CN1888133A - No-brush temperature measuring method and device with CVD system substrate - Google Patents

No-brush temperature measuring method and device with CVD system substrate Download PDF

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Publication number
CN1888133A
CN1888133A CNA2006100408622A CN200610040862A CN1888133A CN 1888133 A CN1888133 A CN 1888133A CN A2006100408622 A CNA2006100408622 A CN A2006100408622A CN 200610040862 A CN200610040862 A CN 200610040862A CN 1888133 A CN1888133 A CN 1888133A
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substrate
temperature measuring
nichrome wire
cvd system
thermopair
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CN100523295C (en
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徐锋
左敦稳
郭魂
卢文壮
曾荡
黎向锋
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Haian Chang Chang Technology Transfer Center Co Ltd
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Nanjing University of Aeronautics and Astronautics
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Abstract

The present invention is no-brush temperature measuring method and device for measuring the temperature of CVD system substrate dynamically. The present invention has swinging, rather than rotating, substrate bench to ensure the homogeneity of temperature on substrate surface and facilitate temperature measurement with thermocouple, and modified no-brush thermocouple structure for real-time monitoring on the temperature of substrate surface.

Description

A kind of no-brush temperature measuring method of CVD system substrate and device
Technical field
The present invention relates to the method and the device of a kind of hot-wire chemical gas-phase deposition (heated filament CVD) method diamond film deposition system substrate temperature field test, especially a kind of can be in the continuous swing process of substrate dynamic measurement big area underlayer temperature field radially with the method and the device of axis multiple spot underlayer temperature, specifically a kind of CVD system substrate temp measuring method and device based on toggle.
Background technology
At present, diamond is an occurring in nature the hardest known material, has high thermal conductivity and transaudient speed, high wear resistance and extremely low frictional coefficient simultaneously, becomes the NEW TYPES OF TOOL MATERIALS with excellent properties.But, natural diamond is rare and extremely expensive, chemical gaseous phase depositing process (CVD) is the nearly 20 years adamantine methods of novel preparation that grow up, and industrialization is just progressively moved towards in the research of CVD diamond film at present, and high quality stable growth diamond film becomes people's research focus.
Nichrome wire CVD quality of forming film is better, and equipment is simple, and parameter is easy to control, and preparation cost is cheap, is fit to the industrialization production of diamond membrane with large area.Studies show that in a large number in the processing parameter of nichrome wire CVD system, the size of underlayer temperature and homogeneity are one of of paramount importance parameters of diamond film growth, very big to the quality and the growth velocity influence of the structure of diamond thin, crystalline form, film.The temperature field of analysing in depth and study heated filament CVD system distributes the technology of understanding adamantine sedimentation mechanism, improvement heated filament CVD device and the preparation of optimization diamond thin is all had great importance.
Nichrome wire CVD method depositing large-area adopts molybdenum as substrate usually, adopts the thermocouple measurement underlayer temperature.The testing method of traditional underlayer temperature field is: thermopair is arranged in substrate central authorities, position about measuring distance substrate surface 1mm, according to heat transfer theory as can be known, temperature herein and substrate surface temperature are more or less the same, when adopting nichrome wire CVD method to prepare diamond film, generally with the temperature of this temperature as the sign substrate surface.
But in nichrome wire CVD system, nichrome wire is arranged and is had directivity, because the distance to nichrome wire is different, substrate surface exists evident difference perpendicular to heated filament direction and the each point temperature that is parallel to the temperature of heated filament direction, therefore, in the depositing diamond membrane process, in order to improve the homogeneity in substrate surface temperature field, usually substrate needs to keep continuous rotary motion in deposition process, measure the radially distribution of multi-point temp field of substrate surface in rotating condition, must adopt mechanisms such as brush, gathering a temperature spot needs a brush, and the multi way temperature signal then needs a plurality of brushes, and each brush can not contact, increase the complicacy of mechanism, and easily loose contact after the wear of brush, influenced the reliability of temp measuring system.Therefore, mostly only measure under the actionless situation of substrate when measuring the substrate surface multi-point temp at present, error is very big, and this is the prominent question that exists in the nichrome wire CVD method depositing diamond membrane process.
Summary of the invention
The objective of the invention is to measure inconvenience or problem that can't dynamic measurement, invent a kind of CVD system substrate temp measuring method and device that can real-time continuous measurement substrate surface temperature distribution based on toggle at underlayer temperature in existing hot-wire chemical gas-phase deposition (heated filament CVD) the method diamond film deposition system.
Technical scheme of the present invention is:
A kind of CVD system substrate temp measuring method based on toggle, it is characterized in that radially and/or axial arranged some thermoelectric sides and draw by the lead that links to each other with the thermopair electrical signal that thermopair is measured and to deliver to Controlling System outside the vacuum chamber along substrate working platform, substrate working platform is linked to each other with swing, make it under the drive of tilting mechanism, do swing, obtain best diamond film deposition effect so that the temperature field on the substrate working platform is in uniform state.
Above-mentioned tilting mechanism can be toggle, especially a kind of three-link mechanism or four-bar mechanism of doing oscillating motion.
The angle of oscillation of described substrate is 90 °~180 °, and its swing rate is per minute 5~8 times.
A kind of no-brush temperature measuring device device of CVD system substrate, comprise nichrome wire 1, electrode 2, substrate 3, thermopair 4, nichrome wire 1 links to each other with electrode 2, nichrome wire 1 is installed in the top of substrate 3, nichrome wire 1 and substrate 3 all are arranged in vacuum chamber, it is characterized in that described substrate 3 is installed on the substrate saddle 5, substrate saddle 5 is connected with drive shaft 6, drive shaft 6 is positioned at the outer end of vacuum chamber and is connected with tilting mechanism 7, this tilting mechanism 7 is connected with drive-motor 8, be embedded with some thermopairs 4 on substrate 3, thermopair 4 is drawn outside the vacuum chamber by the connection lead and is linked to each other with electrical control system.
Above-mentioned tilting mechanism 7 can be toggle, and this toggle is three-link mechanism or four-bar mechanism, and the pivot angle of the connecting rod that it links to each other with drive shaft 6 is 90 °~180 °.
The temperature adjustment water jacket 9 that communicates with substrate saddle 5 is installed on drive shaft 6.
Spacing between the nichrome wire 1 is smaller or equal to 6mm, and the distance between substrate 3 and the nichrome wire 1 is smaller or equal to 10mm, and the scope of arranging of nichrome wire 1 is 1.1 times of substrate diameter, and the length of nichrome wire 1 is more than or equal to 1.5 times of substrate 3 diameters.
Offer the groove that thermopair 4 is installed on substrate 3, thermopair 4 is installed in the described groove.
Three connecting rods in the described toggle 7 satisfy following relational expression:
Figure A20061004086200061
Wherein a represents the length of the crank that links to each other with motor, c represents the length of the short connecting rod that links to each other with drive shaft 6, b represents the long connecting rod that connecting crank links to each other with short connecting rod, and d represents the distance between the center of the center of drive-motor 8 and drive shaft 6, and  is the setting pivot angle of drive shaft.
The present invention has the following advantages:
1, the nichrome wire radiations heat energy can be swung, evenly be accepted to substrate continuously, help adopting simultaneously many thermopairs to monitor substrate surface each point variation of temperature situation in real time, so that Controlling System is in time adjusted the sedimentary province temperature, show that through actual measurement the homogeneity of underlayer temperature field can compare favourably with rotary type substrate temperature field.
2, simplify the structure of entire CVD system greatly, especially saved the brush temperature measuring equipment, made the reliability of equipment improve greatly, reduced maintenance workload, prolonged the trouble-free operation cycle of equipment.
3, help the temperature field distribution situation that records according to many thermopairs, parameters such as the spacing between optimization hot-wire temperature, heated filament and the substrate, heated filament spacing, make that the substrate surface temperature field is more even, further improve the thickness of diamond membrane with large area and the homogeneity of grain size.
4, the thermopair arrangement convenience is simple, can adopt lead directly to link to each other with Controlling System, measures accurately and reliably and can monitor in real time.
5, be the concrete implementation result example of the present invention below:
(1) adopts nichrome wire CVD method, at H 2-C 2H 5Sedimentation diameter is the diamond film of 100mm in the OH atmosphere, adopts the present invention to monitor the changing conditions of underlayer temperature field in real time, and the radial temperature profile of the K type thermocouple measurement substrate that to adopt 5 diameters be 1mm makes thermopair closely contact with the molybdenum substrate.Experimental data shows, the maximum of underlayer temperature appears at substrate center, the substrate center temperature is approximately higher than 50 ℃ of edges of substrate temperature greatly, the substrate radius direction approximately differs 20 ℃ being parallel to the heated filament direction with vertical also different as for the thermograde of substrate direction perpendicular to heated filament direction and the thermograde that is parallel to the heated filament direction.Find that in deposition process the temperature of substrate center remains unchanged substantially, and there is fluctuation in the thermopair of radial direction.And the present invention can only survey the temperature of a central point in the past, and if carry out dynamic measurement, structure will be very complicated, and especially the realization difficulty of brush structure in hot environment is bigger.
