CN113584458B - Method for preparing diamond film on potassium tantalate niobate crystal by microwave plasma chemical vapor deposition technology - Google Patents
Method for preparing diamond film on potassium tantalate niobate crystal by microwave plasma chemical vapor deposition technology Download PDFInfo
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- CN113584458B CN113584458B CN202110756515.4A CN202110756515A CN113584458B CN 113584458 B CN113584458 B CN 113584458B CN 202110756515 A CN202110756515 A CN 202110756515A CN 113584458 B CN113584458 B CN 113584458B
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- 239000013078 crystal Substances 0.000 title claims abstract description 59
- 239000010432 diamond Substances 0.000 title claims abstract description 47
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 46
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 46
- 239000011591 potassium Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 21
- 238000005516 engineering process Methods 0.000 title description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 4
- 229910003468 tantalcarbide Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001534 heteroepitaxy Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
Abstract
The invention belongs to the technical field of crystal synthesis, and particularly relates to a method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method, which comprises the following steps: 1) Placing the potassium tantalate niobate crystal in a cavity of a microwave plasma chemical vapor deposition device, vacuumizing the cavity, introducing hydrogen, adjusting hydrogen flow, air pressure and microwave power to generate plasma to wrap the potassium tantalate niobate crystal so as to heat the potassium tantalate niobate crystal, and adjusting a vacuum fine adjustment valve to keep the air pressure in the cavity within the range of 11-12kPa; 2) After the pressure intensity and the plasma state are stable, introducing methane into the cavity in the step 1), controlling the introduction flow ratio of the methane and the hydrogen, and adjusting a vacuum fine adjustment valve to keep the air pressure in the cavity within the range of 11kPa-12 kPa; and (3) closing the microwave source after methane is introduced for 6-9h, cooling the cavity, and taking out the sample to obtain the diamond film prepared on the potassium tantalate-niobate crystal. The method has the advantages of simple preparation process, high quality of the prepared diamond film, high growth speed and the like.
Description
Technical Field
The invention belongs to the technical field of crystal synthesis, and particularly relates to a method for preparing a diamond film on a potassium tantalate-niobate crystal by a Microwave Plasma Chemical Vapor Deposition (MPCVD) device.
Background
Diamond has extremely high hardness, excellent optical properties, relatively low dielectric constant compared with other materials, high thermal conductivity at room temperature, high chemical inertness and other excellent properties, and is often applied to the fields of optical equipment, optical windows, coatings, semiconductors, electronic devices and the like. The storage capacity of natural diamond is very small, and the demand of diamond is continuously increasing, so the research on the preparation process and technology is particularly urgent for growing and preparing high-speed and high-quality diamond films.
The diamond film prepared by the microwave plasma chemical vapor deposition method has the advantages of high quality, large area and the like, and is one of the effective methods for synthesizing diamond at present. Various substrates (e.g., si, siC, pt, ir) have been used for heteroepitaxial deposition of diamond films by microwave plasma chemical vapor deposition for many years, and higher quality diamond films have been successfully prepared on these substrates. In order to further improve the quality of the diamond film and obtain various diamonds with different requirements (high thermal conductivity, diluted magnetism, semiconductors, X-ray detection, etc.), new substrates need to be explored.
Disclosure of Invention
The invention aims to provide a method for preparing a diamond film by taking potassium tantalate niobate crystals as a novel substrate and utilizing a microwave plasma chemical vapor deposition method for heteroepitaxy.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition device comprises the following steps:
1) Placing the potassium tantalate niobate crystal in a cavity of a microwave plasma chemical vapor deposition device, vacuumizing the cavity, introducing hydrogen, adjusting hydrogen flow, air pressure and microwave power, exciting the gas in the cavity by absorbing microwave energy to generate plasma, wrapping the potassium tantalate niobate crystal by the plasma to heat the potassium tantalate niobate crystal, and adjusting a vacuum fine adjustment valve to keep the air pressure in the cavity within the range of 11-12kPa;
2) After the pressure and the plasma state are stable, introducing methane into the cavity in the step 1), controlling the introduction flow ratio of methane to hydrogen to be 200; and (3) closing the microwave source after methane is introduced for 6-9h, cooling the cavity, and taking out the sample to obtain the diamond film prepared on the potassium tantalate-niobate crystal.
According to the scheme, in the step 1), vacuum pumping is carried out until the vacuum degree is 10-100Pa.
According to the scheme, in the step 1), the microwave power is 1000W, the hydrogen flow is 200sccm, and the gas pressure is 11kPa.
According to the scheme, potassium tantalate niobate crystal is used as a substrate, and the temperature is controlled to be 600-800 ℃. The plasma wraps the surface of the potassium tantalate niobate crystal and heats the potassium tantalate niobate crystal, and the temperature is determined by the heat generated by the microwave energy.
According to the scheme, in the step 2), when the pressure and the plasma state are stable, the pressure, the temperature and the microwave power are stable, namely the pressure is stable within the range of 11kPa-12kPa, and the substrate temperature is stable within the range of 600 ℃ -800 ℃ through the microwave power.
