CN1746332A - Sputtering target and production method therefor - Google Patents
Sputtering target and production method therefor Download PDFInfo
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- CN1746332A CN1746332A CN 200510108996 CN200510108996A CN1746332A CN 1746332 A CN1746332 A CN 1746332A CN 200510108996 CN200510108996 CN 200510108996 CN 200510108996 A CN200510108996 A CN 200510108996A CN 1746332 A CN1746332 A CN 1746332A
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Abstract
A sputtering target which is produced after being gone through a mechanical grinding step, characterized in that, in its first embodiment, micro-cracks having depths and lengths of at least specified values are substantially eliminated when the sputter surface of this target is observed in section, and that, in its second embodiment, the sputter surface of a sputtering target produced after being undergone mechanical grinding is sputtered in advance before shipment. A sputtering target can be provided that effectively reduces arcing, especially, an initial arc generation, and significantly enhances an initial stability.
Description
This application is to be that September 13, application number in 2002 are the applying date: 02802919.4, denomination of invention is the division of female case of " sputtering target and preparation method thereof ".
Technical field
The method that the present invention relates to be used for sputter and film forming target and be used to make described target.
Technical background
So far, known sputtering method is one of film forming method.So-called sputtering method, normally rare gas element is to impact sputtering target under the plasmoid that constitutes in decompression, make the molecule that flies out from target and atomic deposition on base material by this energy, on base material, form film, this method is easy to form large area film and can obtains high performance membrane, therefore can be applicable to industrial.
In recent years, as the sputter mode, known have: carry out the reactive sputtering method of sputter and magnetite is set with the film forming magnetron sputtering method of high speed at back face of target in reactant gas.
In the film that forms by these sputtering methods, particularly contain Indium sesquioxide (In
2O
3) and stannic oxide (SnO
2) at least a oxide compound as the film (hereinafter referred to as " ITO " film) of main ingredient, because visible light transmission height, therefore electroconductibility is also high, is widely used as the nesa coating of liquid crystal indicator and prevents heating film and the infrared reflection film that the glass condensation is used.
The target that is used to form the ITO film is similar to other oxide compound target and equally makes.That is to say that target material is made by powder metallurgical technique (sintering process), this technology comprises the molding raw material powder, afterwards this moulding product of sintering; With the emery wheel that is about #200 described target material is carried out surface grinding then or carry out other mechanical workout make as profile mechanical workout as described in target.
But, when using the sputtering target that makes thus to form high performance thin film, have following problem.
That is, during sputter, particularly the sputter initial stage, can produce the paradoxical discharge (hereinafter being sometimes referred to as " initial arc ") that is called arcing (arcing), this not only damages into membrane stability and produces particle.And described particle adhesion also gathers thereon to sputtering target, forms the black deposit that is called knot grain (nodule), and this knot grain causes the light that generates electricity, and produces new particle thus.In addition, if this particle attached on the film, can make the film performance variation.
Therefore, when using new sputtering target, for fear of the problems referred to above, even be provided with described new sputtering target in the sputter equipment, thereby also must stop to produce electric arc and can make in for some time of goods and dally from beginning to be splashed to, this have influenced the raising of productivity.
Up to now, when grinding the target surface, more can reduce the generation of this arc-over and knot grain by abrasion.Therefore at present, the surface abrasion target with smooth surface becomes main flow.For example, Japanese Patent No.2750483 and No.3152108 communique have been put down in writing by its Roughness Surface on Control is prevented from produce the ITO sputtering target of electric arc and knot grain in specialized range.But for reaching the surfaceness of regulation, this method must be after the preparation target material, carry out rough grinding by mechanical mill,, progressively finally grind (abrasion) then to adjust its thickness, make the target surface smoothing, there is the long and high problem of cost of manufacturing time in this method.In addition,, initial arc can not be effectively prevented, and after new sputtering target is placed sputter equipment, the idle running of relative long period must be carried out even when use has the ITO target of regulation surfaceness.
This problem also exists in ceramic mould target or metal mold target, and described ceramic mould target makes by powder metallurgical technique (sintering process), and contains oxide compound, nitride, carbide and boride etc. except that ITO as main ingredient.
The present inventor furthers investigate these situations, found that in by the prepared sputtering target of mechanical mill operation, cause and be present in the lip-deep primary granule of target by grinding step etc., it partly is the major cause that causes electric arc and knot grain that thermal shocking during perhaps because of sputter forms particulate from sur-face peeling, therefore if remove these primary granules and part, can prevent the generation of initial arc.
The inventor after further research, found that no matter described part is that thermal shocking during by sputter is peeled off from upper layer and formed particle, or depend on the existence of the microfracture that forms to inside from the target surface by mechanical mill rather than described target surfaceness to a great extent.The inventor has been found that also all microfractures can not cause arc-over or knot grain, it is the major cause that causes the initial arc discharge that but the degree of depth and length are not less than the microfracture of prescribed value, therefore, can effectively prevent the generation of initial arc by fully removing this microfracture.Based on described discovery, finished the present invention.
Therefore, the purpose of this invention is to provide sputtering target and the method that is used to make described sputtering target, described sputtering target can prevent the generation of initial arc, and can significantly improve productivity in film shaped.
Summary of the invention
The sputtering target of first embodiment of the invention is the sputtering target of making by the mechanical mill operation, wherein, when the section of the sputtering surface of observing described target, substantially do not find that the degree of depth is not less than 15 microns and length and is not less than 40 microns, the degree of depth that suitable is is not less than 10 microns and length and is not less than 30 microns microfracture.In sputtering target, the degree of depth is not less than 5 microns and be not less than 10 microns but be preferably 5 or still less less than the quantity of 30 microns microfracture in 2.5 mm lengths of sectional width direction less than 10 microns and length.
