CN1614079A - Method for preparing CoSi2 thin film by alloy target material magnetic sputtering method - Google Patents
Method for preparing CoSi2 thin film by alloy target material magnetic sputtering method Download PDFInfo
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- CN1614079A CN1614079A CN 200410066585 CN200410066585A CN1614079A CN 1614079 A CN1614079 A CN 1614079A CN 200410066585 CN200410066585 CN 200410066585 CN 200410066585 A CN200410066585 A CN 200410066585A CN 1614079 A CN1614079 A CN 1614079A
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Abstract
The invention was involved in the method to produce CoSi2 film by alloy target material magnetic force control splutter. Firstly, match Co and Si according to the proportion of CoSi2 and produce alloy by vacuum melting. The alloy target material of sputter was produced by linear cutting process. Using the action of electromagnetic stirring in the melter to uniform the ingredient of target material and guarantee to form standard cube structure of CaF2. Secondly, the target material was equipped into sputter to produce film on the base, which was washed. CoSi2 film was produced by: adjusting power and sputtering speed and adding subsequent treatment, because the ingredients of film and target material were similar. All kinds of CoSi2 films could be produced by the method and the treated films had fine electric conductivity, heat stability and low stress level. At the same time, the production efficiency was improved by the method.
Description
Technical field
The present invention relates to a kind of preparation CoSi
2The method of film specifically is that a kind of alloy target material magnetic sputtering legal system is equipped with CoSi
2The method of film.Be used for technical field of material.
Background technology
Refractory metal silicide is widely used in doing in the large-scale integrated circuit interconnecting material, ohmic contact material and Schottky contacts material.Wherein, CoSi
2Low resistance, lattice parameter and Si with 15-20 μ Ω cm become material of greatest concern near characteristics such as the lattice mismatch rate are little.CoSi
2Method for manufacturing thin film has multiple.Solid phase epitaxy by molecular beam epitaxy (MBE) or short annealing Co/Ti/Si multilayer film can be in Si (100) substrate the good monocrystal epitaxial film of preparation quality.These methods are by 700 ℃ of short annealings, make the Si Elements Diffusion prepared in reaction of Co element and substrate obtain having the CoSi of satisfactory electrical conductivity
2Film.Also can be by the CoSi of annealing co-electrodeposition method preparation
2Noncrystal membrane prepares CoSi
2Film.In the occasion that can not use solid reaction process, when for example substrate was not silicon, the cosputtering thin films had application prospect.In addition, in the multicrystalline silicon compounds structure, can adopt WSi
2Or TiSi
2As electro-conductive material, these films generally adopt alloy target material to utilize the sputter thin films.CoSi
2Film is expected to use in the multicrystalline silicon compounds structure as the material of satisfactory electrical conductivity and low stress level.
Find through literature search prior art, " the Silicide formation in cobalt/amorphous silicon; amorphous Co-Si and bias-induced Co-Si films " that J.Y.Shim delivers on " Thin Solid Films " (thin solid film) (292 (1997) 31-39) (silicide in cobalt/non-crystalline silicon duplicature, amorphous cobalt silicon fiml and the bias voltage cobalt silicon fiml forms) proposes in this article to adopt double target co-sputtering to prepare CoSi
2Film, the thin film sputtering attitude is non-crystalline state, needs just can obtain crystallization thin film through heat-treatment of annealing.Focus on the amorphous crystallization phase research of amorphous cobalt silicon film in the literary composition, to the CoSi after forming
2The performance of film is not reported.
To the document of prior art with CoSi
2Alloy is a target, adopts single target to utilize magnetron sputtering method to prepare in the further retrieval of thin film technique theme, does not find relevant report as yet.
Summary of the invention
The objective of the invention is at above shortcomings in the prior art and defective, provide a kind of alloy target material magnetic sputtering legal system to be equipped with CoSi
2The method of film makes its film for preparing inherit that other method advantage---film has the favorable conductive rate, simultaneously, compares with other method and also to have reduction stress, improves the interface planarization, the characteristics of enhancing productivity.
The present invention is achieved by the following technical solutions, and method is as follows: at first Co and Si according to CoSi
2The stoichiometric ratio composition proportion prepares alloy by vacuum melting, utilizes the line cutting to prepare the alloy target material that meets the sputtering instrument requirement, makes full use of the function composite by electromagnetic stirring of smelting furnace, makes target have uniform composition, and has a cube CaF
2Structure; Then target is packed in the sputtering instrument, go up the preparation film in the substrate of cleaning (for example Si), film and target composition are approaching, by adjustment power and sputtering rate and subsequent disposal, prepare CoSi
2Film.
Below the inventive method is further described, concrete steps are as follows:
(1), target preparation
Pure cobalt and pure silicon are according to CoSi
2The stoichiometric ratio configuration.At first in arc-melting furnace, be smelted into bulk alloy.Vacuum tightness is 10 in the stove
-5Pa, the argon shield state.Then, the bulk alloy after melting is changed over to the vacuum intermediate frequency furnace and continue melting.The vacuum tightness of intermediate frequency furnace is 10
-3Pa, argon shield.Pouring into diameter in the liquation stove is cylinder foundry goods up to specification.After cooling to room temperature with the furnace, be cut into the sputtering target material (thickness 5mm, diameter 76mm) that meets the sputtering instrument requirement through line.Target needs to clean these operations through 150 ℃ of 3 hours oven dry greasy dirts, sand papering and acetone before use.
