CN101671846A - Method for reducing stress of cubic boron nitride thin film - Google Patents
Method for reducing stress of cubic boron nitride thin film Download PDFInfo
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- CN101671846A CN101671846A CN200810119797A CN200810119797A CN101671846A CN 101671846 A CN101671846 A CN 101671846A CN 200810119797 A CN200810119797 A CN 200810119797A CN 200810119797 A CN200810119797 A CN 200810119797A CN 101671846 A CN101671846 A CN 101671846A
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- boron nitride
- cubic boron
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- thin film
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Abstract
The invention discloses a preparation method for reducing the stress of a cubic boron nitride thin film, which comprises the following steps: 1, taking a silicon substrate; 2, placing the silicon substrate on an ion beam assisted deposition system, taking a highly-pure boron target as a sputtering target deposited by the cubic boron nitride thin film, and taking a silicon target as a doped source;3, heating the substrate; 4, adopting two independently adjustable Kaufman broad beam ion sources of which a main ion source adopts Ar<+> ions to bombard the boron target and the silicon target, andsimultaneously taking mixed ion beams of Ar<+> and N2<+> as an auxiliary ion source to bombard the substrate so as to deposit and form the cubic boron nitride thin film on the substrate by the ion beam assisted deposition system; 5, cooling the substrate down in the ion beam assisted deposition system; and 6, taking the prepared substrate out, and performing stress parameter testing to finish thepreparation.
Description
Technical field
The present invention relates to superhard thin film deposition technique field, particularly a kind of preparation method who reduces stress of cubic boron nitride thin film.
Background technology
Cubic boron nitride (c-BN) is the III-V group iii v compound semiconductor material of a kind of superhard, broad-band gap, high heat conductance, high resistivity, high thermal stability and chemical stability.It is be known as third generation semiconductor material after silicon, germanium and gallium arsenide of diamond, silicon carbide and gan, wherein the over-all properties with c-BN is the most excellent again for this, is having a wide range of applications aspect high temperature, high frequency, the high-power electronic device.At present, people can use the method for multiple physical vapor deposition (PVD) and chemical vapor deposition (CVD) to prepare the c-BN film.In the various technologies of preparing of c-BN film, generally use energetic ion (50-1000eV) bombardment, make and have higher internal stress in institute's deposit film, the c-BN film that thickness surpasses 200nm is easy to come off automatically from substrate surface, does not satisfy the needs of industrial coating and microelectronics development.Thereby the internal stress that reduces the c-BN film has very important meaning for the application prospect of c-BN.
Since the end of the eighties in last century, each research group takes various means to reduce internal stress in the c-BN film, as increase transition layer or buffer layer, improving depositing temperature or after annealing handles, reduce the energy of bombarding ion or adopt nucleation and the control of growth substep, and utilize ionizing radiation etc., these methods have reduced the internal stress in the c-BN film to a certain extent, improved the adhesivity of film, but effect is very not remarkable.In addition, for the application facet of c-BN film at high temperature, high frequency, high-power electronic device, methods such as high temperature annealing, high temperature deposition, ionizing radiation, buffer layer all are subjected to certain restriction, as high temperature and ion irradiation between each layer of semiconductor device inside and metal contact all important influence of aspect with semi-conductor, buffer layer has then directly had influence on the design of device architecture.If can reduce the internal stress of c-BN film, for realizing that the application of c-BN film as semiconductor material and industrial coating two aspects all has great significance by mixing.
Summary of the invention
At current present situation, the object of the present invention is to provide a kind of preparation method who reduces stress of cubic boron nitride thin film, thereby effectively reduce the internal stress of c-BN film c-BN thin-film material stress studies.Utilize ion beam assisted deposition to prepare the c-BN film, in preparation process, introduce a spot of silicon in the c-BN film, thereby reduce the internal stress of c-BN film.The size that stretches into shared target area in the main ion source bombardment scope by the adjustment silicon target realizes different silicon doping concentration.
