CN100480419C - Method for preparing magnetron sputtering hemisphere film - Google Patents

Method for preparing magnetron sputtering hemisphere film Download PDF

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Publication number
CN100480419C
CN100480419C CNB2007100725966A CN200710072596A CN100480419C CN 100480419 C CN100480419 C CN 100480419C CN B2007100725966 A CNB2007100725966 A CN B2007100725966A CN 200710072596 A CN200710072596 A CN 200710072596A CN 100480419 C CN100480419 C CN 100480419C
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target
vacuum
minutes
film
hemisphere
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Expired - Fee Related
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CNB2007100725966A
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CN101100740A (en
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朱嘉琦
韩潇
姜春竹
韩杰才
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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 semi-spherical 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 spherical film with uniform thickness and no special device clamping work-piece is needed. Its target different from the prior apparatus is oscillated while the heating table is rotating so as to have high utilization rate of the target material.

Description

A kind of preparation method of magnetron sputtering hemisphere film
Technical field
The present invention relates to the preparation method of hemisphere film.
Background technology
Magnetron sputtering film preparation device in the existing film preparing technology, great majority all are plated films in the plane, minority is also arranged on curved surface or hemisphere internal surface plated film, and at hemisphere face outside surface plated film seldom, and existingly exist not enoughly at hemisphere outside surface film coating apparatus, be embodied in: for when the major diameter hemisphere face appearance facial mask, general target will be done very greatly, the target size is big more, and utilization ratio is often low more, so just causes the huge waste problem of target; Because utilize the property of thin film and the target-substrate distance of magnetically controlled sputter method preparation that substantial connection is arranged, when big target plated the sphere film, the distance of target and spherical substrate in very large range changed, the character of the film that plates will produce considerable change in same aura district like this; Realize mechanism's complexity, the used device of existing plating hemisphere film, its target is fixed, the warm table rotation time is swung, and like this for the fixedly existing problems of unplated piece, and warm table place physical construction is comparatively complicated, the mechanical movement degree of flexibility is relatively poor, the lack of homogeneity of plated film.
Summary of the invention
The present invention is bigger in order to solve the used target size of existing each film of system, like this for hemisphere film, causes plated film character inhomogeneous owing to target-substrate distance changes; And because the target size is big more, target utilization is often low more, thereby causes significant wastage; The device of existing in addition plating hemisphere film, magnetic controlling target maintains static, warm table is swung in the time of the warm table rotation, so just need unit clamp to fix unplated piece, and rotation warm table complicated in mechanical structure, the motion degree of flexibility is relatively poor, is difficult to form the problem of the film of homogeneous character, the invention provides a kind of preparation method of magnetron sputtering hemisphere film, concrete technical scheme adopts following steps to implement:
Step 1, choose Coating Materials as target, and substrate is placed on the rotation warm table, this warm table is positioned at the vacuum storehouse;
Step 2, sealed vacuum storehouse start vacuum acquiring system, and 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, 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 under said temperature;
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, 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, come the rotating speed of stepless control rotation warm table by stepper-motor, rotating speed is controlled in 15 rev/mins, control the running orbit of warm table top target simultaneously with another stepper-motor, making target do step-length along the substrate arc direction is that 0.1~5 geneva motion of spending is to the substrate surface plated film;
After step 6, step 5 are finished, treat to make when temperature is reduced to room temperature in the vacuum storehouse semisphere film.
The present invention has adopted the compound motion form around centre of sphere motion and substrate rotation of magnetron sputtering target, and substrate is easy to fix, and coating process is stable.Prepared film character of the present invention is even; The membrane thickness unevenness degree is less than 10%, and deposition process is easy to control, the utilization ratio height of target.The present invention can utilize less target to prepare the hemisphere film of large-size, and it is very little that little target plated film makes that target surface arrives the variable in distance of semisphere substrate, thereby help the property of thin film homogeneous that plates; Avoided sample table place complex mechanical construction in addition, improved the sensitivity level of mechanical movement, clamping workpiece to be plated is convenient, and property of thin film and thickness are stable.
Description of drawings
Fig. 1 is the planar motion track synoptic diagram that the present invention rotates warm table and target, and Fig. 2 is that target and rotation warm table are overlooked the movement locus synoptic diagram.1 is target among the figure, the 2nd, and warm table.
Embodiment
