CN102127743A - Preparation method of Ta-C-N thin-film - Google Patents
Preparation method of Ta-C-N thin-film Download PDFInfo
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Abstract
The invention relates to the technical field of thin-film preparation, particularly relates to a preparation method of a Ta-C-N thin-film, which comprises the following steps: performing surface activation on a monocrystalline silicon substrate by using a conventional process, separately placing a Ta target, a graphite target and the silicon substrate into a main sputtering chamber and a sample injection chamber, vacuumizing the sputtering chamber and the sample injection chamber, and pre-sputtering the Ta target and the graphite target to remove surface impurities; adjusting the ratio of nitrogen gas flow to argon gas flow (sccm) to 1:(10-100); adjusting the distance between the substrate and the targets to 5-10 centimeters; regulating the Ta target sputtering power to 80-150 W to do firing sputter, regulating the graphite target sputtering power to 100-200 W to do firing sputter, and producing the thin film by adopting simultaneous sputtering and layered sputtering process; and taking the test sample out from the main sputtering chamber to obtain the non-crystalline Ta-C-N ternary thin-film. The preparation method provided by the invention has the characteristics of simple process, short synthesis time, and on the like and is easy to implement.
Description
Technical field
Patent of the present invention relates to a kind of Ta of having, and the preparation method of C and three kinds of element materials of N refers in particular to and adopts direct current and radio frequency magnetron cosputtering to prepare the Ta-C-N film, by the enforcement of this method, can obtain to have the film of Ta-C-N ternary component.
Background technology
The TaN film because have the chemical stability height, temperature coefficient of resistance is little and the resistance variable range is big etc., and characteristics have been widely used in unicircuit, blocking layer and the thin film resistor, the preparation method of TaN film mainly contains ion beam depositing, chemical vapour deposition and reaction magnetocontrol sputtering etc. at present
[1], being compared to binary TaN film, ternary Ta-C-N thin film study is then less relatively.
In the electronic industry development, along with the increase of chip integration and reducing of characteristic dimension, interconnect delay (RC delay) is also increasing; Have on the one hand many researchs in low-k (being called for short low k) material field to reduce interconnection capacitance C, using more on the other hand, the metallic substance of low-resistivity necessitates, copper is very attractive interconnection material, than aluminium better electroconductibility and better electromigration resisting property are arranged, but copper all has higher rate of diffusion in silicon or medium, in case copper atom enters silicon device, just can become the deep energy level acceptor impurity, thereby producing the deathnium reduces carrier lifetime, finally cause device performance degeneration even inefficacy, in addition copper and medium stick performance a little less than, also be vulnerable to corrosion, therefore in copper wiring technique, must introduce suitable diffusion impervious layer simultaneously
[2]
In the early stage research process, once considered to utilize some refractory metals and ternary metal-Si-N(such as Ta-Si-N, W-Si-N etc.) prepare diffusion impervious layer, in these materials, Ta and Ta-N have obtained comparatively extensive studies as diffusion impervious layer with the diffusion that stops copper, this mainly is because Ta has high melt point, and the solid solubility in copper is very little; By systematic study, Ta-C-N film (this film contains a spot of nitrogen) has stability preferably as diffusion impervious layer under higher temperature condition, and causes the concern of Chinese scholars; Human TaC targets such as S.J.Wang (mass ratio 50:50, purity 99.5%) are at certain Ar/N
2Under the throughput ratio, adopt reactive sputtering on N type (100) silicon chip, to synthesize the thick Ta-C-N film of 60nm
[3], people such as H.Wojcik continue to feed the gas mixture of hydrogen and argon gas with the TBTDET presoma, utilize plasma enhanced atomic layer deposition (Atomic layer deposition) method at SiO
2, having synthesized the Ta-C-N film on SiCOH and the Cu matrix, the result shows, even when prepared Ta-C-N film thickness is 1nm, it all can stop the diffusion of copper effectively
[4], in addition, human nitrogen ion beams such as S.H.Kim strengthen deposition method
[5], people such as Y.Ohshita
[6]With people such as E.R.Engbrecht
[7]Use chemical gaseous phase depositing process, make the TaCN film, and studied its prevention diffusion in copper-connection.