(2), substrate is prepared
(such as GaAs and simple substance or polycrystalline Si substrate) determined in the selection of substrate kind according to the object of research and work.Usually use polished silicon single-chip as substrate with (100) and (111) orientation.Pure acetone cleaning by analysis before silicon substrate uses is soaked the several minutes deoxidation then and is handled in 1: 50 HF dilute solution, put into sputtering instrument in deionized water after the rinsing.Other substrate such as glass and polycrystalline silicon substrate all needs to clean these operations through polishing and analytical pure acetone.The cleaning of substrate has significant effects to film in on-chip tack.
(3), sputter prepares film
Target and the substrate corresponding sputtering instrument (as ANELVA SPC-350) of packing into.Vacuum tightness is better than 10 at the bottom of the back of the body of sputtering instrument
-3Pa.Working gas is an argon gas, and operating air pressure is 10
-1Pa.Regulate sputtering power (50-300W), the thickness (100-1000nm) of base reservoir temperature controlling factors sputter rates (20-60nm/min) such as (30-400 ℃) and film.Before the sputter system film, cover baffle plate between substrate and target, target was through 5 minutes pre-sputter clean.Remove baffle plate then, the beginning sputter prepares film.
(4), film subsequent disposal
Sputter attitude film has and CoSi
2The composition that composition is very approaching.In ANELVA SPC-350 sputtering system; the thin film sputtering attitude is crystallization; owing to contain more defective; the initial electrical resistivity of film is 54 μ Ω cm; in argon shield or air atmosphere through 600 ℃ 1-5 minute annealing; the resistivity of film reaches 20 μ Ω cm, with the resistivity basically identical of reaction thin films.
The present invention is by sputter CoSi
2Alloy target material is prepared the film with satisfactory electrical conductivity.Compare with the 1.4GPa of reaction thin films, prepared film has low-stress and is low to moderate 600Mpa.Because film does not need the diffusion by substrate, so film has smooth interface.Compare with dual-target sputtering simultaneously, single target sputter has can reduce production link, enhances productivity.
Description of drawings
The XRD spectral line of Fig. 1 embodiment 1 thin film sputtering attitude
The XRD spectral line of Fig. 2 embodiment 2 thin film sputtering attitudes
The XRD spectral line of Fig. 3 embodiment 3 thin film sputtering attitudes
Embodiment
Content in conjunction with the inventive method provides following examples:
Embodiment 1
(1) target preparation
Pure cobalt and pure silicon are according to CoSi
2The stoichiometric ratio configuration.At first in arc-melting furnace, be smelted into bulk alloy.Vacuum tightness is 10 in the stove
-5Pa, the argon shield state.Then, the bulk alloy after melting is changed over to the vacuum intermediate frequency furnace and continue melting.The vacuum tightness of intermediate frequency furnace is 10
-3Pa, argon shield.Pouring into diameter in the liquation stove is the cylinder foundry goods of 76mm, cool to room temperature with the furnace after, be cut into the sputtering target material (thickness 5mm, diameter 76mm) that meets the sputtering instrument requirement through line.Target 150 ℃ of 3 hours oven dry greasy dirts, sand papering and acetone clean.
(2) substrate is prepared
Use (100) orientation polished silicon single-chip as substrate.Pure acetone ultrasonic cleaning by analysis before silicon substrate uses is soaked 3 minutes deoxidations then and is handled in 1: 50 HF dilute solution, put into sputtering instrument in deionized water after the rinsing.
(3) sputter prepares film
Target and the substrate corresponding sputtering instrument (ANELVA SPC-350) of packing into.Before the sputter system film, cover baffle plate between substrate and target, target was through 5 minutes pre-sputter clean.Remove baffle plate then, the beginning sputter prepares film.Vacuum tightness is 1 * 10 at the bottom of the back of the body of sputtering instrument
-3Pa.Working gas is an argon gas, and operating air pressure is 1.6 * 10
-1Pa, sputtering power 100W, 30 ℃ of base reservoir temperatures, sputter rate 20nm/min, the thickness 600nm of film.The initial electrical resistivity of film is 54 μ Ω cm.The film original texture through X-ray scanning as shown in Figure 1, the thin film sputtering attitude is crystallization, with CoSi
2Standard diagram is compared, and (111) peak wants big with the strength ratio at (220) peak, shows to have stronger (111) orientation silk weaving structure.
(4) film subsequent disposal
600 ℃ of annealing in 3 minutes of argon shield, the resistivity of film reaches 20 μ Ω cm.
Embodiment 2
Repeat step (1)-(4) among the embodiment 1, the sputtering power that changes in the step (3) is 150W, sputter rate is 30nm/min, base reservoir temperature is 250 ℃, the structure of prepared film as shown in Figure 2, compared to Figure 1, (111) intensity is higher with the ratio of (220) intensity, and stronger (111) texture is described.Close among the resistivity of subsequent heat treatment rear film and the embodiment 1.Texture strengthens the mechanical property that helps improving film, improves the erosion resistance of film and deelectric transferred ability or the like.
