obtained above to L=200mm; Pickling: HF:HCL:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Heat-treated by niobium ingot after pickling, temperature is 1200 DEG C, insulation 60min;
The niobium ingot of the above-mentioned 100mm of obtaining × 100mm is clapped flat forging, 100mm × 100mm → B160 × H50mm, forging feed L=80 ~ 120mm, draught Δ h=30 ~ 50mm, be out of shape comparatively uniformly for obtaining, when clapping flat forging operation, the feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopt standard gauge block as cushion block; Pickling: HF:HCl:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Heat-treated by niobium ingot after pickling, temperature is 1200 DEG C, insulation 60min; Finished product rolling: be rolled down to δ=6.5mm; Finished product thermal treatment: thermal treatment temp is 1200 DEG C, insulation 90min; Finally adopt levelling machine smoothing, sampling, blanking, surperficial rubbing down, finished product processing, obtain plane niobium target.As shown in Figure 1, Fig. 1 is the metallograph of niobium target prepared by the present embodiment, and as seen from the figure, the grain fineness number of niobium target prepared by the present embodiment is 55 μm.
Embodiment 2
The niobium ingot of Φ 285mm × L is carried out successively the radial direction side of beating and axially pull out, obtain the niobium ingot being of a size of 190mm × 190mm × Lmm, forging feed L=100 ~ 150mm, draught Δ h=40 ~ 60mm, be out of shape comparatively uniformly for obtaining, when pulling operates, the feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopt standard gauge block as cushion block; By above-mentioned niobium ingot length saw material to L=400mm; Pickling: HF:HCl:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Niobium ingot pickling obtained is heat-treated, and temperature is 1200 DEG C, insulation 60min;
Above-mentioned niobium ingot is clapped flat forging, first time claps flat forging, 190mm × 190mm → B200 × H100mm, forging feed L=80 ~ 120mm, draught Δ h=30 ~ 50mm, be out of shape comparatively uniformly for obtaining, when clapping flat forging operation, feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopts standard gauge block as cushion block; Pickling: HF:HCl:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Heat-treated by niobium ingot after pickling, temperature is 1100 DEG C, insulation 60min; Second time claps flat forging, B200 × H100mm → B200 × H50mm, forging feed L=80 ~ 120mm, draught Δ h=30 ~ 50mm, be out of shape comparatively uniformly for obtaining, when clapping flat forging operation, the feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopt standard gauge block as cushion block; Pickling: HF:HCl:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Heat-treated by niobium ingot after pickling, temperature is 1100 DEG C, insulation 60min; Finished product rolling: be rolled down to δ=10mm; Finished product thermal treatment: thermal treatment temp is 1200 DEG C, insulation 60min; Finally smooth, sample, blanking, surperficial rubbing down, finished product processing, obtain plane niobium target.Fig. 2 is the metallograph of niobium target prepared by the present embodiment, and as seen from the figure, the grain fineness number of niobium target prepared by the present embodiment is 80 μm.
Embodiment 3
The niobium ingot of Φ 190mm × L is carried out successively the radial direction side of beating and axially pull out, obtain the niobium ingot being of a size of 120mm × 120mm × Lmm, feed L=100 ~ the 150mm of forging, draught Δ h=40 ~ 50mm, be out of shape comparatively uniformly for obtaining, when pulling operates, the feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopt standard gauge block as cushion block; By above-mentioned niobium ingot length saw material to L=400mm; Pickling: HF:HCl:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Niobium ingot pickling obtained is heat-treated, and temperature is 1000 DEG C, insulation 90min;
Above-mentioned niobium ingot is clapped flat forging, 120mm × 120mm → B170 × H70mm, forging feed L=80 ~ 120mm, draught Δ h=30 ~ 40mm, be out of shape comparatively uniformly for obtaining, when clapping flat operation, the feed entrance point before and after should making during each time compression is interlaced to be opened, unanimously controlled in order to ensure each pressure, adopt standard gauge block as cushion block; Pickling: HF:HCl:HNO
3=1:2:3 (volume ratio), remove surface impurity, visual inspection visible niobium metal gloss is without assorted spot; Thermal treatment: thermal treatment temp is 1000 DEG C, insulation 90min; By niobium ingot finished product obtained above rolling: be rolled down to δ=15mm; Finished product thermal treatment: thermal treatment temp is 1100 DEG C, insulation 90min; Finally smooth, sample, blanking, surperficial rubbing down, finished product processing, obtain plane niobium target.Fig. 3 is the metallograph of niobium target prepared by the present embodiment, and as seen from the figure, the grain fineness number of niobium target prepared by the present embodiment is 45 μm.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (9)
1. a preparation method for plane niobium target, comprises the following steps:
A), forged by niobium ingot, the mode of described forging is that radial direction beats square shaft to pulling; Niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated;
B), by steps A) the niobium ingot that obtains forges, and the mode of described forging is for flattening forging; Niobium ingot after forging is carried out pickling, the niobium ingot after pickling is heat-treated;
C), by step B) the niobium ingot that obtains is rolled, heat-treated by the niobium plate after rolling, obtain plane niobium target.
2. preparation method according to claim 1, is characterized in that, steps A) described in forging working modulus be greater than 50%.
3. preparation method according to claim 1, is characterized in that, step B) described in forging working modulus be greater than 30%.
4. preparation method according to claim 1, is characterized in that, step C) described in the working modulus of rolling be greater than 50%.
5. preparation method according to claim 1, steps A) described in the feed of forging be 100 ~ 150mm, draught is 40 ~ 60mm.
6. preparation method according to claim 1, step B) described in the feed of forging be 80 ~ 120mm, draught is 30 ~ 50mm.
7. preparation method according to claim 1, it is characterized in that, steps A) with step B) described in the mixing solutions of the hydrofluoric acid of the solution of pickling to be volume ratio be 1:2:3, hydrochloric acid and nitric acid, the concentration of described hydrofluoric acid is 40wt%, the concentration of described hydrochloric acid is 37wt%, and the concentration of described nitric acid is 65wt%.
8. preparation method according to claim 1, is characterized in that, steps A) described in heat treated temperature be 1000 DEG C ~ 1300 DEG C, described heat treated soaking time is 60 ~ 120min; Step B) described in heat treated temperature be 1000 ~ 1300 DEG C, described heat treated soaking time is 60 ~ 120min; Step C) described in heat treated temperature be 1100 DEG C ~ 1300 DEG C, described heat treated soaking time is 90 ~ 120min.
9. preparation method according to claim 1, is characterized in that, the diameter of described niobium ingot is 150mm ~ 350mm.
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| CN109706427A (en) * | 2018-12-28 | 2019-05-03 | 宁夏东方钽业股份有限公司 | The preparation method of plane niobium target |
| CN113718110A (en) * | 2021-08-11 | 2021-11-30 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate for controlling plate structure by accumulated energy |
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| CN113718110A (en) * | 2021-08-11 | 2021-11-30 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate for controlling plate structure by accumulated energy |
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