In addition, the carbon/nitride of fourth officer family and the 5th subgroup element gets most of the attention because of its unique physics-chem characteristic, as high-melting-point, and high rigidity, excellent heat and chemical stability, corrosion-resistant and excellent conducting performance etc.; Wang Guangfu and Zhang Huixing
[8]With magnetic filtering cathode vacuum arc plasma deposition method in different N
2Divide and depress, on the Si substrate, synthesized Ta-C (N) film, XPS and Raman analysis revealed, deposition target chamber nitrogen partial pressure in the following synthetic amorphous carbon of 0.1Pa nitrogen film the N/C atomic ratio between 0.098-0.31, and along with the increase of nitrogen air input, the N content in the film increases sp
3The key proportion reduces, and further increases nitrogen partial pressure, and sedimentation rate can reduce significantly, in synthetic amorphous carbon nitrogen film N mainly with the N=C key with the combination of C atom.
The present invention adopts Ta target and graphite target, direct current and radio frequency magnetron cosputtering prepare the Ta-C-N ternary film, compare with the listed method in front, having the target source easily obtains, characteristics such as technology is simple to operation, the enforcement of conditions such as the sputtering power by adjusting the source target, sputtering time, reaction atmosphere obtains to have the film of Ta, C, N ternary component, for inquiring into its physicals, and then inquire into its may use in electron device, wear-resistant coating and establish the material preparation basis.
Reference:
[1] Kang Jie, Zhang Wanli, Wu Chuangui etc., the influence that nitrogen partial pressure prepares the TaN film performance to magnetron sputtering, electronic component and material, 2009,28(6), 46-48;
[2] Xie Qi, the research of advanced diffusion impervious layer in the integrated circuit copper interconnecting technology, Fudan University, doctorate paper, 2008,12;
[3]?Shui?Jinn?Wang,?Hao?Yi?Tsai,?S.C.?Sun?et?al,?Characterization?of?Sputtered?Ta-C-N?Film?in?the?Cu/barrier/Si?Contact?System,?Journal?of?Electronic?Materials,?2001,?30(8),917-924；
[4]?H.Wojcik,?M.Friedemann,?F.Feustel?et?al,?A?comparative?study?of?thermal?and?plasma?enhanced?ALD?Ta-N-C?films?on?SiO
2,?SiCOH?and?Cu?substrates,?International?Interconnect?Technology?Conference,?IEEE,?4-6?June?2007,19-21；
[5]?Soo-Hyum?Kim,?Se-Joon?Im,?Ki-Bum?Kim,?The?effect?of?ion?beam?bombardment?on?the?properties?of?Ta(C)N?films?deposited?from?pentakis-diethylamido-tantalum,?Thin?Solid?Films,?2002,?415,?177-186；
[6]?Y.Ohshita,?A.Ogura,?A.Hoshino?et?al,?Low-pressure?chemical?vapor?deposition?of?TaCN?films?by?pyrolysis?of?ethylamido-tantalum,?Journal?of?Crystal?Growth,?2000,?220,?604-609；
[7]?E.R.Engbrecht,?Y.-M?Sun,?S.Smith?et?al,?Chemical?vapor?deposition?growth?and?properties?of?TaCxNy,?Thin?Solid?Films,?2002,?418,?145-150；
[8] Wang Guangfu, Zhang Huixing, FCVAD synthesize Ta-C (N) film and Raman and XPS analysis, luminous journal, 2003,24 (5), 535-539.
Summary of the invention
The purpose of this invention is to provide a kind of magnetron sputtering and prepare film process, obtain the novel thin film of three kinds of components of Ta-C-N.
