CN111945130A - Arrangement method of filaments of hot filament CVD diamond equipment - Google Patents
Arrangement method of filaments of hot filament CVD diamond equipment Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 110
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004050 hot filament vapor deposition Methods 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 82
- 238000000576 coating method Methods 0.000 claims abstract description 28
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims abstract description 17
- 230000008021 deposition Effects 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 6
- 238000005260 corrosion Methods 0.000 claims abstract description 4
- 230000007797 corrosion Effects 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 3
- 230000007547 defect Effects 0.000 claims description 3
- 238000005087 graphitization Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000001737 promoting effect Effects 0.000 claims description 3
- 239000002344 surface layer Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 abstract description 19
- 238000009776 industrial production Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 description 14
- 238000012876 topography Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000006911 nucleation Effects 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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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
- C23C16/271—Diamond only using hot filaments
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/279—Diamond only control of diamond crystallography
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for arranging filaments of hot filament CVD diamond equipment, which specifically comprises the following steps: preparing a plurality of N hot wires, wherein the hot wires are arranged at the upper end part of a base body, the base body is arranged at the upper end part of a bottom plate, and the hot wire intervals Tw are different from each other from the middle to the two sides; carrying out acid-base corrosion treatment on the substrate on the bottom plate; putting the treated substrate into chemical vapor deposition equipment for diamond coating deposition; and observing the diamond micro-morphology of four different positions of the substrate, analyzing the purity and the grain orientation of the diamond, and testing the bonding strength of the diamond coating and the substrate and the diamond micro-morphology and purity of the central substrate. According to the arrangement method of the filaments of the hot filament CVD diamond equipment, the arrangement mode of the filaments is improved, so that the temperature distribution in the deposition chamber is uniform, and the surface appearance and the internal stress distribution of the prepared CVD diamond film product are more uniform during large-batch industrial production.
Description
Technical Field
The invention belongs to the technical field of filaments, and particularly relates to a filament arrangement method of hot filament CVD diamond equipment.
Background
The hot wire chemical vapor deposition method for preparing the diamond coating has simple equipment and low cost, and is very suitable for the industrial production of large-area diamond coatings. In addition to ensuring the excellent performance of the diamond coating, ensuring the uniformity of the performance of the diamond coating is another important factor limiting the industrial production thereof. The uniformity of the temperature field and the gas flow field can seriously affect the uniformity of diamond coatings deposited on the surface of a substrate at different positions in the same batch and the uniformity of diamond nucleation density and growth speed at different positions on the same substrate, thereby affecting the uniformity of the performance of the diamond coatings. Thus, good stability and uniformity of the physical field in the vicinity of the substrate and the hot wire is required by changing the deposition conditions for depositing a good quality diamond coating.
In a common hot wire CVD device, a hot wire array can influence the uniformity of a diamond coating on the surface of a substrate to cause an edge effect and a shadow effect, so that the temperature field on the surface of the substrate is not uniform, the content of non-diamond components in the central part and the edge part of a diamond film and the stress of the film have larger difference, and the appearance of the diamond film below a filament and the appearance of the diamond film between the filaments have larger difference.
Disclosure of Invention
The invention aims to provide a filament arrangement method of a hot filament CVD diamond device, which solves the technical problem that the filament arrangement mode in the traditional device is uneven in temperature distribution in a deposition chamber, designs a reasonable filament arrangement structure, and makes the surface appearance and the internal stress distribution of the prepared CVD diamond film product more uniform during large-scale industrial production.
A method for arranging filaments of hot filament CVD diamond equipment specifically comprises the following steps:
step S1: preparing a plurality of N hot wires, arranging the hot wires at the upper end part of a substrate, arranging the substrate at the upper end part of a bottom plate, wherein the hot wire intervals Tw are different from the middle to the two sides, arranging an interval HY between the hot wires and the bottom plate, and arranging four positions on the substrate for carrying out a diamond coating deposition test;
step S2: carrying out pretreatment, namely acid-base corrosion treatment, on the substrate on the bottom plate;
step S3: putting the pretreated substrate into chemical vapor deposition equipment, putting the substrate well, and depositing a diamond coating;
step S4: and observing the microscopic morphology of the diamond at four different positions of the substrate, analyzing the purity and the grain orientation of the diamond, testing the bonding strength of the diamond coating and the substrate, and testing the microscopic morphology and the purity of the diamond at five different positions of the central substrate.
