CN102808150A - Cu-Ni-Nb ternary alloy film with low resistivity and high chemical inertia and preparation process thereof - Google Patents
Cu-Ni-Nb ternary alloy film with low resistivity and high chemical inertia and preparation process thereof Download PDFInfo
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Abstract
The invention provides a Cu-Ni-Nb ternary alloy film with low resistivity and high chemical inertia and a preparation process thereof, and belongs to the field of materials. Under the guidance of a cluster model of a stable solid solution, the selection and the addition quantity of alloying elements in the Cu film are determined, and factors such as the enthalpy of mixing, a cluster structure and atomic radius dimension are comprehensively considered, so that the solid solution alloy film with relatively high thermal stability and relatively low chemical reaction activity is formed. By adopting a solid solution structure, resistivity rising caused by mass precipitation of solute elements is avoided; due to the introduction of an element Nb with a large atomic radius, interdiffusion between Cu and surrounding media can be effectively blocked; and due to the proportional addition of the second group of elements Ni, the addition quantity of Nb can be greatly reduced, thereby reducing an electron scattering effect caused by large atom selves to a large extent, facilitating the stabilization of the Cu film and guaranteeing that the resistivity of the Cu film is minimally influenced. The Cu-Ni-Nb ternary alloy film can be expected to simultaneously have a diffusion blocking effect as well as high temperature stability.
Description
Technical field
The present invention relates to a kind of have low-resistivity and high chemically inert Cu-Ni-Nb ternary alloy film and preparation technology thereof, Cu-Ni-Nb ternary alloy film is its main alloy element with Ni, need add a small amount of the 3rd constituent element Nb simultaneously, belongs to field of new.
Background technology
Copper has low resistivity and deelectric transferred preferably ability, is widely used in the various VLSI as the interconnection line metal.Yet, the diffusion of Cu with and and surrounding medium between the reaction problem hinder it always and bring into play premium properties to greatest extent, such as, Cu just can react with silicon or silicon oxide etc. down in lower temperature (about 200 ℃), causes the electron device damage.Need around the Cu lead, add diffusion impervious layer in order to address the above problem.Development along with large-scale integrated circuit; Dwindling gradually of device feature size; Require the thickness of diffusion impervious layer also will reduce accordingly; In the yardstick of several nanometers, promptly will reach the diffusion barrier effect and keep higher thermostability again, traditional diffusion impervious layer preparation technology has run into very big difficulty.Therefore proposed to make the method for electroplating the preceding Cu seed layer alloying of Cu lead; The characteristics of this method are to prepare diffusion impervious layer specially; Select certain alloy element when sputter copper seed layer, directly to add; The amount of element that adds will be seldom and not with Cu chemical combination, make it play the diffusion barrier effect, to the overall resistivity of interconnection line not had a negative impact when improving thermostability.
In the early stage research, selected alloying element is generally more intense with the oxygen binding ability, for example Mg and Al, after the thermal treatment, can be on the film top layer and the interface form the thin passivation layer of one deck, compare with pure Cu film, film base interface binding ability strengthens.But the interface passivation layer relatively thick (about 20nm) that forms like this, along with the reducing gradually of chip features size (＜45nm), they can't satisfy the development of interconnection technique.
Existing document is main in copper, to add the insoluble metal element with thick atom radius mainly.Because of adding the low solid solubility of metallic element, so it mainly is in outside the Cu lattice, crystal boundary and film defects etc. is located.Can when stopping the Cu diffusion, improving film heat stability, reduce effectively like this because the resistivity that the copper crystal lattice distortion causes increases.But in practical study, find; The pinning effect of second phase of separating out makes that a large amount of column crystal, dislocation and crystal boundaries can't be eliminated in the sputter attitude film; Increased the electron scattering of copper film on the contrary, finally caused the resistivity of sputter Cu film not to be reduced to desirable category through subsequent anneal.
Actually rare for the research of in the Cu film, adding the Nb element separately at present, people such as T. Mahalingam
[2]On the sheet glass that cleaned, plated and contain the different Cu film of Nb atomic percent, the copper film resistivity that wherein contains Nb2.7at.% is minimum, but still maintains higher level.It is thus clear that it is unsatisfactory directly in sputter Cu film, to add Nb result.
