CN103911596B - A kind of device preparing diamond film and use the method that this device prepares diamond film - Google Patents
A kind of device preparing diamond film and use the method that this device prepares diamond film Download PDFInfo
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Abstract
The present invention provides a kind of device preparing diamond film, it adopts microwave plasma CVD device, this device includes microwave system, vacuum system, air supply system and plasma reaction chamber, plasma reaction chamber is provided with a spinning chip bench, the microwave that in work process, microwave system produces enters plasma reaction chamber, the gas that air supply system provides is excited to produce plasma ball above spinning chip bench, being also arranged above refractory metal annulus at spinning chip bench, this refractory metal annulus is positioned at the internal the latter half of plasmasphere.
Description
Technical field
The invention belongs to vacuum microelectronics technique field, be specifically related to a kind of device preparing diamond film and the method using this device to prepare diamond film.
Background technology
Diamond has high hardness, and at room temperature has the excellent properties such as high thermal conductivity, low thermal coefficient of expansion, high chemical inertness, can be used to make cutting element and wear parts, is widely used in field of machining.It addition, it still makes the ideal material of the devices such as surface pressure sensor, radio-resisting semiconductor device, high power semiconductor lasers and high density anticorrosion antiwear infrared optical window.But natural diamond quantity shortcoming that is rare, expensive and that be difficult to process constrains widely using of diamond.The diamond of High Temperature High Pressure (HTHP) the method synthesis that the fifties in last century grows up is Powdered, grows oarse-grained diamond costly, and application is restricted and containing metallic catalyst impurity.Since Matsumto et al. has invented after chemical vapor deposition (CVD) method prepares diamond film in nineteen eighty-two, people have seen the dawn of diamond film applied research.Today, people about the research more actuality of cvd diamond, both at home and abroad about high speed, high-quality, Large-Area-Uniform growing diamond film technology of preparing become the problem that research worker is currently wanted urgently to solve.
Adopt CVD to prepare the technique of diamond film, have been developed over a variety of at present, wherein mainly have: heat wire method (HFCVD), microwave method (MPCVD), direct-current plasma torch method and oxy-acetylene combustion flame etc..Wherein microwave method is to carry out provocative reaction gas with electromagnetic wave energy, and owing to being electrodless discharge, plasma is pure, the region of discharge of microwave is concentrated and is not extended simultaneously, activating and produce various atomic radicals such as atomic hydrogen etc., the maximum kinetic energy of the ion of generation is low, will not corrode the diamond generated.Microwave plasma CVD (MPCVD) method is prepared the performance of diamond and is sufficiently close to even partial properties with natural diamond and has surmounted natural diamond, and this makes the preparation of MPCVD diamond film become the study hotspot of each scientific research institution.
Microwave plasma CVD (MPCVD) device generally comprises microwave system, vacuum system, air supply system and plasma reaction chamber, plasma reaction chamber is provided with a spinning chip bench, prepare in the process of diamond, the microwave that microwave system produces enters plasma reaction chamber, the gas that air supply system provides is excited to produce plasma ball above spinning chip bench, plasma ball is close to substrate surface, and sp2 structure carbon-containing group becomes diamond film in substrate surface deposition.Owing to above the spinning chip bench of plasma-reaction-chamber zone line, microwave energy is the strongest, in plasma ball, energy density distribution is different, plasma zone line density is higher than the density of marginal area, cause that in plasma ball, active group Density Distribution is different, the temperature of plasma ball contact substrate surface also there will be height difference, thus the diamond membrane with large area layer thickness homogeneity grown out is bad, thick middle and thin edge.Diamond film zone line and marginal area thickness difference are typically in about 15-20%, and the polishing of diamond film is caused difficulty and is a kind of waste greatly to diamond by this.
Summary of the invention
The technical problem to be solved is for above shortcomings in prior art, it is provided that a kind of device preparing diamond film and use the method that this device prepares diamond film, and technique is simple, and prepared diamond film area is big and thickness is uniform.
