CN104831242B - Large scale integration aluminium neodymium rotary target material and preparation method thereof - Google Patents
Large scale integration aluminium neodymium rotary target material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of integrated large scale aluminium neodymium rotary target material and preparation method thereof; wherein preparation method includes pretreatment and electric arc spraying bottoming stainless steel base penstock; ball milling shaping is carried out to the aluminium neodymium powder of purity 99.99%, plasma cold spraying neodymium aluminium powder is to formation neodymium aluminium rotary target material in nickel aluminium transition zone stainless steel base penstock in vacuum or protective atmosphere.The aluminium neodymium rotary target material thickness prepared using the present invention can reach 3 ~ 16mm, and target relative density is more than 97%, and purity reaches 99.99%, and oxygen content is less than 200ppm.The present invention can play the advantages such as airless spraying purity is high, oxygen content is low, and and can has given play to cold spraying consistency height, the advantages that even tissue, can increase substantially target quality, target is applied to wider field.
Description
Technical field
The invention belongs to target preparation field, more particularly to a kind of preparation of large scale integration aluminium neodymium rotary target material.
Background technology
Aluminium neodymium target be mainly used for flat-panel screens, touch-screen glass substrate electrode layer plated film.Presently mainly
With vacuum melting and hot-pressing sintering method research and development and production small size flat target, large scale target is spliced to form by small size.
Due to not being that integrated (needing to splice) easily produces arc discharge, therefore quality of forming film is poor, it is difficult to is really applied to high quality
Display screen, on touch-screen.Although people are using vacuum melting production hollow aluminum neodymium target target pipe, and welded and bound by indium
Aluminium neodymium rotary target material is produced on to stainless steel penstock.Because indium solder expensive (accounting for whole target cost 50%) causes aluminium neodymium to rotate
The cost of target is high；On the other hand, due to being that a section section target pipe is spliced in the presence of section seam, electric arc is easily formed when in use and is put
Electricity, reduce quality of forming film.Further, since being welded using the indium of low melting point, generate heat during target use, easily cause phenomenon of missing the target,
Thermal contraction is not easily controlled when also aluminium neodymium target pipe welds, and welding difficulty is big.
Vacuum melting and hot-pressing technique are because uneven components easily produce segregation, along with target shape is restricted,
The requirement that target material composition is uniform, large scale is integrated can not have been met.
Sputter-deposition technology is widely used in solar cell, flat-panel screens, CD, micro-structural circuit etc.；
Particularly, with the development in large size of display screen in recent years, touch-screen, sputtering technology has been display screen, touch-screen pushes away
It is old to go out newly to have made huge contribution.But existing method is required for follow-up target binding technique, i.e., by target and backboard (generally
It is metal copper plate) it is bound together by brazing mode, binding technology is a complicated process in itself, and bound device is held high
It is expensive；Meanwhile once binding effect is poor, then target can be brought rapidly up and cause target sealing-off, target fusing, apparatus overheat etc.
Problem, sputtering equipment can be out of order or scrap when serious.
The new rotary target material for being used to prepare the integration of high density high-purity large scale of invention has important practical significance
It is worth with huge technique.
The content of the invention
Goal of the invention：It is an object of the invention to provide a kind of aluminium neodymium of the large scale that technique is simple, cost is cheap integration
Rotary target material preparation method.
Technical scheme：A kind of preparation method of large scale integration aluminium neodymium rotary target material provided by the invention, including it is following
Step：
(1) ultrasonic wave cleaning, drying and sandblasting pretreatment are carried out to stainless steel base penstock surface；
(2) electric arc spraying ni-al alloyed wire is to forming transition zone, thickness 0.1 in the stainless steel base penstock pre-processed
~0.3mm；
(3) by purity not less than the aluminium neodymium powder batch mixing shaping 3-5 hours that 99.99%, D50 is 50~100 μm；
(4) in vacuum or protective atmosphere, the neodymium of integration will be formed in neodymium aluminium mixed-powder cold spraying to stainless steel base
Aluminium rotary target material.