The technical scheme that technical solution problem of the present invention is adopted is:
The invention provides a kind of preparation method who reduces stress of cubic boron nitride thin film, it is characterized in that, comprise the steps:
Step 1: get a silicon substrate;
Step 2: silicon substrate is placed in the ion beam assisted depositing system, and as the sedimentary sputtering target of cubic boron nitride film, silicon target is as doped source with the high purity boron target;
Step 3: substrate is heated;
Step 4: the ion beam assisted depositing system adopt two can independent regulation Kaufman wide beam ion source, Ar is adopted in the main ion source
+Ion bombardment boron target and silicon target are simultaneously with Ar
+And N
2 +Ion beam mixing as assisting ion source bombardment substrate, make formation of deposits cubic boron nitride film on the substrate;
Step 5: in the ion beam assisted depositing system, substrate is lowered the temperature;
Step 6: take out the substrate after preparing, carry out the stress parameters test, finish preparation.
Wherein silicon substrate is silicon (a 001) single crystalline substrate.
Wherein the background vacuum pressure of ion beam assisted depositing system is 1 * 10
-5Pa.
Underlayer temperature T when wherein depositing cubic boron nitride film
sBe 200-800 ℃, working gas pressure P
DBe 1.0-5.0 * 10
-2Pa.
Main ion source Ar when wherein depositing cubic boron nitride film
+Ion energy be U
1, U
1Span 1200-1500eV, beam current density is J
1, J
1Span 200-400 μ A/cm
2
Assisting ion source Ar when wherein depositing cubic boron nitride film
++ N
2 +Ion energy be U
2, U
2Span 300-500eV, beam current density J
2, J
2Span 60-90 μ Q/cm
2, Ar
+: N
2 +Line be 1: 1 than m.
Wherein silicon doping concentration is n
Si, n
SiSpan 0-3.3at.%.
Invention is compared the significative results that is had with background technology
Utilize the ion beam assisted depositing system to the mode that the c-BN film carries out silicon doping, realized the release of c-BN film internal stress, can effectively reduce the internal stress of c-BN film.Silicon doping and c-BN growth for Thin Film are carried out simultaneously in this method, do not need extra step, and be simple and easy to do.Than methods such as high temperature annealing, high temperature deposition, ionizing radiation, buffer layers, this method is more suitable for the application of c-BN film aspect semiconducter device; In addition, compare with additive method, this method can more effective release stress.
Description of drawings
For further specifying feature of the present invention and technical scheme, below in conjunction with embodiment and accompanying drawing the present invention is done a detailed description, wherein:
Fig. 1 prepares the structural representation of the ion beam assisted depositing system of silicon doping c-BN film for the present invention;
Fig. 2 is the Fourier transform infrared spectroscopy figure of the Different Silicon doping content c-BN film of inventive embodiments preparation;
Fig. 3 is the internal stress of the Different Silicon doping content c-BN film of the embodiment of the invention preparation variation diagram with silicon doping concentration.
