CN106755891B - A kind of surface treatment method of high pure metal sputtering target material - Google Patents
A kind of surface treatment method of high pure metal sputtering target material Download PDFInfo
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- CN106755891B CN106755891B CN201611102780.6A CN201611102780A CN106755891B CN 106755891 B CN106755891 B CN 106755891B CN 201611102780 A CN201611102780 A CN 201611102780A CN 106755891 B CN106755891 B CN 106755891B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0068—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for particular articles not mentioned below
Abstract
The invention belongs to target processing technology of preparing fields, and in particular to a kind of surface treatment method of high pure metal sputtering target material.Target is machined through surface accurate, surface grinding, after surface clean, using continuous wave laser heat treating process, scanning beam method or non-coherent broad band frequency Light Source Method to target material surface rapid thermal treatment, pass through the skin effect of rapid thermal treatment, recrystallize target material surface hardened layer, the stress and dislocation in hardened layer are eliminated, obtains the recrystallized structure basically identical with matrix.This method is simple for process, speed is fast, versatility is high, material is pollution-free suitable for different size targets, preparation process, spillage of material is small, and the method is environmentally protective.
Description
Technical field
The invention belongs to target processing technology of preparing fields, and in particular to a kind of surface treatment of high pure metal sputtering target material
Method.
Background technology
The metal sputtering target that semiconductor integrated circuit (IC) uses when machining (such as turning, grinding, mechanical polishing),
Common cobalt target, titanium target, included a tantalum target, nickel target and its alloy target material in hardened layer, particularly integrated circuit are always introduced, because material is hard
Degree is big, product size is big, and during surface turnery processing is carried out, cutter can be worn, and is cut after tool wear passivation
Reduced capability introduces a large amount of dislocations and stress in metal surface, increases surface layer roughness and hardness.The hardened layer of material surface
So that surface metal atoms work function increase during target as sputter, lead to that target as sputter speed is small, uniformity of film of initial stage sputtering
Difference.
In order to eliminate the influence of target material surface hardened layer, target will carry out pre-sputtering before formal use, also referred to as burn target.It burns
Target process is generally carried out sputtering and is removed skim-coat using high-power, and the material hardening layer of different-thickness needs the different burning target time,
This process results a large amount of time cost and material costs.Carry out largely to eliminate target material surface hardened layer researcher
It works, target material surface is processed in patent CN101700616, is sprayed in process using alcohol, pass through to polish and improve
Target finish, since alcohol is inflammable, this method is dangerous high；It is polished after target is machined in patent US6749103
Processing, then bite is carried out, this method needs pickling solution, and target easily corrodes target in acid solution soaking process
Back veneer material, operation difficulty is big and pollutes the environment；Using magnetron sputtering apparatus to target material surface in patent WO2008067150
Sputter process is carried out, eliminates target case-hardening layer, this method uses specific sputtering machine table to target as sputter, without general
Property.
Invention content
The purpose of the present invention is to propose to a kind of surface treatment methods of high pure metal sputtering target material, and target is under vacuum
Surface rapid thermal treatment is carried out, makes surface that shallow-layer recrystallization occur, eliminates case-hardening.Specific technical solution is as follows：
A kind of surface treatment method of high pure metal sputtering target material, includes the following steps：
1) target carries out surface accurate machining；
2) target obtained by step 1) carries out surface grinding, and then surface is cleaned；
3) target obtained by step 2) carries out surface rapid thermal treatment under vacuum；
The surface rapid thermal treatment uses continuous wave laser heat treating process, scanning beam method or non-coherent broad band frequency light
Source method.
Target material surface roughness≤0.8 μm in step 1) after accurate machining.
The scan mode of the continuous wave laser heat treating process and scanning beam method is overlap joint shuttle-scanning mode or spiral shell
Revolve scan mode.
