CN109706431A - A kind of tantalum spattering target material, preparation method and magnetically controlled sputter method - Google Patents
A kind of tantalum spattering target material, preparation method and magnetically controlled sputter method Download PDFInfo
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- CN109706431A CN109706431A CN201910128676.1A CN201910128676A CN109706431A CN 109706431 A CN109706431 A CN 109706431A CN 201910128676 A CN201910128676 A CN 201910128676A CN 109706431 A CN109706431 A CN 109706431A
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- tantalum
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Abstract
The invention discloses a kind of tantalum spattering target material, preparation method and magnetically controlled sputter method, the average crystal grain diameter of the tantalum spattering target material is more than or equal to 20mm, and by mass percentage, purity is more than or equal to 99.995%.The tantalum spattering target material of the embodiment of the present invention has the crystal grain of larger size, reduces impurity content, improves the purity of tantalum spattering target material.Moreover, large-sized crystal grain makes that the calendering manufacturing procedure such as forging, rolling, heat treatment can be reduced when preparing tantalum spattering target material, reduces processing step, reduce production cost.
Description
Technical field
The present invention relates to sputtering target material, in particular to a kind of tantalum spattering target material, preparation method and magnetically controlled sputter method.
Background technique
Copper resistance is small, highly effective as integrated circuit wiring material, but since copper itself is active metal, exists
Diffuse to interlayer dielectric and cause pollute and fail the problem of, need between thin copper film and interlayer dielectric formed Ta film,
The diffusion barrier layers such as TaN film.
In general, Ta film, TaN film are formed a film by metal tantalum target magnetic control sputtering.At present it is known that is contained in included a tantalum target is various miscellaneous
Ta film when matter, gas componant, density, crystallite dimension, crystal planar orientation etc. are to sputtering, TaN film film forming speed, film thickness it is uniform
Property, particle generate etc. filming performances will cause influence.Traditional tantalum spattering target material often through vacuum melting, forging, anneal, roll
Prepared by the complicated technologies such as system, heat treatment, this preparation process is complicated, process is long, and process is caused to bring pollutant into, because
And tantalum target at least haves the defects that low purity, high production cost, stability are poor at present.
Summary of the invention
In order to solve the above technical problems, the embodiment of the invention provides a kind of tantalum spattering target material, preparation method and magnetic controls to splash
Shooting method.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
The embodiment of the invention provides a kind of tantalum spattering target material, the average crystal grain diameter of the tantalum spattering target material is more than or equal to
20mm, by mass percentage, purity are more than or equal to 99.995%.Further, the average crystal grain diameter of the tantalum spattering target material
For 20 ~ 150mm；
Or/and the purity of the tantalum spattering target material is more than or equal to 99.9995%.
Further, in the tantalum spattering target material: every kind of refractory metal impurity content is less than or equal to 1ppm mass, and every kind
Interstitial impurity is less than or equal to 0.02ppm mass, and every kind of radioimpurity radioactive impurity content is less than or equal to 0.0005ppm mass, by quality hundred
Divide than meter, gaseous impurity total content is less than 0.005%.
Further, the refractory metal impurity includes at least one of W, Mo, Zr, and the interstitial impurity includes
At least one of Fe, Ni, K, Na, S, P；The radioimpurity radioactive impurity includes U or/and Th, and the gaseous impurity includes in O, N, C
At least one.
Further, the average grain size of the tantalum spattering target material is greater than the thickness of the tantalum spattering target material.
The embodiment of the invention also provides a kind of preparation method of tantalum spattering target material, the tantalum spattering target material is above-mentioned tantalum
Sputtering target material；The preparation method comprising steps of
S10, tantalum blank is produced using method of smelting, the average crystal grain of the tantalum blank is more than or equal to 20mm；
S20, cutting processing is carried out to the tantalum blank, forms slab；
S30, the slab is heat-treated, obtains target blank；
S40, the target blank is finished, obtains the tantalum spattering target material.
Further, in step S10, the total impurities content of the tantalum blank is less than or equal to 10ppm.
