CN109082637A - A kind of high uniformly fine grain tin target and preparation method thereof of high-purity - Google Patents
A kind of high uniformly fine grain tin target and preparation method thereof of high-purity Download PDFInfo
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- CN109082637A CN109082637A CN201810929068.6A CN201810929068A CN109082637A CN 109082637 A CN109082637 A CN 109082637A CN 201810929068 A CN201810929068 A CN 201810929068A CN 109082637 A CN109082637 A CN 109082637A
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- tin
- purity
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- high purity
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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
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The invention discloses a kind of preparation method of the high uniformly fine grain tin target of high-purity, S1: the raw material refined tin that purity is 99.99% is carried out melting and casting, obtains high purity tin ingot casting by vacuum melting；S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, and rolling reduction is 50% or more；S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 60~140 DEG C, and annealing time is 60~120min, and air-cooled or water cooling obtains high purity tin target blank；S4: high purity tin target blank is machined by machining, the high uniformly fine grain tin target of the high-purity needed.The preparation method of the high uniformly fine grain tin target of high-purity, it is simple and convenient, it is low in cost, implement convenient for operation.It is lower to production equipment requirement in entire production process, equipment cost investment can be greatly reduced, further reduced production cost.The preparation method universality is high, is suitable for scale industrial production.
Description
Technical field
The present invention relates to the technical fields of metal material, specifically, refer to a kind of high uniformly fine grain tin target of high-purity
Material and preparation method thereof.
Background technique
With the high speed development of the high-tech industries such as electronics industry and semi-conductor industry, have more to the performance of thin-film material
High requirement, and sputtering method is to prepare one of major technique of thin-film material, has consistency with the film that target as sputter deposits
The advantages that height, adhesion is good.
Target restricts and affects coating quality, and existing product cannot fully meet the market demand, thus study tool
High-purity target preparation process of standby superperformance, to high-purity metal target possess the more and more extensive market competitiveness have it is far-reaching
Meaning.
Summary of the invention
The first purpose of this invention is to provide a kind of preparation method of the high uniformly fine grain tin target of high-purity, energy
Enough performances improved to target as sputter film, while the preparation method is easy to operate, it is low in cost, it is raw to be suitable for large-scale industrial
It produces.
Second object of the present invention is to provide a kind of high-purity high uniformly fine grain tin target, can be improved to target
The performance of the sputtered film of material.
The embodiment of the present invention is achieved in that
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting, obtains high purity tin ingot casting by vacuum melting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: heat treatment, the high purity tin after cold rolling is annealed, annealing temperature be 60~140 DEG C, annealing time be 60~
120min, air-cooled or water cooling obtain high purity tin target blank；
S4: high purity tin target blank is machined by machining, obtains the high uniformly fine grain tin target of high-purity
Material.
The beneficial effect of the embodiment of the present invention is:
By a series of technique of raw material refined tin progress for being 99.99% to purity, so that it is high uniformly to obtain high-purity
Fine grain tin target, therefrom step includes vacuum melting, rolling processing, heat treatment and machining, is done at this to above-mentioned steps
Further instruction.
Vacuum melting is that the raw material refined tin for being 99.99% by purity carries out melting and casting in a vacuum furnace, passes through control
Vacuum condition processed further obtains high purity tin ingot casting, and in an embodiment of the present invention, the vacuum degree in vacuum drying oven is not less than 6
×10-1MPa, while smelting temperature is 250~350 DEG C.
Rolling processing is will to obtain the plane milling of high purity tin ingot casting surface, and plane milling mainly removes high purity tin ingot casting surface
Impurity, thus further obtain purer high purity tin ingot casting, by plane milling after high purity tin ingot casting roll, be convenient for subsequent place
Reason.
Heat treatment, the high purity tin after cold rolling is annealed, and further limit annealing conditions, specifically annealing temperature is
60~140 DEG C, annealing time is 60~120min, to obtain high purity tin target blank.
Machining after processing high purity tin target blank by mechanical means, just can obtain the high uniform fine grain of high-purity
Grain tin target.
The preparation method of the high uniformly fine grain tin target of high-purity, it is simple and convenient, it is low in cost, implement convenient for operation.It is whole
It is lower to production equipment requirement in a production process, equipment cost investment can be greatly reduced, further reduced production cost.
The preparation method universality is high, is suitable for scale industrial production.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described, the person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out, reagents or instruments used without specified manufacturer, is the conventional production that can be obtained by commercially available purchase
Product.
Have below to a kind of preparation method of the high uniformly fine grain tin target of high-purity provided in an embodiment of the present invention
Body explanation.
The embodiment of the present invention provides a kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting, obtains high purity tin ingot casting by vacuum melting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: heat treatment, the high purity tin after cold rolling is annealed, annealing temperature be 60~140 DEG C, annealing time be 60~
120min, air-cooled or water cooling obtain high purity tin target blank；
S4: high purity tin target blank is machined by machining, obtains the high uniformly fine grain tin target of high-purity
Material.
