CN102002666A - Preparation method of tantalum nitride diffusion impervious layer for copper interconnection - Google Patents

Preparation method of tantalum nitride diffusion impervious layer for copper interconnection Download PDF

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Publication number
CN102002666A
CN102002666A CN 201010515721 CN201010515721A CN102002666A CN 102002666 A CN102002666 A CN 102002666A CN 201010515721 CN201010515721 CN 201010515721 CN 201010515721 A CN201010515721 A CN 201010515721A CN 102002666 A CN102002666 A CN 102002666A
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tantalum
nitride diffusion
copper
barrier layer
diffusion barrier
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CN102002666B (en
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朱嘉琦
王建东
张建隆
张雯婷
曹世成
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to a preparation method of a tantalum nitride diffusion impervious layer for copper interconnection, relating to a preparation method of the tantalum nitride diffusion impervious layer and solving the problems of poor impervious effect of tantalum nitride diffusion impervious layer, which is caused by large thickness and poor compactness of the tantalum nitride diffusion impervious layer prepared by the traditional tantalum nitride deposition technology. The preparation method comprises the following steps of: cleaning a substrate, and then placing the cleaned substrate on a sample platform inside a vacuum cavity of filtering cathode arc deposition equipment; then carrying out ion cleaning on the substrate; vacuumizing, heating the sample platform, introducing nitrogen, then importing scanning waveforms, and setting deposition parameters; and then starting the filtering cathode arc deposition equipment. The tantalum nitride diffusion impervious layer for the copper interconnection has the thickness of 10-20 nm, good compactness and uniform and smooth surface and can ensure the excellent quality of a subsequent electrodeposition copper layer; and in addition, the tantalum nitride diffusion impervious layer has high high-temperature diffusion imperviousness and does not generate copper-silicon compounds after being subjected to heat treatment at the temperature of 600 DEG C for 90 minutes.