The sputtering target of first embodiment of the invention should any one handles prepared sputtering target in sputter process, laser treatment and the dry etch process by its sputtering surface is carried out.
The sputtering target of first embodiment of the invention should comprise the target material by the powder metallurgic method preparation, and should contain in Indium sesquioxide and the stannic oxide at least a as main ingredient.
In the sputtering target of first embodiment of the invention, the surface roughness Ra of described sputtering surface can be not less than 1.0 microns.
The sputtering target of second embodiment of the invention is the sputtering target of making by the mechanical mill operation, and the sputtering surface of described sputtering target had carried out sputter process before shipment.
In the sputtering target of second embodiment of the invention, in sputter process, be applied to the integration electric energy (integrated electric energy) on the sputtering surface of sputtering target, be not less than 0.005 watt/centimetre
2Being advisable, better is to be not less than 0.01 watt/centimetre
2, be more preferably and be not less than 0.02 watt/centimetre
2
In the sputtering target of second embodiment of the invention, when the shipment of described target, should be on the sputtering surface of sputtering target the adhesive surface protective membrane.
The sputtering target of second embodiment of the invention is preferably the sputtering target that makes by sintering process.
The sputtering target of second embodiment of the invention should contain Indium sesquioxide as main ingredient, perhaps should contain oxide compound at least a in Indium sesquioxide and the stannic oxide (ITO).
The method of making the sputtering target of second embodiment of the invention comprises mechanical mill target surface, preferably the target surface that makes by sintering process; Before shipment, the sputtering surface at least of described target carries out sputter process then.
When the sputtering target of second embodiment of the invention is the ITO sputtering target, the method of making described ITO sputtering target comprises that mechanical mill makes ITO target surface by the material that sintering contains Indium sesquioxide and stannic oxide main ingredient, and the sputtering surface of described at least target carries out sputter process before shipment then.
Brief Description Of Drawings
Shown in Figure 1 is the synoptic diagram of the microfracture example found when observing described target sputtering surface section.
Implement best mode of the present invention
Below, the present invention is specifically described.
The sputtering target of the first embodiment of the invention and second embodiment all makes by the mechanical mill operation.
That is to say that sputtering target of the present invention only is the sputtering target that makes by the mechanical mill operation.The target material used to the present invention do not have particular restriction, and for example, it can be the ceramic mould target that contains oxide compound as main ingredient, nitride, carbide, boride etc., perhaps can be the target that is made by metal.The example of this target material comprises and contains In
2O
3And SnO
2In at least a material (ITO) as main ingredient, contain In
2O
3With at least a material (IZO), ZnO-Al among the ZnO as main ingredient
2O
3, In
2O
3, SnO
2, ZnO, Al
2O
3, SiO
2, Ta
2O
5, MgO, NiO, SiN
3, AlN, SiC, Mo, W, Cr, Ti, Zr, Hf, Nb, Ta and Al.Wherein, described ITO sputtering target especially can be effectively applied to first and second embodiments of the present invention, and its reason is in order to carry out sputter efficiently, to need high primary stability.
The method for preparing described target material there is not particular restriction, for example, described ceramic mould target can pass through sintering process (powder metallurgical technique) preparation, wherein, mixture with the raw material powder of given mixed feedstock production, perhaps homogenizing mixture of the raw material powder that makes by co-deposition method etc. carries out sintering then and carries out mechanical mill by known drying process of various routines or humidity method molding.For the situation of metal mold target, can use the dissolving of the mixture vacuum of raw material powder, cast then, the vacuum dissolution process of plastic working and mechanical mill; Or the mixture by HIP (hot isostatic pressing) method or CIP (isostatic cool pressing) method molding raw material powder, the powder metallurgical technique that carries out sintering and plastic working then.
The example of drying process comprises CP (colding pressing) method, HP (hot pressing) method and HIP (hot isostatic pressing) method.The CP method is raw material powder mixture to be packed into make moulding product in the mould the described moulding product of roasting under air atmosphere or oxygen atmosphere (sintering).The HP method is that the mixture of raw material powder is packed in the mould of electric furnace inside, carries out moulding and sintering under heating and pressurizing simultaneously.The HIP method is that raw material powder mixture or prefabricated component are sealed in the rubber sack or at high temperature form nappe with tinsel, inserts after the degassing in the container again, and the feeding inert media adds in isotropy depresses heat-agglomerating.
Damp process for example Japanese Patent discloses the filtering type method of forming of putting down in writing among the communique No.286002/1999.In the filtering type method of forming, use the filtering type shaping dies.Described filtration mould is the shaping dies of being made by non-water soluble material, obtains moulding product by the late water of decompression from the ceramic raw material slurries.As for this method, example is gone into the slurries of being made up of raw material powder mixture, ion exchanged water and organic additive in the filtering type shaping dies, and decompression removes to anhydrate from slurries down and prepares moulding product then, and with described moulding product drying, degreasing, sintering then.
Maturing temperature in above-mentioned each method should be according to raw materials used definite suitable temp.
After the raw material die for molding, sintering prepares target material as mentioned above, and described target material carries out mechanical mill such as surface grinding, to form given size or to grind its surface.That is to say that described sputtering surface is made by the mechanical mill operation usually at least.