Embodiment
See also shown in Figure 1ly, a kind of preparation method who reduces stress of cubic boron nitride thin film of the present invention is characterized in that, comprises the steps:
Step 1: get a silicon substrate, this silicon substrate is silicon (a 001) single crystalline substrate;
Step 2: silicon substrate is placed in the ion beam assisted depositing system sample holder 1, and as the sedimentary sputtering target of cubic boron nitride film, silicon target is as doped source with high purity boron target 2;
Step 3: substrate is heated; Underlayer temperature T
sBe 200-800 ℃, working gas pressure P
DBe 1.0-5.0 * 10
-2Pa;
Step 4: the ion beam assisted depositing system adopt two can independent regulation Kaufman wide beam ion source, Ar are adopted in main ion source 2
+Ion bombardment boron target 3 and silicon target 4 are simultaneously with Ar
+And N
2 +Ion beam mixing as assisting ion source 5 bombardment substrates, make formation of deposits cubic boron nitride film on the substrate; The background vacuum pressure of this ion beam assisted depositing system is 1 * 10
-5Pa; Main ion source Ar when wherein depositing cubic boron nitride film
+Ion energy be U
1, U
1Span 1200-1500eV, beam current density is J
1, J
1Span 200-400 μ A/cm
2Assisting ion source Ar wherein
++ N
2 +Ion energy be U
2, U
2Span 300-500eV, beam current density J
2, J
2Span 60-90 μ A/cm
2, Ar
+: N
2 +Line be 1: 1 than m; The control silicon target is by the silicon doping of the size realization different concns of main ion source bombardment area, silicon doping concentration n
SiBetween 0-3.3at.%; Film thickness h is 120nm;
Step 5: in the ion beam assisted depositing system, substrate is cooled to room temperature;
Step 6: take out the cubic boron nitride film of preparation, carry out the stress parameters test, finish preparation.Growth result
According to above-mentioned processing condition, on silicon (001) substrate, deposited the c-BN film of Different Silicon doping content.Fig. 1 is for realizing the structural representation of the ion beam assisted depositing system that the present invention adopts.We bombard regional shared scope by the control silicon target in the main ion source size realizes the silicon doping of different concns.Fig. 2 is the Fourier transform infrared spectroscopy figure that utilizes the Different Silicon doping content c-BN film of above-mentioned technological process preparation.As can see from Figure 2, three infrared absorption peak intensity of all c-BN films remain unchanged substantially, demonstrate when silicon doping concentration is not higher than 3.3at.%, silicon doping is to not influence of the phase structure in the c-BN film, and the c-BN film still has higher cube phase content.We can also see from Fig. 2, and along with the increase of silicon doping concentration, the peak position of cube phase absorption peak of c-BN film moves the 1107cm when never mixing gradually to the lower wave number direction
-1Move to the 1074cm of doping content when being 3.3at.%
-1The peak position of cube phase absorption peak moves relevant with the stress in the c-BN film in the c-BN film.C-BN film cube phase absorption peak peak position that there are some researches show zero stress state is positioned at 1055cm
-1, the every increase of stress 1GPa in the c-BN film, cube phase absorption peak moves 5cm to high wave number direction
-1, promptly the internal stress σ in the c-BN film can be calculated by following formula, σ (GPa)=(v
TO-1055)/5.09GPa.Fig. 3 utilizes the variation diagram of the internal stress of the Different Silicon doping content c-BN film that following formula calculates with silicon doping concentration.We see from Fig. 3, do not have adulterated c-BN film, its internal stress 10.4GPa, and along with the increase of silicon doping concentration, the internal stress in the c-BN film reduces gradually, and when silicon doping concentration was 3.3at%, the internal stress in the c-BN film was reduced to 3.8GPa.Obvious a spot of silicon doping makes the internal stress of c-BN film significantly reduce.Therefore, utilizing the stress of the method reduction c-BN film of silicon doping is a kind of fruitful method in semiconductor film deposition field and superhard thin film deposition field.
So far invention has been described in conjunction with the preferred embodiments.Should be appreciated that those skilled in the art can carry out various other change, replacement and interpolations under the situation that does not break away from the spirit and scope of the present invention.Therefore, scope of the present invention is not limited to above-mentioned specific embodiment, and should be limited by claims.
Claims (7)
1, a kind of preparation method who reduces stress of cubic boron nitride thin film is characterized in that, comprises the steps:
Step 1: get a silicon substrate;
Step 2: silicon substrate is placed in the ion beam assisted depositing system, and as the sedimentary sputtering target of cubic boron nitride film, silicon target is as doped source with the high purity boron target;
Step 3: substrate is heated;
Step 4: the ion beam assisted depositing system adopt two can independent regulation Kaufman wide beam ion source, Ar is adopted in the main ion source
+Ion bombardment boron target and silicon target are simultaneously with Ar
+And N
2 +Ion beam mixing as assisting ion source bombardment substrate, make formation of deposits cubic boron nitride film on the substrate;
Step 5: in the ion beam assisted depositing system, substrate is lowered the temperature;
Step 6: take out the substrate after preparing, carry out the stress parameters test, finish preparation.