Description

The interconnected preparation method of a kind of copper with the tantalum-nitride diffusion barrier layer
Technical field
The present invention relates to a kind of preparation method of tantalum-nitride diffusion barrier layer.
Background technology
Along with the development of integrated circuit technology, the Cu substitute for Al becomes the interconnecting material of a new generation.Cause in the Si device that device performance is impaired and improve Cu and Si, SiO in order to prevent that Cu from diffusing into 2Adhesivity, must be at Cu interconnection line external parcel one deck diffusion impervious layer.Tantalum nitride has very good barrier material performance, and the performance of, a series of excellences such as fusing point high, the intensity of activation height of character and crystal boundary diffusion, interface stability low as resistivity is the preferred material of current diffusion impervious layer.When the characteristic dimension of unicircuit during less than 45nm, performance requriementss such as the thickness of barrier film, blocking effect are further improved, the thickness on blocking layer should be less than 3.3nm, the depth-to-width ratio of circuit groove increases, current main deposition technique can not guarantee that the tantalum nitride barrier layer of preparing still has good diffusion barrier performance and step coverage, existing deposition technique is mainly magnetron sputtering, vacuum evaporation etc., the tantalum nitride barrier layer thickness for preparing excessive (greater than 100nm), blocking layer compactness is poor, causes blocking effect poor.
Summary of the invention
The objective of the invention is that the tantalum nitride barrier layer thickness that existing deposition of tantalum-nitride technology prepares is big, compactness is poor in order to solve, the problem that causes the blocking effect difference of tantalum nitride barrier layer provides a kind of copper interconnected preparation method with the tantalum-nitride diffusion barrier layer.
The interconnected preparation method of copper of the present invention with the tantalum-nitride diffusion barrier layer, realize by following steps: one,, then monocrystalline substrate is placed on the sample table in the filtering cathode arc deposited equipment vacuum storehouse monocrystalline substrate ultrasonic cleaning 30~40min; Two, will be evacuated to 1.0 * 10 in the vacuum storehouse -6~9.9 * 10 -6Feed argon gas behind the Torr, the control argon flow amount is 50cm 3/ min, pressure reaches 8.0 * 10 in the hole capital after selling all securities of taking seriously -5~1.0 * 10 -4During Torr, sample table is gone to the ion cleaning positions, ion is carried out on the monocrystalline substrate surface clean 10~20min, close argon gas then, again sample table is gone to deposition position; Three, continue the vacuum storehouse is vacuumized, when vacuum tightness reaches 1.0 * 10 -6~9.9 * 10 -6During Torr, sample table is heated to 200~600 ℃ again, feeds nitrogen then, nitrogen flow is controlled at 2.6~8.8cm 3/ min calls in sweep waveform then, deposition parameter is set be: flame current is 120~150A, and the scanning duration is 10min, and playing radian frequency is 10~15s/ time, and the substrate direct-current biasing is 20~200V; Four, the interior vacuum tightness of hole capital after selling all securities is 4.0 * 10 surely -4~7.0 * 10 -4During Torr, open filtering cathode arc deposited equipment, begin the tantalum target is applied the starting the arc of pulse power characteristic, adopt flat characteristic power supply stabilising arc then, to monocrystalline substrate surface deposition plated film, deposition promptly obtains the tantalum-nitride diffusion barrier layer on the monocrystalline substrate surface after finishing, and realizes the interconnected preparation with the tantalum-nitride diffusion barrier layer of copper.
The interconnected preparation method with the tantalum-nitride diffusion barrier layer of copper of the present invention utilizes the filtered cathodic vacuum arc technology to obtain the tantalum-nitride diffusion barrier layer that thickness only is 10~20nm on monocrystalline substrate, and the tantalum-nitride diffusion barrier layer compactness for preparing is good, the surface is evenly smooth, can guarantee the excellent quality of follow-up electric deposited copper floor; It is 600 ℃ thermal treatment after 90 minutes that the height of High temperature diffusion block simultaneously, tantalum-nitride diffusion barrier layer are subjected to temperature, no copper silicon compound generation.
The interconnected preparation method's technology with the tantalum-nitride diffusion barrier layer of copper of the present invention is simple, and preparation cycle is short, is suitable for industrial applications.Preparation method of the present invention can realize the requirement that depth-to-width ratio was at least 9: 1, can satisfy the performance requriements of current semiconductor industry.
Description of drawings
Fig. 1 is glancing incidence X-ray diffraction (GIXRD) the test spectrogram of the sample after the thermal treatment in the embodiment 13, " ■ " is (111) crystal orientation cube phase TaN among the figure, " " is (200) crystal orientation cube phase TaN, " ◆ " is (111) crystal orientation cube phase Cu, " ◇ " is (200) crystal orientation cube phase Cu, " ▲ " is (220) crystal orientation cube phase TaN, and " △ " is (220) crystal orientation cube phase Cu.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment is the interconnected preparation method with the tantalum-nitride diffusion barrier layer of copper, realize by following steps: one,, then monocrystalline substrate is placed on the sample table in the filtering cathode arc deposited equipment vacuum storehouse monocrystalline substrate ultrasonic cleaning 30~40min; Two, will be evacuated to 1.0 * 10 in the vacuum storehouse -6~9.9 * 10 -6Feed argon gas behind the Torr, the control argon flow amount is 50cm 3/ min, pressure reaches 8.0 * 10 in the hole capital after selling all securities of taking seriously -5~1.0 * 10 -4During Torr, sample table is gone to the ion cleaning positions, ion is carried out on the monocrystalline substrate surface clean 10~20min, close argon gas then, again sample table is gone to deposition position; Three, continue the vacuum storehouse is vacuumized, when vacuum tightness reaches 1.0 * 10 -6~9.9 * 10 -6During Torr, sample table is heated to 200~600 ℃ again, feeds nitrogen then, nitrogen flow is controlled at 2.6~8.8cm 3/ min calls in sweep waveform then, deposition parameter is set be: flame current is 120~150A, and the scanning duration is 10min, and playing radian frequency is 10~15s/ time, and the substrate direct-current biasing is 20~200V; Four, the interior vacuum tightness of hole capital after selling all securities is 4.0 * 10 surely -4~7.0 * 10 -4During Torr, open filtering cathode arc deposited equipment, begin the tantalum target is applied the starting the arc of pulse power characteristic, adopt flat characteristic power supply stabilising arc then, to monocrystalline substrate surface deposition plated film, deposition promptly obtains the tantalum-nitride diffusion barrier layer on the monocrystalline substrate surface after finishing, and realizes the interconnected preparation with the tantalum-nitride diffusion barrier layer of copper.
The purpose of ultrasonic cleaning is to remove the pollutent on monocrystalline substrate surface in the present embodiment step 1, as oil stain, dust etc.