On the target surface of making by the mechanical mill operation as mentioned above, usually there be primary granule or the part that produces by grinding step, they separate and become particle from upper layer by the thermal shocking sputter, and these particles are attached in sputter procedure in the substrate, form film defects; Perhaps adhere again on the target, gather thereon and form the black accumulation that is called the knot grain, it can cause arc-over further to form the gains in depth of comprehension particle thus.
Therefore among the present invention, make the sputtering surface of the sputtering target that makes by the mechanical mill operation carry out hereinafter described concrete processing, can remove, effectively reduce initial arc thus because of isolating particle of thermal shocking sputter and part.
First embodiment of invention
At first, first embodiment of the present invention is described.The characteristics of the sputtering target of first embodiment of the invention are: described sputtering target makes by the basic working procedure in the above-mentioned common process, and after making or in manufacturing processed, described sputtering target carries out the processing of the following stated, to remove microfracture.
Because described mechanical mill is that it excises the method for grinding work-piece by cutting the striker with the abrasive particle of high speed rotating emery wheel, because the contact stress of abrasive particle, inside at surface of target (especially carrying out the surface of sputter, hereinafter referred to as " sputtering surface ") and target forms the crack.As for described crack, those observed from the teeth outwards cracks are considered to grind damage or mechanical defect, still, and the micro-cracks (hereinafter referred to as " microfracture ") that does not have research to extend internally from sputtering surface.
As long as carry out described mechanical mill, inevitably microfracture can appear just, have nothing in common with each other though degree such as the shape (degree of depth, length etc.) and the quantity etc. of microfracture occur.The degree that microfracture takes place is subjected to the influence of the shape of the weight of used emery wheel in the mechanical mill and speed, abrasive particle and workpiece material etc.
In first embodiment of the invention, note this microfracture, and by removing the microfracture that the degree of depth and length are not less than prescribed value substantially, can provide the target that has effectively prevented to produce initial arc.
That is to say, not all these microfractures can not produce initial arc, but the degree of depth and the length microfracture that is not less than prescribed value can cause producing initial arc as mentioned above, therefore, by fully removing these specific microfractures, make when section is observed described target sputtering surface and can not find microfracture, can effectively prevent the generation of initial arc.
Especially, the sputtering target of first embodiment of the invention is the sputtering target that makes by the mechanical mill operation, wherein, when section is observed described target sputtering surface, substantially can not find that the degree of depth is not less than 15 microns and length and is not less than 40 microns microfracture, suitable is, its degree of depth is not less than 10 microns and length and is not less than 30 microns.
The removal of carrying out microfracture on described target " is not found microfracture " and is meant in statement used herein substantially, when observing described target sputtering surface when section, can not find that substantially the degree of depth and length are not less than the microfracture of prescribed value.
Specifically be meant, when section is observed described target sputtering surface, substantially do not find that in width r 2.5 mm length zones the degree of depth is not less than 15 microns and length and is not less than 40 microns crackle, suitable is, the degree of depth is not less than 10 microns and length and is not less than 30 microns microfracture.Even this means to have the degree of depth and the length microfracture less than above-mentioned value, this microfracture itself can not cause producing electric arc yet, and can not become the particle source yet, and this is because the thermal shocking of sputter can not bring fragment.
More specifically, when section is observed described target sputtering surface, require not find that the degree of depth and length are not less than the microfracture of prescribed value, and with 2.5 millimeters length-gauge on the sectional width direction, the degree of depth is not less than 5 microns but less than 10 microns, and length is not less than 10 microns but be 5 or still less less than the quantity of 30 microns microfracture, is preferably 3 or still less, is more preferably 1 or still less.
Certainly best is, when section is observed described target sputtering surface, even do not find that the degree of depth is not less than 5 microns but less than 10 microns, and length is not less than 10 microns but less than 30 microns microfracture, promptly with 2.5 millimeters length-gauge on the sectional width direction, the quantity of above-mentioned microfracture is 0.
But, when the quantity of described microfracture is 5 or still less, be preferably 3 or still less, be more preferably 1 or still less the time, can effectively reduce initial arc, like this, in sputter, just can not have problems.
Section is observed the microscopic instrument of the device of described target sputtering surface for (for example) use opticmicroscope, electron microscope or scanning electronic microscope (SEM).
The sputtering surface of described target has small projection and depression, and this is because described target has carried out the mechanical mill operation as mentioned above, and the degree of depth and the length that how to define microfracture become a problem.Therefore, below with reference to Fig. 1 the definition to the microfracture degree of depth and length in this specification sheets is described.
In this manual, as shown in Figure 1, the degree of depth of microfracture is the depth D of the top at crestal line (ridgeline) climax that forms of sputtering surface 1 corresponding from the zone that is existed by microfracture and section 3 to the position, deep of microfracture 5, described crestal line.
In this specification sheets, as shown in Figure 1, the length of microfracture is the maximum length L of microfracture 5 in the horizontal direction on the section 3.
The sputtering target of first embodiment of the invention only has does not have the degree of depth and length to be not less than the microfracture of prescribed value basically, and the surfaceness of sputtering target (arithmetic average roughness of roughness curve) Ra (recording according to JIS B0601 (1994)) can be not less than 1.0 microns, perhaps can be not less than 1.5 microns, perhaps be not less than 2.0 microns.
Therefore in the sputtering target of first embodiment of the invention, the target surface is not always need polish to think the reduction surfaceness, is different from conventional target, can cancel grinding steps.Therefore, described production method can be simplified, and can improve the productivity of target.
But its policy is that the present invention can use the Ra less than 1.0 microns.