In step S1, the number of hot wires N is 10, Tw1＝14mm、Tw2＝10mm、Tw3＝10mm、Tw4＝8mm、Tw5＝8mm,HY＝8mm。
In step S2, the method specifically includes the following steps:
step S201: firstly, polishing the substrate for 3min by using P1500 abrasive paper, then continuously polishing the substrate for 3min by using P2000 abrasive paper, removing surface impurities and leaving scratches;
step S202: placing the polished substrate into an acid solution (formula V (H2SO 4): V (H2O 2): 1: 10) for treatment for 20s, and removing cobalt on the surface of the substrate;
step S203: ultrasonically treating with alkali solution (Murakami solution, formula of w (KOH): w (K3[ Fe (CN) 6): w (H2O): 1: 10 (mass ratio)) for 30min to corrode WC particles on the surface of the substrate and expose cobalt on the surface layer;
step S204: and continuously performing ultrasonic treatment for 3min by using an acid solution to remove metal Co which has a certain depth and is used for promoting the graphitization of the diamond on the surface of the matrix.
Step S205: putting the substrate into mixed diamond micro powder acetone suspension, and carrying out ultrasonic grinding treatment for 30min to increase the defect density of the substrate surface, wherein the suspension is prepared by adding diamond micro powder with the granularity of M0.5/1, M2.5/5 and M5/10 into a proper amount of acetone solution according to the mass ratio of 1:1:1 and uniformly mixing.
The distance between the filaments is determined by the groove distance of the molybdenum plate used in the filament fixing device, and after the filaments which are arranged at equal intervals are electrified, the temperature distribution on the surface of the substrate on the sample table is uneven, and the uniformity of the temperature distribution on the surface of the substrate is usually ensured by rotating the sample table and the like. If mass industrial production is required, the number of the matrixes on the sample table is large, the requirement on the uniformity of the temperature distribution is higher, and the uniformity of diamond deposition is directly determined by the temperature distribution. The invention adopts filament arrangement with unequal intervals, thereby ensuring the uniformity of the temperature distribution on the surface of the substrate in the first step and reducing the difficulty of subsequent work.
The basic working principle of the invention is as follows: since the only energy source of the hot filament CVD diamond apparatus is the filament, the temperature is high at a position closer to the filament, and is low otherwise. When the filaments are arranged at equal intervals, the temperature right below the filaments is highest, the temperature at the edge part is lower, the temperature distribution is seriously uneven, the interval of the middle filaments is properly enlarged, the interval of the edge filaments is reduced, and a more uniform temperature field can be obtained.
The method is realized by utilizing chemical vapor deposition equipment to perform diamond layer deposition and obtain a diamond film, belongs to the prior art and is not detailed herein.
The invention achieves the following remarkable effects:
(1) when the CVD diamond film is produced industrially in large batch, the diamond coatings deposited on different positions of the surface of the matrix in the same batch and the uniformity of the nucleation density and the growth speed of the diamond on different positions of the same matrix can be ensured, so that the uniformity of the performance of the diamond coatings is ensured;
(2) the diamond film prepared by the filament arrangement mode of the invention has more uniform surface appearance and film stress distribution and less non-diamond component content.
Drawings
Fig. 1 is a schematic structural diagram of a placement position of a substrate in an embodiment of the invention.
FIG. 2 is a schematic view of the temperature field distribution of the base and the filament in the embodiment of the present invention.
Fig. 3 is a schematic of the diffraction peaks of the non-diamond component at position 1 in an example of the invention.
Fig. 4 is a schematic of the diffraction peak of the non-diamond component at position 2 in an example of the present invention.
Fig. 5 is a schematic of the diffraction peak at position 3 of the non-diamond component of the example of the present invention.
Fig. 6 is a schematic of a diffraction peak at position 4 of a non-diamond component in an example of the present invention.
