CN1304630C - 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
- Publication number
- CN1304630C CN1304630C CNB2004100665853A CN200410066585A CN1304630C CN 1304630 C CN1304630 C CN 1304630C CN B2004100665853 A CNB2004100665853 A CN B2004100665853A CN 200410066585 A CN200410066585 A CN 200410066585A CN 1304630 C CN1304630 C CN 1304630C
- Authority
- CN
- China
- Prior art keywords
- film
- sputtering
- target material
- target
- alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to a method for preparing CoSiO2 membranes by an alloy target material magnetron sputtering method, which is used for the technical field of material preparation. The present invention comprises: firstly, co and Si are mixed proportionally according to the stoichiometric ratio of CoSiO2 and melted into alloy in vacuum, the alloy is prepared into alloy target material by wire cutting in accordance with the requirements of a sputtering instrument, and the alloy target material is made to have uniform components and a standard cubic CaF2 structure by fully utilizing the electromagnetic mixing action of a smelting furnace; secondly, the alloy target material is put into the sputtering instrument, a membrane is prepared on a cleaned substrate, and the components of the membrane are approach to that of the alloy target material; a CoSiO2 membrane is prepared through the regulation of power and sputtering speed, and subsequent treatment. With the present invention, CoSiO2 membranes of various states can be prepared, the CoSiO2 membranes has favorable electric conductive performance, favorable thermal stability and low stress level after treatment, and meanwhile, when the present invention is used for preparing the CoSiO2 membranes, the productive efficiency can be raised.
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 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 10 at the bottom of the back of the body of sputtering instrument
-3Pa, working gas is an 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, between substrate and target, cover baffle plate, 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 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100665853A CN1304630C (en) | 2004-09-23 | 2004-09-23 | Method for preparing CoSi2 thin film by alloy target material magnetic sputtering method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100665853A CN1304630C (en) | 2004-09-23 | 2004-09-23 | Method for preparing CoSi2 thin film by alloy target material magnetic sputtering method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1614079A CN1614079A (en) | 2005-05-11 |
| CN1304630C true CN1304630C (en) | 2007-03-14 |
Family
ID=34764917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100665853A Expired - Fee Related CN1304630C (en) | 2004-09-23 | 2004-09-23 | Method for preparing CoSi2 thin film by alloy target material magnetic sputtering method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1304630C (en) |
Families Citing this family (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 |
| CN112509805B (en) * | 2020-10-19 | 2022-05-27 | 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020064605A1 (en) * | 2000-10-11 | 2002-05-30 | Kiyoharu Hatakenaka | Method of coating a substrate and vane for vane-type compressor |
| CN1449002A (en) * | 2002-03-28 | 2003-10-15 | 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
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020064605A1 (en) * | 2000-10-11 | 2002-05-30 | Kiyoharu Hatakenaka | Method of coating a substrate and vane for vane-type compressor |
| CN1449002A (en) * | 2002-03-28 | 2003-10-15 | 华邦电子股份有限公司 | Method for preparing self-aligning silicide of metal oxide semiconductor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1614079A (en) | 2005-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107354506B (en) | A method of preparing super smooth copper single crystal film | |
| JP5621764B2 (en) | Transparent conductive film, transparent conductive film laminate, manufacturing method thereof, and silicon-based thin film solar cell | |
| KR101789347B1 (en) | Transparent conductive films | |
| TWI476159B (en) | Composite oxide sintered body, amorphous composite oxide film manufacturing method, amorphous composite oxide film, crystal composite oxide film manufacturing method and crystalline composite oxide film | |
| TWI395826B (en) | An amorphous composite oxide film, a crystal composite oxide film, an amorphous composite oxide film, a method for producing a crystalline composite oxide film, and a composite oxide sintered body | |
| JP4797712B2 (en) | ZnO-Al2O3-based sintered body, sputtering target, and method for producing transparent conductive film | |
| KR20120051656A (en) | Oxide sinter, method for producing same, target and transparent conductive film | |
| JPH04219359A (en) | Electrically conductive zinc oxide sintered compact | |
| WO2010018707A1 (en) | Gallium oxide-tin oxide based oxide sintered body and oxide film | |
| JPH11302835A (en) | Production of zinc oxide base sintered compact | |
| JPH11236219A (en) | Zinc oxide-base sintered compact and its production | |
| TW201240123A (en) | Method of manufacturing transparent conductive film, and method of manufacturing thin-film solar cell | |
| CN1684251A (en) | Heat interface material and its producing method | |
| CN113336549A (en) | Tellurium-selenium-cadmium target material and preparation method thereof | |
| CN1766158A (en) | The preparation method of low resistivity metal oxide lanthanum nickelate | |
| CN1304630C (en) | Method for preparing CoSi2 thin film by alloy target material magnetic sputtering method | |
| JPH11256320A (en) | Zno base sintered compact | |
| CN103237910B (en) | Low resistivity high thermal-stability copper-nickel-molybdenum alloy film and producing method thereof | |
| JP4092764B2 (en) | ZnO-based sintered body | |
| CN109554674A (en) | A kind of preparation method of the bismuth telluride thermal electric film with heterojunction structure | |
| CN1949459A (en) | Method for directly preparing Cr-Si silicide resistance film on surface of monocrystalline silicon substrate | |
| CN102522241B (en) | CuCr alloy contact material and preparation method thereof | |
| JPH11171539A (en) | Zno-base sintered compact and its production | |
| JP4917725B2 (en) | Transparent conductive film, method for producing the same, and use thereof | |
| JP2000129432A (en) | Electroconductive metallic oxide sinetred body and its use |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070314 Termination date: 20091023 |