In addition, the addition of insoluble metal element is difficult to confirm.Addition does not then reach the effect of effective diffusion barrier very little, addition too much then resistivity obviously increase.How to design the addition that adds element, lack the theoretical direction foundation.
Based on above-mentioned deficiency, the present invention proposes based on the dual element of stablizing sosoloid group clustering model and add the alloying novel method altogether, through selecting the appropriate collocation of two dvielements, preparation has low-resistivity and high chemically inert alloying Cu film.
Summary of the invention
The present invention is in order to overcome the deficiency of the no diffusion impervious layer Cu film that has the refractory element interpolation now, and the dual element that preparation has high unreactiveness, low-resistivity adds ternary Cu alloy film altogether.
Technical scheme of the present invention is: a kind of have low-resistivity and a high chemically inert Cu-Ni-Nb ternary alloy film, in the Cu film, adds the Ni and the Nb of certain atomic percent, and Ni is as solid solution element, and Nb is as the diffusion barrier element; Nb and Cu are positive enthalpy of mixing 3 kJ/mol, are negative enthalpy of mixing-30 kJ/mol with Ni; It is 0.02 ~ 0.70% that the adding proportion of Nb/Ni keeps the atomic percent proportional range; The atomic percent that NiNb adds total amount is 0.20 ~ 1.50%.
Described preparation technology with low-resistivity and high chemically inert Cu-Ni-Nb ternary alloy film adopts the following step:
(1) preparation alloy sputtering target, its step is following:
1. get the raw materials ready: according to Ni recited above, Nb atomic percent, take by weighing each constituent element value, for use, the purity of Ni, Nb raw metal is more than 99.99%;
2. the melting of Ni-Nb alloy pig: the compound of metal is placed in the water jacketed copper crucible of smelting furnace, adopts the method for vacuum arc melting under the protection of argon gas, to carry out melting, at first be evacuated to 10
-2Pa, charging into argon gas to air pressure then is 0.03 ± 0.01MPa, the span of control of melting current density is 150 ± 10A/cm
2, after the fusing, continuing 10 seconds of melting again, outage lets alloy be cooled to room temperature with copper crucible, then with its upset, places again in the water jacketed copper crucible, carries out the melting second time; Aforementioned process melt back at least 3 times obtains the uniform Ni-Nb alloy pig of composition;
3. the preparation of Ni-Nb alloy bar: the Ni-Nb alloy pig is placed in the water jacketed copper crucible that is connected with negative pressure suction casting equipment, under argon shield,, at first be evacuated to 10 with above-mentioned vacuum arc melting method molten alloy
-2Pa, charging into argon gas to air pressure then is 0.03 ± 0.01MPa, the used current density of melting is 150 ± 10A/cm
2, after the fusing, continuing 10 seconds of melting again, the negative pressure absorbing and casting device is opened in outage simultaneously, lets alloy melt charge in the cylindrical, copper model cavity, is cooled to room temperature, obtains the Ni-Nb alloy bar of certain specification;
4. the preparation of alloy paster: the alloy small pieces that alloy bar are cut into desired thickness with the low speed saw;
5. the preparation of alloy sputtering target: using conductive silver glue that the Ni-Nb alloy slice is sticked on the used purity of sputter is on the 99.999% basic Cu target, and perhaps the Ni-Nb alloy slice directly being mounted to foraminous purity is to process the combined alloy sputtering target material on the 99.999% basic Cu target.
(2) the polynary codoped Cu film of preparation, its step is following:
1. the Si substrate of magnetron sputtering film preparation cleans; The monocrystalline silicon piece of (100) orientation earlier through acetone, alcohol and deionized water ultrasonic cleaning, is put into 5% HF then and soaked 2～3 minutes, adopt N
2Put into Vakuumkammer after drying up;
2. magnetron sputtering equipment extracting vacuum; After sample and target were all put into Vakuumkammer, the plant machinery pump slightly was evacuated to below the 5Pa, adopted molecular pump to carry out essence then and vacuumized, and vacuum tightness is evacuated to 5.4 * 10
-4Pa;
3. after vacuum tightness reaches required high vacuum, charge into argon gas to the air pressure 2Pa, let the target build-up of luminance; Regulate argon flow amount then to 8.0Sccm, operating air pressure modulation 0.4Pa, sputtering power 75w; Target-substrate distance is 8-12cm, and sputtering time is 25min, after sputter finishes; Apparatus cools 30min takes out ternary Cu alloy firm sample.