Fig. 7 is a microstructure of a position 1 diamond in accordance with an example of the present invention.
Fig. 8 is a plot of the position 2 diamond microtopography in accordance with an example of the present invention.
Fig. 9 is a position 3 diamond micro-topography map according to an embodiment of the present invention.
Fig. 10 is a location 4 diamond micro-topography map according to an example of the invention.
FIG. 11 is a microstructure of diamond at point A at position 2 in accordance with an embodiment of the present invention.
FIG. 12 is a microstructure of diamond at point B at position 2 in accordance with an embodiment of the present invention.
FIG. 13 is a microstructure of diamond at point C at position 2 in accordance with an embodiment of the present invention.
FIG. 14 is a graph of the microstructure of diamond at point D at position 2 in accordance with an embodiment of the present invention.
FIG. 15 is a microstructure of diamond at point E at position 2 in accordance with an embodiment of the present invention.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is described below by way of specific embodiments.
Referring to fig. 1 and 2, a method for arranging filaments of a hot-filament CVD diamond device specifically includes the following steps:
step S1: preparing a plurality of N hot wires, arranging the hot wires at the upper end part of a substrate, arranging the substrate at the upper end part of a bottom plate, wherein the hot wire intervals Tw are different from the middle to the two sides, arranging an interval HY between the hot wires and the bottom plate, and arranging four positions on the substrate for carrying out a diamond coating deposition test;
step S2: carrying out pretreatment, namely acid-base corrosion treatment, on the substrate on the bottom plate;
step S3: putting the pretreated substrate into chemical vapor deposition equipment, putting the substrate well, and depositing a diamond coating;
step S4: and observing the microscopic morphology of the diamond at four different positions of the substrate, analyzing the purity and the grain orientation of the diamond, testing the bonding strength of the diamond coating and the substrate, and testing the microscopic morphology and the purity of the diamond at five different positions of the central substrate.
In step S1, the number of hot wires N is 10, Tw1＝14mm、Tw2＝10mm、Tw3＝10mm、Tw4＝8mm、Tw5＝8mm,HY＝8mm。
In step S2, the method specifically includes the following steps:
step S201: firstly, polishing the substrate for 3min by using P1500 abrasive paper, then continuously polishing the substrate for 3min by using P2000 abrasive paper, removing surface impurities and leaving scratches;
step S202: placing the polished substrate into an acid solution (formula V (H2SO 4): V (H2O 2): 1: 10) for treatment for 20s, and removing cobalt on the surface of the substrate;
step S203: ultrasonically treating with alkali solution (10gKOH +10gK3[ Fe (CN)6] +100ml H2O) at a formula of w (KOH): w (K3[ Fe (CN) 6): w (H2O): 1: 10 (mass ratio)) for 30min, and corroding WC particles on the surface of the substrate to expose cobalt on the surface layer;
step S204: and continuously performing ultrasonic treatment for 3min by using an acid solution to remove metal Co which has a certain depth and is used for promoting the graphitization of the diamond on the surface of the matrix.
Step S205: putting the substrate into mixed diamond micro powder acetone suspension, and carrying out ultrasonic grinding treatment for 30min to increase the defect density of the substrate surface, wherein the suspension is prepared by adding diamond micro powder with the granularity of M0.5/1, M2.5/5 and M5/10 into a proper amount of acetone solution according to the mass ratio of 1:1:1 and uniformly mixing.
The distance between the filaments is determined by the groove distance of the molybdenum plate used in the filament fixing device, and after the filaments which are arranged at equal intervals are electrified, the temperature distribution on the surface of the substrate on the sample table is uneven, and the uniformity of the temperature distribution on the surface of the substrate is usually ensured by rotating the sample table and the like. If mass industrial production is required, the number of the matrixes on the sample table is large, the requirement on the uniformity of the temperature distribution is higher, and the uniformity of diamond deposition is directly determined by the temperature distribution. The invention adopts filament arrangement with unequal intervals, thereby ensuring the uniformity of the temperature distribution on the surface of the substrate in the first step and reducing the difficulty of subsequent work.
