CN100494479C - Method for preparing thin film by using magnetron sputtering - Google Patents

Method for preparing thin film by using magnetron sputtering Download PDF

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CN100494479C
CN100494479C CNB2007100725951A CN200710072595A CN100494479C CN 100494479 C CN100494479 C CN 100494479C CN B2007100725951 A CNB2007100725951 A CN B2007100725951A CN 200710072595 A CN200710072595 A CN 200710072595A CN 100494479 C CN100494479 C CN 100494479C
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minutes
film
vacuum
target
pressure
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CN101100739A (en
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朱嘉琦
姜春竹
韩潇
梁军
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

A process to prepare film by magnet sputter deposition is carried out by: (1) selecting target, and potting substrate in a rotary heating table; (2) vacuuming the heating table in a cabin, passing Ar gas, and ionization cleaning; (3) heating to the working temperature of deposition and keeping the temperature; (4) passing ignition gas, providing sputter power, controlling gas fluid volume, providing negative bias-voltage, shifting off buffer to begin deposition onto substrate; (5) controlling tracks of the two step motors rotating the heating table and the target respectively; and (6) cooling to atmosphere. It can produce large area film as traditional large target and thickness of the film is easily controlled with high uniform.

Description

A kind of method that adopts magnetron sputtering to prepare film
Technical field
The present invention relates to the preparation method of film.
Background technology
Magnetron sputtering film preparation device in the existing film preparing technology, can realize metal, plated film such as non-metal simple-substance and compound, but it is generally little than the magnetron sputtering target area at the prepared film size that goes out of existing planar magnetic control sputtering device, homogeneity is relatively poor, be embodied in: because the plasma density that existing magnetron sputtering equipment is produced is inhomogeneous, the target particle distribution of institute's sputter is inhomogeneous, the particle density in general target middle portion aura district is higher, so during film forming, middle portion is thicker, the edge is thinner, and the area of thicker homogeneous area is much smaller than the size of target in the middle of the film; In order to prepare large-area uniform thin film, will do middle uniform parts greatly as far as possible, usual method is to do the size of target very big, because the size of target is big more, utilization ratio is often low more, thereby causes the significant wastage of target.
Summary of the invention
The present invention is little than the magnetic controlling target area for the film size that solves existing planar magnetic control sputtering device and sputtered, homogeneity is relatively poor, the problem that the target waste is serious provides a kind of method that adopts magnetron sputtering to prepare film, and the concrete technical scheme that addresses the above problem is as follows:
The present invention adopts magnetron sputtering deposition to prepare the method for film, and the step of this method is as follows:
Step 1, select for use required Coating Materials as target, and substrate is placed on the rotation warm table, this warm table is positioned at the vacuum storehouse;
Step 2, with vacuum storehouse sealing, by vacuum acquiring system, will be evacuated in the vacuum storehouse, when vacuum tightness reaches 1.0 * 10 -4~9.9 * 10 -4During handkerchief, feed Ar gas, when pressure is 3~5 handkerchiefs in the hole capital after selling all securities of taking seriously, start the ionization power supply, substrate surface is carried out ionization clean, ionization was cleaned 3~5 minutes;