Embodiment one: the method for present embodiment adopts following steps:
Step 1, to select Si (silicon) for use be substrate, is the rete target with Ge (germanium) material, and substrate material is placed on the rotation warm table, and this warm table is positioned at the vacuum storehouse;
Step 2, sealed vacuum storehouse start vacuum acquiring system, and 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, 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 the needed temperature of deposit film, Heating temperature to 25~750 ℃, and insulation 10 minutes~1 hour under said temperature;
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, 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, come the rotating speed of stepless control rotation warm table by stepper-motor, rotating speed is controlled in 15 rev/mins and changes, control the running orbit of warm table top target simultaneously with another stepper-motor, make target do step-length and control to the substrate surface plated film less than the geneva motion of 5 degree along the plating piece arc direction; The plated film time is determined according to the area and the thickness of film, the principle that concrete controlled variable is selected is: hemisphere face is spent with 10 respectively, 17 degree, 16 degree, 16 degree, 16 degree, 15 degree are divided into 6 parts from the head-to-foot face of ball, each part is divided into some small portions again, the coating process of each part is controlled with a controlled variable, this controlled variable is the coefficient of a time series, this time series is that target is when doing geneva motion, the time series of forming in the residence time of each small portion, the ratio of each number is approximately equal to the area ratio of each small portion in the time series.For certain part, controlled variable increases, and thick at this part coating film thickness, controlled variable reduces, and is thin at this part coating film thickness; In order to obtain uniform semisphere film, will select suitable controlled variable.
After step 6, step 5 are finished, treat to make when temperature is reduced to room temperature in the vacuum storehouse semisphere film.
Embodiment two: the difference of present embodiment and embodiment one is to adopt in the step 1 Φ 164mm Si hemisphere face, and the preparation thickness is 90nm on hemisphere face, adopts the Ge material as the rete target, and the target diameter is 49mm, and thickness is 3mm; Step 2 is taken seriously, and vacuum tightness reaches 4.6 * 10 in the hole capital after selling all securities -4During handkerchief, when pressure was 3 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 5 minutes; Step 3 is plated film at room temperature, and the Ar airshed is made as 60sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 3 handkerchiefs, opens the radio-frequency power supply starter, and power is made as 50 watts; The pre-sputter of step 4 is after 5 minutes, and regulating pressure in vacuum tank is 0.6 handkerchief; It is 1.0,1.0,2.3,4.5 that step 5 is set controlled variable, behind the position of 5.2,8.4 revolutions that come the controls revolution warm table and target, removes baffle plate, begins plated film; The step 6 plated film time is 1 hour 43 minutes, promptly makes the semisphere film.Other step is identical with embodiment one.
Sedimentary thickness is about 88.2nm through recording, and differs 2% with designed film thickness, and unevenness is 9.8% in the film, less than the unevenness 10% of service requirements.
Embodiment three: the difference of present embodiment and embodiment one is to adopt in the step 1 Φ 300mm Si hemisphere face, and the preparation thickness is 280nm on hemisphere face, adopts the Ge material as the rete target, and the target diameter is 49mm, and thickness is 3mm; Step 2 is taken seriously, and vacuum tightness reaches 2.0 * 10 in the hole capital after selling all securities -4During handkerchief, when pressure was 4 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 4 minutes; Step 3 starts the heating lamp group and is heated to 200 degree, is incubated 30 minutes, and the Ar airshed is made as 40sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 5 handkerchiefs, opens the radio-frequency power supply starter, and power is made as 150 watts; The pre-sputter of step 4 is after 3 minutes, and regulating pressure in vacuum tank is 0.8 handkerchief; It is 1.0,2.0,2.6,2.5 that step 5 is set controlled variable, behind the position of 3.0,8.0 revolutions that come the controls revolution warm table and target, removes baffle plate, begins plated film; The step 6 plated film time is 1 hour 27 minutes, promptly makes the semisphere film.Other step is identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is to adopt in the step 1 Φ 270mm Si hemisphere face, and the preparation thickness is 460nm on hemisphere face, adopts the Ge material as the rete target, and the target diameter is 49mm, and thickness is 3mm; Step 2 is taken seriously, and vacuum tightness reaches 7.5 * 10 in the hole capital after selling all securities -4During handkerchief, when pressure was 5 handkerchiefs in the hole capital after selling all securities of taking seriously, ionization was cleaned 3 minutes; Step 3 starts the heating lamp group and is heated to 350 ℃, is incubated 20 minutes, and the Ar airshed is made as 20sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 4 handkerchiefs, opens the radio-frequency power supply starter, and power is made as 200 watts; Step 4, pre-sputter are after 4 minutes, and regulating pressure in vacuum tank is 1 handkerchief; It is 1.0,1.7,2.8,3.8 that step 5 is set controlled variable, behind the position of 6.5,9.0 revolutions that come the controls revolution warm table and target, removes baffle plate, begins plated film; The step 6 plated film time is 2 hours 2 minutes, promptly makes the semisphere film.Other step is identical with embodiment one.

Claims (9)