Basically do not have the degree of depth and length to be not less than the target of the microfracture of prescribed value in order to obtain the sputtering target of first embodiment of the invention, promptly to have, need remove microfracture up to not finding aforesaid microfracture.
Method as for the target (removing microfracture) that obtains not have substantially microfracture can adopt any method that the method for fully removing microfracture is provided.For example, can on the sputtering surface of target, carry out strictly to control precise finiss, sputter process, laser treatment, dry etch process and the sandblasting of emery wheel weight or rotation rotating speed.
Wherein, considering from good target productivity, is good with sputter process, laser treatment and dry etch process.
With the method that tiny crack is removed in embodiment description below, this method is carried out sputter process for making the target surface.
When described sputter process during as the method for the target (removing microfracture) that obtains not have substantially microfracture, described sputtering condition such as sputter mode, sputter gas and air pressure there are not particular restriction, can suitably select as required.For example, should use as the rare gas element of argon gas and oxygen (if needs), and to set air pressure be 1-10 millitorr (mTorr) as sputter gas.
The integration electric energy (watt/centimetre that is used for sputter process
2), the integration electric energy of per unit area that promptly is used for the target of sputter process is preferably 0.1-10 watt/centimetre
2, be more preferably 0.5-5 watt/centimetre
2
When the integration electric energy that is applied is in above-mentioned scope, can remove microfracture basically, and it is good to make required time of target and throughput such as production cost.
Specifically, the target of making by the mechanical mill operation (can be bonded on the chassis) places the sputter equipment that uses the DC magnetron sputtering system, and use the sputter gas of above-mentioned composition to carry out sputter, up to reaching above-mentioned integration electric energy, can obtain the sputtering target of first embodiment of the invention thus.
In thus obtained sputtering target, when observing sputtering surface, section do not find that substantially the degree of depth and length are not less than the microfracture of prescribed value, and when using sputter that this target is used for when film shaped, described target can effectively prevent the generation of initial arc, and presents good initial arc performance.
When using target through above-mentioned processing to carry out when film shaped, promptly when using this target to carry out sputter, cumulative frequency that the initial arc performance of the sputtering target of first embodiment of the invention can occur according to electric arc and the integration electric energy that is applied (watt/centimetre
2) between relation estimate.The cumulative frequency that described electric arc occurs is measured by using μ Electric arc monitoring device (MAM Genesis is made by Landmark Technology Co.).In the use of sputtering target described in the first embodiment of the invention, the cumulative frequency that electric arc occurs is low, and described sputtering target presents good initial arc performance.
Second embodiment of the invention
Below, second embodiment of the invention is described.
Being characterized as of the sputtering target of second embodiment of the invention: before sputtering target manufacturers loads and transports, carried out sputter process through the target sputtering surface that obtains after the mechanical mill target material.
As mentioned above, the cause of described initial arc is that existence is easy to separating particles or part because of the sputter thermal shocking on the sputtering surface of the sputtering target that passes through the manufacturing of mechanical mill operation.
Therefore, easily can carry out sputter process by the sputtering surface itself that makes described sputtering target and remove, can reduce described initial arc effectively because of the isolating particle of sputter thermal shocking or part.
And in this case, no matter described part is separated because of the sputter thermal shocking, perhaps do not depend on the microfracture from the target surface to inside that forms because of mechanical mill, the degree of depth and length especially occurring, to be not less than the microfracture and the first embodiment of the invention of prescribed value similar.
Therefore in second embodiment and first embodiment of the invention similar, the sputtering surface of described sputtering target also should carry out sputter process in advance, and the target that does not have the degree of depth and length to be not less than the microfracture of prescribed value substantially is provided.But, and if do not require the performance that reaches this degree, described sputtering target is not limited thereto.
That is to say that in second embodiment of the invention, the integration electric energy that is applied on the sputtering surface that has carried out sputter process in advance is not less than 0.005 watt/centimetre
2Being advisable, better is to be not less than 0.01 watt/centimetre
2, be more preferably and be not less than 0.02 watt/centimetre
2, preferably be not less than 0.1 watt/centimetre
2Term used herein " integration electric energy (watt/centimetre
2) " be meant the integration electric energy of unit surface on the sputtering surface that before shipment, carries out being applied in the sputter process described target.
When described integration electric energy is not less than 0.005 watt/centimetre
2The time, the target that has carried out sputter process in advance presents good initial arc performance, and can effectively prevent the generation of described initial arc.Therefore on the use face of sputtering target, the sputter that is used for shaping surface can be not carrying out using described sputtering target to carry out immediately under the idle condition substantially, to improve film shaped productivity and effectively to carry out described film shaped.
The sputtering condition that carries out sputter process is not in advance had particular restriction, can under normal condition, carry out sputter up to reaching above-mentioned integration electric energy.
In second embodiment of the invention, the upper limit of integration electric energy does not have particular restriction, but from making required time of described sputtering target and productivity such as cost consideration, described integration electric energy should not be above 10 watts/centimetre
2
The initial arc performance of described target can be according to being 6 inches target carry out sputter the time when using diameter, applies integration electric energy (watt/centimetre
2) be not less than 10 seconds up to the interval that electric arc takes place and estimate.Specifically be, survey the electric arc when carrying out sputter process by using electric arc counter (making) by Landmark Technology Co., and to measure up to described diameter be the integration electric energy that the initial arc of 6 inches target is applied when assembling (converge), promptly up to the integration electric energy that electric arc occurs and occur once more being applied when interval between the electric arc is not less than 10 seconds.According to the observed value of integration electric energy, estimate described initial arc performance.When the value reduction of described integration electric energy, when perhaps the cumulative frequency that occurs when electric arc reduced, the initial arc performance of described target became better.