The basic working principle of the invention is as follows: since the only energy source of the hot filament CVD diamond apparatus is the filament, the temperature is high at a position closer to the filament, and is low otherwise. When the filaments are arranged at equal intervals, the temperature right below the filaments is highest, the temperature at the edge part is lower, the temperature distribution is seriously uneven, the interval of the middle filaments is properly enlarged, the interval of the edge filaments is reduced, and a more uniform temperature field can be obtained.
The method is realized by utilizing chemical vapor deposition equipment to perform diamond layer deposition and obtain a diamond film, belongs to the prior art and is not detailed herein.
For further illustration, referring to fig. 2, the technical effect brought by the arrangement method of the filament in the present invention patent can be seen that the temperature fields at four positions on the substrate are uniformly distributed;
referring to fig. 3-6, no graphite peak appears in the diamond coating of the substrate at four different positions, the characteristic peaks of diamond are obvious and sharp, the diamond has high purity and good crystal orientation, the three characteristic peaks of diamond appear simultaneously, the diffraction intensities of the (111) and (220) crystal planes are high, and the diffraction intensity of the (311) crystal plane is lower, which indicates that the diamond crystal grains mainly present the (111) and (220) crystal planes. The diffraction intensities of the (111) and (220) crystal planes in the four-site base diamond coating are highest at position 2, next to position 1 and position 3, and finally position 4, but the difference is not great because the grains at position 1 and position 2 are slightly coarse and the grain orientation is good, but the difference is not great overall, and the crystal forms of the four samples are good, so the diffraction peaks are all strong.
Referring to fig. 7-10, SEM images of the topography of the diamond coating on the substrate surface at 4 different locations are shown. It can be seen that the shapes of diamonds in the coatings of 4 substrates at different positions are basically the same, diamond grains are clear, crystal edges are obvious and have obvious orientations, crystal faces (111) and (220) are mainly presented, the crystal grains are aggregated and connected with each other to form a polycrystalline, the size of the crystal grains is large, the crystal grains are densely stacked, no holes or isolated crystal grains are generated, the quality of the coatings is good, and the surface roughness is large. On the whole, the diamond grain sizes of the position 1 and the position 2 on the substrate are slightly larger than the grain sizes of the diamond coatings on the surfaces of the position 3 and the position 4 substrates, and the diamond grain accumulation densities of the position 1 sample and the position 2 sample are lower than those of the position 3 and the position 4, which shows that the temperature of the surface of the middle substrate is slightly higher than that of the substrates on the two sides, and the gas flow rate is slightly lower than that of the substrates on the two sides. And the shape of the crystal grains of the diamond on the surface of the substrate is not greatly different when the diamond is singly compared with the shape of the diamond on the surface of the substrate parallel to the direction of the hot wire.
Referring to fig. 11-15, scanning electron micrographs of the five points are selected to observe the surface topography of the diamond at different positions on the substrate at position 2. The 5 points on the substrate at position 2, namely the four points of the tool and the center of the tool, were selected and named A, B, C, D, E in turn.
From the SEM images of the diamond surface topography at 5 different observation points, it can be seen that the diamond topography is substantially the same at four angular positions A, B, C, D of the tool, and the diamond particles are of comparable size, but the diamond particles coated at the E position in the middle of the substrate are slightly smaller in size than at several other positions, and the particle packing density is slightly greater than at four other positions. According to the distribution of the temperature field and the airflow field, under the experimental condition, because of the hot wire effect, the four corners are positioned below the hot wires, the temperature of the edge of the middle substrate is slightly higher than that of the central area, the airflow velocity is slightly lower at the central position of the surface of the substrate and is higher far away from the central position, and the combined action of the temperature field and the airflow field enables the diamond nucleation density at the central position to be high, the growth rate to be relatively low, the diamond nucleation density to be aggregated into clusters, the grain size to be small, and the grain stacking density to be relatively high. On the whole, the diamond has good uniformity and high density. In practical application, the cutting edges of the diamond coated cutter which have the cutting function are positioned at four corners of the cutter, so that the growth uniformity of diamonds at the cutting edges and the bonding strength of the coating and a substrate have obvious influence on the service performance and stability of the cutter, and therefore, the service performance of the coated cutter is better under the deposition condition. The whole growth of the diamond is relatively uniform, and the actual deposition experiment result is identical with the simulation result.