Technique scheme selects Ni as main alloy element, and itself and Cu dissolve each other fully, add an amount of thick atom radius diffusion barrier element nb simultaneously, and preparation Cu-Ni-Nb film is measured alloy Cu membrane resistance rate and thermostability.Because the complete solid solution of alloy element or most solid solution make the Cu film have higher thermostability and low chemical reactivity in the Cu lattice, avoided because the resistivity that causes of separating out in a large number of solute element raises; The introducing of thick atom radius element nb can effectively stop the mutual diffusion between Cu and the surrounding medium; With the proportional interpolation of the second constituent element Ni addition of Nb is reduced significantly; Thereby cut down the electron scattering effect that thick atom itself causes largely, helped stablizing the Cu film and guarantee that simultaneously its resistivity receives minimum influence.Can expect that such alloy has diffusion barrier effect and high-temperature stability simultaneously.
Advantage of the present invention is: the selection and the addition that 1. do not have diffusion impervious layer Cu film interalloy element all carry out under theory instructs; Take all factors into consideration factors such as enthalpy of mixing, group's clustering architecture and atomic size, prepared the alloying Cu film that solid solution element Ni and diffusion barrier element nb add altogether.2. dual element adds the characteristic that the Cu alloy firm has stable sosoloid altogether; After the 400 ℃/40h annealing; Grain growth resistivity is still kept lower level in the film; Crystal grain is grown up in annealing process very soon, can eliminate the electron scattering effect that dislocation and crystal boundary etc. increase largely, makes resistivity keep lower level.3. the addition of diffusion barrier element nb is greatly reduced; Can be reduced to 0.01at % (0.03wt %); The electron scattering that the attenuating thick atom of the very big degree of this meeting causes itself helps when stablizing the Cu film, keeping its resistivity to receive minimum influence.
Embodiment
Be described in detail specific embodiment of the present invention below in conjunction with technical scheme.
Be Cu below with the composition
99.68Ni
0.29Nb
0.03(atomic percent) [Cu
99.69Ni
0.27Nb
0.04(weight percent)] tell about step of preparation process for example:
The first step, preparation combined alloy target
Get the raw materials ready: according to the Ni in the design mix, Nb composition, take by weighing each constituent element value, for use, the purity requirement of Ni, Nb raw metal is more than 99.99%;
The melting of Ni-Nb alloy pig: the compound of metal is placed in the water jacketed copper crucible of arc-melting furnace, adopts the non-consumable arc melting method under the protection of argon gas, to carry out melting, at first be evacuated to 10
-2Pa, charging into argon gas to air pressure then is 0.03 ± 0.01MPa, the span of control of melting current density is 150 ± 10A/cm
2, after the fusing, continuing 10 seconds of melting again, outage lets alloy be cooled to room temperature with copper crucible, then with its upset, places again in the water jacketed copper crucible, carries out melting second time, and melt back like this at least 3 times obtains the uniform Ni-Nb alloy pig of composition;
The preparation of Ni-Nb alloy bar: the Ni-Nb alloy pig is placed in the water jacketed copper crucible that is connected with negative pressure suction casting equipment, under argon shield,, at first be evacuated to 10 with non-consumable arc melting method molten alloy
-2Pa, charging into argon gas to air pressure then is 0.03 ± 0.01MPa, the used current density of melting is 150 ± 10A/cm
2, after the fusing, continuing 10 seconds of melting again, the negative pressure absorbing and casting device is opened in outage simultaneously, and draught head is 0.01 ± 0.005MPa, lets alloy melt charge in the cylindrical, copper model cavity, is cooled to room temperature, obtains diameter and be the Ni-Nb alloy bar of specification such as 3mm;
The preparation of alloy paster: alloy bar is cut into the alloy small pieces that thickness is about 1mm with the low speed saw.
The preparation of alloy sputtering target: the Ni-Nb alloy slice is sticked on the used basic target of sputter with conductive silver glue---purity 99.999% is processed the combined alloy sputtering target material on the Cu target.