Present embodiment obtains the tantalum-nitride diffusion barrier layer that thickness only is 10~20nm on monocrystalline substrate, and the tantalum-nitride diffusion barrier layer compactness for preparing is good, and the surface is evenly smooth, can guarantee the excellent quality of follow-up electric deposited copper floor; It is 600 ℃ thermal treatment after 90 minutes that the height of High temperature diffusion block simultaneously, tantalum-nitride diffusion barrier layer are subjected to temperature, no copper silicon compound generation.
The interconnected preparation method's technology with the tantalum-nitride diffusion barrier layer of the copper of present embodiment is simple, and preparation cycle is short, is suitable for industrial applications.Preparation method of the present invention can realize the requirement that depth-to-width ratio was at least 9: 1, can satisfy the performance requriements of current semiconductor industry.
Embodiment two: what present embodiment and embodiment one were different is will to be evacuated to 3.0 * 10 in the vacuum storehouse in the step 2 -6~8 * 10 -6Feed argon gas behind the Torr, the control argon flow amount is 50cm 3/ min, pressure reaches 8.5 * 10 in the hole capital after selling all securities of taking seriously -5~9.5 * 10 -5During Torr, sample table is gone to the ion cleaning positions.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is will to be evacuated to 6.0 * 10 in the vacuum storehouse in the step 2 -6Feed argon gas behind the Torr, the control argon flow amount is 50cm 3/ min, pressure reaches 9 * 10 in the hole capital after selling all securities of taking seriously -5During Torr, sample table is gone to the ion cleaning positions.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment and embodiment one, two or three are different is to reach 3.0 * 10 when vacuum tightness in the step 3 -6~8 * 10 -6During Torr, sample table is heated to 300~500 ℃ again.Other step and parameter are identical with embodiment one, two or three.
Embodiment five: present embodiment and embodiment one, two or three are different is to reach 6 * 10 when vacuum tightness in the step 3 -6During Torr, sample table is heated to 400 ℃ again.Other step and parameter are identical with embodiment one, two or three.
Embodiment six: what present embodiment was different with one of embodiment one to five is that nitrogen flow is controlled at 3~8cm in the step 3 3/ min.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different with one of embodiment one to five is that nitrogen flow is controlled at 4~6cm in the step 3 3/ min.Other step and parameter are identical with one of embodiment one to five.
Embodiment eight: what present embodiment was different with one of embodiment one to five is that nitrogen flow is controlled at 5cm in the step 3 3/ min.Other step and parameter are identical with one of embodiment one to five.
Embodiment nine: what present embodiment was different with one of embodiment one to eight is deposition parameter to be set in the step 3 be: flame current is 125~145A, the scanning duration is 10min, playing radian frequency is 11~14s/ time, and the substrate direct-current biasing is 80~150V.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different with one of embodiment one to eight is deposition parameter to be set in the step 3 be: flame current is 135A, and the scanning duration is 10min, and playing radian frequency is 12s/ time, and the substrate direct-current biasing is 120V.Other step and parameter are identical with one of embodiment one to eight.
Embodiment 11: present embodiment is different with one of embodiment one to ten is to take seriously in the step 4 that vacuum tightness is 4.8 * 10 in the hole capital after selling all securities -4~6.2 * 10 -4During Torr, open filtering cathode arc deposited equipment.Other step and parameter are identical with one of embodiment one to ten.
Embodiment 12: present embodiment is different with one of embodiment one to ten is to take seriously in the step 4 that vacuum tightness is 5.6 * 10 in the hole capital after selling all securities -4During Torr, open filtering cathode arc deposited equipment.Other step and parameter are identical with one of embodiment one to ten.
Embodiment 13: present embodiment is the interconnected preparation method with the tantalum-nitride diffusion barrier layer of copper, realize by following steps: one, monocrystalline substrate is used ultrasonic cleaning 30min, then monocrystalline substrate is placed on the sample table in the filtering cathode arc deposited equipment vacuum storehouse; Two, will be evacuated to 6 * 10 in the vacuum storehouse -6Feed argon gas behind the Torr, the control argon flow amount is 50cm 3/ min, pressure reaches 9.0 * 10 in the hole capital after selling all securities of taking seriously -5During Torr, sample table is gone to the ion cleaning positions, ion is carried out on the monocrystalline substrate surface clean 20min, close argon gas then, again sample table is gone to deposition position; Three, continue the vacuum storehouse is vacuumized, when vacuum tightness reaches 6 * 10 -6During Torr, sample table is heated to 400 ℃ again, feeds nitrogen then, nitrogen flow is controlled at 5cm 3/ min calls in sweep waveform then, deposition parameter is set be: flame current is 135A, and the scanning duration is 10min, and playing radian frequency is 12s/ time, and the substrate direct-current biasing is 120V; Four, the interior vacuum tightness of hole capital after selling all securities is 5.6 * 10 surely -4During Torr, open filtering cathode arc deposited equipment, begin the tantalum target is applied the starting the arc of pulse power characteristic, adopt flat characteristic power supply stabilising arc then, to monocrystalline substrate surface deposition plated film, deposition promptly obtains the tantalum-nitride diffusion barrier layer on the monocrystalline substrate surface after finishing, and realizes the interconnected preparation with the tantalum-nitride diffusion barrier layer of copper.
Present embodiment only is 15nm at the tantalum-nitride diffusion barrier layer thickness that the monocrystalline silicon surface deposition prepares, and the tantalum-nitride diffusion barrier layer compactness for preparing is good, and the surface is evenly smooth, can guarantee the excellent quality of follow-up electric deposited copper floor; It is 600 ℃ thermal treatment after 90 minutes that the height of High temperature diffusion block simultaneously, tantalum-nitride diffusion barrier layer are subjected to temperature, no copper silicon compound generation.
The silicon single crystal that present embodiment will deposit the tantalum-nitride diffusion barrier layer carries out copper facing again, make that forming the layer of copper film on the tantalum-nitride diffusion barrier layer obtains sample, it put under 600 ℃ the condition thermal treatment after 90 minutes with sample then, sample after adopting X ' Pert-Pro type X-ray diffractometer that Dutch Philips company produces to thermal treatment then carries out glancing incidence X-ray diffraction (GIXRD) test, test result as shown in Figure 1, " ■ " is (111) crystal orientation cube phase TaN among the figure, " " is (200) crystal orientation cube phase TaN, " ◆ " is (111) crystal orientation cube phase Cu, " ◇ " is (200) crystal orientation cube phase Cu, " ▲ " is (220) crystal orientation cube phase TaN, and " △ " is (220) crystal orientation cube phase Cu.As seen, present embodiment obtains the tantalum-nitride diffusion barrier layer, and to be subjected to temperature be 600 ℃ thermal treatment after 90 minutes on the monocrystalline substrate surface among Fig. 1, and no copper silicon compound produces, and diffusion barrier performance is good.