Preferred embodiment is as follows：
In step (1), the pretreatment includes derusting, ultrasonic wave decontamination and matrix surface is carried out at sandblasting roughening
Reason.The shot blasting particles that sandblasting roughening treatment uses are steel sand, and steel sand granularity is 16~30 mesh.In step (2), the nickel alumin(i)um alloy
Silk is diameter 1-3 millimeters.In step (4), the gas in described protective atmosphere is inert gas argon gas or nitrogen.
The neodymium rotary target material thickness is 3~16mm, and target relative density is more than 97%, and purity is not less than 99.99%, contains
Oxygen amount is less than 200ppm.
Beneficial effect：The preparation method of neodymium aluminium rotary target material provided by the invention is using vacuum or protective gas less than conjunction
(cold spraying) neodymium aluminium mixed-powder is sprayed under golden melting temperature neodymium aluminium rotary target material, technique letter are formed to stainless steel cylindrical base member
It is single, easy to operate, cost is cheap, the target size produced is big, integration, density is high, porosity is low, composition is uniform, crystal grain
It is tiny, yield is high, quality is good, overcomes the binding process in existing method, obtained target can be used directly.
Specifically, the present invention has advantage following prominent relative to prior art：
(1) technique is simple, yield is high, cost is cheap：This method need not subsequently bind process, and technique is simple, operation side
Just, cost is cheap, it is not necessary to complicated molding, has good economic benefit ratio；
(2) good product quality：Using the target length that this method is produced from 50 centimetres to 400 centimetres, 12 centimetres of diameter
To 15 centimetres, the thickness of neodymium aluminium alloy is from 3 millimeters to 16 millimeters；With density high (＞ 95%), porosity it is low (<0.5%), into
Point uniformly, the features such as crystal grain tiny (particle diameter be less than 100 μm), the defects of isolating of macroscopic view is not had.
(3) rotary target material large scale, integration, it is no to splice, without binding.The target of preparation is not size-limited, without spelling
Connect and bind, target fully integratedization, do not save gap, arc discharge is greatly decreased, improve the plating membrane efficiency of target, ensure film
Uniformity.
(4) rotary target material purity is high：Vacuum or protective atmosphere spraying technology significantly reduce oxygen content and other impurities
It is mixed into, simultaneously because cold spraying with respect to thermal spraying is worked at a temperature of far below material melting point, avoids oxidation and generation not
The thing phase needed, ensure that the high-purity of target.
(5) rotary target material density is high：Because cold spraying relative to thermal spraying particle produces strong plasticity with high-speed impact
Coating is formed, and the impact of follow-up particle produces the effect of densification to coating early stage, and coating is not by melting
The volume contraction process of state cooling, therefore the porosity low-density of target is high.
(6) the uniform segregation-free of rotary target material composition：The volume contraction that cold spray technique technique is not cooled down by molten condition
Process, which can avoid segregation of the high temperature on coating, to be influenceed.
Embodiment
Embodiment 1
A kind of preparation of integrated large scale aluminium neodymium rotary target material,
(1) select 304 stainless steels to be used as basal body pipe, the oxide layer of matrix surface is removed with the method for mechanical grinding, with surpassing
The method of sound cleaning removes the dirt of matrix surface, then carries out blasting treatment to matrix surface, matrix surface is reached suitable
Roughness, in favor of the combination of coating and matrix, blasting treatment uses steel sand, and granularity is 16~30 mesh.
(2) electric arc spraying nickel alclad B alloy wire is used, prime coat thickness is 0.15mm.
(3) purity is selected to be not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder, ball milling shaping in 3 hours.
(4) vacuum is extracted to vacuum cold spray tank body using 3 groups of vacuum pump sets, vacuum is detected using vacuum detecting meter,
When vacuum reaches 1Pa, stop extracting vacuum, argon gas is then filled with to vacuum cold spray tank interior by air intake valve and is used as
Protective gas.