The laser power of the continuous wave laser heat treating process be 1~3kW, laser defocus distance be 20~50mm, hot spot
A diameter of 10~50mm, sweep speed are 10~50mm/s, and the temperature of heating is 350~450 DEG C.
Target angle of inclination is 10 °~30 ° in the continuous wave laser heat treating process scanning process.
The beam spot power density of the scanning beam method is 1~3kW/cm2, sweep speed is 10~50mm/s,
Heating speed is 100~200 DEG C/s, and the temperature of heating is 350~450 DEG C.
The scan mode of the non-coherent broad band frequency Light Source Method is whole radiation mode, and non-coherent broad band frequency light source is halogen light
Lamp, arc lamp, graphite heater or infrared equipment.
The heating speed of the non-coherent broad band frequency Light Source Method is 50~100 DEG C/s, and the temperature of heating is 350~450 DEG C,
Soaking time is 1~10min.
Beneficial effects of the present invention are：The method that the present invention uses target material surface rapid thermal treatment, passes through rapid thermal treatment
Skin effect, recrystallize target material surface hardened layer, eliminate hardened layer in stress and dislocation, obtain basic with matrix
Consistent recrystallized structure.This method is simple for process, speed is fast, versatility is high, suitable for different size targets, preparation process
Material is pollution-free, spillage of material is small, and the method is environmentally protective.
Description of the drawings
Fig. 1 is the process flow for carrying out surface treatment figure of target in the present invention.
Fig. 2 is cobalt target longitudinal section micro-structure diagram in embodiment 1.
Fig. 3 is cobalt target longitudinal section micro-structure diagram in comparative example 1, and wherein a represents hardened layer.
Fig. 4 schemes for embodiment and cobalt target longitudinal section hardness profiles versus in comparative example.
Fig. 5 is embodiment and cobalt target sputtered film uniformity variation tendency comparison diagram in comparative example.
Specific embodiment
The present invention proposes a kind of surface treatment method of high pure metal sputtering target material, with reference to embodiment to the present invention
It is described further.
The preferred technical solution of the present invention is as follows：Target carries out accurate machining first, then carries out surface grinding processing,
Reduce the reflectivity of target material surface；Surface is cleaned later, removes surface contamination；Cleaned target is carried out under vacuum
Rapid thermal treatment eliminates target material surface hardened layer.The present invention solves cementation zone in existing machining technique and is difficult to eliminate
The problem of, and whole process speed is fast, does not interfere with target interior tissue and backboard performance.
(1) target precision machines：Target material surface carries out accurate machining, accurately processed in finishing passes the depth of cut with
Process rotating speed.Machining parameter will be controlled strictly to each target, be consistent the hardened layer of target, in this way, target into
The thickness for needing to recrystallize hardened layer is easier to control in row rapid thermal treatment process.
(2) surface grinding：Target is higher by Precision Machining rear surface reflectance, under these conditions according to fast speed heat
Processing carries out flash annealing, can be due to reflectance height, and target material surface, which absorbs infrared heat, to be reduced, it is difficult to carry out fast speed heat to surface
Processing.Therefore, it is necessary to be ground processing to target material surface, target material surface is made to form unrestrained transmitting, reflectivity reduces, subsequent
Heat can be absorbed well in surface short annealing heat treatment process.Grinding technics will reduce target material surface reflectivity and reach
Uniformly, unanimously, such target material surface can uniformly absorb heat in rapid thermal treatment.