The Si substrate of second step, magnetron sputtering film preparation cleans
The monocrystalline silicon piece of (100) orientation earlier through acetone, alcohol and deionized water ultrasonic cleaning, is put into 5% HF then and soaked 2～3 minutes, adopt N
2Put into Vakuumkammer after drying up.
The 3rd step, magnetron sputtering equipment extracting vacuum
After sample was put into Vakuumkammer, the plant machinery pump slightly was evacuated to below the 5Pa, adopted molecular pump to carry out essence then and vacuumized, and vacuum tightness is evacuated to 5.4 * 10
-4Pa.
The 4th step, sputter procedure
After vacuum tightness reaches required high vacuum, charge into argon gas to the air pressure 2Pa, let the target build-up of luminance, regulate argon flow amount then to 8.0 sccm, operating air pressure modulation 0.4Pa, sputtering power 75W, target-substrate distance are about 10cm.The not also inartificial cooling of heating of substrate during sputter.Sputtering time is 25min, after sputter finishes, behind the apparatus cools 30min, takes out Cu alloy firm sample.The step appearance records the about 350nm of film thickness.For preventing the sample oxidation, after the sample sputter is accomplished, do not take out as early as possible, take out sample after half a hour again with apparatus cools.
The 5th step, annealing
Adopt vacuum annealing, vacuum tightness is superior to 7 * 10
-4Pa, temperature rise rate are about 1 ℃/s, naturally cooling during cooling.At first respectively 400 ℃, 500 ℃, 600 ℃ annealing 1 hour.Further under 500 ℃, carry out long-time cycle annealing: 10 hours for one-period, carries out 4 cycles totally 40 hours long term annealings.
The 6th step, analysis
Adopt the EPMA-1600 electron microprobe examination monitoring thin film composition of day island proper Tianjin company, adopt German Brooker D8 discover film X-ray diffractometer (XRD), Philips Technai G2 type transmission electron microscope that film is carried out microstructure analysis.Adopt two electrical measurement four point probe testers that the square resistance of Cu-Ni-Nb film before and after the annealing is measured.
The content of each Cu, Ni, three kinds of elements of Nb is followed successively by in the EPMA analysed film, 99.68 at.%, 0.29 at.%, 0.03 at.%.The atomic ratio of Ni, Nb is 12:1.2.Total doping in the Cu film is 0.32 at.%.Getting alloying constituent at last is Cu
99.68Ni
0.29Nb
0.03(atomic percent) Cu
99.69Ni
0.27Nb
0.04(weight percent).
XRD result shows that the Cu-Ni-Nb film is respectively 400 ℃, 500 ℃, 600 ℃ annealing 1 hour; Cu is main diffraction peak; 400 ℃ of long-time vacuum annealings are after 40 hours; Still the diffraction peak of having only Cu does not detect the diffraction peak of Cu-Si compound, shows that the thermal stability of Cu-Ni-Nb film is good.X-ray diffraction spectrum before and after contrast is annealed in addition, can find: the halfwidth degree of 1.Cu diffraction peak obviously reduces, and crystal grain is obviously grown up.This and the simple Nb that adds, Ru etc. are different with the situation of the immiscible element of copper: Nb, elements such as Ru are in copper film and separate out attitude; Become second phase that hinders grain growth; Therefore research shows that the columnar crystal structure of sputter copper film can remain to higher temperature, and annealing grains is not obviously grown up.Abundant residues stress can not merge recovery in the growth at crystal grain, and crystal boundary makes that too much the resistivity of this binary Cu alloy firm is all very high.2. anneal in differing temps and time, the Cu peak position does not all have obviously to move, and this shows that lattice parameter keeps stablizing constant.These two phenomenons are all explained, add in the element annealing process and from copper crystal lattice, do not separate out, and keep stablizing the structure of sosoloid.
TEM results shows, mainly is the about 20～30nm column crystal of width in the Cu alloy firm under the sputter attitude, film and matrix the thick intrinsic silicon oxide amorphous layer of one deck～3nm arranged at the interface.Cross-sectional sample after the 500 ℃/40h annealing shows, film still keeps concordant, even at the interface, do not have hole with matrix, does not have the generation of Cu-Si compound; Intrinsic interface amorphous layer thickens～5nm simultaneously; Columnar crystal structure disappears, and crystal grain grows up to bulk crystal grain gradually, and is consistent with XRD result.