Further, in the step S1, vacuum degree is not less than 6 × 10 when melting-1MPa, 250 DEG C~350 DEG C of smelting temperature,
High purity tin ingot casting is cast as in water cooling swage.
Further, in the step S1, vacuum degree is not less than 6 × 10 when melting-1MPa, 300 DEG C of smelting temperature, in water cooling
High purity tin ingot casting is cast as in swage.
Further, in the step S3, the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 100 DEG C,
Annealing time is 60~120min, and air-cooled or water cooling obtains tin target blank.
Further, in the step S3, the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 60~140
DEG C, annealing time 90min, air-cooled or water cooling obtains tin target blank.
The preparation method of uniformly fine grain tin target high to high-purity does specific explanations explanation below:
Target restricts the Physical and mechanical properties of sputtering thin film, affects coating quality, tin target magnetic in the prior art
Property sputtering metallic film performance it is poor, studied for a long period of time discovery by researcher, target is basic in magnetron sputtering process
Consumptive material, not only usage amount is big, but also the quality of target quality plays vital decisive action to the performance of metallic film, because
This, target is the critical material of magnetron sputtering process.
And determine target performance mainly according to the high-purity of target, high uniform fine grain.Specifically from these three sides
Face:
(1) purity: requirement of the target to purity is namely to the requirement of content of impurities, and content of impurities is lower, purity
Higher, the purity of target is very big on the influence of the performance of sputtered film, and the purity of target is higher, and the performance of sputtered film is better,
But difference purposes target is different to purity requirement, the purity requirement of high purity tin target is not less than in the present invention
99.999%.
(2) consistency: the consistency of target not only influences deposition rate, the density and electric discharge of sputtering peplomer when sputtering
Phenomenon etc. has an effect on the electrical and optical performance of sputtered film, therefore target is finer and close, and the density of sputtered film particle is got over
Low, electric discharge phenomena are weaker, and the performance of film is also better.
(3) crystallite dimension and distribution: the target of same ingredient, the sputter rate of fine size crystal grain target is than coarse grain target
Fastly, while crystallite dimension differs lesser uniform target, and the thickness distribution for depositing film is also more uniform.
Performance Assessment to tin target is also mainly in terms of above three:
Tin has a wide range of applications as a kind of common metal material, and purity is not less than 99.999% high purity tin, inhales
Thermal energy power is strong, stable mechanical performance, with excellent electric conductivity, the tin plating and diffusing, doping work that is widely used in electronics industry
The fields such as skill, semi-conductor industry and manufacture superconducting alloy.High purity tin has high purity alloys, compound partly to lead for the product of preparation
Body, superconductor such as Nb3Sn (niobium tin), the dopant of solder and compound semiconductor, tin indium oxide target material (ITO), optics
The fields such as the sputtering target material used for solar batteries of the large-area glass plated film of film industry and solar photovoltaic industry, therefore select
The raw material refined tin that purity is 99.99% can satisfy the requirement of purity.
By a series of technique of raw material refined tin progress for being 99.99% to purity, so that it is high uniformly to obtain high-purity
Fine grain tin target, therefrom step includes vacuum melting, rolling processing, heat treatment and machining, is done at this to above-mentioned steps
Further instruction.
Vacuum melting is that the raw material refined tin for being 99.99% by purity carries out melting and casting in a vacuum furnace, passes through control
Vacuum condition processed further obtains high purity tin ingot casting, and in an embodiment of the present invention, the vacuum degree in vacuum drying oven is not less than 6
×10-1MPa, while smelting temperature is 250~350 DEG C.
Rolling processing is will to obtain the plane milling of high purity tin ingot casting surface, and plane milling mainly removes high purity tin ingot casting surface
Impurity, thus further obtain purer high purity tin ingot casting, by plane milling after high purity tin ingot casting roll, be convenient for subsequent place
Reason.
Heat treatment, the high purity tin after cold rolling is annealed, and further limit annealing conditions, specifically annealing temperature is
60~140 DEG C, annealing time is 60~120min, to obtain high purity tin target blank.
Machining after processing high purity tin target blank by mechanical means, just can obtain the high uniform fine grain of high-purity
Grain tin target.
By above-mentioned preparation method, selecting purity is 99.99% refined tin raw material, and this is carried out melting, can be obtained
To the high purity tin of high-purity 99.999%, obtained high purity tin target has strong heat absorption capacity, stable mechanical performance, excellent leads
The advantages that electrical.
It is well known that the purity of pure metal material is higher, internal grain is easier to grow up, prepare high-purity and it is tiny
Even crystal grain, difficulty is quite larger, because according to Principles of Metallography, the purity of pure metal material is higher, and internal grain is easier
It grows up, and rear tin target obtained through the above steps, to change the crystalline texture of tin target, and then control internal grain
Variation, proved by long-term experiment, the crystallite dimension of the tin target can control in 100um hereinafter, and grain size variation
When being maintained within 20%, the quality of sputtered film is substantially increased, and then improve sputter rate.