(3) surface rapid thermal treatment：Using continuous wave laser heat treating process, scanning beam method or non-coherent broad band frequency light
Source method.Wherein non-coherent broad band frequency Light Source Method can be halogen lamp or arc lamp etc..It is fast that these types of method can be used for metal surface
Speed heat processing.Target material surface is cleaned before heat treatment, prevents surface contamination from influencing thermal treatment quality.Rapid thermal treatment process
Metal surface is made to be heated to close to recrystallization temperature, slight recrystallization occurs for metal surface, and surface layer dislocation is reduced, and hardness declines,
Metallic hardfacing layer tissue is after treatment close to interior tissue.After stopping heating, the heat that superficial layer is obtained passes through work
The heat transfer of part itself disperses rapidly, and heating surface is made to cool down quickly.Since cooling rate is fast, target interior tissue is not sent out substantially
Changing does not interfere with target entirety sputtering performance.The oxide layer of target material surface can cause paradoxical discharge in sputtering process to generate
Particle.To prevent target from being aoxidized in processing procedure, rapid thermal treatment process carries out under vacuum.In scanning process
Can overlap joint shuttle-scanning mode or spiral shell may be used for point type heat source according to the different scan mode of the formal character of heat source
Scan mode is revolved, simple scanning mode may be used for linear heat source, face formula heat source is added by the way of integrally irradiating
Heat.Heating process will ensure that target surface is heated evenly, unanimously.The speed of the temperature of heating, the time of heat preservation and scanning will be according to not
It is determined with the material category of target and the thin hardened layer on surface.
In the following, it is specifically described by taking the method that cobalt target is processed and is surface-treated as an example.
Embodiment 1
(1) surface accurate processing, the control finishing depth of cut and processing are carried out to cobalt target with the higher diamond tool of hardness
Rotating speed, depth of cut control in 0.5mm hereinafter, the control of machine tooling rotating speed is at 200 revolutions per seconds, the μ of processing rear surface roughness≤0.8
m；
(2) target material surface obtained by step (1) is made target material surface form unrestrained transmitting, is reduced table using wire drawing cloth milled processed
Face reflectance；Target material surface is cleaned, prevents surface contamination from influencing thermal treatment quality；
(3) under vacuum condition, carbon dioxide laser machine is using target table obtained by overlap joint shuttle-scanning mode scanning step (2)
Face, the power of laser machine are 2kW, and target tilts 15 ° in scanning process, prevents the light beam that surface is reflected from burning laser head；To carry
High laser heat treatment efficiency, laser defocus distance are 50mm, and spot diameter 13mm, sweep speed 40mm/s are heated to 420
DEG C, the target scanning process of one piece of a diameter of Φ 440mm takes around 5min.Target material surface recrystallizes, and eliminates material
Cementation zone.
Fig. 1 is the process flow for carrying out surface treatment figure of target.
Fig. 2 is cobalt target longitudinal section micro-structure diagram in embodiment 1.It can be seen from the figure that target surface layer and internal group
Knit no difference.
Embodiment 2
Step (1) and (2) are the same as embodiment 1；
(3) under vacuum condition, using electronics beam scanning metal targets sputter face, beam spot power density during heating surface
Control is in 2kW/cm2, heating speed is 100 DEG C/s, is heated to 420 DEG C, soaking time 10s makes metal surface be heated to again
It is more than crystallization temperature.Using spiral scan mode, sweep speed 40mm/s, one piece of a diameter of Φ 440mm target in scanning process
Material, scanning process take around 5min.Make target material surface that faster recrystallization occur, eliminate material surface work hardening layer.
Embodiment 3
Step (1) and (2) are the same as embodiment 1；
(3) under vacuum condition, rapid thermal treatment carries out metal targets sputter face using halogen lamp, mode of heating is whole for target surface
Body irradiates, and heating speed is 50 DEG C/s, is heated to 420 DEG C, soaking time 60s, target heat treatment time is irradiated model by halogen lamp
Influence is enclosed, Φ 440mm targets a diameter of to one piece irradiate, and take around 3min.Target material surface is recrystallized, is eliminated
Material surface work hardening layer.
Comparative example 1
High-purity cobalt target surface is subjected to accurate machining, the diamond cutter for selecting hardness higher carries out surface machining,
The control finishing depth of cut and rotating speed, depth of cut control is in 0.5mm hereinafter, the control of machine tooling rotating speed is processed at 200 revolutions per seconds
Rear surface roughness≤0.8 μm.Target hardening layer analysis is carried out after the processing of surface, Fig. 3 is that the cobalt target longitudinal section of comparative example 1 is microcosmic
Structure chart.
