CN119465396B - Growth method for heterogeneous growth of large-size polycrystalline diamond - Google Patents
Growth method for heterogeneous growth of large-size polycrystalline diamond Download PDFInfo
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- CN119465396B CN119465396B CN202510042150.7A CN202510042150A CN119465396B CN 119465396 B CN119465396 B CN 119465396B CN 202510042150 A CN202510042150 A CN 202510042150A CN 119465396 B CN119465396 B CN 119465396B
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 95
- 239000010432 diamond Substances 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 28
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 60
- 239000011733 molybdenum Substances 0.000 claims abstract description 60
- 239000000758 substrate Substances 0.000 claims abstract description 54
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 51
- 239000010935 stainless steel Substances 0.000 claims abstract description 51
- 238000000151 deposition Methods 0.000 claims abstract description 28
- 230000008021 deposition Effects 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 238000010583 slow cooling Methods 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 claims 20
- 238000002360 preparation method Methods 0.000 claims 1
- 230000002829 reductive effect Effects 0.000 abstract description 15
- 239000013078 crystal Substances 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 11
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 7
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 2
- 210000002381 plasma Anatomy 0.000 description 10
- 238000009966 trimming Methods 0.000 description 6
- 239000003570 air Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 2
- 239000012080 ambient air Substances 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a growth method of heterogeneous growth large-size polycrystalline diamond, which relates to the technical field of chemical vapor deposition, wherein a detachable substrate combination consisting of a molybdenum carrier disc and a stainless steel ring can be detached and cleaned conveniently, the substrate combination can be recycled and reused with high efficiency, the surface energy of the stainless steel ring is larger than that of diamond deposition materials, so that carbon atoms cannot be stably attached, the temperature field in a preset diamond deposition target area is more uniform, the defect that a microwave system is applied to the growth process of the polycrystalline diamond is overcome, the defect that the stainless steel ring and a diamond lattice are larger in phase difference, a continuous and uniform crystal structure cannot be formed on the stainless steel ring, the situation that the polycrystalline diamond grows on the side edge of the molybdenum carrier disc, and a wafer cannot be separated or the wafer is broken in the separation process is avoided, and the possibility that the polycrystalline diamond grown on the molybdenum carrier disc is broken in the extraction stage is reduced.
Description
Technical Field
The invention relates to the technical field of chemical vapor deposition, in particular to a method for growing large-size polycrystalline diamond in a heterogeneous manner.
Background
The microwave plasma chemical vapor deposition technology is one of the accepted ideal means for preparing large-size high-quality single crystal diamond, and is mainly characterized in that after microwaves are resonated through a specially designed resonant cavity, a concentrated electric field is formed in an area above a sample stage, raw material gases such as hydrogen, methane and the like are dissociated to form atomic hydrogen and a series of carbon-containing precursor plasmas, and then diamond is deposited on the surface of a seed crystal cooled to a certain temperature:
For example, the application of the prior patent application number 202410702675.4 provides an MPCVD (multi-point chemical vapor deposition) device of a substrate table system, which comprises a microwave reflection table and a large molybdenum table which are arranged in a stacked manner, wherein the substrate table is arranged on one side of the large molybdenum table away from the microwave reflection table, an annular bulge is arranged on one side of the large molybdenum table away from the microwave reflection table, and the annular bulge is coaxial with the substrate table and surrounds the periphery of the substrate table.
Taking the MPCVD equipment of the substrate table system as an example, the substrate table is a main supporting structure for diamond growth, but gap pits exist on the supporting structure around the substrate table, diamond and derivatives can be deposited in the gap pits in the diamond growth process, the subsequent equipment cleaning is troublesome, the common substrate table is made of monocrystalline silicon wafer materials, the detachment of a diamond sheet is realized by dissolving the substrate table by strong acid, the material loss is large, and the pollution is serious.
Disclosure of Invention
The invention aims to provide a growth method for heterogenously growing large-size polycrystalline diamond, which aims to solve the problems in the prior art.