Further, in step S20, the cutting processing is Cutting indexes or linear cutter, the thickness of the slab
For 5 ~ 15mm.
Further, in step S30, the temperature of the heat treatment is 1200 ~ 1400 DEG C.
Further, step S30 further include: by after the heat treatment slab and copper or copper alloy backing plate through Diffusion Welding
Or hot isostatic press welding is bound into the target blank.
The embodiment of the invention also provides a kind of magnetically controlled sputter methods, form sputtered film using above-mentioned tantalum spattering target material.
The tantalum spattering target material of the embodiment of the present invention has the crystal grain of larger size, reduces impurity content, improves tantalum and splash
It shoots at the target the purity of material.Moreover, large-sized crystal grain makes that forging, rolling, heat treatment equipressure can be reduced when preparing tantalum spattering target material
Prolong manufacturing procedure, reduce processing step, reduces production cost.Reduce quality fluctuation, ensure that the matter of tantalum spattering target material
Measure stability.
Detailed description of the invention
Fig. 1 is that tantalum spattering target material carries out XRD(X x ray diffraction in the embodiment of the present invention one) test of crystal grain orientation analysis
Hkl distribution map.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, rather than whole embodiments.Based on described the embodiment of the present invention, those skilled in the art institute
The every other embodiment obtained, belongs to the scope of the present invention.
The embodiment of the invention provides a kind of tantalum spattering target material, the average crystal grain diameter of tantalum spattering target material is more than or equal to
20mm, by mass percentage, purity are more than or equal to 99.995%.Further, the average crystal grain diameter of tantalum spattering target material is 20
~ 150mm, such as: the average crystal grain diameter of tantalum spattering target material is 20 ~ 120mm, such as: the average crystal grain diameter of tantalum spattering target material
For 50 ~ 150mm.Further, the purity of tantalum spattering target material is more than or equal to 99.9995%.
Again for example: the average crystal grain diameter of tantalum spattering target material be 20mm, 25mm, 30mm, 40mm, 50mm, 55mm, 60mm,
70mm、85mm、90mm、100mm、110mm、120mm、130mm、150mm。
Metal tantalum impurities of materials element is mainly distributed on crystal boundary, the crystalline substance that the embodiment of the present invention passes through raising tantalum spattering target material
Particle size reduces the impurity content in tantalum spattering target material, improves the purity of tantalum spattering target material.
In the embodiment of the present invention, in tantalum spattering target material: every kind of refractory metal impurity content is less than or equal to 1ppm mass, often
Kind interstitial impurity is less than or equal to 0.02ppm mass, and every kind of radioimpurity radioactive impurity content is less than or equal to 0.0005ppm mass, by quality
Percentages, gaseous impurity total content is less than 0.005%.
Further, the refractory metal impurity includes at least one of W, Mo, Zr, and the interstitial impurity includes
At least one of Fe, Ni, K, Na, S, P；The radioimpurity radioactive impurity includes U or/and Th, and the gaseous impurity includes in O, N, C
At least one.
In a specific embodiment of the invention, W content is less than or equal to 1ppm mass in tantalum spattering target material, and Mo content is small
In being equal to 1ppm mass, Zr content is less than or equal to 1ppm mass；Fe content be less than or equal to 0.02ppm mass, Ni content be less than etc.
In 0.02ppm mass, K content is less than or equal to 0.02ppm mass, and Na content is less than or equal to 0.02ppm mass, and S content is less than etc.
In 0.02ppm mass, P content is less than or equal to 0.02ppm mass；U content is less than or equal to 0.001ppm mass, and Th content is less than
Equal to 0.001ppm mass；By mass percentage, gaseous impurity, such as: O, N, C total content are less than 0.005%.Further, gas
Body impurity, such as: O, N, C total content are less than 0.001%.Experiments verify that by mass percentage, the tantalum of the embodiment of the present invention splashes
The content of various metal impurities and interstitial impurity element in material of shooting at the target is 30-50% lower than conventional tantalum spattering target material.