2, the method for reduction stress of cubic boron nitride thin film according to claim 1 is characterized in that, wherein silicon substrate is silicon (a 001) single crystalline substrate.
3, the method for reduction stress of cubic boron nitride thin film according to claim 1 is characterized in that, wherein the background vacuum pressure of ion beam assisted depositing system is 1 * 10
-5Pa.
4, the method for reduction stress of cubic boron nitride thin film according to claim 1 is characterized in that, underlayer temperature T when wherein depositing cubic boron nitride film
sBe 200-800 ℃, working gas pressure P
DBe 1.0-5.0 * 10
-2Pa.
5, the method for reduction stress of cubic boron nitride thin film according to claim 1 is characterized in that, main ion source Ar when wherein depositing cubic boron nitride film
+Ion energy be U
1, U
1Span 1200-1500eV, beam current density is J
1, J
1Span 200-400 μ A/cm
2
6, the method for reduction stress of cubic boron nitride thin film according to claim 1 is characterized in that, assisting ion source Ar when wherein depositing cubic boron nitride film
++ N
2 +Ion energy be U
2, U
2Span 300-500eV, beam current density J
2, J
2Span 60-90 μ A/cm
2, Ar
+: N
2 +Line be 1: 1 than m.
7, the method for reduction stress of cubic boron nitride thin film according to claim 1 is characterized in that, wherein silicon doping concentration is n
Si, n
SiSpan 0-3.3at.%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534534A (en) * | 2012-01-19 | 2012-07-04 | 张金凤 | Optical thin film with excellent performances |
| CN102560357A (en) * | 2012-01-19 | 2012-07-11 | 张金凤 | Preparation method of boron nitride optical film |
| CN104313684A (en) * | 2014-09-30 | 2015-01-28 | 中国科学院半导体研究所 | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal |
| CN106119798A (en) * | 2016-08-19 | 2016-11-16 | 南京航空航天大学 | The preparation method of anode film linear ion source auxiliary cubic boron nitride coated cutting tool |
| CN106702337A (en) * | 2016-12-09 | 2017-05-24 | 北京科技大学 | In-situ control method for stress of hard coating |
| CN107219030A (en) * | 2016-03-21 | 2017-09-29 | 中国科学院深圳先进技术研究院 | Membrane stress tester and its method of testing |
| CN110660657A (en) * | 2019-09-30 | 2020-01-07 | 福建北电新材料科技有限公司 | Method for releasing residual stress on surface of substrate slice |
-
2008
- 2008-09-10 CN CN200810119797A patent/CN101671846A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534534A (en) * | 2012-01-19 | 2012-07-04 | 张金凤 | Optical thin film with excellent performances |
| CN102560357A (en) * | 2012-01-19 | 2012-07-11 | 张金凤 | Preparation method of boron nitride optical film |
| CN104313684A (en) * | 2014-09-30 | 2015-01-28 | 中国科学院半导体研究所 | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal |
| CN107219030A (en) * | 2016-03-21 | 2017-09-29 | 中国科学院深圳先进技术研究院 | Membrane stress tester and its method of testing |
| CN106119798A (en) * | 2016-08-19 | 2016-11-16 | 南京航空航天大学 | The preparation method of anode film linear ion source auxiliary cubic boron nitride coated cutting tool |
| CN106702337A (en) * | 2016-12-09 | 2017-05-24 | 北京科技大学 | In-situ control method for stress of hard coating |
| CN106702337B (en) * | 2016-12-09 | 2019-04-16 | 北京科技大学 | A kind of hard coat stress in-situ control method |
| CN110660657A (en) * | 2019-09-30 | 2020-01-07 | 福建北电新材料科技有限公司 | Method for releasing residual stress on surface of substrate slice |
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Open date: 20100317 |