In order to achieve the above purpose, the invention provides a method for growing heterogenous-growth large-size polycrystalline diamond, which comprises the following steps:
step one, ultrasonic cleaning of a substrate combination;
step two, purging and drying the substrate combination CDA;
step three, placing the substrate in an MPCVD water cooling table in a combined way;
fourthly, MPCVD equipment works;
Step five, introducing deposition gas;
Step six, growing and depositing for a plurality of time periods;
Step seven, cooling and furnace withdrawal;
step eight, separating the polycrystalline diamond sheet;
the substrate combination comprises a molybdenum carrying disc and a stainless steel ring sleeved on the outer side of the molybdenum carrying disc.
Preferably, the method comprises the following steps of placing the molybdenum carrying disc and the stainless steel ring into deionized water for ultrasonic cleaning for 30 minutes, and cleaning foreign matters and dirt on the molybdenum carrying disc and the stainless steel ring so as to prevent impurities on the substrate combination from affecting the crystal quality.
Preferably, the second step is to put the molybdenum carrying disc and the stainless steel ring into CDA environment for blowing and drying to remove surface moisture.
Preferably, the third step is that a molybdenum carrying disc is placed in a stainless steel ring to complete the assembly of the substrate combination, and the substrate combination is placed on an MPCVD carrying water cooling table.
Preferably, the fourth step is specifically as follows:
closing the MPCVD cavity, and pumping air in the MPCVD cavity for 30 minutes by using a mechanical pump to ensure that the vacuum degree in the MPCVD cavity is below 0.001 Torr;
igniting, namely introducing 300-500sccm hydrogen to maintain the cavity pressure in the MPCVD cavity at about 6Torr, starting a microwave power supply, preheating a power supply filament, starting microwaves after the preheating is finished, and setting the microwave power to be 1000W;
Heating, namely adjusting the internal pressure and microwave power of the MPCVD cavity to enable the temperature in the MPCVD cavity to reach 600-800 ℃ to finish heating;
And various parameters in the MPCVD cavity are adjusted to avoid the reaction between gases when the deposition gases are injected subsequently.
Preferably, the fifth step is specifically as follows:
Injecting gas, namely introducing 10-50sccm of methane into the MPCVD cavity, introducing less than 0.5sccm of nitrogen into the MPCVD cavity, and introducing 0.2-1sccm of oxygen into the MPCVD cavity;
The deposition environment is controlled by trimming the cavity pressure in the MPCVD cavity to be 120-180Torr, trimming the microwave power to be 7000-9000W and trimming the temperature in the MPCVD cavity to be 700-900 ℃;
Controlling MPCVD work to maintain the deposition environment achieved in the fifth step for a plurality of times according to the target thickness of the polycrystalline diamond, and slowly depositing and growing the polycrystalline diamond on the substrate combination.
Preferably, the step seven is specifically as follows:
stopping the gas injection, namely stopping the supply of methane, nitrogen and oxygen;
The slow cooling is carried out, namely the cooling, pressure relief and microwave power reduction time is set to be 300 minutes, the slow cooling is carried out, the cooling period of the diamond sheet is prolonged, the material reaction of thermal expansion and cold contraction is reduced, and the occurrence of cracks of the diamond sheet can be effectively reduced;
And (3) annealing, namely when the cavity pressure in the MPCVD cavity reaches 3Torr, the microwave power reaches 1000W, and the wafer temperature is 60-90 ℃, turning off the microwave power supply.
Preferably, the step eight is specifically as follows:
Cooling, namely closing hydrogen, and waiting for the wafer to cool for 15 minutes;
Exhausting, namely opening a mechanical pump, and pumping out residual reaction gas in the cavity to enable the cavity pressure in the MPCVD cavity to reach 0.01Torr;
The air pressure control is that nitrogen is injected into the MPCVD cavity, the inside of the MPCVD cavity is separated from the vacuum environment, and the nitrogen is injected after the crystal diamond is formed, so that the possibility of chemical reaction of the crystal diamond sheet is reduced, the cavity pressure in the MPCVD cavity reaches the atmospheric pressure, the stress of the crystal diamond sheet caused by the pressure difference between the inside and the outside of the MPCVD cavity is avoided, and the possibility of crack occurrence of the crystal diamond sheet is reduced;
And taking out the substrate combination, and taking out the polycrystalline diamond.