Solve the technology of the present invention problem and be employed technical scheme comprise that this is prepared the device of diamond film and adopts microwave plasma CVD device, this device includes microwave system, vacuum system, air supply system and plasma reaction chamber, plasma reaction chamber is provided with a spinning chip bench, the microwave that in work process, microwave system produces enters plasma reaction chamber, the gas that air supply system provides is excited to produce plasma ball above spinning chip bench, it is also arranged above refractory metal annulus at spinning chip bench, this refractory metal annulus is positioned at the internal the latter half of plasmasphere.Refractory metal annulus is positioned at plasma ball, near plasma ball border.
By such scheme, setting up more than one non-metal frame in described spinning chip bench surrounding, the resistance to 1200 DEG C of high temperature above of non-metal frame, described refractory metal annulus is connected by tungsten filament or tantalum wire are fixing with non-metal frame.
By such scheme, non-metal frame is preferably alumina holder or SiO2, the ceramics bracket such as SiC.Described support can pass through microwave, microwave field is not affected and physical and chemical stability is good.
By such scheme, described refractory metal annulus is the tungsten filament that processes of surface carbonation or the diameter of tantalum wire, tungsten filament or tantalum wire is 0.8-1.5mm.
The present invention also provides for a kind of method preparing diamond film, and it adopts said apparatus to prepare, and comprises the following steps:
(1) substrate of surface ungrease treatment is put on the spinning chip bench that plasma reaction is indoor, base vacuum taken out by article on plasma reative cell, microwave system generation hydrogen plasma is opened time high-purity hydrogen to vacuum is 1-2kPa with backward plasma reaction chamber passes into, utilize microwave radiation heating substrate to 800-1000 DEG C, with hydrogen plasma, substrate surface is performed etching process, etch period is 15min, obtains the substrate of clean surface；
(2) in plasma reaction chamber, methane is passed into, it is formed over plasma ball at spinning chip bench, adjust microwave plasma CVD device technological parameter and make the refractory metal annulus above plasma ball covering step (1) gained substrate surface and spinning chip bench, making diamond at described substrate surface forming core, nucleated time is 10-60min；
(3) adjusting microwave plasma CVD device technological parameter and carry out the growth of diamond film, growth time is 10-100 hour, obtains diamond film in uniform thickness.
By such scheme, step (1) described surface ungrease treatment is place the substrates in grind 30 minutes with the bortz powder of granularity 100nm on abrasive disk, then ultrasonic 30min in the acetone soln containing a small amount of 100nm bortz powder, and dry with absorbent cotton after ultrasonic 5min in acetone.
Substrate of the present invention can be silicon chip or molybdenum sheet.Preferably, described substrate is P type (100) monocrystalline silicon piece.P type (100) monocrystalline silicon piece purity is high, and the diamond film quality of deposition is good.
Step (1) described base vacuum refers to that vacuum is 10-2-10Pa.Described high-purity hydrogen purity is more than 99.999v%.
By such scheme, the described microwave plasma CVD device technological parameter of step (2) is microwave power 750W, plasma reaction indoor operating air pressure 7.8kPa, methane flow 5sccm, hydrogen flowing quantity 200sccm, nucleated time 30min, substrate temperature 800-850 DEG C.
By such scheme, the described microwave plasma CVD device technological parameter of step (3) is microwave power 800W, plasma reaction indoor operating air pressure 8.8kPa, methane flow 3sccm, hydrogen flowing quantity 200sccm, growth time 30min, substrate temperature 820-880 DEG C.
The invention has the beneficial effects as follows: on the original architecture basics of MPCVD equipment, article on plasma reative cell has carried out design repacking, add refractory metal annulus, plasma is utilized easily to be adsorbed in the characteristic of metal surface, thus changing plasma density distribution, reach to improve the purpose of diamond membrane with large area deposition uniformity.
Accompanying drawing explanation
Fig. 1 is the installation site schematic diagram of refractory metal annulus of the present invention；
Fig. 2 is the work process schematic diagram of refractory metal annulus of the present invention；
Fig. 3 is the film thickness distribution figure of the diamond film prepared by embodiment one；
Fig. 4 is the film thickness distribution figure of the diamond film prepared by embodiment two；
Fig. 5 is the film thickness distribution figure of the diamond film prepared by embodiment three；
Fig. 6 is the film thickness distribution figure of the diamond film prepared by comparative example 1.