In second embodiment of the invention, the sputtering surface of described target carries out sputter in advance, and the surface roughness Ra that makes the target sputtering surface is usually greater than the initial value that records immediately after the mechanical mill.Therefore, the Ra of the sputtering target of second embodiment of the invention can be greater than 0.5 micron, and this is commonly referred to be suitable.Certainly, be not more than 0.5 micron Ra and can be used for second embodiment of the invention.
In specification sheets of the present invention, described surface roughness Ra is meant the arithmetic average roughness of the roughness curve that records according to JIS B 0601 (1994).
More particularly, when proceeding sputter, if do not consider the words of initial value, the Ra value of the sputtering target of second embodiment of the invention focuses on almost value, and the productivity from sputter process considers that the Ra value of described sputtering target can be the 0.1-5.0 micron, perhaps is the 0.1-3.0 micron.
The sputtering target of second embodiment of the invention is preferably the sputtering target with surface protection film, and described protective membrane is adhered on the sputtering surface after described sputtering surface carries out sputter process immediately.By described surface protection film is adhered on the sputtering surface, can prevent that the lip-deep impurity of target from adhering to or gas adsorption.
Described surface protection film only adheres at least on the sputtering surface, adhere to or gas adsorption to prevent the lip-deep impurity of target, but described surface protection film can be adhered on the whole target naturally.Can be by resin film being bonded to sputtering surface or sealing entire target with the resin film vacuum and come bonding described surface protection film.Wherein, should use vacuum to seal, this is because hardly can residual bubble between film and target.The described resin film that is used for surface protection film is not had particular restriction, but, do not contain peelable particulate resin film for better in order to prevent transfer of granules to sputtered film.
Below, the method for the sputtering target of making second embodiment of the invention is described.
Make the method for the sputtering target of second embodiment of the invention, it is characterized by: with the target surface, better be that mechanical mill is carried out on the target surface that sintering process makes, then before shipment, the sputtering surface of target at least carried out sputter process.
When the sputtering target of second embodiment of the invention is the ITO sputtering target, make being characterized as of method of ITO sputtering target: will contain Indium sesquioxide and stannic oxide and carry out mechanical mill as the surface that the raw material of main ingredient makes the ITO sputtering target, before shipment, make the sputtering surface at least of ITO sputtering target carry out sputter process then.
As for the method for the sputtering target of making second embodiment of the invention, the method for making conventional sputtering target is feasible, except the sputtering surface of sputtering target carries out sputter process.
That is to say, raw material is in die for molding, and carry out sintering or cast by the vacuum dissolution process by sintering process (powder metallurgical technique), prepare target material, make described target material carry out mechanical mill then, as surface grinding, it is formed give sizing or make described surface smoothing.After the mechanical mill, described target is bonded to usually and prepares sputtering target on the chassis.
For mechanical mill, can adopt suitable Ginding process as required, as surface grinding, rotation abrasion or sandblasting (blasting).After above-mentioned shaping thing ground, described surface is roughly ground and is regulated its thickness, the emery wheel that uses sand grains to reduce gradually then finish grindes (hereinafter being sometimes referred to as " abrasion "), further polish described surface, perhaps use granulated glass sphere, aluminum oxide globule, zirconia bead etc. to carry out sandblasting (sandblasting and correct grinding combine, and hereinafter are sometimes referred to as " abrasion ") as blast media.
In the method for the sputtering target of making second embodiment of the invention, sputter process then before shipment, is carried out with the sputtering surface of target at least in the described target of mechanical mill surface as mentioned above, makes described sputtering target.This sputter process can be carried out after roughly grinding, perhaps in correct grinding or sandblasting or carry out after it is bonded to the chassis.
By as mentioned above sputtering surface at least being carried out sputter, can remove because of grinding the burr that forms and crumb powder or, therefore, can effectively reducing described initial arc because of the sputter thermal shocking is easy to separated portions.
So according to, even the abrasion of face level is not always carried out on second embodiment of the invention target surface, do not reduce surfaceness even perhaps do not use the fine sand globule to carry out sandblasting, also can make the target that reduces initial arc and carry out effective sputter.That is to say, when using the target of second embodiment of the invention, can not make sputtering target by the target sputtering surface is carried out sputter process not denuding operation.
The invention effect
First embodiment of the invention can effectively reduce the generation of generation, the especially initial arc of the electric arc that the microfracture that formed by mechanical mill causes, and can significantly improve primary stability.And because described abrasion operation can be saved, the productivity of described target can be simplified and can be improved to production technique.
Second embodiment of the invention can obtain effectively to reduce the sputtering target that primary stability appears and improve in initial arc.By using this sputtering target to carry out sputter, can form the performance film efficiently with high productivity.And because described abrasion operation can be saved, described grinding technics can be simplified and can carry out under low cost.
Embodiment
Be described more specifically the present invention with reference to following embodiment, but the invention is not restricted to these embodiment.
The embodiment and the Comparative Examples of first embodiment of the invention at first, are described.
Preparation embodiment A 1
The preparation of target
Prepare the used target of embodiment A 1-A3 and comparative example A 1 in the following manner.
With In
2O
3Powder and SnO
2Powder was with 90: 10 weight % (In
2O
3: SnO
2) mixed.By described mixture, make the ITO sintered compact with common method, and described sintered compact is as target material.The relative density of described target material is 99.7%.