Compared with the prior art, the invention has the beneficial effects that:
1. The substrate combination consists of a molybdenum carrying disc and a stainless steel ring at the outer side of the molybdenum carrying disc, the detachable substrate combination consisting of the molybdenum carrying disc and the stainless steel ring can be detached, the molybdenum carrying disc and the stainless steel ring are placed into deionized water for ultrasonic cleaning for 30 minutes, dirt on the molybdenum carrying disc and the stainless steel ring is subjected to direct and indirect effects, so that a fine dirt layer is dispersed, emulsified and stripped to comprehensively and thoroughly clean the molybdenum carrying disc and the stainless steel ring, and the substrate combination can be recycled with high efficiency;
2. According to the application, due to the fact that edge discharge phenomenon exists in the microwave system application, the stainless steel ring guides a secondary plasma field to the stainless steel, and the diamond deposition needs to have proper surface energy on the molybdenum carrying disc, carbon atoms can be adsorbed, decomposed and deposited, the surface energy of the stainless steel ring is greatly different from diamond deposition materials, so that carbon atoms cannot be stably attached, the temperature field in a preset diamond deposition target area is more uniform, the defect of the microwave system applied in the polycrystalline diamond growth process is overcome, and the quality of polycrystalline diamond generated by utilizing a microwave plasma chemical vapor deposition technology is improved;
3. According to the application, the stainless steel ring and the diamond lattice match have larger phase difference, a continuous and uniform crystal structure cannot be formed on the stainless steel ring, the situation that polycrystalline diamond grows on the side edge of the molybdenum carrying disc, and the wafer cannot be separated or the wafer is broken in the separation process is avoided, the possibility that the polycrystalline diamond growing on the molybdenum carrying disc is broken in the extraction stage is reduced, the stainless steel ring is used as a traction ring in the MPCVD polycrystalline deposition process, a graphite-like amorphous carbon substance is formed on the surface of the stainless steel ring, the substance cannot adhere to the target polycrystalline diamond, the parameters such as the ambient air pressure, the temperature and the electric field of the polycrystalline diamond are slowly changed in the substrate combination cooling and annealing process, the situation that the polycrystalline diamond cracks due to the material thermal stress change caused by rapid cooling is avoided, the situation that the polycrystalline diamond cracks formed on the molybdenum carrying disc occur is reduced, the crack of the polycrystalline diamond chip is effectively reduced, and the problem of cracking caused by the side wall adhesion in the diamond growth and separation process is solved.
Drawings
FIG. 1 is a schematic diagram of a growth method according to the present invention.
Fig. 2 is a schematic structural diagram of a substrate assembly according to the present invention.
Fig. 3 is a schematic partial structure of the molybdenum carrier disk of the present invention.
In the figure, the reference numeral is 1, molybdenum carrying disk, 2, stainless steel ring.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment as shown in fig. 1-3, the present invention provides a technical scheme of a method for heterogeneous growth of large-size polycrystalline diamond, comprising the following steps:
step one, ultrasonic cleaning of a substrate combination;
step two, purging and drying the substrate combination CDA;
step three, placing the substrate in an MPCVD water cooling table in a combined way;
fourthly, MPCVD equipment works;
Step five, introducing deposition gas;
Step six, growing and depositing for a plurality of time periods;
Step seven, cooling and furnace withdrawal;
step eight, separating the polycrystalline diamond sheet;
the substrate combination comprises a molybdenum carrying disc 1 and a stainless steel ring 2 sleeved on the outer side of the molybdenum carrying disc 1.
The specific steps in the growth method of the polycrystalline diamond by using the substrate combination are as follows:
The method comprises the steps of firstly, ultrasonically cleaning a substrate combination, namely, placing a molybdenum carrying disc 1 and a stainless steel ring 2 into deionized water for 30 minutes, and directly and indirectly acting on dirt on the molybdenum carrying disc 1 and the stainless steel ring 2 by utilizing cavitation, acceleration and direct flow action of ultrasonic waves in liquid, so that a fine dirt layer is dispersed, emulsified and stripped to comprehensively and thoroughly clean the molybdenum carrying disc 1 and the stainless steel ring 2, and foreign matters and dirt on the substrate combination consisting of the molybdenum carrying disc 1 and the stainless steel ring 2 are removed, thereby avoiding that the crystal quality is affected by the existence of fine dirt on the substrate combination for precipitating and growing polycrystalline diamond.