In figure: 1 plasma ball；2 refractory metal annulus；3 substrates；4 spinning chip bench；5 tungsten filaments；6 alumina holder.
Detailed description of the invention
For making those skilled in the art be more fully understood that technical scheme, below in conjunction with embodiment, the present invention is described in further detail.
The embodiment of the present invention provides a kind of device preparing diamond film.Microwave plasma CVD device used by the present invention is antenna coupling quartz bell cover type micro-wave plasma CVD device, and its spinning chip bench diameter is 30mm, and microwave power is 800W.Density of hydrogen used by the present invention is 99.999v%, and methane concentration used is 99.995v%.
Embodiment one
Refractory metal ring textures carbonization treatment: selecting diameter is that the tantalum wire of 1.0mm is to make the refractory metal annulus that diameter is 10mm, tantalum wire is placed on plasma reaction indoor and carries out surface carbonation process { microwave power 800W, operating air pressure 8.8kPa, methane flow 10sccm (sccm), hydrogen flowing quantity 200sccm, time 15min}.Refractory metal annulus after being processed by surface carbonation lies in a horizontal plane in distance spinning chip bench vertical height 5mm place.Its installation site schematic diagram is as shown in Figure 1.Setting up an alumina holder 6 in spinning chip bench 4 surrounding, refractory metal annulus 2 is connected by tungsten filament 5 is fixing with alumina holder 6.
Using diameter be 20mm, thickness be 1mm P type (100) monocrystalline silicon piece as substrate deposition diamond film.Silicon chip is ground 30 minutes with the bortz powder of granularity 100nm on abrasive disk, then ultrasonic 30min in the acetone soln containing a small amount of 100nm bortz powder, and dry with absorbent cotton after ultrasonic 5min in acetone, obtain the substrate of surface ungrease treatment.
Following steps are adopted to prepare diamond film:
(1) being put into by the substrate of above-mentioned surface ungrease treatment on the spinning chip bench 4 that plasma reaction is indoor, base vacuum 10 taken out by article on plasma reative cell-2Pa, microwave system generation hydrogen plasma is opened time high-purity hydrogen to vacuum is 1.5kPa with backward plasma reaction chamber passes into, utilize microwave radiation heating substrate to 800 DEG C of (microwave power 700W, operating air pressure 7.8kPa, hydrogen flowing quantity 200sccm), with hydrogen plasma, substrate surface being performed etching process, etch period is 15min, obtains the substrate 3 of clean surface；
(2) in plasma reaction chamber, methane is passed into, it is formed over plasma ball at spinning chip bench, adjust microwave plasma CVD device technological parameter (microwave power 750W, operating air pressure 8.8kPa, methane flow 5sccm, hydrogen flowing quantity 200sccm, substrate temperature 830 DEG C) make the refractory metal annulus (now plasma bulb diameter is 25mm) above plasma ball 1 covering step (1) gained substrate surface and spinning chip bench, making diamond at described substrate 3 surface forming core, operating diagram is as shown in Figure 2.Nucleated time is 30min；
(3) microwave plasma CVD device technological parameter (microwave power 800W, operating air pressure 8.8kPa, methane flow 3sccm are adjusted, hydrogen flowing quantity 200sccm, substrate temperature 850 DEG C) carry out the growth of diamond film, growth time is 50 hours, obtains diamond film in uniform thickness.
Diamond film film thickness distribution prepared by the present embodiment is tested, 19 points are equidistantly taken in diamond film diametric(al), diamond film diameter is divided into 20 equal portions, from left to right survey the thickness of each point, its film thickness distribution figure is as it is shown on figure 3, the diamond film middle edge thickness difference prepared by the present embodiment is 5.3%.
Embodiment two
Refractory metal ring textures carbonization treatment: select diameter be the tantalum wire of 1.0mm to make the refractory metal annulus that diameter is 15mm, adopt, with embodiment one identical method, tantalum wire carried out surface carbonation process.Refractory metal annulus after being processed by surface carbonation lies in a horizontal plane in distance spinning chip bench vertical height 7mm place.