It is 8 sheets of 101.6 millimeters that described target material is cut into diameter.Then, they are placed on the identical surface grinder(lathe), and grind the sputtering surface of each sheet and bonded surface (adhesive surface), make thickness and respectively be 6 millimeters target No.a1-a8 with the #170 diamond wheel.
Embodiment A 1
Remove microfracture
Target No.a1 and a2 that preparation embodiment A 1 is made are bonded on the copper chassis separately.Then, described target is placed sputter equipment (EX-3013M is made by Shinkuu KiKai Kogyo K.K.), and carry out sputter process under the following conditions, to remove microfracture.
Sputtering condition:
Sputtering system: DC magnetron sputtering machine
Handle gas: Ar
Pressure during processing: 3 milli torrs
Oxygen partial pressure: 0.03 milli torr
Apply electric energy: 3 watts/centimetre
2
Apply the integration electric energy: 10 watts/centimetre
2
Press JIS B 0601 (1994), use surface roughness measuring gauge SE1700 (making) by KosaKa KenKysho measure sputter process under the following conditions before and the surfaceness of target No.a1 and a2 sputtering surface separately afterwards: the probe radius is 2 microns, input speed is 0.5 mm/second, and block (cut-off) c λ being 0.8 millimeter is 4 millimeters with the length of estimating.The results are shown in table 1.
The section of target is observed
Using grinding machine (being made by Okamoto Kosaku Kikai K.k.), is that 205 millimeters and thickness are that 1 millimeter #180 Buddha's warrior attendant cutters cut with the target No.a1 that carries out sputter process along its thickness direction diameter.
Then, use grinding machine (being made by Okamoto Kosaku Kikai K.k.), using diameter is that 205 millimeters and thickness are the cutting surface that 10 millimeters #600 diamond wheel grinds target No.a1.
Use single face refining mills (making) then, denude the cutting surface of target No.a1 with the shatter value grain of GC#1000 by speedfam Co..
Then, using single face refining mills (being made by Speedfam Co.), is the cutting surface of 0.1 micron diamond abrasive grain abrasion target No.a1 with median size.
Observe the cutting surface of target No.a1 by opticmicroscope (BX5-33P (being equipped with the speculum means of illumination), by Olympus opticalCo., Ltd. makes).The results are shown in table 1.
The evaluation of initial arc performance
To carry out sputter process similarly with target No.a1 removes the target No.a2 of microfracture and places sputter equipment (EX-3013M, make by Shinkuu KiKai Kogyo K.K.), and be the film shaped sputter process of carrying out under the following conditions, use the electric arc that produces in μ Electric arc monitoring device ((MAM Genesis is made by Landmark Technology Co.)) the monitoring sputter.Described sputtering condition and Electric arc monitoring condition are as follows.The results are shown in Table 1.
Sputtering condition:
Sputtering system: DC magnetron sputtering machine
Handle gas: Ar
Processing pressure: 3 milli torrs
Oxygen partial pressure: 0.02 milli torr
Apply electric power: 3 watts/centimetre
2
Integration electric energy: 5 watts/centimetre
2
μ Electric arc monitoring device measuring condition
Monitoring mode: energy
Electric arc monitoring voltage: 100V
High medium energy limit: 50mJ
Hard arc minimum time: 100 μ s
Embodiment A 2
Repeat the step of embodiment A 1, replace target No.a1 and a2 except using target No.a3 and a4, and in the sputtering condition, the integration electric energy that applies is from 10 watts/centimetre in removing the sputter process of microfracture
2Change 6 watts/centimetre into
2Outward.The results are shown in Table 1.
Embodiment A 3
Repeat the step of embodiment A 1, replace target No.a1 and a2 except using target No.a5 and a6, and in the sputtering condition, the integration electric energy that applies is from 10 watts/centimetre in removing the sputter process of microfracture
2Change 3 watts/centimetre into
2Outward.The results are shown in Table 1.
The comparative example A 1
Repeat the step of embodiment A 1, replace target No.a1 and a2, and do not carry out beyond microfracture removes except using target No.a7 and a8.The results are shown in Table 1.
Table 1
| Target number | The microfracture number * | Sputter front surface roughness (removing the crack) Ra (μ m) | Sputter rear surface roughness (removing the crack) Ra (μ m) | The electric arc frequency of occurrences (number of times) | |||
| D≥15 | D≥10 | D≥5 | |||||
| L≥40 | L≥30 | L≥10 | |||||
| Embodiment A 1 | a1 | 0 | 0 | 0 | 1.1 | 1.3 | - |
| a2 | - | - | - | 1.2 | 1.2 | 1 | |
| Embodiment A 2 | a3 | 0 | 0 | 1 | 1.1 | 1.1 | - |
| a4 | - | - | - | 1.0 | 1.2 | 2 | |
| Embodiment A 3 | a5 | 0 | 0 | 3 | 1.1 | 1.1 | - |
| a6 | - | - | - | 1.0 | 1.1 | 7 | |
| The comparative example A 1 | | 5 | 8 | 10 | 1.1 | - | - |
| a8 | - | - | - | 1.2 | - | 21 | |
*: D is the degree of depth (μ m) of microfracture.
L is the length (μ m) of microfracture.
Below, the embodiment of second embodiment of the invention is described.