The object of the present invention is achieved like this:
1. to the target material surface polishing, with drying after the alcohol wipe;
To the Si substrate routinely technology carry out surface activation process;
3. magnetron sputtering technique process:
Ta target, graphite target and Si substrate are put into main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are vacuumized, Ta target and graphite target are carried out pre-sputter clean to remove surface impurity; Regulate nitrogen and argon flow amount (sccm) than being 1:(10 ~ 100); Regulating base material and target distance is 5 ~ 15cm; Regulate Ta target sputtering power in the sputter of 80 ~ 150W build-up of luminance, the graphite target sputtering power is in the sputter of 100 ~ 200W build-up of luminance, adopt the technical process of sputter simultaneously or intersection sputter to prepare film, take out sample from main sputtering chamber after the sputter, obtain amorphous Ta-C-N ternary film.
Adopt X-ray diffractometer (XRD) to carry out the material phase analysis of film; The component analysis of film is carried out in energy spectrum analysis (EDS); The indentation load of nano-hardness tester analysed film and displacement relation; Atomic force microscope (AFM) viewing film surface topography.
By the enforcement of present method, make prepared Ta-C-N ternary film have following several characteristics: (1) is compared with document [3-7]: (a) present method adopts Ta target and graphite target, and need not adopt TaC target or other presoma, and target is easy to get; (b) sputter deposition rate is big; (c) but the independent control target power realizes the control of the component proportions of prepared film, and TaC target (mass ratio 50:50, purity 99.5%) in the document [3], its target composition is constant, the difficult control that realizes the component proportions of film; (2) with the independent Ta target that adopts, adopting magnetron sputtering method to prepare Ta-N binary film compares: (a) Ta-C-N ternary film nano hardness height, the equal conditions Ta-C-N ternary film nano hardness of preparation down can reach 9.5GPa, and Ta-N binary film has only 4.7GPa; (b) Ta-C-N ternary film surfacing densification, all square roughness in surface (RMS) is little, and the equal conditions Ta-C-N ternary film RMS of preparation down is 1.93nm, and Ta-N binary film RMS is 2.85nm; (c) Ta-C-N ternary film frictional coefficient is low, and the equal conditions Ta-C-N ternary film frictional coefficient of preparation down is 0.237, and Ta-N binary film friction coefficient is 0.315.
Description of drawings
The XRD figure of Fig. 1 Ta-C-N ternary film;
The energy spectrum analysis figure of Fig. 2 Ta-C-N ternary film;
Fig. 3 Ta-C-N ternary film and Ta-N binary film nano indentation load and displacement relation curve;
Fig. 4 Ta-C-N ternary film and Ta-N binary film surface appearance (AFM).
Embodiment
Adopt magnetron sputtering technique to prepare the Ta-C-N film, the invention will be further described below in conjunction with example.
Example 1
(1) processing of magnetic control spattering target
Commercially available Ta target and graphite target surface are polished with sand paper, remove surface possible impurity and oxide compound, with drying after the alcohol wipe;
(2) to single crystalline Si substrate surface activation treatment
The Si substrate is immersed in the ethanol ultrasonic cleaning 15min; Use the solution soaking 15min of hydrogen peroxide: the vitriol oil=1:2 again; Put into after the taking-up and fill HF: the solution 30s of deionized water=1:10; Last Si substrate dries up with nitrogen;
(3) magnetron sputtering technique process
Ta target, graphite target and Si substrate are put into main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are evacuated to 1 * 10
-5Pa;
Ta target and graphite target are carried out the pre-sputter of 20min with cleaning target material surface impurity.Sputtering atmosphere is argon gas and nitrogen flow ratio=1:100.Regulating target and base material spacing is 5cm, is reaching vacuum tightness 3 * 10
-3Regulate Ta target sputtering power 80W during Pa, graphite target sputtering power 100W build-up of luminance sputter simultaneously, sputtering pressure is 3Pa, sputtering time is 60min, takes out sample from main sputtering chamber after the sputter, obtains amorphous film that spatters altogether.