(5) when spraying：Operating pressure is 1.8Mpa at cold spraying nozzle inlet, and temperature is 250 DEG C, and working gas temperature is
400 DEG C, pressure 2.5Mpa, nitrogen is selected as working gas, nitrogen flow 35m3/ h, spray distance 50mm.
The Lv Nv rotary target materials dense structure prepared by the present invention, porosity is low, and composition is uniform, and purity is high, target
Size is unrestricted, and thickness can reach 12mm, and relative density is more than 97%, and oxygen content is less than 200ppm.
It is 300mm in length, external diameter is the aluminium neodymium rotation that vacuum cold spray thickness is 5mm in 90mm 304 stainless steel penstocks
Turn target.
Embodiment 2
A kind of preparation of integrated large scale aluminium neodymium rotary target material,
(1) select 304 stainless steels to be used as basal body pipe, the oxide layer of matrix surface is removed with the method for mechanical grinding, with surpassing
The method of sound cleaning removes the dirt of matrix surface, then carries out blasting treatment to matrix surface, reaches matrix surface suitable
Roughness, in favor of the combination of coating and matrix, blasting treatment uses steel sand, and granularity is 24 mesh.
(2) electric arc spraying nickel alclad B alloy wire is used, prime coat thickness is 0.2mm；
(3) purity is selected to be not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder.
(4) vacuum is extracted to vacuum cold spray tank body with vacuum pump set, be filled with by air intake valve to spraying tank interior
Argon gas is as protective gas.
(5) when spraying：Operating pressure is 2.2Mpa at cold spraying nozzle inlet, and temperature is 280 DEG C, and working gas temperature is
500 DEG C, pressure 2.8Mpa, nitrogen flow 40m3/ h, spray distance 40mm.
The microstructure morphology and composition that this example prepares aluminium neodymium target are observed with SEM, uses Archimedes
Method surveys target porosity, and the porosity of target is analyzed with metallographic microscope.Lv Nv targets dense structure manufactured in the present embodiment, hole
Gap rate is low, composition is uniform, and purity is high.Thickness is 5mm, relative density 98%, porosity 1.9%.
Embodiment 3
A kind of preparation of integrated large scale aluminium neodymium rotary target material,
It is 300mm in length, external diameter is the aluminium neodymium rotation that vacuum cold spray thickness is 9mm in 133mm 304 stainless steel penstocks
Turn target.
(1) select 304 stainless steels to be used as basal body pipe, the oxide layer of matrix surface is removed with the method for mechanical grinding, with surpassing
The method of sound cleaning removes the dirt of matrix surface, then carries out blasting treatment to matrix surface, reaches matrix surface suitable
Roughness, in favor of the combination of coating and matrix, blasting treatment uses steel sand, and granularity is 24 mesh.
(2) electric arc spraying nickel alclad B alloy wire is used, prime coat thickness is 0.2mm；
(3) purity is selected to be not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder.
(4) vacuum is extracted to vacuum cold spray tank body with vacuum pump set, be filled with by air intake valve to spraying tank interior
Argon gas is as protective gas.
(5) when spraying：Operating pressure is 1.5Mpa at cold spraying nozzle inlet, and temperature is 330 DEG C, and working gas temperature is
450 DEG C, pressure 2.8Mpa, nitrogen flow 45m3/ h, spray distance 60mm.
The microstructure morphology and composition that this example prepares aluminium neodymium target are observed with SEM, uses Archimedes
Method surveys target porosity, and the porosity of target is analyzed with metallographic microscope.Lv Nv targets dense structure manufactured in the present embodiment, hole
Gap rate is low, composition is uniform, and purity is high.Thickness is 9mm, relative density 97.5%, porosity 2%.