Using diameter be 20mm, thickness be 1mm P type (100) monocrystalline silicon piece as substrate deposition diamond film.Adopt the method identical with embodiment one that substrate surface is carried out ungrease treatment.
Following steps are adopted to prepare diamond film:
(1) being put into by the substrate of above-mentioned surface ungrease treatment on the spinning chip bench that plasma reaction is indoor, base vacuum 10 taken out by article on plasma reative cell-2Pa, microwave system generation hydrogen plasma is opened time high-purity hydrogen to vacuum is 1.5kPa with backward plasma reaction chamber passes into, utilize microwave radiation heating substrate to 800 DEG C of (microwave power 700W, operating air pressure 7.8kPa, hydrogen flowing quantity 200sccm), with hydrogen plasma, substrate surface being performed etching process, etch period is 15min, obtains the substrate of clean surface；
(2) in plasma reaction chamber, methane is passed into, it is formed over plasma ball at spinning chip bench, adjust microwave plasma CVD device technological parameter (microwave power 750W, operating air pressure 8.8kPa, methane flow 5sccm, hydrogen flowing quantity 200sccm, substrate temperature 830 DEG C) make the refractory metal annulus (now plasma bulb diameter is 25mm) above plasma ball covering step (1) gained substrate surface and spinning chip bench, making diamond at described substrate surface forming core, nucleated time is 30min；
(3) microwave plasma CVD device technological parameter (microwave power 800W, operating air pressure 8.8kPa, methane flow 3sccm are adjusted, hydrogen flowing quantity 200sccm, substrate temperature 850 DEG C) carry out the growth of diamond film, growth time is 50 hours, obtains diamond film in uniform thickness.
Adopt the method identical with embodiment one that the diamond film film thickness distribution prepared by the present embodiment is tested, its film thickness distribution figure is as shown in Figure 4, there are similar three peak values in the diamond film film thickness distribution curve obtained, and interpeak is maximum, occurs in that two a little bit smaller peak values immediately below annulus.Diamond film middle edge thickness difference is 5.1%.
Embodiment three
Refractory metal ring textures carbonization treatment: select thin tantalum wire to make the refractory metal annulus that diameter is 20mm, adopts the method identical with embodiment one that tantalum wire is carried out surface carbonation process.Refractory metal annulus after being processed by surface carbonation lies in a horizontal plane in distance spinning chip bench vertical height 9mm place.
Using diameter be 20mm, thickness be 1mm P type (100) monocrystalline silicon piece as substrate deposition diamond film.Adopt the method identical with embodiment one that substrate surface is carried out ungrease treatment.
Following steps are adopted to prepare diamond film:
(1) being put into by the substrate of above-mentioned surface ungrease treatment on the spinning chip bench that plasma reaction is indoor, base vacuum 10 taken out by article on plasma reative cell-2Pa, microwave system generation hydrogen plasma is opened time high-purity hydrogen to vacuum is 1.5kPa with backward plasma reaction chamber passes into, utilize microwave radiation heating substrate to 800 DEG C of (microwave power 700W, operating air pressure 7.8kPa, hydrogen flowing quantity 200sccm), with hydrogen plasma, substrate surface being performed etching process, etch period is 15min, obtains the substrate of clean surface；
(2) in plasma reaction chamber, methane is passed into, it is formed over plasma ball at spinning chip bench, adjust microwave plasma CVD device technological parameter (microwave power 750W, operating air pressure 8.8kPa, methane flow 5sccm, hydrogen flowing quantity 200sccm, substrate temperature 830 DEG C) make the refractory metal annulus above plasma ball covering step (1) gained substrate surface and spinning chip bench, making diamond at described substrate surface forming core, nucleated time is 30min；
(3) microwave plasma CVD device technological parameter (microwave power 800W, operating air pressure 8.8kPa, methane flow 3sccm are adjusted, hydrogen flowing quantity 200sccm, substrate temperature 850 DEG C) carry out the growth of diamond film, growth time is 50 hours, obtains diamond film.