Example 2
(1) processing of magnetic control spattering target
Commercially available Ta target and graphite target surface are polished with sand paper, remove surface possible impurity and oxide compound, with drying after the alcohol wipe;
(2) to single crystalline Si substrate surface activation treatment
The Si substrate is immersed in the ethanol ultrasonic cleaning 15min; Use the solution soaking 15min of hydrogen peroxide: the vitriol oil=1:2 again; Put into after the taking-up and fill HF: the solution 30s of deionized water=1:10; Last Si substrate dries up with nitrogen;
(3) magnetron sputtering technique process
Tantalum target, graphite target and Si substrate are put into main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are evacuated to 1 * 10
-5Pa;
The pre-sputter of Ta target and graphite target being carried out 20min is with cleaning target material surface impurity, and sputtering atmosphere is argon gas and nitrogen flow ratio=1:10.Regulating target and base material spacing is 10cm, is reaching vacuum tightness 3 * 10
-3Regulate tantalum target sputtering power 100W during Pa, graphite target sputtering power 150W build-up of luminance sputter simultaneously, sputtering pressure is 3Pa, sputtering time is 45min, takes out sample from main sputtering chamber after the sputter, obtains amorphous film that spatters altogether.
Example 3
(1) processing of magnetic control spattering target
Commercially available Ta target and graphite target surface are polished with sand paper, remove surface possible impurity and oxide compound, with drying after the alcohol wipe;
(2) to single crystalline Si substrate surface activation treatment
The Si substrate is immersed in the ethanol ultrasonic cleaning 15min; Use the solution soaking 15min of hydrogen peroxide: the vitriol oil=1:2 again; Put into after the taking-up and fill HF: the solution 30s of deionized water=1:10; Last Si substrate dries up with nitrogen;
(3) magnetron sputtering technique process
Tantalum target, graphite target and Si substrate are put into main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are evacuated to 1 * 10
-5Pa;
The pre-sputter of tantalum target and graphite target being carried out 20min is with cleaning target material surface impurity, and sputtering atmosphere is argon gas and nitrogen flow ratio=1:100, and adjusting target and base material spacing are 15cm, are reaching vacuum tightness 3 * 10
-3During Pa, regulate Ta target sputtering power 150W, sputtering pressure is 3.5Pa, behind the sputter 15min, stop the sputter of Ta target, regulate graphite target power 200W, sputter 15min, the following difference of the same terms is sputter Ta target and each 15min of graphite target again, takes out sample from main sputtering chamber after the intersection sputter, obtains amorphous layering sputtered film.
Table 1 provides three groups of example approach of the present invention.Prepare the Ta-C-N film by changing parameters such as sputtering atmosphere, sputtering time, sputtering technology.
The processing parameter of table 1 preparation Ta-C-N film
Adopt X-ray diffractometer (XRD) to carry out the material phase analysis of film; The component analysis of film is carried out in energy spectrum analysis (EDS); The indentation load of nano-hardness tester analysed film and displacement relation; Atomic force microscope (AFM) viewing film surface topography.
As seen from Figure 1, prepared synthetic film is a non-crystalline state; Zhi Bei film contains Ta as shown in Figure 2, C and N element (contain the O element and be film be placed in the air due to the oxidation); As shown in Figure 3, institute's made membrane has higher nano hardness; As shown in Figure 4, the smooth densification of made film surface.
Claims (3)
1. the preparation method of a Ta-C-N film is characterized in that, carries out according to following steps:
(1) to the target material surface polishing, with drying after the alcohol wipe;
(2) substrate routinely technology carry out surface activation process;
(3) sputtering technology process:
Ta target, graphite target and Si substrate are put into main sputtering chamber and Sample Room respectively, and main sputtering chamber and Sample Room are vacuumized, tantalum target and graphite target are carried out pre-sputter clean to remove surface impurity; Regulate nitrogen and argon flow amount (sccm) than being 1:(10 ~ 100); Regulating base material and target distance is 5 ~ 15cm; Regulate Ta target sputtering power in the sputter of 80 ~ 150W build-up of luminance, the graphite target sputtering power takes out sample from main sputtering chamber in the sputter of 100 ~ 200W build-up of luminance after the sputter, obtains amorphous Ta-C-N ternary film.