Claims (10)

1. the interconnected preparation method of a copper with the tantalum-nitride diffusion barrier layer, it is characterized in that the interconnected preparation method with the tantalum-nitride diffusion barrier layer of copper realizes by following steps: one,, then monocrystalline substrate is placed on the sample table in the filtering cathode arc deposited equipment vacuum storehouse with monocrystalline substrate ultrasonic cleaning 30~40min; Two, will be evacuated to 1.0 * 10 in the vacuum storehouse -6~9.9 * 10 -6Feed argon gas behind the Torr, the control argon flow amount is 50cm 3/ min, pressure reaches 8.0 * 10 in the hole capital after selling all securities of taking seriously -5~1.0 * 10 -4During Torr, sample table is gone to the ion cleaning positions, ion is carried out on the monocrystalline substrate surface clean 10~20min, close argon gas then, again sample table is gone to deposition position; Three, continue the vacuum storehouse is vacuumized, when vacuum tightness reaches 1.0 * 10 -6~9.9 * 10 -6During Torr, sample table is heated to 200~600 ℃ again, feeds nitrogen then, nitrogen flow is controlled at 2.6~8.8cm 3/ min calls in sweep waveform then, deposition parameter is set be: flame current is 120~150A, and the scanning duration is 10min, and playing radian frequency is 10~15s/ time, and the substrate direct-current biasing is 20~200V; Four, the interior vacuum tightness of hole capital after selling all securities is 4.0 * 10 surely -4~7.0 * 10 -4During Torr, open filtering cathode arc deposited equipment, begin the tantalum target is applied the starting the arc of pulse power characteristic, adopt flat characteristic power supply stabilising arc then, to monocrystalline substrate surface deposition plated film, deposition promptly obtains the tantalum-nitride diffusion barrier layer on the monocrystalline substrate surface after finishing, and realizes the interconnected preparation with the tantalum-nitride diffusion barrier layer of copper.
2. the interconnected preparation method with the tantalum-nitride diffusion barrier layer of a kind of copper according to claim 1 is characterized in that working as in the step 3 vacuum tightness and reaches 3.0 * 10 -6~8 * 10 -6During Torr, sample table is heated to 300~500 ℃ again.
3. the interconnected preparation method with the tantalum-nitride diffusion barrier layer of a kind of copper according to claim 1 is characterized in that working as in the step 3 vacuum tightness and reaches 6 * 10 -6During Torr, sample table is heated to 400 ℃ again.
4. according to claim 1, the interconnected preparation method of 2 or 3 described a kind of copper, it is characterized in that nitrogen flow is controlled at 3~8cm in the step 3 with the tantalum-nitride diffusion barrier layer 3/ min.
5. according to claim 1, the interconnected preparation method of 2 or 3 described a kind of copper, it is characterized in that nitrogen flow is controlled at 4~6cm in the step 3 with the tantalum-nitride diffusion barrier layer 3/ min.
6. according to claim 1, the interconnected preparation method of 2 or 3 described a kind of copper, it is characterized in that nitrogen flow is controlled at 5cm in the step 3 with the tantalum-nitride diffusion barrier layer 3/ min.
7. according to claim 1, the interconnected preparation method of 2 or 3 described a kind of copper with the tantalum-nitride diffusion barrier layer, it is characterized in that being provided with in the step 3 deposition parameter is: flame current is 125~145A, the scanning duration is 10min, playing radian frequency is 11~14s/ time, and the substrate direct-current biasing is 80~150V.
8. according to claim 1, the interconnected preparation method of 2 or 3 described a kind of copper with the tantalum-nitride diffusion barrier layer, it is characterized in that being provided with in the step 3 deposition parameter is: flame current is 135A, the scanning duration is 10min, and playing radian frequency is 12s/ time, and the substrate direct-current biasing is 120V.
9. according to claim 1, the interconnected preparation method with the tantalum-nitride diffusion barrier layer of 2 or 3 described a kind of copper, vacuum tightness is 4.8 * 10 in the hole capital after selling all securities that it is characterized in that taking seriously in the step 4 -4~6.2 * 10 -4During Torr, open filtering cathode arc deposited equipment.
10. according to claim 1, the interconnected preparation method with the tantalum-nitride diffusion barrier layer of 2 or 3 described a kind of copper, vacuum tightness is 5.6 * 10 in the hole capital after selling all securities that it is characterized in that taking seriously in the step 4 -4During Torr, open filtering cathode arc deposited equipment.
CN2010105157218A 2010-10-22 2010-10-22 Preparation method of tantalum nitride diffusion impervious layer for copper interconnection Expired - Fee Related CN102002666B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8518825B1 (en) 2012-12-24 2013-08-27 Shanghai Huali Microelectronics Corporation Method to manufacture trench-first copper interconnection