According to the scheme, in the step 2), the flow rate of methane is 5sccm.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts microwave plasma chemical vapor deposition method (MPCVD method), utilizes methane/hydrogen mixed gas to prepare the diamond film on potassium tantalate niobate (KTN) crystal for the first time, and has the advantages of high quality, high purity, high growth speed and the like.
Drawings
FIG. 1 is an XRD pattern of a starting substrate (labeled Beforee in FIG. 1) and a prepared diamond film (labeled After in FIG. 1) in example 1 of the present invention.
Fig. 2 is an XRD pattern of the diamond films prepared in examples 1 and 2, respectively, of the present invention.
Fig. 3 is a view showing the structure of a diamond film prepared in example 1 of the present invention under an optical microscope at a magnification of 500.
FIG. 4 is a schematic structural diagram of a microwave plasma CVD apparatus for producing a diamond film according to the present invention.
In fig. 4: 1-a substrate table; 2-a metal flange; 3-a cavity; 4-an air inlet; 5-a pumping hole of a vacuum pump; 6-compressing the rectangular waveguide; 7-quartz glass tube.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
In the following examples, potassium tantalate niobate (formula KTa) 1-x Nb x O 3 Abbreviated as KTN) crystal, and the value of X is in the range of 0-0.37. The following examples specifically employ KTa with an X value of 0.23 1-x Nb x O 3 The crystal is taken as a representative. The potassium tantalate niobate crystal is prepared by a pulling method, and can be referred to as the following documents: [1]Growth and Performance Studies of Wangxxuping, KTN series crystals [ D]University of Shandong, 2008. However, the present invention is not limited to the specific production of KTN crystalsThe preparation method is as follows. The KTN crystal was previously ultrasonically cleaned with ethanol and acetone and dried.
In the following embodiments, as shown in fig. 4, a microwave plasma cvd apparatus for preparing a diamond film includes a substrate stage 1, a metal flange 2, and a chamber 3. The substrate table 1 is positioned in the cavity 3, the substrate table 1 is installed on a lifting mechanism (the substrate table 1 can be lifted), the cavity 3 is provided with an air inlet 4 and a vacuum pump air exhaust opening 5, hydrogen and methane are introduced from the air inlet 4, the vacuum pump air exhaust opening 5 is connected with a vacuum pump through a vacuum pipeline (used for pumping air in the cavity 3 to vacuum), and the vacuum pipeline is provided with a vacuum fine adjustment valve. The middle part (the position close to the substrate) of the cavity 3 is provided with a quartz glass tube 7 in series (the cavity 3 is circular, the middle part of the cavity 3 is the quartz glass tube 7), the cavity 3 is fixed with an upper metal flange and a lower metal flange, the upper metal flange is positioned above the quartz glass tube 7, the lower metal flange is positioned below the quartz glass tube 7, and the cavity 3 is connected with the compressed rectangular waveguide by the upper metal flange and the lower metal flange 2 (the upper metal flange and the lower metal flange are sealed with the quartz glass tube 7 by rubber rings). The compressed rectangular waveguide 6 is connected with a microwave generator (microwave energy generated by the microwave generator enters the cavity 3 from the compressed rectangular waveguide 6 through a quartz glass tube 7). 2.45GHz microwave is transmitted through the rectangular waveguide and coupled in the cavity, and the gas absorbs the excitation of microwave energy to generate plasma after entering the cavity.
Example 1
A method for preparing a diamond film on a potassium tantalate niobate crystal by a microwave plasma chemical vapor deposition device comprises the following steps:
(1) Sequentially using ethanol and acetone solution to carry out ultrasonic cleaning on the potassium tantalate-niobate crystal to remove surface impurities; then, placing the potassium tantalate-niobate crystal at the central position above the substrate table, sealing the metal flange, and vacuumizing the cavity;
(2) Introducing hydrogen into the cavity, adjusting microwave power, hydrogen flow and gas pressure, exciting the gas by absorbing microwave energy to generate plasma, and using the following process parameters: the hydrogen flow rate was 200sccm, the working gas pressure was 11kPa, and the microwave power was 800W.
(3) Adjusting the height of the substrate table to enable the plasma to wrap the surface of the crystal and heat the crystal (the temperature is 600-800 ℃), and adjusting a vacuum fine adjustment valve to keep the air pressure in the cavity at 11-12kPa;
(4) When the pressure and the plasma state are stable, methane is introduced to adjust the gas flow and the gas ratio (adjusting the volume ratio of hydrogen to methane to be H) 2 :CH 4 =200, methane 5sccm, hydrogen 200 sccm); and after the deposition reaction is finished for 6h, closing the microwave source, cooling the cavity, and taking out a sample (marked as sample No. 1) to obtain the diamond film prepared on the potassium tantalate-niobate crystal.
From the XRD spectrum of fig. 1, it can be seen that the 2 θ angles corresponding to the (111) and (220) crystal planes of diamond are 43.9 ° and 75.2 °, respectively. In sample # 1, there is a diffraction peak for a portion of the tantalum carbide, indicating that tantalum carbide is formed during the growth process. The diamond crystal orientation in sample # 1 has (111) and (220) planes, and the (111) plane has a distinct advantage. Therefore, the diamond film prepared on the potassium tantalate niobate crystal in the embodiment has obvious diamond diffraction peaks except a small amount of tantalum carbide, and the diamond film is proved to be successfully grown on the potassium tantalate niobate crystal.