1, a kind of preparation method of magnetron sputtering hemisphere film is characterized in that the step of this method is as follows:
Step 1, choose Coating Materials as target, and the hemisphere face substrate is placed on the rotation warm table, this warm table is positioned at the vacuum storehouse;
Step 2, sealed vacuum storehouse start vacuum acquiring system, and vacuum tightness reaches 1.0 * 10 in the vacuum storehouse -4~9.9 * 10 -4Handkerchief feeds Ar gas, when pressure is 3~5 handkerchiefs in the vacuum storehouse, starts the ionization power supply, substrate surface is carried out ionization clean, and 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 under said temperature;
Step 4, in the vacuum storehouse, feed starter gas, gas pressure intensity starter when 3~5 handkerchiefs in the vacuum storehouse, apply sputtering power, 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, 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, make target do step-length and control to the substrate surface plated film less than the geneva motion of 5 degree along the substrate arc direction;
After step 6, step 5 are finished, when treating that temperature is reduced to room temperature in the vacuum storehouse, promptly make hemispheric film.
2, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1 is characterized in that adopting in the step 1 Φ 300mm Si hemisphere face, and the preparation thickness is 280nm on hemisphere face.
3, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1 is characterized in that adopting the Ge material as target, and the target diameter is 49mm, and thickness is 3mm.
4, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1 is characterized in that vacuum tightness reaches 2.0 * 10 in the step 2 vacuum storehouse -4Handkerchief, when pressure was 4 handkerchiefs in the vacuum storehouse, ionization was cleaned 4 minutes.
5, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1, after it is characterized in that end is cleaned in step 3 ionization, start the heating lamp group and be heated to 200 ℃, be incubated 30 minutes, the Ar airshed is made as 40sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 5 handkerchiefs, open the radio-frequency power supply starter, power is made as 150 watts.
6, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1 is characterized in that step 4, pre-sputter after 3 minutes, and regulating pressure in vacuum tank is 0.8 handkerchief.
7, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1 is characterized in that it is 1.0,2.0,2.6,2.5 that step 5 is set controlled variable, 3.0,8.0 come the position of the revolution of controls revolution warm table and target after, remove baffle plate; The step 5 plated film time is 1 hour 27 minutes, promptly makes the semisphere film.
8, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1, it is characterized in that adopting in the step 1 Φ 164mm Si hemisphere face, the preparation thickness is 90nm on hemisphere face, adopts the Ge material as target, the target diameter is 49mm, and thickness is 3mm; Step 2 is taken seriously, and vacuum tightness reaches 4.6 * 10 in the hole capital after selling all securities -4Handkerchief, when pressure was 3 handkerchiefs in the vacuum storehouse, ionization was cleaned 5 minutes; After step 3 ionization clean to finish, plated film at room temperature, the Ar airshed is made as 60sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 3 handkerchiefs, opens the radio-frequency power supply starter, and power is made as 50 watts; The pre-sputter of step 4 is after 5 minutes, and regulating pressure in vacuum tank is 0.6 handkerchief; It is 1.0,1.0,2.3,4.5 that step 5 is set controlled variable, 5.2,8.4 come the position of the revolution of controls revolution warm table and target after, remove baffle plate; The step 5 plated film time is 1 hour 43 minutes, promptly makes the semisphere film.
9, the preparation method of a kind of magnetron sputtering hemisphere film according to claim 1, it is characterized in that adopting in the step 1 Φ 270mm Si hemisphere face, the preparation thickness is 460nm on hemisphere face, adopts the Ge material as target, the target diameter is 49mm, and thickness is 3mm; Vacuum tightness reaches 7.5 * 10 in the step 2 vacuum storehouse -4Handkerchief, when pressure was 5 handkerchiefs in the vacuum storehouse, ionization was cleaned 3 minutes; After step 3 ionization is cleaned and finished, start the heating lamp group and be heated to 350 degree, be incubated 20 minutes, the Ar airshed is made as 20sccm, turns down slide valve simultaneously, when treating that gas pressure in vacuum is 4 handkerchiefs, opens the radio-frequency power supply starter, and power is made as 200 watts; Step 4, pre-sputter are after 4 minutes, and regulating pressure in vacuum tank is 1 handkerchief; It is 1.0,1.7,2.8,3.8 that step 5 is set controlled variable, 6.5,9.0 come the position of the revolution of controls revolution warm table and target after; The step 5 plated film time is 2 hours 2 minutes, promptly makes the semisphere film.
CNB2007100725966A 2007-08-02 2007-08-02 Method for preparing magnetron sputtering hemisphere film Expired - Fee Related CN100480419C (en)

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CN102409304A (en) * 2011-06-13 2012-04-11 星弧涂层科技(苏州工业园区)有限公司 Method for coating films on focusing mirrors
CN105334557A (en) * 2015-11-10 2016-02-17 东莞鑫泰玻璃科技有限公司 High-reflection sun light reflection mirror and manufacturing method thereof
CN105671509B (en) * 2016-03-31 2018-06-29 成都西沃克真空科技有限公司 A kind of spherical target cathode mechanism and Sputting film-plating apparatus
CN107500559B (en) * 2017-10-12 2020-06-19 信利光电股份有限公司 Curved surface glass coating device
CN107723675A (en) * 2017-11-17 2018-02-23 东莞颠覆产品设计有限公司 Pvd equipment and physical gas-phase deposite method
CN109182991B (en) * 2018-11-06 2020-11-10 哈尔滨工业大学 Relative movement mechanism of magnetron sputtering coating device suitable for coating film on conformal substrate surface and coating method thereof
CN110699653B (en) * 2019-10-30 2021-08-03 哈尔滨工业大学 Metal film preparation device and method suitable for polyhedral reflector
CN110760812B (en) * 2019-12-02 2024-05-28 江苏铁锚玻璃股份有限公司 Hemispherical glass outer surface coating device and coating method

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