Fig. 4 schemes for embodiment and cobalt target longitudinal section hardness profiles versus in comparative example.It can be seen from the figure that embodiment 1,
The thin hardened layer of target material surface is declined in embodiment 2 and embodiment 3, and the target material surface of comparative example 1 hardening thickness
About 50 μm of degree.Treated that target can obtain film in homogeneous thickness at sputtering initial stage for three kinds of methods.
Fig. 5 is embodiment and cobalt target sputtered film uniformity variation tendency comparison diagram in comparative example.It can be seen from the figure that
The target of comparative example 1 is poor in sputtering initial film uniformity, and target uniformity of film after 7kWh is used just is changed
It is kind.The target as sputter 3.5kWh rear films thickness evenness of embodiment 1, embodiment 2 and embodiment 3 improves.Relative to comparative example
The burning target time of middle target reduces about 50% by the target burning target time of Surface heat-treatent.
Claims (5)
1. a kind of surface treatment method of high pure metal sputtering target material, which is characterized in that include the following steps：
1) target carries out surface accurate machining；
2) target obtained by step 1) carries out surface grinding, and then surface is cleaned；
3) target obtained by step 2) carries out surface rapid thermal treatment under vacuum；
The surface rapid thermal treatment uses continuous wave laser heat treating process, scanning beam method or non-coherent broad band frequency light source
Method；
The laser power of the continuous wave laser heat treating process be 1~3kW, laser defocus distance be 20~50mm, spot diameter
For 10~50mm, sweep speed is 10~50mm/s, and the temperature of heating is 350~450 DEG C；
The beam spot power density of the scanning beam method is 1~3kW/cm2, sweep speed is 10~50mm/s, and heating is fast
It spends for 100~200 DEG C/s, the temperature of heating is 350~450 DEG C；
The heating speed of the non-coherent broad band frequency Light Source Method is 50~100 DEG C/s, and the temperature of heating is 350~450 DEG C, heat preservation
Time is 1~10min.
2. according to the method described in claim 1, it is characterized in that, target material surface roughness in step 1) after accurate machining
≤0.8μm。
3. according to the method described in claim 1, it is characterized in that, the continuous wave laser heat treating process and scanning beam method
Scan mode be overlap joint shuttle-scanning mode or spiral scan pattern.
4. according to the method described in claim 1, it is characterized in that, target in the continuous wave laser heat treating process scanning process
Angle of inclination is 10 °~30 °.
5. according to the method described in claim 1, it is characterized in that, the scan mode of the non-coherent broad band frequency Light Source Method is whole
Body radiation mode, non-coherent broad band frequency light source are halogen light lamp, arc lamp, graphite heater or infrared equipment.
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| CN113001114B (en) * | 2021-03-01 | 2023-12-29 | 宁波江丰电子材料股份有限公司 | Turning method of rotary target sputtering surface |
| CN113073297B (en) * | 2021-03-23 | 2023-05-02 | 熔创金属表面科技(常州)有限公司 | Device for remanufacturing rotary silicon-aluminum target and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1504584A (en) * | 2002-11-28 | 2004-06-16 | 中国科学院力学研究所 | Laser strengthening and toughening method for interface between ground-mass and coating |
| CN102513789A (en) * | 2011-12-21 | 2012-06-27 | 宁波江丰电子材料有限公司 | Manufacturing method of tungsten target material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1504584A (en) * | 2002-11-28 | 2004-06-16 | 中国科学院力学研究所 | Laser strengthening and toughening method for interface between ground-mass and coating |
| CN102513789A (en) * | 2011-12-21 | 2012-06-27 | 宁波江丰电子材料有限公司 | Manufacturing method of tungsten target material |
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