The specific working process of the invention is as follows:
the detailed operation flow is described in detail before, and is not described in detail here.
The technical features of the present invention which are not described in the above embodiments may be implemented by or using the prior art, and are not described herein again, of course, the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and variations, modifications, additions or substitutions which may be made by those skilled in the art within the spirit and scope of the present invention should also fall within the protection scope of the present invention.
Claims (3)
1. A method for arranging filaments of hot filament CVD diamond equipment is characterized by comprising the following steps:
step S1: preparing a plurality of N hot wires, arranging the hot wires at the upper end part of a substrate, arranging the substrate at the upper end part of a bottom plate, wherein the hot wire intervals Tw are different from the middle to the two sides, arranging an interval HY between the hot wires and the bottom plate, and arranging four positions on the substrate for carrying out a diamond coating deposition test;
step S2: carrying out pretreatment, namely acid-base corrosion treatment, on the substrate on the bottom plate;
step S3: putting the pretreated substrate into chemical vapor deposition equipment, putting the substrate well, and depositing a diamond coating;
step S4: and observing the microscopic morphology of the diamond at four different positions of the substrate, analyzing the purity and the grain orientation of the diamond, testing the bonding strength of the diamond coating and the substrate, and testing the microscopic morphology and the purity of the diamond at five different positions of the central substrate.
2. The method of claim 1, wherein in step S1, the number of filaments N-10, T is 10w1＝14mm、Tw2＝10mm、Tw3＝10mm、Tw4＝8mm、Tw5＝8mm,HY＝8mm。
3. The method for arranging filaments of a hot wire CVD diamond apparatus according to claim 2, wherein the step S2 specifically comprises the following steps:
step S201: firstly, polishing the substrate for 3min by using P1500 abrasive paper, then continuously polishing the substrate for 3min by using P2000 abrasive paper, removing surface impurities and leaving scratches;
step S202: placing the polished substrate into an acid solution (formula V (H2SO 4): V (H2O 2): 1: 10) for treatment for 20s, and removing cobalt on the surface of the substrate;
step S203: ultrasonically treating with alkali solution (Murakami solution, formula of w (KOH): w (K3[ Fe (CN) 6): w (H2O): 1: 10 (mass ratio)) for 30min to corrode WC particles on the surface of the substrate and expose cobalt on the surface layer;
step S204: and continuously performing ultrasonic treatment for 3min by using an acid solution to remove metal Co which has a certain depth and is used for promoting the graphitization of the diamond on the surface of the matrix.
Step S205: putting the substrate into mixed diamond micro powder acetone suspension, and carrying out ultrasonic grinding treatment for 30min to increase the defect density of the substrate surface, wherein the suspension is prepared by adding diamond micro powder with the granularity of M0.5/1, M2.5/5 and M5/10 into a proper amount of acetone solution according to the mass ratio of 1:1:1 and uniformly mixing.
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Cited By (2)
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| CN116121728A (en) * | 2023-01-30 | 2023-05-16 | 江苏开放大学（江苏城市职业学院） | Method for preparing novel diamond composite thick film cutter |
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2020
- 2020-07-20 CN CN202010700039.XA patent/CN111945130A/en active Pending
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| CN113026001A (en) * | 2021-05-26 | 2021-06-25 | 苏州香榭轩表面工程技术咨询有限公司 | Method for preparing diamond by metastable state control |
| CN113026001B (en) * | 2021-05-26 | 2021-08-17 | 苏州香榭轩表面工程技术咨询有限公司 | Method for preparing diamond by metastable state control |
| CN113026001B8 (en) * | 2021-05-26 | 2021-09-14 | 上海征世科技股份有限公司 | Method for preparing diamond by metastable state control |
| CN116121728A (en) * | 2023-01-30 | 2023-05-16 | 江苏开放大学（江苏城市职业学院） | Method for preparing novel diamond composite thick film cutter |
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