Shown in the subordinate list 1, the Cu-Ni-Nb film resiativity reduces the trend that afterwards increases earlier along with the rising of annealing temperature appears, and resistivity is minimum when 500 ℃/1h, is about 2.73 μ Ω-cm, and the back of 600 ℃/1h annealing subsequently resistivity raises slightly, is about 2.74 μ Ω-cm.Select 500 ℃ of Detection of Stability temperature commonly used, resistivity is still kept lower level behind the annealing 40h, is about 2.77 μ Ω-cm.So the sosoloid Cu alloy film under this clustering model instructs has effectively been protected the continuity of Cu layer, has stopped the Cu-Si mutual diffusion, has guaranteed the electric property that it is good simultaneously.
Through above-mentioned experimental analysis; Is the allusion quotation example with Ni, Nb as being total to alloy element; Can draw following result: among the present invention program, utilize group's clustering model of stablizing solid solution alloy, take all factors into consideration factors such as enthalpy of mixing, group's clustering architecture and atomic size; The dissolve each other Ni of element and the scheme of the common alloying of diffusion barrier element have been selected with Cu; Can prepare no diffusion impervious layer Cu alloy firm, through guaranteeing alloy ratio and content, we have obtained satisfying the high unreactiveness of industry member demand and the Cu alloy film of low-resistivity.
Subordinate list 1 Cu
99.68Ni
0.29Nb
0.03Change in resistance under the different annealing conditions of film
Claims (2)
1. one kind has low-resistivity and high chemically inert Cu-Ni-Nb ternary alloy film, it is characterized in that: in the Cu film, add the Ni and the Nb of certain atomic percent, Ni is as solid solution element, and Nb is as the diffusion barrier element; Nb and Cu are positive enthalpy of mixing 3 kJ/mol, are negative enthalpy of mixing-30 kJ/mol with Ni; It is 0.02 ~ 0.70% that the adding proportion of Nb/Ni keeps the atomic percent proportional range; The atomic percent that NiNb adds total amount is 0.20 ~ 1.50%.
2. the preparation technology with low-resistivity and high chemically inert Cu-Ni-Nb ternary alloy film according to claim 1, it is characterized in that: it adopts the following step:
(1) preparation alloy sputtering target, its step is following:
1. get the raw materials ready: according to Ni recited above, Nb atomic percent, take by weighing each constituent element value, for use, the purity of Ni, Nb raw metal is more than 99.99%;
2. the melting of Ni-Nb alloy pig: the compound of metal is placed in the water jacketed copper crucible of smelting furnace, adopts the method for vacuum arc melting under the protection of argon gas, to carry out melting, at first be evacuated to 10
-2Pa, charging into argon gas to air pressure then is 0.03 ± 0.01MPa, the span of control of melting current density is 150 ± 10A/cm
2, after the fusing, continuing 10 seconds of melting again, outage lets alloy be cooled to room temperature with copper crucible, then with its upset, places again in the water jacketed copper crucible, carries out the melting second time; Aforementioned process melt back at least 3 times obtains the uniform Ni-Nb alloy pig of composition;
3. the preparation of Ni-Nb alloy bar: the Ni-Nb alloy pig is placed in the water jacketed copper crucible that is connected with negative pressure suction casting equipment, under argon shield,, at first be evacuated to 10 with above-mentioned vacuum arc melting method molten alloy
-2Pa, charging into argon gas to air pressure then is 0.03 ± 0.01MPa, the used current density of melting is 150 ± 10A/cm
2, after the fusing, continuing 10 seconds of melting again, the negative pressure absorbing and casting device is opened in outage simultaneously, lets alloy melt charge in the cylindrical, copper model cavity, is cooled to room temperature, obtains the Ni-Nb alloy bar of certain specification;
4. the preparation of alloy paster: the alloy small pieces that alloy bar are cut into desired thickness with the low speed saw;
5. the preparation of alloy sputtering target: using conductive silver glue that the Ni-Nb alloy slice is sticked on the used purity of sputter is on the 99.999% basic Cu target, and perhaps the Ni-Nb alloy slice directly being mounted to foraminous purity is to process the combined alloy sputtering target material on the 99.999% basic Cu target.