In some embodiment of the invention, the average grain size of tantalum spattering target material is greater than the thickness of tantalum spattering target material.It protects
It has demonstrate,proved tantalum spattering target material sputter face and the distribution of sputter face vertical direction all crystal grains is consistent with crystal planar orientation, ensure that tantalum sputters
Target life phase filming performance is consistent, improves the diffusion barrier layers forming thin film performance such as Ta film, TaN film.
The embodiment of the invention also provides a kind of preparation method of tantalum spattering target material, tantalum spattering target material is that above-mentioned tantalum sputters
Target；Preparation method comprising steps of
S10, tantalum blank is produced using method of smelting, the average crystal grain of tantalum blank is more than or equal to 20mm；
S20, cutting processing is carried out to tantalum blank, forms slab；
S30, slab is heat-treated, obtains target blank；
S40, target blank is finished, obtains tantalum spattering target material.
It in existing preparation method, needs by processes such as hammer cogging, rollings, in the preparation method of the embodiment of the present invention
It can be omitted the processes such as hammer cogging, rolling, simple process, production process are easily-controllable, pollution are not likely to produce, so being easier to make tantalum
The performance of sputtering target material reaches the technical requirements of semiconductor circuit diffusion barrier layer film.
Further, method of smelting is vacuum electron beam melting or other vacuum oriented solidification method of smelting.Tantalum blank
Average crystal grain is preferably 20 ~ 150mm, and further, the average crystal grain of tantalum blank is preferably 50 ~ 150mm.Such as: tantalum blank
Average crystal grain is 20mm, 30mm, 50mm, 80mm, 90mm, 100mm, 120mm, 130mm, 140mm, 150mm.In the present invention
In embodiment, in step S10, the total impurities content of tantalum blank is less than or equal to 10ppm.Further, with refractory metal impurity,
If the low metallurgical Ta powder of tungsten, molybdenum, content of niobium or/and tantalum item do raw material, general refractory metal impurity content control is in 1-
Within 5ppm mass, raw material produces big crystal grain by 2-3 vacuum electron beam melting or other vacuum oriented solidification melting techniques
Tantalum blank, such as tantalum ingot.
In other embodiments of the invention, in step S20, cutting processing is Cutting indexes or linear cutter, slab
With a thickness of 5 ~ 15mm.
In some other embodiment of the present invention, in step S30, the temperature of heat treatment is 1200 ~ 1400 DEG C.Further
Ground, step S30 further include: by after heat treatment slab and copper or copper alloy backing plate bind through Diffusion Welding or hot isostatic press welding
At target blank.Heat treatment is for eliminating stress, and specifically, slab eliminates stress through 1200-1400 DEG C of vacuum heat treatment, heat
Treated slab and copper or copper alloy backing plate are through Diffusion Welding or hot isostatic pressing (HIP) welding binding (Bonding) at target
Blank, then finished product tantalum spattering target material is fabricated to after numer centre Precision Machining.
The manufacture of the big crystal grain tantalum spattering target material of the embodiment of the present invention does not need to carry out the processes such as hammer cogging, rolling, work
Skill is simple, production process is easily-controllable, is not easy to generate pollution to material, reduces production cost, stable product quality is good.
The embodiment of the invention also provides a kind of magnetically controlled sputter methods, form sputtered film using above-mentioned tantalum spattering target material.
Magnetically controlled sputter method well-known to those skilled in the art can be used in specific magnetically controlled sputter method, will herein be described in detail.
Technical scheme is described further combined with specific embodiments below, it is to be understood that the present invention
It is not limited to following embodiment:
Embodiment one
Raw material is done no more than the metallurgical Ta powder and tantalum item of 5ppm mass with refractory metal impurity, such as tungsten, molybdenum, content of niobium,
Above-mentioned raw materials are fabricated to tantalum blank using the method for vacuum electron beam melting, the average crystal grain of tantalum blank is 22mm.Tantalum blank
Through Cutting indexes or linear cutter at the slab of 8mm thickness, slab eliminates stress through 1300-1400 DEG C of vacuum heat treatment,
Slab and copper backboard after heat treatment are bound into target blank through hot isostatic press welding, then make after numer centre Precision Machining
At finished product tantalum spattering target material.