2. the preparation method of a kind of Ta-C-N film as claimed in claim 1, it is characterized in that: step (3) but Ta target and graphite target co-sputtered also can be intersected sputter: promptly first sputter Ta target, sputter graphite target again, then at sputter Ta target, sputter graphite target again.
3. the preparation method of a kind of Ta-C-N film as claimed in claim 1 is characterized in that: the sputtering pressure of co-sputtered or intersection sputter is 3～3.5Pa, and the time is 45～60min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924190A (en) * | 2014-04-02 | 2014-07-16 | 江苏科技大学 | Tavcn hard nanometer structure thin film and preparation method thereof |
| CN103952672A (en) * | 2014-03-12 | 2014-07-30 | 江苏科技大学 | TaCN (tantalum carbon nitrogen) hard nanostructured film and preparation method |
| CN105057235A (en) * | 2015-07-06 | 2015-11-18 | 山东金鼎电子材料有限公司 | ITO film sputtering target material cleaning method |
| CN107986792A (en) * | 2017-12-06 | 2018-05-04 | 中国人民解放军国防科技大学 | Ta-C-N ceramic precursor synthesis method |
| CN108085641A (en) * | 2017-11-09 | 2018-05-29 | 吉林大学 | It is a kind of that there is high hard and hydrophobic property protective coating and preparation method and application |
| CN112481591A (en) * | 2020-11-11 | 2021-03-12 | 中国科学院宁波材料技术与工程研究所 | Self-adaptive high-low temperature cycle resistant low-friction functional protective coating and preparation method and application thereof |
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| CN101710577A (en) * | 2009-11-19 | 2010-05-19 | 复旦大学 | Method for inhibiting oxidization of copper in copper interconnect structure |
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2011
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952672A (en) * | 2014-03-12 | 2014-07-30 | 江苏科技大学 | TaCN (tantalum carbon nitrogen) hard nanostructured film and preparation method |
| CN103952672B (en) * | 2014-03-12 | 2016-10-12 | 江苏科技大学 | TaCN hard nanometer structural membrane and preparation method |
| CN103924190A (en) * | 2014-04-02 | 2014-07-16 | 江苏科技大学 | Tavcn hard nanometer structure thin film and preparation method thereof |
| CN103924190B (en) * | 2014-04-02 | 2016-06-08 | 江苏科技大学 | TaVCN hard nanometer structural membrane and preparation method |
| CN105057235A (en) * | 2015-07-06 | 2015-11-18 | 山东金鼎电子材料有限公司 | ITO film sputtering target material cleaning method |
| CN108085641A (en) * | 2017-11-09 | 2018-05-29 | 吉林大学 | It is a kind of that there is high hard and hydrophobic property protective coating and preparation method and application |
| CN108085641B (en) * | 2017-11-09 | 2019-11-05 | 吉林大学 | A kind of protective coating and preparation method and application hard with height and hydrophobic property |
| CN107986792A (en) * | 2017-12-06 | 2018-05-04 | 中国人民解放军国防科技大学 | Ta-C-N ceramic precursor synthesis method |
| CN107986792B (en) * | 2017-12-06 | 2020-05-29 | 中国人民解放军国防科技大学 | Ta-C-N ceramic precursor synthesis method |
| CN112481591A (en) * | 2020-11-11 | 2021-03-12 | 中国科学院宁波材料技术与工程研究所 | Self-adaptive high-low temperature cycle resistant low-friction functional protective coating and preparation method and application thereof |
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Application publication date: 20110720 |