Step 3, ionization start the heating lamp group after cleaning and finishing, and are heated to 25~750 ℃ of the needed temperature of deposit film, and are incubated 10 minutes~1 hour;
Step 4, feed starter gas in the vacuum storehouse, gas pressure intensity starter when 3~5 handkerchiefs in the hole capital after selling all securities of taking seriously applies sputtering power, and sputtering power is 50~400 watts, pre-sputter 3~10 minutes; Gas flow is controlled at 10sccm~90sccm, and gas pressure intensity is reduced to 0.1~2 handkerchief in the vacuum storehouse, applies 0~600 volt negative bias on substrate, removes baffle plate;
Step 5, employing stepper-motor come the rotating speed of stepless control rotation warm table, rotating speed is controlled in 15 rev/mins, control the running orbit of warm table top target simultaneously with another stepper-motor, target is that the geneva motion of 2~5mm control to substrate surface plated film to cylindrical with step-length along the warm table center of circle;
After step 6, step 5 were finished, powered-down treated that (sediment chamber) makes required film in the vacuum storehouse when temperature is reduced to room temperature.
The invention solves existing target size and the contradiction between the sedimentary film dimensions, promptly changed the existing present situation that could prepare large area film with big target of having only, can deposit the large-sized film that has good uniformity with little target is the same, improve the utilization ratio of target simultaneously.The target size is far smaller than the sedimentary uniform thin film size of wanting; Compare with existing magnetically controlled sputter method, thickness is easy to control, and the uniformity coefficient height of film, and homogeneity satisfies industry general requirement (general requirement of industry is that unevenness is less than 10%)
Embodiment
Embodiment one: the step of the method for present embodiment is as follows:
Step 1, be that substrate and Ge (germanium) are target with Si (silicon), the target diameter is 49mm, and target thickness is 3mm, and substrate is placed on the rotation warm table, and this warm table is positioned at the vacuum storehouse;
Step 2, with vacuum storehouse sealing, by vacuum acquiring system, will be evacuated in the vacuum storehouse, vacuum tightness reaches 1.0 * 10 in the hole capital after selling all securities of taking seriously -4~9.9 * 10 -4During handkerchief, feed Ar gas, when pressure is 3~5 handkerchiefs in the hole capital after selling all securities of taking seriously, start the ionization power supply, the Si substrate surface is carried out ionization clean, ionization was cleaned 3~5 minutes;
Step 3, ionization start the heating lamp group after cleaning and finishing, and are heated to 25~750 ℃ of the needed temperature of deposit film, and are incubated 10 minutes~1 hour;
Step 4, in the vacuum storehouse, feed starter gas, starter when gas pressure intensity reaches 3~5 handkerchiefs, apply sputtering power, sputtering power is 50~400 watts, carry out pre-sputter 3~10 minutes, gas flow is controlled at 10sccm~90sccm, and gas pressure intensity is reduced to 0.1~2 handkerchief in the vacuum storehouse, on substrate, apply 0~600 volt negative bias, remove baffle plate;
Step 5, employing stepper-motor come the rotating speed of stepless control rotation warm table, rotating speed is controlled in 15 rev/mins, control the running orbit of warm table top target simultaneously with another stepper-motor, target is that the geneva motion of 2~5mm control to substrate surface plated film (plated film time according to area and the thickness of film determine) to cylindrical with step-length along the warm table center of circle; Control the homogeneity of plated film by the moving process of above-mentioned two motors.