Diamond film film thickness distribution prepared by the present embodiment is tested, and its film thickness distribution figure is as it is shown in figure 5, diamond film film thickness distribution class of a curve is similar to W-shape.Thickness difference is 5.8%.
Comparative example 1
Be added without refractory metal annulus, using diameter be 20mm, thickness be 1mm P type (100) monocrystalline silicon piece as substrate deposition diamond film.The method identical with embodiment one is adopted to process substrate surface.Refractory metal annulus after being processed by surface carbonation lies in a horizontal plane in distance spinning chip bench vertical height 5mm place.Prepare concretely comprising the following steps of diamond film:
(1) being put into by the substrate of above-mentioned surface ungrease treatment on the spinning chip bench that plasma reaction is indoor, base vacuum 10 taken out by article on plasma reative cell-2Pa, microwave system generation hydrogen plasma is opened time high-purity hydrogen to vacuum is 1.5kPa with backward plasma reaction chamber passes into, utilize microwave radiation heating substrate to 800 DEG C of (microwave power 700W, operating air pressure 7.8kPa, hydrogen flowing quantity 200sccm), with hydrogen plasma, substrate surface being performed etching process, etch period is 15min, obtains the substrate of clean surface；
(2) in plasma reaction chamber, methane is passed into, it is formed over plasma ball at spinning chip bench, adjust microwave plasma CVD device technological parameter (microwave power 750W, operating air pressure 8.8kPa, methane flow 5sccm, hydrogen flowing quantity 200sccm, substrate temperature 830 DEG C) make plasma ball covering step (1) gained substrate surface, making diamond at described substrate surface forming core, nucleated time is 30min；
(3) microwave plasma CVD device technological parameter (microwave power 800W, operating air pressure 8.8kPa, methane flow 3sccm are adjusted, hydrogen flowing quantity 200sccm, substrate temperature 850 DEG C) carry out the growth of diamond film, growth time is 50 hours, obtains diamond film in uniform thickness.
Diamond film film thickness distribution prepared by the present embodiment is tested, and as shown in Figure 6, thicknesses of layers distribution curve presents typical normal distribution curve to its film thickness distribution figure.Middle high rim is low, and thickness difference is 14.5%.When not adding ring, plasma ball internal density is unevenly distributed, and diameter is in the plasma ball of about 25mm, and the closer to outer edge area, plasma density is more low.Energy density of plasma skewness, the energy radiation to substrate silicon chip is also uneven, and growth deposition meron silicon chip surface diamond film presents the thickness distribution that middle high rim is low.
By the above detailed description to the embodiment of the present invention, it will be appreciated that the invention solves conventional MPCVD method and prepare the problem that diamond film is in uneven thickness.Utilizing plasma to be easily adsorbed in the characteristic of metal surface, add a refractory metal annulus in substrate upper horizontal, change the Energy distribution of microwave electric field, thus changing plasma density distribution, reaching to improve the purpose of diamond membrane with large area deposition uniformity.Diamond film zone line and marginal area thickness difference are reduced to 5.1-5.8% by do not add refractory metal annulus 14.5%.The chip processing of diamond film can only be used diamond, and costly, the uniformity of rete improves the thickness that can be greatly reduced the required chip of processing, thus being substantially reduced processing cost.
It is understood that the principle that is intended to be merely illustrative of the present of embodiment of above and the illustrative embodiments that adopts, but the invention is not limited in this.For those skilled in the art, without departing from the spirit and substance in the present invention, it is possible to make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (7)
1. the device preparing diamond film, it adopts microwave plasma CVD device, this device includes microwave system, vacuum system, air supply system and plasma reaction chamber, plasma reaction chamber is provided with a spinning chip bench, the microwave that in work process, microwave system produces enters plasma reaction chamber, the gas that air supply system provides is excited to produce plasma ball above spinning chip bench, it is characterized in that: be also arranged above refractory metal annulus at spinning chip bench, this refractory metal annulus is positioned at the internal the latter half of plasmasphere；
Described refractory metal annulus is the tungsten filament that processes of surface carbonation or the diameter of tantalum wire, tungsten filament or tantalum wire is 0.8-1.5mm.