Gained tantalum spattering target material average crystal grain diameter is 20mm, by mass percentage, purity 99.999%.It is resulting
The corresponding test result of tantalum spattering target material is shown in Table 1.
Obtained tantalum spattering target material target is installed on sputtering equipment, and is sputtered.And it sputters on substrate at thin
Film.The film resistor for measuring 50 points on substrate, calculates its standard deviation (σ), specific structure is shown in Table 2.Corresponding test result is shown in
Tables 1 and 2.
As shown in Figure 1, wherein hkl is Miller indices, i.e. the indices of crystallographic plane.The crystalline substance of the resulting tantalum spattering target material of the present embodiment
The predominance of crystal planes of grain is (200) and (400), wherein crystal face (200) distribution proportion concentrates on 40% or more, crystal face (400)
Distribution proportion concentrates on 20% or more.
Embodiment two
With with refractory metal impurity, the metallurgical grade tantalum item as tungsten, molybdenum, content of niobium are no more than 5ppm mass does raw material, utilizes
The method of vacuum electron beam melting produces tantalum blank, and the average crystal grain of tantalum blank is 100mm.Tantalum blank is cut through Cutting indexes or line
Cut the slab for being processed into 10mm thickness, slab eliminates stress through 1200-1300 DEG C of vacuum heat treatment, after heat treatment slab and
Copper alloy backing plate is bound into target blank through Diffusion Welding, then finished product tantalum spattering target is fabricated to after numer centre Precision Machining
Material.
Resulting tantalum spattering target material average crystal grain diameter is 100mm, by mass percentage, purity 99.9996%.Institute
The corresponding test result of tantalum spattering target material obtained is shown in Table 1.
Obtained tantalum spattering target material target is installed on sputtering equipment, and is sputtered on substrate into film.It measures on substrate
50 points of film resistor calculates its standard deviation (σ), and specific structure is shown in Table 22.
Embodiment three
With with refractory metal impurity, the metallurgical grade tantalum item as tungsten, molybdenum, content of niobium are no more than 5ppm mass does raw material, utilizes
The method of vacuum electron beam melting produces tantalum blank, and the average crystal grain of tantalum blank is 80mm.Tantalum blank is cut through Cutting indexes or line
Cut the slab for being processed into 10mm thickness, slab eliminates stress through 1200-1300 DEG C of vacuum heat treatment, after heat treatment slab and
Copper alloy backing plate is bound into target blank through Diffusion Welding, then finished product tantalum spattering target is fabricated to after numer centre Precision Machining
Material.
Resulting tantalum spattering target material average crystal grain diameter is 100mm, by mass percentage, purity 99.9998%.Institute
The corresponding test result of tantalum spattering target material obtained is shown in Table 1.
Obtained tantalum spattering target material target is installed on sputtering equipment, and is sputtered on substrate into film.It measures on substrate
50 points of film resistor calculates its standard deviation (σ), and specific structure is shown in Table 2.Corresponding test result is shown in Table 1.
The test result of three gained tantalum spattering target material of 1 embodiment one of table, embodiment two and embodiment
In 2 embodiment of table, embodiment two and embodiment three on substrate film thickness substep variation
As known from the above, in the embodiment of the present invention, from sputtering initial stage to later period film in distribution of resistance variation it is small (2.0% ~
2.4%), the variation of film thickness distribution is small, and quality of forming film and consistency are good.