Embodiment B 1
With In
2O
3Powder and SnO
2Powder was with 90: 10 (In
2O
3: SnO
2) mixed of weight %.By described mixture, make the ITO sintered compact with common method, and described sintered compact is as target material.It is after 6 inches the thin slice that described target material is cut into diameter, grinds each sheet with surface grinder(lathe) and will and want bonded surface (bonding surface) by the surface of sputter (sputtering surface), and its thickness is adjusted to 5 millimeters.Then, grind the sputtering surface of each sheet, make target No.b1-b4 with varigrained diamond wheel.Then, except described sputtering surface stands to use aluminum oxide as the sandblasting that blast media carries out, beyond the grinding that replaces carrying out with diamond wheel, identical as mentioned above mode prepares target No.b5.
Then, described target is bonded on the copper chassis separately, places the sputter equipment of self-chambering then, under following adjusting, carry out sputter.
Sputtering condition:
Sputtering system: DC magnetron sputtering machine
Handle gas: Ar
Processing pressure: 3 milli torrs
Oxygen partial pressure: 0.03 milli torr
Apply electric energy: 1.64 watts/centimetre
2
In above-mentioned sputtering operation, use μ Electric arc monitoring device (MAM Genesis, make by Landmark TechnologyCo.) under following monitoring energy model measuring condition, carry out arc detection as the electric arc counter:, arc detection voltage is 100V, high medium energy limit is 50mJ, the hard arc minimum time is 100 μ s, and measures the integration electric energy that is applied when described initial arc is assembled (become at interval up to described electric arc and be not less than 10 seconds).Then, proceeding sputter is 0.1 watt/centimetre up to described integration electric energy
2The results are shown in Table 2.
And, according to the surface roughness Ra of each target sputtering surface before JIS B 0601 (1994) the measurement sputter.The results are shown in Table 2.Use surface roughness measuring gauge SE1700 (being made by KosaKa KenKysho) measure surface roughness under the following conditions: the probe radius is 2 microns, and input speed is 0.5 mm/second, and blocking λ c and be 0.8 millimeter and evaluation length is 4 millimeters.
Table 2
| Sample number into spectrum | Relative density | Density (g/cm 3) | Sputter front surface roughness (removing the crack) Ra (μ m) | The integration electric energy that applies (watt/centimetre 2)*1 | The electric arc frequency of occurrences (number of times) * 2 |
| b1 | 99.1 | 7.09 | 0.35 | 0.0100 | 261 |
| b2 | 99.5 | 7.12 | 1.38 | 0.0120 | 1119 |
| b3 | 99.1 | 7.09 | 1.01 | 0.0073 | 740 |
| b4 | 99.3 | 7.10 | 0.79 | 0.0091 | 83 |
| b5 | 99.6 | 7.13 | 2.47 | 0.0064 | 1052 |
* 1: the integration electric energy that when the interval that electric arc occurs is not less than 10 seconds, is applied.
* 2: the frequency that electric arc occurs after the interval that electric arc occurs is not less than 10 seconds.
Embodiment B 2
Sample used in the Embodiment B 1 is taken out from the sputter equipment of self-chambering, carry out vacuum then and seal, and left standstill one day.Afterwards, with sample taking-up from described vacuum is sealed, placing above-mentioned self-chambering sputter equipment, carry out sputter under the sputtering condition identical with Embodiment B 1, is 5 watts/centimetre up to described integration electric energy
2, comprise the integration electric energy of Embodiment B 1.And, with surface roughness Ra before Embodiment B 1 identical mode is measured sputter process.The results are shown in Table 3.
Table 3
| Sample number into spectrum | The integration electric energy that is applied before the sputter (watt/centimetre 2) | Sputter process front surface roughness Ra (μ m) | The integration electric energy that applies (watt/centimetre 2)*1 | The electric arc frequency of occurrences (number of times) * 2 |
| b1 | 0.1 | 0.37 | 0.0004 | 2 |
| b2 | 0.1 | 1.35 | 0.0009 | 2 |
| b3 | 0.1 | 1.09 | 0.0005 | 3 |
| b4 | 0.1 | 0.81 | 0.0009 | 4 |
| b5 | 0.1 | 2.48 | 0.0004 | 2 |
* 1: be not less than the integration electric energy that was applied in 10 seconds up to the interval that electric arc occurs.
* 2: the frequency that electric arc occurs after the interval that electric arc occurs is not less than 10 seconds.
As seen from Table 3, the described sample that carries out sputter process has good initial arc performance, and this is fast because of concentrating immediately of electric arc after the sputter, and the frequency that electric arc occurs reduces.
Embodiment B 3
Sample used in the Embodiment B 2 being taken out from the sputter equipment of self-chambering, and then be placed in one, and carry out sputter under the sputtering condition identical with Embodiment B 1, is 6 watts/centimetre up to described integration electric energy
2, comprise the integration electric energy of Embodiment B 1 and B2.As a result, arbitrary target electric arc all can not occur at interval less than 10 seconds electric arc.And, with surface roughness Ra before Embodiment B 1 identical mode is measured sputter process.The results are shown in Table 4.
Table 4
| Sample number into spectrum | The integration electric energy that is applied before the sputter (watt/centimetre 2) | Sputter process front surface roughness Ra (μ m) | The integration electric energy that applies (watt/centimetre 2)*1 | The electric arc frequency of occurrences (number of times) * 2 |
| b1 | 5.0 | 2.01 | 0 | 0 |
| b2 | 5.0 | 1.74 | 0 | 0 |
| b3 | 5.0 | 2.23 | 0 | 0 |
| b4 | 5.0 | 2.92 | 0 | 0 |
| b5 | 5.0 | 2.36 | 0 | 0 |
* 1: be not less than the integration electric energy that was applied in 10 seconds up to the interval that electric arc occurs.
* 2: the frequency that electric arc occurs after the interval that electric arc occurs is not less than 10 seconds.