2. the device preparing diamond film according to claim 1, it is characterized in that: set up more than one non-metal frame in described spinning chip bench surrounding, the resistance to 1200 DEG C of high temperature above of non-metal frame, described refractory metal annulus is connected by tungsten filament or tantalum wire are fixing with non-metal frame.
3. the method preparing diamond film, it is characterised in that adopt device described in claim 1 or 2 to prepare, comprise the following steps:
(1) substrate of surface ungrease treatment is put on the spinning chip bench that plasma reaction is indoor, base vacuum taken out by article on plasma reative cell, microwave system generation hydrogen plasma is opened time high-purity hydrogen to vacuum is 1.0-2.0kPa with backward plasma reaction chamber passes into, utilize microwave radiation heating substrate to 800-1000 DEG C, with hydrogen plasma, substrate surface is performed etching process, etch period is 15min, obtains the substrate of clean surface；
(2) in plasma reaction chamber, methane is passed into, it is formed over plasma ball at spinning chip bench, adjust microwave plasma CVD device technological parameter and make the refractory metal annulus above plasma ball covering step (1) gained substrate surface and spinning chip bench, making diamond at described substrate surface forming core, nucleated time is 10-60min；
(3) adjusting microwave plasma CVD device technological parameter and carry out the growth of diamond film, growth time is 10-100 hour, obtains diamond film in uniform thickness.
4. the method preparing diamond film according to claim 3, it is characterized in that: step (1) described surface ungrease treatment is place the substrates in grind 30 minutes with the bortz powder of granularity 100nm on abrasive disk, then ultrasonic 30min in the acetone soln containing a small amount of 100nm bortz powder, and dry with absorbent cotton after ultrasonic 5min in acetone.
5. the method preparing diamond film according to claim 3, it is characterised in that: described substrate is P type (100) monocrystalline silicon piece.
6. the method preparing diamond film according to claim 3, it is characterized in that: the described microwave plasma CVD device technological parameter of step (2) is microwave power 750W, plasma reaction indoor operating air pressure 7.8kPa, methane flow 5sccm, hydrogen flowing quantity 200sccm, nucleated time 30min, substrate temperature 800-850 DEG C.
7. the method preparing diamond film according to claim 3, it is characterized in that: the described microwave plasma CVD device technological parameter of step (3) is microwave power 800W, plasma reaction indoor operating air pressure 8.8kPa, methane flow 3sccm, hydrogen flowing quantity 200sccm, growth time 30min, substrate temperature 820-880 DEG C.
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| CN107164740B (en) * | 2017-05-12 | 2019-05-07 | 中国工程物理研究院应用电子学研究所 | A method of diamond film is prepared using MPCVD method |
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| CN110512195A (en) * | 2019-09-20 | 2019-11-29 | 武汉工程大学 | A kind of tubular material inner surface carries out the method and device of MPCVD |
| CN110938811A (en) * | 2019-12-30 | 2020-03-31 | 广东达蒙得半导体科技有限公司 | Method for rotatably growing diamond in microwave plasma chemical vapor deposition |
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| CN112063996B (en) * | 2020-09-18 | 2021-04-20 | 上海征世科技有限公司 | Microwave plasma reaction chamber and accommodating base thereof |
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| CN113529050B (en) * | 2021-07-05 | 2022-09-20 | 云南民族大学 | Plasma etching method for polishing diamond film and product thereof |
| CN114684818B (en) * | 2022-04-01 | 2022-09-02 | 佛山曜世新材料科技有限公司 | Diamond plasma device and diamond preparation method |
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Address after: 201799 west side of Building 2, No. 500, Huapu Road, Qingpu District, Shanghai Patentee after: Shanghai Zhengshi Technology Co.,Ltd. Address before: 201799 west side of Building 2, No. 500, Huapu Road, Qingpu District, Shanghai Patentee before: SHANGHAI ZHENGSHI TECHNOLOGY Co.,Ltd. |