(2) the polynary codoped Cu film of preparation, its step is following:
1. the Si substrate of magnetron sputtering film preparation cleans; The monocrystalline silicon piece of (100) orientation earlier through acetone, alcohol and deionized water ultrasonic cleaning, is put into 5% HF then and soaked 2～3 minutes, adopt N
2Put into Vakuumkammer after drying up;
2. magnetron sputtering equipment extracting vacuum; After sample and target were all put into Vakuumkammer, the plant machinery pump slightly was evacuated to below the 5Pa, adopted molecular pump to carry out essence then and vacuumized, and vacuum tightness is evacuated to 5.4 * 10
-4Pa;
3. after vacuum tightness reaches required high vacuum, charge into argon gas to the air pressure 2Pa, let the target build-up of luminance; Regulate argon flow amount then to 8.0Sccm, operating air pressure modulation 0.4Pa, sputtering power 75w; Target-substrate distance is 8-12cm, and sputtering time is 25min, after sputter finishes; Apparatus cools 30min takes out ternary Cu alloy firm sample.
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| CN103014627A (en) * | 2013-01-17 | 2013-04-03 | 大连理工大学 | Fe-Si-Al ternary amorphous thin film with adjustable band gap width and preparation method of thin film |
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| CN103074553A (en) * | 2013-01-17 | 2013-05-01 | 大连理工大学 | Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and preparation method thereof |
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| CN108985004A (en) * | 2018-06-27 | 2018-12-11 | 广东工业大学 | A kind of calculation method of ternary amorphous alloy maximum negative heat of mixing |
| CN109706429A (en) * | 2018-11-15 | 2019-05-03 | 江苏科技大学 | A kind of self assembly diffusion barrier layer copper interconnection material and preparation method thereof |
| CN109930124A (en) * | 2019-04-12 | 2019-06-25 | 大连理工大学 | One kind being applied to anti-corrosion Ti-Nb-Ta alloy film material of detecting head surface high-temperature electric conduction and preparation method thereof |
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| CN103014627A (en) * | 2013-01-17 | 2013-04-03 | 大连理工大学 | Fe-Si-Al ternary amorphous thin film with adjustable band gap width and preparation method of thin film |
| CN103046000A (en) * | 2013-01-17 | 2013-04-17 | 大连理工大学 | Bandgap-variable Fe-B-Si three-element semiconductor amorphous film and preparation method thereof |
| CN103074553A (en) * | 2013-01-17 | 2013-05-01 | 大连理工大学 | Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and preparation method thereof |
| CN103014627B (en) * | 2013-01-17 | 2014-10-22 | 大连理工大学 | Fe-Si-Al ternary amorphous thin film with adjustable band gap width and preparation method of thin film |
| CN103074553B (en) * | 2013-01-17 | 2014-12-10 | 大连理工大学 | Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and preparation method thereof |
| CN105648402A (en) * | 2016-01-06 | 2016-06-08 | 大连理工大学 | High-hardness Cu alloy film for stabilizing N through cluster solid solution model and preparing method of high-hardness Cu alloy film |
| CN105648402B (en) * | 2016-01-06 | 2018-06-22 | 大连理工大学 | A kind of high-hardness Cu alloy firm of cluster solid solution model stability N and preparation method thereof |
| CN108985004A (en) * | 2018-06-27 | 2018-12-11 | 广东工业大学 | A kind of calculation method of ternary amorphous alloy maximum negative heat of mixing |
| CN108985004B (en) * | 2018-06-27 | 2022-02-25 | 广东工业大学 | Method for calculating maximum negative mixing enthalpy of ternary amorphous alloy |
| CN109706429A (en) * | 2018-11-15 | 2019-05-03 | 江苏科技大学 | A kind of self assembly diffusion barrier layer copper interconnection material and preparation method thereof |
| CN109930124A (en) * | 2019-04-12 | 2019-06-25 | 大连理工大学 | One kind being applied to anti-corrosion Ti-Nb-Ta alloy film material of detecting head surface high-temperature electric conduction and preparation method thereof |
| CN109930124B (en) * | 2019-04-12 | 2020-06-12 | 大连理工大学 | High-temperature conductive corrosion-resistant Ti-Nb-Ta alloy film material applied to probe surface and preparation method thereof |
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Application publication date: 20121205 |