In conclusion the tantalum spattering target material of the embodiment of the present invention can by the calendering manufacturing procedure such as removal forging, rolling
Secondary pollution of the calendering process to tantalum target is greatly decreased, guarantee tantalum spattering target material purity.Crystal grain in tantalum spattering target material
Size is greater than thickness, ensure that tantalum spattering target material sputter face and the distribution of sputter face vertical direction all crystal grains and crystal face take
To consistent, guarantee that tantalum sputter tantalum target life phase filming performance is consistent, improve diffusion barrier layer forming thin film performance；This hair
In bright embodiment, by improving the crystallite dimension and control crystal planar orientation of included a tantalum target, the electric discharge of tantalum spattering target material is effectively reduced
Voltage inhibits the voltage drift in film forming to be easy to produce plasma；In the preparation method of tantalum spattering target material, pass through
The calendering manufacturing procedure such as forging, rolling, heat treatment is reduced, quality fluctuation can be greatly decreased, reduce processing cost.The present invention is real
The tantalum spattering target material for applying example forms a film through magnetron sputtering to be tested, and filming performance reaches the skill of semiconductor circuit diffusion barrier layer film
Art requirement, quality of forming film and consistency are good.
Other operations according to an embodiment of the present invention and corresponding processing step are all to those skilled in the art
It is understood that and easy to accomplish, therefore is not described in detail.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of tantalum spattering target material, which is characterized in that the average crystal grain diameter of the tantalum spattering target material is more than or equal to 20mm, by matter
Percentages are measured, purity is more than or equal to 99.995%.
2. tantalum spattering target material according to claim 1, which is characterized in that the average crystal grain diameter of the tantalum spattering target material is
20~150mm；
Or/and the purity of the tantalum spattering target material is more than or equal to 99.9995%.
3. tantalum spattering target material according to claim 1, which is characterized in that in the tantalum spattering target material: every kind of high-melting-point gold
Belong to impurity content and be less than or equal to 1ppm mass, every kind of interstitial impurity is less than or equal to 0.02ppm mass, every kind of radioimpurity radioactive impurity content
Less than or equal to 0.0005ppm mass, by mass percentage, gaseous impurity total content is less than 0.005%.
4. tantalum spattering target material according to claim 3, which is characterized in that the refractory metal impurity includes W, Mo, Zr
At least one of, the interstitial impurity includes at least one of Fe, Ni, K, Na, S, P；The radioimpurity radioactive impurity includes U
Or/and Th, the gaseous impurity include at least one of O, N, C.
5. tantalum spattering target material according to claim 1, which is characterized in that the average grain size of the tantalum spattering target material is big
In the thickness of the tantalum spattering target material.
6. a kind of preparation method of tantalum spattering target material, which is characterized in that the tantalum spattering target material is any one of claim 1 to 5
The tantalum spattering target material；The preparation method comprising steps of
S10, tantalum blank is produced using method of smelting, the average crystal grain of the tantalum blank is more than or equal to 20mm；
S20, cutting processing is carried out to the tantalum blank, forms slab；
S30, the slab is heat-treated, obtains target blank；
S40, the target blank is finished, obtains the tantalum spattering target material.
7. preparation method according to claim 6, which is characterized in that in step S10, the total impurities content of the tantalum blank
Less than or equal to 10ppm.
8. preparation method according to claim 6, which is characterized in that in step S20, the cutting processing is Cutting indexes
Or linear cutter, the slab with a thickness of 5 ~ 15mm.
9. preparation method according to claim 6, which is characterized in that in step S30, the temperature of the heat treatment is 1200
~1400℃；
Or/and step S30 further include: by after the heat treatment slab and copper or copper alloy backing plate it is quiet through Diffusion Welding or heat etc.
Pressure welding, which connects, is bound into the target blank.
10. a kind of magnetically controlled sputter method, which is characterized in that formed using described in any one of claim 1 to 55 described in any item tantalum spattering target materials
Sputtered film.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114207179A (en) * | 2019-08-14 | 2022-03-18 | 霍尼韦尔国际公司 | Large grain tin sputtering target |
-
2019
- 2019-02-21 CN CN201910128676.1A patent/CN109706431A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114207179A (en) * | 2019-08-14 | 2022-03-18 | 霍尼韦尔国际公司 | Large grain tin sputtering target |
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