By the above method, high-purity, high uniform, fine grain tin target can be obtained, and the preparation method is simple
It has been operated that, while low in cost, be more suitable for enterprise and produce on a large scale.
Embodiment 1:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 250 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 60 DEG C, annealing time 60min, empty
Cold or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Embodiment 2:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 250 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 60 DEG C, annealing time 120min, empty
Cold or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Embodiment 3:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 300 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 100 DEG C, annealing time 90min, empty
Cold or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Embodiment 4:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 350 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 140 DEG C, annealing time 60min, empty
Cold or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Embodiment 5:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 350 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 140 DEG C, annealing time 120min,
Air-cooled or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Comparative example 1:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.95% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 250 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 40 DEG C, annealing time 30min, empty
Cold or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Comparative example 2:
A kind of preparation method of the high uniformly fine grain tin target of high-purity,
The following steps are included:
S1: the raw material refined tin that purity is 99.95% is carried out melting and casting in a vacuum furnace, melted by vacuum melting
Temperature control vacuum degree at 400 DEG C, melting is not less than 6 × 10-1MPa obtains high purity tin ingot casting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, rolling reduction 50% with
On；
S3: the high purity tin after cold rolling is annealed in heat treatment, and annealing temperature is 180 DEG C, annealing time 150min,
Air-cooled or water cooling obtains high purity tin target blank；
S4: high purity tin target blank is machined by machining, the high uniform fine grain of the high-purity needed
Tin target.
Experimental data:
By above-mentioned experimental example and comparative example comparison it is found that the tin target that Examples 1 to 5 obtains is that high-purity is high uniformly
Fine grain, and the tin raw material that the purity of the use of comparative example 1 and 2 is not high, and there is also larger differences for parameter during preparation method
Different, finally obtained tin target does not all reach requirement on purity, uniformity and crystal grain.
It is simple and convenient for preparing the high uniformly preparation method of fine grain tin target of high-purity, it is low in cost, convenient for operation
Implement.It is lower to production equipment requirement in entire production process, equipment cost investment can be greatly reduced, further reduced life
Produce cost.The preparation method universality is high, is suitable for scale industrial production.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of the high uniformly fine grain tin target of high-purity, it is characterised in that: the following steps are included:
S1: the raw material refined tin that purity is 99.99% is carried out melting and casting, obtains high purity tin ingot casting by vacuum melting；
S2: rolling processing will carry out at room temperature cold rolling after the plane milling of high purity tin ingot casting surface, and rolling reduction is 50% or more；
S3: heat treatment, the high purity tin after cold rolling is annealed, annealing temperature be 60~140 DEG C, annealing time be 60~
120min, air-cooled or water cooling obtain high purity tin target blank；
S4: high purity tin target blank is machined by machining, obtains the high uniformly fine grain tin target of high-purity.
2. preparation method according to claim 1, it is characterised in that: in the step S1, vacuum degree is not less than 6 when melting
×10-1MPa, is cast as high purity tin ingot casting in water cooling swage by 250 DEG C~350 DEG C of smelting temperature.
3. preparation method according to claim 2, it is characterised in that: in the step S1, vacuum degree is not less than 6 when melting
×10-1MPa, is cast as high purity tin casting in water cooling swage by 300 DEG C of smelting temperature.
4. preparation method according to claim 1, it is characterised in that: in the step S3, heat treatment, by the height after cold rolling
Pure tin is annealed, and annealing temperature is 100 DEG C, and annealing time is 60~120min, and air-cooled or water cooling obtains tin target blank.
5. preparation method according to claim 1, it is characterised in that: in the step S3, heat treatment, by the height after cold rolling
Pure tin is annealed, and annealing temperature is 60~140 DEG C, and annealing time 90min, air-cooled or water cooling obtains tin target blank.
6. the high uniformly fine grain tin target of high-purity, the tin target is made in any one preparation method according to claim 1~5
Purity >=99.999% of material, relative density >=99%, mean grain size≤100um.
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| CN201810929068.6A CN109082637A (en) | 2018-08-15 | 2018-08-15 | A kind of high uniformly fine grain tin target and preparation method thereof of high-purity |
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Cited By (3)
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| CN110938799A (en) * | 2019-12-17 | 2020-03-31 | 宁波海秀丰科技有限公司 | High-purity high-uniformity gold target material and preparation method and application thereof |
| CN112725675A (en) * | 2020-12-23 | 2021-04-30 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN114207179A (en) * | 2019-08-14 | 2022-03-18 | 霍尼韦尔国际公司 | Large grain tin sputtering target |
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| CN101307429A (en) * | 2008-07-14 | 2008-11-19 | 中南大学 | Process for preparing high-purity metallic nickel target of superfine crystal particle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114207179A (en) * | 2019-08-14 | 2022-03-18 | 霍尼韦尔国际公司 | Large grain tin sputtering target |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181225 |
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| RJ01 | Rejection of invention patent application after publication |