Industrial applicability
Sputtering target of the present invention can reduce the appearance of initial arc effectively, and is conducive to thus with acting on sputter and film shaped target.
Claims (16)
1. the sputtering target of making by the mechanical mill operation is characterized in that the sputtering surface of described sputtering target had carried out sputter process before shipment.
2. the described sputtering target of claim 1, the integration electric energy that it is characterized in that being input in sputter process on the sputtering target sputtering surface is not less than 0.005 watt/centimetre
2
3. the described sputtering target of claim 1, the integration electric energy that it is characterized in that being input in sputter process on the sputtering target sputtering surface is not less than 0.01 watt/centimetre
2
4. the described sputtering target of claim 1, the integration electric energy that it is characterized in that being input in sputter process on the sputtering target sputtering surface is not less than 0.02 watt/centimetre
2
5. each described sputtering target of claim 1-4 is characterized in that surface protection film being adhered on the sputtering surface of sputtering target when the described target of shipment.
6. each described sputtering target of claim 1-4 is characterized in that described sputtering target makes by sintering process.
7. each described sputtering target of claim 1-4 is characterized in that described sputtering target contains Indium sesquioxide as main ingredient.
8. each described sputtering target of claim 1-4 is characterized in that described sputtering target is to contain oxide compound at least a in Indium sesquioxide and the stannic oxide (ITO).
9. the described sputtering target of claim 5 is characterized in that described sputtering target makes by sintering process.
10. the described sputtering target of claim 5 is characterized in that described sputtering target contains Indium sesquioxide as main ingredient.
11. the described sputtering target of claim 6 is characterized in that described sputtering target contains Indium sesquioxide as main ingredient.
12. the described sputtering target of claim 5 is characterized in that described sputtering target is to contain oxide compound at least a in Indium sesquioxide and the stannic oxide (ITO).
13. the described sputtering target of claim 6 is characterized in that described sputtering target is to contain oxide compound at least a in Indium sesquioxide and the stannic oxide (ITO).
14. make the method for the described sputtering target of claim 1, described method comprises mechanical mill target surface, before shipment, makes the sputtering surface at least of described target carry out sputter process then.
15. the method for the described manufacturing sputtering target of claim 14 is characterized in that described target makes by sintering process.
16. make the method for the described sputtering target of claim 14, described method comprises that mechanical mill contains Indium sesquioxide and the stannic oxide surface as the prepared ITO target of the material of main ingredient by sintering, before shipment, make the sputtering surface at least of described ITO target carry out sputter process then.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001283658A JP2003089869A (en) | 2001-09-18 | 2001-09-18 | Sputtering target, and production method therefor |
| JP2001283658 | 2001-09-18 | ||
| JP2001376247 | 2001-12-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB028029194A Division CN100457961C (en) | 2001-09-18 | 2002-09-13 | Sputtering target, and production method therefor |
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| Publication Number | Publication Date |
|---|---|
| CN1746332A true CN1746332A (en) | 2006-03-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510108996 Pending CN1746332A (en) | 2001-09-18 | 2002-09-13 | Sputtering target and production method therefor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105555997A (en) * | 2014-03-27 | 2016-05-04 | 吉坤日矿日石金属株式会社 | Tantalum sputtering target and production method therefor |
| CN105925942A (en) * | 2015-02-27 | 2016-09-07 | Ｊｘ金属株式会社 | Sputtering Target And Manufacturing Method Of Sputtering Target |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006316339A (en) * | 2005-04-12 | 2006-11-24 | Kobe Steel Ltd | Aluminum-based sputtering target |
| JP4948633B2 (en) * | 2010-08-31 | 2012-06-06 | Ｊｘ日鉱日石金属株式会社 | Indium target and manufacturing method thereof |
| JP4948634B2 (en) | 2010-09-01 | 2012-06-06 | Ｊｘ日鉱日石金属株式会社 | Indium target and manufacturing method thereof |
| JP5140169B2 (en) | 2011-03-01 | 2013-02-06 | Ｊｘ日鉱日石金属株式会社 | Indium target and manufacturing method thereof |
| JP5026611B1 (en) | 2011-09-21 | 2012-09-12 | Ｊｘ日鉱日石金属株式会社 | Laminated structure and manufacturing method thereof |
| JP5074628B1 (en) | 2012-01-05 | 2012-11-14 | Ｊｘ日鉱日石金属株式会社 | Indium sputtering target and method for manufacturing the same |
| KR20160085907A (en) | 2012-08-22 | 2016-07-18 | 제이엑스금속주식회사 | Cylindrical indium sputtering target and process for producing same |
| US9922807B2 (en) | 2013-07-08 | 2018-03-20 | Jx Nippon Mining & Metals Corporation | Sputtering target and method for production thereof |
-
2001
- 2001-09-18 JP JP2001283658A patent/JP2003089869A/en active Pending
-
2002
- 2002-09-13 CN CN 200510108996 patent/CN1746332A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105555997A (en) * | 2014-03-27 | 2016-05-04 | 吉坤日矿日石金属株式会社 | Tantalum sputtering target and production method therefor |
| CN105555997B (en) * | 2014-03-27 | 2017-09-26 | 吉坤日矿日石金属株式会社 | Tantalum spattering target and its manufacture method |
| CN105925942A (en) * | 2015-02-27 | 2016-09-07 | Ｊｘ金属株式会社 | Sputtering Target And Manufacturing Method Of Sputtering Target |
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|---|---|
| JP2003089869A (en) | 2003-03-28 |
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