(2) owing to can adopt the dynamic real-time thermometric, therefore can carry out parameters Optimization to heated filament CVD method depositing diamond, significantly improve the quality of diamond film according to the homogeneity of hot-wire temperature field.Optimized parameters is as follows: hot-wire temperature T f=2600 ℃, heated filament radical n=18, heated filament spacing H l=6mm, heated filament length l=150mm, the distance H of heated filament and substrate S=5mm, heated filament cover substrate the time, the substrate center temperature is 850 ℃, the edges of substrate temperature is 826 ℃, the difference of the center of diamond film and the thickness at edge and grain-size is significantly reduced.
Description of drawings
Fig. 1 is a temperature measuring equipment structural representation of the present invention.
Fig. 2 is the arrangement synoptic diagram of thermopair of the present invention.
Fig. 3 is the schematic diagram of toggle of the present invention.
Embodiment
The present invention is further illustrated for following structure drawings and Examples.
As shown in Figure 1, 2, 3.
A kind of no-brush temperature measuring method of CVD system substrate may further comprise the steps:
At first, radially and/or axial arranged some thermoelectric sides along substrate working platform;
Secondly, the electrical signal that thermopair is recorded is drawn vacuum chamber with the lead that is attached thereto and is delivered to electrical control system outward and handle;
The 3rd, substrate working platform is linked to each other with a toggle, make its swing of under the drive of toggle, making 90 °~180 °, per minute 5~8 times so that the temperature field on the substrate working platform is in uniform state, obtain best diamond film deposition effect.
The concrete device that matches with aforesaid method can be:
A kind of no-brush temperature measuring device of CVD system substrate comprises nichrome wire 1, electrode 2, substrate 3 (can adopt the molybdenum materials quality), thermopair 4, as shown in Figure 1, nichrome wire 1 links to each other with electrode 2, nichrome wire 1 is installed in the top of substrate 3, nichrome wire 1 and substrate 3 all are arranged in vacuum chamber, described substrate 3 is installed on the substrate saddle 5, substrate saddle 5 is connected with drive shaft 6, the temperature adjustment water jacket 9 that communicates with substrate saddle 5 is installed on drive shaft 6, drive shaft 6 is positioned at the outer end of vacuum chamber and is connected with tilting mechanism 7 and (specifically can be toggle, also can be other similar tilting mechanism, as the cam tilting mechanism, the structure of the swing motor direct-drive of also can serving as reasons), toggle is connected with drive-motor 8, drive-motor 8 should be selected slowspeed machine for use, also can adopt the structure formation of common electric machine acceleration and deceleration device, axially be embedded with 3-10 thermopair 4 (as shown in Figure 2) at substrate 3 radially or along drive shaft 6, the quantity of thermopair also can increase and decrease according to the size of substrate working platform during concrete enforcement, and each thermopair 4 is all drawn outside the vacuum chamber by the connection lead and linked to each other with electrical control system.Spacing between the nichrome wire 1 is smaller or equal to 6mm, and the distance between substrate 3 and the nichrome wire 1 is smaller or equal to 10mm, and the scope of arranging of nichrome wire 1 is 1.1 times of substrate diameter, and the length of nichrome wire 1 is more than or equal to 1.5 times of substrate 3 diameters.
The mounting means of thermopair 4 can be by being the hole of 1mm at big area molybdenum substrate surface radial direction drill diameter, pitch-row is 1mm from the distance of substrate surface, placement diameter is the K type thermopair of 1mm in the hole, the position in hole and number are generally 3-10 according to the position and the number decision of required mensuration substrate surface temperature spot.Because substrate 3 is to swing back and forth, signal wire can not be intertwined, and can avoid using many brushes structure that temperature signal is drawn.
In addition, thermopair 4 also can realize that thermopair 4 is installed in the described groove and gets final product by the method for offering groove on substrate 3.
Toggle 7 can adopt three-link mechanism as shown in Figure 3, and the pivot angle of the connecting rod that it links to each other with drive shaft 6 is 90 °~180 °, and swing rate is per minute 5~8 times.
Three connecting rods in the described toggle 7 satisfy following relational expression:
Figure A20061004086200081
Wherein a represents the length of the crank that links to each other with motor, c represents the length of the short connecting rod that links to each other with drive shaft 6, b represents the long connecting rod that connecting crank links to each other with short connecting rod, and d represents the distance between the center of the center of drive-motor 8 and drive shaft 6, and  is the setting pivot angle of drive shaft.
Concrete size can be with reference to following table.
a(mm) b(mm) c(mm) d(mm)
90 50 141.4 70.7 150
100 50 144.0 65.2 150
110 50 145.8 61.0 150
120 50 147.1 57.7 150
130 50 148.1 55.1 150
140 50 148.8 53.2 150
150 50 149.4 51.7 150
160 50 149.7 50.7 150
170 50 149.9 50.1 150
180 50 150 50 200
The part that present embodiment does not relate to, as the structure of CVD cvd furnace, electric control part is graded all same as the prior art.
Make substrate working platform do swing so that the mode that substrate surface is heated evenly replaces traditional rotary type substrate working platform is key of the present invention, characteristics just because of swinging structure, make the installation of temperature thermocouple and collection, the conduction of temperature become very simple and convenient, all all kinds of devices of this method and structures utilized all are considered to equivalence replacement of the present invention, present embodiment has only provided an embodiment, but is not limited only to this structure.