After step 6, step 5 are finished, close all power supplys, treat that (sediment chamber) makes required film in the vacuum storehouse when temperature is reduced to room temperature.
Embodiment two: it is that 300mm, thickness are that the circular flat film of 168nm is an example that the difference of present embodiment and embodiment one is with the preparation diameter, and step 2 is taken seriously, and pressure is 7.5 * 10 in the hole capital after selling all securities -4During handkerchief, feed Ar gas, when pressure was 3 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 5 minutes; Step 3 is heated to 200 ℃ of insulations 30 minutes; The step 4 flow is made as 60sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 3 handkerchiefs, open the radio-frequency power supply starter, sputtering power is 80 watts, and pre-sputter is after 5 minutes, regulating pressure in vacuum tank is 0.7 handkerchief, and the plated film starting point of setting target is the warm table center of circle, and plated film target controlled variable is 2.0,2.0,2.1,2.4,2.8,2.9 control the position of the revolution of warm table and target after, on substrate, add 300 volts negative bias, remove baffle plate, the beginning plated film, the plated film time is 46 minutes 29 seconds (seeing Table one).Other step is identical with embodiment one.The thick 166nm of being about of film that makes through survey, with designed thickness error be 1.2%, the membrane thickness unevenness degree is less than 8.5%, satisfies the membrane thickness unevenness degree less than 10% industry general requirement.
Embodiment three: the difference of present embodiment and embodiment one is that with the preparation diameter be that 300mm, thickness are that 121nm circular flat film is an example, and step 2 is taken seriously, and pressure is 1.5 * 10 in the hole capital after selling all securities -4During handkerchief, feed Ar gas, when pressure was 4 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 4 minutes; Step 3 is heated to 50 ℃ of insulations 50 minutes; The step 4 flow is made as 20sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 4 handkerchiefs, open the radio-frequency power supply starter, sputtering power is 200 watts, and pre-sputter is after 4 minutes, regulating pressure in vacuum tank is 0.5 handkerchief, and the plated film starting point of setting target is the warm table center of circle, plated film controlled variable 1.0,1.0,1.1,1.2,1.4,1.45 control the position of the revolution of warm table and target after, on substrate, add 50 volts negative bias, remove baffle plate, the beginning plated film, the plated film time is 18 minutes and 46 seconds.Other step is identical with embodiment one.
Embodiment four: it is that 160mm, thickness are that the thin circular flat film of 122nm is an example that the difference of present embodiment and embodiment one is with the preparation diameter, and step 2 is taken seriously, and pressure is 8.5 * 10 in the hole capital after selling all securities -4During handkerchief, feed Ar gas, when pressure was 5 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 3 minutes; Step 3 is heated to 700 ℃ of insulations 20 minutes; The step 4 flow is made as 80sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 1 handkerchief, open the radio-frequency power supply starter, sputtering power is 80 watts, and pre-sputter is after 5 minutes, regulating pressure in vacuum tank is 1 handkerchief, and the plated film starting point of setting target is plated film controlled variable 1.33,1.2,1.4,1.6,1.87, behind the revolution of 0 control warm table and the position of target, on substrate, add 450 volts negative bias, the beginning plated film, the plated film time is 10 minutes and 15 seconds.Other step is identical with embodiment one.
Table one, be the preparation diameter be that 300mm, thickness are the running orbit and the plated film time data of the circular flat film target of 168nm
Figure C200710072595D00071
Figure C200710072595D00081