Embodiment 4
A kind of preparation of integrated large scale aluminium neodymium rotary target material,
It is 300mm in length, external diameter is the aluminium neodymium that vacuum cold spray thickness is 10mm in 133mm 304 stainless steel penstocks
Rotary target material.
(1) select 304 stainless steels to be used as basal body pipe, the oxide layer of matrix surface is removed with the method for mechanical grinding, with surpassing
The method of sound cleaning removes the dirt of matrix surface, then carries out blasting treatment to matrix surface, reaches matrix surface suitable
Roughness, in favor of the combination of coating and matrix, blasting treatment uses steel sand, and granularity is 24 mesh.
(2) electric arc spraying nickel alclad B alloy wire is used, prime coat thickness is 0.2mm；
(3) purity is selected to be not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder.
(4) vacuum is extracted to vacuum cold spray tank body with vacuum pump set, be filled with by air intake valve to spraying tank interior
Argon gas is as protective gas.
(5) when spraying：Operating pressure is 2.4Mpa at cold spraying nozzle inlet, and temperature is 360 DEG C, and working gas temperature is
560 DEG C, pressure 2.2Mpa, nitrogen flow 25m3/ h, spray distance 40mm.
The microstructure morphology and composition that this example prepares aluminium neodymium target are observed with SEM, uses Archimedes
Method surveys target porosity, and the porosity of target is analyzed with metallographic microscope.Lv Nv targets dense structure manufactured in the present embodiment, hole
Gap rate is low, composition is uniform, and purity is high.Thickness is 10mm, relative density 97%, porosity 2.5%.
Embodiment 5
A kind of preparation of integrated large scale aluminium neodymium rotary target material,
(1) select 304 stainless steels to be used as basal body pipe, the oxide layer of matrix surface is removed with the method for mechanical grinding, with surpassing
The method of sound cleaning removes the dirt of matrix surface, then carries out blasting treatment to matrix surface, matrix surface is reached suitable
Roughness, in favor of the combination of coating and matrix, blasting treatment uses steel sand, and granularity is 16~30 mesh.
(2) electric arc spraying nickel alclad B alloy wire is used, prime coat thickness is 0.15mm.
(3) purity is selected to be not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder.
(4) vacuum is extracted to vacuum cold spray tank body using 3 groups of vacuum pump sets, vacuum is detected using vacuum detecting meter,
When vacuum reaches 1Pa, stop extracting vacuum, argon gas is then filled with to vacuum cold spray tank interior by air intake valve and is used as
Protective gas.
(5) when spraying：Operating pressure is 2.6Mpa at cold spraying nozzle inlet, and temperature is 400 DEG C, and working gas temperature is
300 DEG C, pressure 2.2Mpa, nitrogen is selected as working gas, nitrogen flow 25m3/ h, spray distance 50mm.
The Lv Nv rotary target materials dense structure prepared by the present invention, porosity is low, and composition is uniform, and purity is high, target
Size is unrestricted, and thickness can reach 10mm, and relative density is more than 97%, and oxygen content is less than 200ppm.
Embodiment 6
A kind of preparation of integrated large scale aluminium neodymium rotary target material,
(1) select 304 stainless steels to be used as basal body pipe, the oxide layer of matrix surface is removed with the method for mechanical grinding, with surpassing
The method of sound cleaning removes the dirt of matrix surface, then carries out blasting treatment to matrix surface, matrix surface is reached suitable
Roughness, in favor of the combination of coating and matrix, blasting treatment uses steel sand, and granularity is 16~30 mesh.
(2) electric arc spraying nickel alclad B alloy wire is used, prime coat thickness is 0.15mm.
(3) purity is selected to be not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder.
(4) vacuum is extracted to vacuum cold spray tank body using 3 groups of vacuum pump sets, vacuum is detected using vacuum detecting meter,
When vacuum reaches 1Pa, stop extracting vacuum, argon gas is then filled with to vacuum cold spray tank interior by air intake valve and is used as
Protective gas.