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Publication number Priority date Publication date Assignee Title
US20030124262A1 (en) * 2001-10-26 2003-07-03 Ling Chen Integration of ALD tantalum nitride and alpha-phase tantalum for copper metallization application
CN101100739A (en) * 2007-08-02 2008-01-09 哈尔滨工业大学 Method for preparing thin film by using magnetron sputtering
CN101515580A (en) * 2009-03-31 2009-08-26 中南大学 SiCN medium diffusion barrier film for copper interconnection and preparation process thereof
CN101702406A (en) * 2009-11-24 2010-05-05 四川大学 Preparation technique of gradient diffusion impervious layer used for deep submicron integrated circuit Cu interconnection

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030124262A1 (en) * 2001-10-26 2003-07-03 Ling Chen Integration of ALD tantalum nitride and alpha-phase tantalum for copper metallization application
CN101100739A (en) * 2007-08-02 2008-01-09 哈尔滨工业大学 Method for preparing thin film by using magnetron sputtering
CN101515580A (en) * 2009-03-31 2009-08-26 中南大学 SiCN medium diffusion barrier film for copper interconnection and preparation process thereof
CN101702406A (en) * 2009-11-24 2010-05-05 四川大学 Preparation technique of gradient diffusion impervious layer used for deep submicron integrated circuit Cu interconnection

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《功能材料》 20070531 陈秀华等 超大规模集成电路铜布线扩散阻挡层TaN薄膜的制备研究 期刊第750-752页 1-10 第38卷, 第5期 2 *

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8518825B1 (en) 2012-12-24 2013-08-27 Shanghai Huali Microelectronics Corporation Method to manufacture trench-first copper interconnection

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