Claims (4)

1, a kind of method that adopts magnetron sputtering deposition to prepare film is characterized in that the step of this method is as follows:
Step 1, select for use and need Coating Materials as target, and substrate is placed on the rotation warm table, this warm table is positioned at the vacuum storehouse;
Step 2, with vacuum storehouse sealing, by vacuum acquiring system, will be evacuated in the vacuum storehouse, vacuum tightness reaches 9.9 * 10 in the hole capital after selling all securities of taking seriously -4~1.0 * 10 -4During handkerchief, feed Ar gas, when pressure is 3~5 handkerchiefs in the hole capital after selling all securities of taking seriously, start the ionization power supply, substrate surface is carried out ionization clean, ionization was cleaned 3~5 minutes;
Step 3, ionization start the heating lamp group after cleaning and finishing, and are heated to 25~750 ℃ of the needed temperature of deposit film, and are incubated 10 minutes~1 hour;
Step 4, in the vacuum storehouse, feed starter gas, the interior gas pressure intensity starter when 3~5 handkerchiefs of the hole capital after selling all securities of taking seriously, apply sputtering power, sputtering power is 50~400 watts, carry out pre-sputter 3~10 minutes, gas flow is controlled at 10sccm~90sccm, and gas pressure intensity is reduced to 0.1~2 handkerchief in the vacuum storehouse, on substrate, add 0~600 volt negative bias, remove baffle plate;
Step 5, employing stepper-motor come the rotating speed of stepless control rotation warm table, rotating speed is controlled in 15 rev/mins, control the running orbit of warm table top target simultaneously with another stepper-motor, target is that the geneva motion of 2~5mm control to substrate surface plated film to cylindrical with step-length along the warm table center of circle;
After step 6, step 5 were finished, powered-down treated to make when temperature is reduced to room temperature in the vacuum storehouse required film.
2, a kind of method that adopts magnetron sputtering deposition to prepare film according to claim 1, it is characterized in that preparing diameter is that 300mm, thickness are the circular flat film of 168nm, step 2 is taken seriously, and pressure is 7.5 * 10 in the hole capital after selling all securities -4During handkerchief, feed Ar gas, when pressure was 3 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 5 minutes; Step 3 is heated to 200 ℃ of insulations 30 minutes; The step 4 flow is made as 60sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 3 handkerchiefs, open the radio-frequency power supply starter, sputtering power is 80 watts, and pre-sputter is after 5 minutes, regulating pressure in vacuum tank is 0.7 handkerchief, sets the plated film controlled variable 2.0,2.0 of target, 2.1,2.4,2.8,2.9 control the position of the revolution of warm table and target after, on substrate, add 300 volts negative bias, remove baffle plate; Step 5 begins plated film, and the plated film time is closed all power supplys after being 46 minutes and 29 seconds, treat that vacuum chamber returns to room temperature after, open the vacuum storehouse, make required film.
3, a kind of method that adopts magnetron sputtering deposition to prepare film according to claim 1, it is characterized in that preparing diameter is that 300mm, thickness are 121nm circular flat film, step 2 is taken seriously, and pressure is 1.5 * 10 in the hole capital after selling all securities -4During handkerchief, feed Ar gas, when pressure was 4 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 4 minutes; Step 3 is heated to 50 ℃ of insulations 50 minutes; The step 4 flow is made as 20sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 4 handkerchiefs, open the radio-frequency power supply starter, sputtering power is 200 watts, and pre-sputter is after 4 minutes, regulating pressure in vacuum tank is 0.5 handkerchief, set the plated film controlled variable 1.0,1.0,1.1 of target, 1.4,1.45 after controlling the position of the revolution of warm table and target, on substrate, add 50 volts negative bias, remove baffle plate; Step 5 begins plated film, and the plated film time is closed all power supplys after being 18 minutes and 46 seconds, treat that vacuum chamber returns to room temperature after, open the vacuum storehouse, make required film.
4, a kind of method that adopts magnetron sputtering deposition to prepare film according to claim 1, it is characterized in that preparing diameter is that 160mm, thickness are the thin circular flat film of 122nm, step 2 is taken seriously, and pressure is 8.5 * 10 in the hole capital after selling all securities -4During handkerchief, feed Ar gas, when pressure was 5 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 3 minutes; Step 3 is heated to 700 ℃ of insulations 20 minutes; The step 4 flow is made as 80sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 1 handkerchief, open the radio-frequency power supply starter, sputtering power is 80 watts, and pre-sputter is after 5 minutes, regulating pressure in vacuum tank is 1 handkerchief, sets the plated film controlled variable 1.33,1.2 of target, 1.4,1.6, behind the revolution of 1.87,0 control warm tables and the position of target, on substrate, add 450 volts negative bias, remove baffle plate; Step 5 begins plated film, and the plated film time is closed all power supplys after being 10 minutes and 15 seconds, treat that vacuum chamber returns to room temperature after, open the vacuum storehouse, make required film.
CNB2007100725951A 2007-08-02 2007-08-02 Method for preparing thin film by using magnetron sputtering Expired - Fee Related CN100494479C (en)

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CN101492811B (en) * 2009-02-20 2012-01-25 电子科技大学 Self-air-suction vacuum plating method
CN102002666B (en) * 2010-10-22 2012-06-27 哈尔滨工业大学 Preparation method of tantalum nitride diffusion impervious layer for copper interconnection
CN102251214B (en) * 2011-07-04 2013-02-20 哈尔滨工业大学 Preparation method of boron phosphide wear-resistant corrosion-resistant coating
CN105088153B (en) * 2015-08-17 2017-09-26 宁波中车时代传感技术有限公司 The preparation method of semiconductor silicon germanium film
CN112760608A (en) * 2020-12-14 2021-05-07 兰州空间技术物理研究所 Method for preventing interlayer air bleeding in carbon fiber composite material surface film deposition process

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