Embodiment 3
Repeat step (1)-(4) among the embodiment 1, the sputtering power that changes in the step (3) is 300W, sputter rate is 60nm/min, base reservoir temperature is 400 ℃, the structure of prepared film as shown in Figure 3, compare with Fig. 2, (111) intensity descends on the contrary, and its (111) texture of sedimentary film dies down when showing too high substrate.Close among the resistivity of subsequent heat treatment rear film and the embodiment 1.
Claims (3)
1, a kind of alloy target material magnetic sputtering legal system is equipped with CoSi
2The method of film is characterized in that, at first Co and Si according to CoSi
2The stoichiometric ratio composition proportion prepares alloy by vacuum melting, utilizes the line cutting to prepare the alloy target material that meets the sputtering instrument requirement, makes full use of the function composite by electromagnetic stirring of smelting furnace, makes target have uniform composition, and has cube CaF of standard
2Structure is packed target in the sputtering instrument into then, prepares film in the substrate of cleaning, and film and target composition are approaching, by adjusting power and sputtering rate and subsequent disposal, prepares CoSi
2Film.
2, alloy target material magnetic sputtering legal system according to claim 1 is equipped with CoSi
2The method of film is characterized in that, below method is done further to limit, and concrete steps are as follows:
(1), target preparation
Pure cobalt and pure silicon are according to CoSi
2The stoichiometric ratio configuration, at first in arc-melting furnace, be smelted into bulk alloy, the argon shield state, then, bulk alloy after melting is changed over to the vacuum intermediate frequency furnace continue melting, argon shield, casting is the cylinder foundry goods in the liquation stove, after cooling to room temperature with the furnace, be cut into the sputtering target material that meets the sputtering instrument requirement through line gradually;
(2), substrate is prepared
Polished silicon single-chip as substrate has (100) and (111) orientation, pure acetone cleaning by analysis before silicon substrate uses, soaking deoxidation then in 1: 50 HF dilute solution handles, put into sputtering instrument in deionized water after the rinsing, glass and substrate all need through polishing and analytical pure acetone matting;
(3), sputter prepares film
Target and the substrate corresponding sputtering instrument of packing into, vacuum tightness is better than 10 at the bottom of the back of the body of sputtering instrument
-3Pa, working gas are argon gas, regulate sputtering pressure, sputtering power, substrate temperature control sputter rate, the thickness of film and the state of thin film sputtering attitude of vacuum chamber.Before the sputter system film, cover baffle plate between substrate and target, target is removed baffle plate then through 5 minutes pre-sputter clean, and the beginning sputter prepares film;
(4), film subsequent disposal
Sputter attitude film has and CoSi
2The composition that composition is very approaching; the thin film sputtering attitude is crystallization; owing to contain more defective; the initial electrical resistivity of film is 54 μ Ω cm; in argon shield or air atmosphere through 600 ℃ 1-5 minute annealing; the resistivity of film reaches 20 μ Ω cm, with the resistivity basically identical of reaction thin films.
3, alloy target material magnetic sputtering legal system according to claim 2 is equipped with CoSi
2The method of film is characterized in that, in the step (1), vacuum tightness is better than 10 in the arc-melting furnace stove
-5Pa, the vacuum tightness of vacuum intermediate frequency furnace is 10
-3Pa, sputtering target material thickness 5mm, diameter 76mm, target need before use through 150 ℃ of 3 hours oven dry greasy dirt, sand papering and acetone mattings.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101921988A (en) * | 2010-05-05 | 2010-12-22 | 广州市尤特新材料有限公司 | Silicon-base alloy rotary target material and preparation method thereof |
CN112509805A (en) * | 2020-10-19 | 2021-03-16 | 山东麦格智芯机电科技有限公司 | Method for optimizing magnetic property of cobalt-based magnetic thin film inductance material |
CN115274295A (en) * | 2022-09-28 | 2022-11-01 | 季华实验室 | Magnetic film, magnetic code assembly comprising same and preparation method |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2002115045A (en) * | 2000-10-11 | 2002-04-19 | Token Thermotec:Kk | Film deposition method, and vane for movable vane compressor |
CN1206711C (en) * | 2002-03-28 | 2005-06-15 | 华邦电子股份有限公司 | Method for preparing self-aligning silicide of metal oxide semiconductor |
-
2004
- 2004-09-23 CN CNB2004100665853A patent/CN1304630C/en not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101921988A (en) * | 2010-05-05 | 2010-12-22 | 广州市尤特新材料有限公司 | Silicon-base alloy rotary target material and preparation method thereof |
CN112509805A (en) * | 2020-10-19 | 2021-03-16 | 山东麦格智芯机电科技有限公司 | Method for optimizing magnetic property of cobalt-based magnetic thin film inductance material |
CN115274295A (en) * | 2022-09-28 | 2022-11-01 | 季华实验室 | Magnetic film, magnetic code assembly comprising same and preparation method |
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