(5) when spraying：Operating pressure is 3Mpa at cold spraying nozzle inlet, and temperature is 200 DEG C, and working gas temperature is
600 DEG C, pressure 2.6Mpa, nitrogen is selected as working gas, nitrogen flow 50m3/ h, spray distance 45mm.
The Lv Nv rotary target materials dense structure prepared by the present invention, porosity is low, and composition is uniform, and purity is high, target
Size is unrestricted, and thickness can reach 12mm, and relative density is more than 97%, and oxygen content is less than 200ppm.
Detect aluminium neodymium rotary target material prepared by embodiment 1 to 6.
The measuring instrument used has：Electron scanning Electronic Speculum, metallographic microscope, high accuracy balance, penetron, porosity
Measuring instrument, ICP mass-spectrometer measurement instrument etc..Measurement the results are shown in Table 1.
Aluminium neodymium rotary target material parameter prepared by the embodiment 1 to 6 of table 1
| Relative density | Porosity | Oxygen content | Average grain size | Sputtering performance | |
| 1 | 98% | ≤ 1.9% | ≤200ppm | <150μm | Sputtering is stable |
| 2 | 97.5% | ≤ 2% | ≤200ppm | <150μm | Sputtering is stable |
| 3 | 97% | ≤ 2.5% | ≤200ppm | <150μm | Sputtering is stable |
| 4 | 98.2% | ≤ 1.7% | ≤200ppm | <150μm | Sputtering is stable |
| 5 | 97.3% | ≤ 2.2% | ≤200ppm | <150μm | Sputtering is stable |
| 6 | 98.5% | ≤ 2.4% | ≤200ppm | <150μm | Sputtering is stable |
In a word, compared with the conventional method, want to obtain high-purity, high-compactness, low oxygen content, large scale, integration are not
The rotary target material rotated by shape, vacuum or protective atmosphere are essential.Meanwhile spraying technology can have equipment letter
It is single, operating personnel, integration, the characteristics of limitation by target shape.Cold spraying as plasma spray technology supplement can avoid height
Adverse effect of the temperature to coating.Due to low temperature, avoid oxidation and generate unwanted thing phase, particularly suitable for prepare metal and
Its alloy etc. is easy to the coating of oxidation material.Small on materials microstructure influence, the residual stress of induction is small；Due to high-velocity particles
Realize and deposit by severe plastic deformation, coating structure is fine and close, and produces larger compression, therefore prepared painting applying interlayer
The heat conductivity and electrical conductivity of layer are good；Compared with hot-spraying coating, the density and hardness of cold spraying coating is higher, porosity
It is low.Coating is formed because cold spraying particle produces intense plastic strain with high-speed impact, and the impact of follow-up particle is to preceding
Phase coating produces the effect of densification, and the volume contraction process that coating is not cooled down by molten condition, therefore porosity is relatively low；
Coating has higher adhesion with matrix；Composite coating can be prepared, and very dissimilar material can be processed.Due to material
Significant physicochemical change does not occur in spraying process, collects and recycles particle (powder can reach using the rate of recovery
100%) cost, has been saved, has added processing safety.
The target prepared using the present invention is not limited by geomery, target fully integratedization, without splicing and binding,
And the uniform segregation-free of target material composition, vacuum or protective atmosphere cold spraying ensure that the high-purity of target, and the densification of target
Degree.Due to one-shot forming, without binding, production cost is greatly reduced.This method is sprayed using vacuum or protective atmosphere plasma cold
The neodymium aluminium rotary target material painted, overcomes the binding process in existing method, and technique is simple and convenient to operate, cost is cheap, production
The target integration that goes out, large scale, density is high, porosity is low, composition is uniform, crystal grain is tiny, yield is high, quality is good.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of equivalents can be carried out to technical scheme, this
A little equivalents belong to protection scope of the present invention.It is further to note that described in above-mentioned embodiment
Each particular technique feature, in the case of reconcilable, can be combined by any suitable means.In order to avoid not
Necessary repetition, the present invention no longer separately illustrate to various combinations of possible ways.In addition, a variety of implementations of the present invention
It can also be combined between mode, as long as it without prejudice to the thought of the present invention, it is public that it should equally be considered as institute of the invention
The content opened.