Claims (10)

1, a kind of no-brush temperature measuring method of CVD system substrate, it is characterized in that radially and/or axial arranged some thermoelectric sides and draw by the lead that links to each other with the thermopair electrical signal that thermopair is measured and to deliver to Controlling System outside the vacuum chamber along substrate working platform, substrate working platform is linked to each other with swing, make it under the drive of tilting mechanism, do swing, obtain best diamond film deposition effect so that the temperature field on the substrate working platform is in uniform state.
2, the no-brush temperature measuring method of CVD system substrate according to claim 1 is characterized in that described tilting mechanism is a toggle.
3, the no-brush temperature measuring method of CVD system substrate according to claim 1, the angle of oscillation that it is characterized in that described substrate are 90 °~180 °, and its swing rate is per minute 5~8 times.
4, a kind of device of realizing the described temp measuring method of claim 1, comprise nichrome wire (1), electrode (2), substrate (3), thermopair (4), nichrome wire (1) links to each other with electrode (2), nichrome wire (1) is installed in the top of substrate (3), nichrome wire (1) and substrate (3) all are arranged in vacuum chamber, it is characterized in that described substrate (3) is installed on the substrate saddle (5), substrate saddle (5) is connected with drive shaft (6), drive shaft (6) is positioned at the outer end of vacuum chamber and is connected with tilting mechanism (7), and this tilting mechanism (7) is connected with drive-motor (8); Be provided with some thermopairs (4) on substrate (3), thermopair (4) is drawn outside the vacuum chamber by the connection lead and is linked to each other with electrical control system.
5, the no-brush temperature measuring device of CVD system substrate according to claim 4 is characterized in that described tilting mechanism (7) is a toggle.
6, according to the no-brush temperature measuring device of claim 4 or 5 described CVD system substrate, it is characterized in that described toggle is a three-link mechanism, the pivot angle of the connecting rod that it links to each other with drive shaft (6) is 90 °~180 °.
7, the no-brush temperature measuring device of CVD system substrate according to claim 4 is characterized in that being equipped with the temperature adjustment water jacket (9) that communicates with substrate saddle (5) on drive shaft (6).
8, the no-brush temperature measuring device of CVD system substrate according to claim 4, it is characterized in that spacing between the nichrome wire (1) is smaller or equal to 6mm, distance between substrate (3) and the nichrome wire (1) is smaller or equal to 10mm, the scope of arranging of nichrome wire (1) is 1.1 times of substrate diameter, and the length of nichrome wire (1) is more than or equal to 1.5 times of substrate (3) diameter.
9, the no-brush temperature measuring device of CVD system substrate according to claim 4 is characterized in that offering the groove that thermopair (4) is installed on substrate (3), and thermopair (4) is installed in the described groove.
10,, it is characterized in that three connecting rods in the described toggle satisfy following relational expression according to the no-brush temperature measuring device of claim 2 or 5 described CVD system substrate:
Figure A2006100408620003C1
Wherein a represents the length of the crank that links to each other with motor, c represents the length of the short connecting rod that links to each other with drive shaft (6), b represents the long connecting rod that connecting crank links to each other with short connecting rod, and d represents the distance between the center of the center of drive-motor (8) and drive shaft (6), and  is the setting pivot angle of drive shaft.
CNB2006100408622A 2006-07-31 2006-07-31 No-brush temperature measuring method and device with CVD system substrate Expired - Fee Related CN100523295C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102102196A (en) * 2009-12-16 2011-06-22 丽佳达普株式会社 Temperature control method for chemical vapor deposition apparatus
CN105887042A (en) * 2016-05-26 2016-08-24 无锡特固新材料有限公司 Vibration hot filament chemical vapor deposition device and application in diamond coating deposition

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102102196A (en) * 2009-12-16 2011-06-22 丽佳达普株式会社 Temperature control method for chemical vapor deposition apparatus
CN102102196B (en) * 2009-12-16 2013-05-29 丽佳达普株式会社 Temperature control method for chemical vapor deposition apparatus
CN105887042A (en) * 2016-05-26 2016-08-24 无锡特固新材料有限公司 Vibration hot filament chemical vapor deposition device and application in diamond coating deposition
CN105887042B (en) * 2016-05-26 2018-05-22 张家港市微纳新材料科技有限公司 Vibrate hot-filament chemical vapor deposition equipment and the purposes in Diamond coating deposition

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