By observing the diamond film prepared on the potassium tantalate niobate crystal in the embodiment under an optical microscope, as shown in fig. 3, it can be seen that the crystal grains are relatively uniform in size, closely arranged, and poor in surface flatness.
Example 2
A method for preparing a diamond film on a potassium tantalate niobate crystal by a microwave plasma chemical vapor deposition device comprises the following steps:
(1) Sequentially using ethanol and acetone solution to carry out ultrasonic cleaning on the potassium tantalate-niobate crystal to remove surface impurities; then, placing the crystal at the central position above the substrate table, sealing the metal flange, and vacuumizing the cavity;
(2) Introducing hydrogen into the cavity, adjusting microwave power, hydrogen flow and gas pressure, exciting the gas by absorbing microwave energy to generate plasma, and using the following process parameters: hydrogen flow of 200sccm, working pressure of 11kPa and microwave power of 800W;
(3) The height of the substrate stage is adjusted to allow the plasma to wrap and heat the crystal surface (temperature is 600-800 ℃). Adjusting the vacuum fine-tuning valve to keep the air pressure in the cavity at 11-12kPa;
(4) When the pressure and the plasma state are stable, methane is introduced to adjust the gas flow and the gas ratio (adjusting the volume ratio of hydrogen to methane to be H) 2 :CH 4 And = 5, methane 5sccm and hydrogen 200 sccm), closing the microwave source after the deposition reaction is finished for 9h, cooling the cavity, and taking out a sample (marked as sample # 2) to obtain the diamond film prepared on the potassium tantalate-niobate crystal.
In this example, diamond films were prepared on potassium tantalate niobate crystals and exfoliated, and the XRD patterns thereof are shown in fig. 2. It can be seen that in sample # 2, no diffraction peak of potassium tantalate niobate crystal is generated due to peeling of the film from the substrate, and tantalum carbide is still generated. The diamond crystal grain orientation of the sample No. 2 has (111) and (220) planes, the (111) plane is in absolute dominance, compared with the sample No. 1, two diffraction peaks of the diamond are more obvious, the film thickness increases along with the increase of the reaction time, and the successful growth of the diamond film on the potassium tantalate niobate crystal is also shown.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the scope of the present invention.
Claims (7)
1. A method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method is characterized by comprising the following steps:
1) Placing the potassium tantalate-niobate crystal in a cavity of a microwave plasma chemical vapor deposition device, vacuumizing the cavity, introducing hydrogen, adjusting hydrogen flow, air pressure and microwave power, generating plasma to wrap the potassium tantalate-niobate crystal to heat the potassium tantalate-niobate crystal, and adjusting a vacuum fine-tuning valve to keep the air pressure in the cavity within the range of 11-12kPa;
2) After the pressure intensity and the plasma state are stable, introducing methane into the cavity in the step 1), controlling the introduction flow ratio of hydrogen and methane, and adjusting a vacuum fine adjustment valve to keep the air pressure in the cavity within the range of 11kPa-12 kPa; and (3) closing the microwave source after methane is introduced for 6-9h, cooling the cavity, and taking out the sample to obtain the diamond film prepared on the potassium tantalate-niobate crystal.
2. The method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method according to claim 1, wherein the microwave power in step 1) is 800-1200W.
3. The method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method according to claim 1, wherein the hydrogen flow rate in step 1) is 150 to 250 seem.
4. The method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method according to claim 1, wherein the potassium tantalate niobate crystal is used as a substrate, and the temperature of the substrate is controlled to be 600 ℃ -800 ℃.
5. The method for preparing a diamond film on a potassium tantalate niobate crystal by using the microwave plasma chemical vapor deposition method according to claim 1, wherein in the step 2), the flow ratio of hydrogen to methane introduced is controlled to be 200.
6. The method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method according to claim 1, wherein the potassium tantalate niobate crystal is previously ultrasonically cleaned with ethanol and acetone and dried.
7. The method for preparing a diamond film on a potassium tantalate niobate crystal by using a microwave plasma chemical vapor deposition method according to claim 1, wherein the vacuum degree in step 1) is evacuated to 10 to 100Pa.
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| CN106012003A (en) * | 2016-06-07 | 2016-10-12 | 武汉工程大学 | Two-dimensional expansion method for CVD monocrystal diamond |
| CN111775354A (en) * | 2020-06-19 | 2020-10-16 | 山东省科学院新材料研究所 | Method for processing and manufacturing potassium tantalate niobate monocrystal substrate element |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106012003A (en) * | 2016-06-07 | 2016-10-12 | 武汉工程大学 | Two-dimensional expansion method for CVD monocrystal diamond |
| CN111775354A (en) * | 2020-06-19 | 2020-10-16 | 山东省科学院新材料研究所 | Method for processing and manufacturing potassium tantalate niobate monocrystal substrate element |
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