Claims (1)
- A kind of 1. method for preparing large scale integration aluminium neodymium rotary target material, it is characterised in that comprise the following steps：（1）Stainless steel tube is selected matrix surface oxide layer to be removed with the method for mechanical grinding, with ultrasonic cleaning as matrix penstock Method remove the dirt of matrix surface, blasting treatment then is carried out to matrix surface, matrix surface is reached suitable coarse Degree, in favor of the combination of coating and matrix；The blasting treatment uses steel sand, and steel sand granularity is 16~30 mesh；（2）Electric arc spraying ni-al alloyed wire is to forming transition zone, thickness 0.15mm in the stainless steel base penstock pre-processed；（3）Purity is not less than 99.99%, granularity is 20~100 μm of aluminium neodymium powder ball milling shaping in 3 hours；（4）Vacuum is extracted to vacuum cold spray tank body, vacuum is detected using vacuum detecting meter, when vacuum reaches 1Pa, is stopped Vacuum is extracted, argon gas is then filled with to vacuum cold spray tank interior by air intake valve and is used as protective gas；（5）The aluminium neodymium rotary target material of integration will be formed in aluminium neodymium powder cold spraying to stainless steel base；Cold spraying nozzle inlet Place's operating pressure is 1.8Mpa, and temperature is 250 DEG C, and working gas temperature is 400 DEG C, pressure 2.5Mpa, selects nitrogen conduct Working gas, nitrogen flow 35m3/ h, spray distance 50mm；The coating thickness is 5mm；Target relative density is more than 97%, oxygen content is less than 200ppm.
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| CN105058923A (en) * | 2015-08-17 | 2015-11-18 | 基迈克材料科技（苏州）有限公司 | Sputtering target capable of enhancing wear resistance and corrosion resistance of coated glass and manufacturing method |
| CN105714254A (en) * | 2016-04-21 | 2016-06-29 | 广州市尤特新材料有限公司 | Target material assembly and preparation method thereof |
| CN106011758B (en) * | 2016-07-20 | 2018-10-19 | 浙江舒玛新材料有限公司 | A kind of optic communication and magnetic store plated film rare earth-transition metal rotary target material and preparation method thereof |
| CN106498350A (en) * | 2016-10-13 | 2017-03-15 | 法柯特科技（江苏）有限公司 | The preparation method of sial sputtering target material |
| CN107267945A (en) * | 2017-07-17 | 2017-10-20 | 绍兴斯普瑞涂层技术有限公司 | A kind of high-compactness high-purity sputters the preparation method of rotating silver target material |
| CN107619972B (en) * | 2017-11-09 | 2020-07-07 | 韶关市欧莱高新材料有限公司 | Manufacturing method of aluminum-neodymium alloy for magnetron sputtering target material |
| US11584985B2 (en) * | 2018-08-13 | 2023-02-21 | Honeywell International Inc. | Sputter trap having a thin high purity coating layer and method of making the same |
| CN109706422A (en) * | 2019-01-16 | 2019-05-03 | 广州市尤特新材料有限公司 | A kind of aluminium rotary target material and its manufacturing method |
| CN110004417A (en) * | 2019-03-18 | 2019-07-12 | 苏州康科斯柔性电子有限公司 | A kind of rotary target material preparation and its method storing plated film for optic communication and magnetic |
| CN112048703A (en) * | 2020-07-22 | 2020-12-08 | 基迈克材料科技（苏州）有限公司 | Aluminum-neodymium alloy rotary sputtering target material and preparation method thereof |
| CN113604770B (en) * | 2021-07-23 | 2022-08-09 | 常州大学 | Preparation method and device of rotary spraying integrated coating |
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