And step two, the substrate combination is subjected to CDA purging and drying, the molybdenum carrying disc 1 and the stainless steel ring 2 are placed into a CDA environment to be purged and dried, surface moisture is removed, the molybdenum carrying disc 1 and the stainless steel ring 2 are dried by using CDA gas of which main components are nitrogen, oxygen and a small amount of rare gas, the conditions of gas adhesion and static electricity generation on the substrate combination formed by the molybdenum carrying disc 1 and the stainless steel ring 2 are reduced, the stability of the chemical structure of the surface layer of the substrate combination is ensured, and the stability of the combination of polycrystalline diamond and the substrate combination is improved.
Placing the substrate combination on an MPCVD water cooling table, firstly placing the molybdenum carrying disc 1 into the stainless steel ring 2, then placing the substrate combination on the MPCVD water cooling table, and thoroughly cleaning the detachable substrate combination consisting of the molybdenum carrying disc 1 and the stainless steel ring 2 after being detached, so that the substrate combination can be recycled with high efficiency.
Step four, MPCVD equipment works:
Firstly, performing preliminary work, closing an MPCVD cavity, enabling the MPCVD cavity to enter a state of being separated from the outside, pumping air in the MPCVD cavity for 30 minutes by using a mechanical pump, simulating a vacuum state in the MPCVD cavity, avoiding influence of suspended matters and partial gases contained in air on the growth process of polycrystalline diamond, ensuring the quality of the polycrystalline diamond, and controlling the mechanical pump to stop working until the vacuum degree in the MPCVD cavity is lower than 0.001 Torr;
Then ignition is carried out, namely 300-500sccm hydrogen is introduced into the MPCVD cavity, after the cavity pressure in the MPCVD cavity is maintained to be about 6Torr, a microwave power supply is started, a power supply filament is preheated, microwaves are started after the preheating is completed, and the microwave power is set to be 1000W;
Finally, heating is carried out, the internal pressure and microwave power of the MPCVD cavity are regulated, after the temperature in the MPCVD cavity reaches 600-800 ℃, the heating is finished, and a thermal expansion gap exists between the molybdenum carrying disc 1 and the stainless steel ring 2, so that the molybdenum carrying disc 1 and the stainless steel ring 2 are convenient to assemble and disassemble, and in the step, the molybdenum carrying disc 1 is expanded and tightly attached to the stainless steel ring 2, and the gap between the molybdenum carrying disc 1 and the stainless steel ring 2 is removed.
Step five, introducing a deposition gas,
Firstly, injecting gas, namely 10-50sccm of methane is introduced into an MPCVD cavity, nitrogen is introduced into the MPCVD cavity, the injection amount of the nitrogen is controlled below 0.5sccm, and 0.2-1sccm of oxygen is introduced into the MPCVD cavity, so that the polycrystalline diamond raw material supplying work is completed;
and then performing deposition environment control work, namely trimming cavity pressure in the MPCVD cavity to maintain the cavity pressure at 120-180Torr, trimming microwave power to maintain the cavity pressure at 7000-9000W, trimming the temperature in the MPCVD cavity to maintain the cavity pressure at 700-900 ℃, and eliminating the change of the polycrystalline diamond growth environment parameters caused by injecting methane, nitrogen and oxygen into the MPCVD cavity to ensure the growth quality of the polycrystalline diamond.
Step six, growing and depositing for a plurality of time periods, controlling MPCVD work to maintain the deposition environment achieved in the step five for a plurality of time periods according to the preset target thickness of the polycrystalline diamond finished product, in the process, forming a strong electric field area above the substrate combination by microwaves with specific power, dissociating hydrogen gas and methane gas to form atomic hydrogen and a series of carbon-containing precursor plasmas, depositing the plasmas on the substrate combination with lower temperature to form a diamond growth phenomenon, and slowly depositing and growing polycrystalline diamond on the substrate combination along with the time;
The substrate combination is composed of the molybdenum carrying disc 1 and the stainless steel ring 2 outside the molybdenum carrying disc 1, because the edge discharge phenomenon exists in the application of the microwave system, if no stainless steel ring 2 is arranged, a secondary plasma field is generated at the edge of the molybdenum carrying disc 1, in this case, a growth product is raised at the most edge, and because of different temperatures and different thermal stresses, the growth product is easy to deform and break, which is also a main disadvantage of the application of the microwave plasma chemical vapor deposition technology, the stainless steel ring 2 guides the secondary plasma field to the stainless steel, and as the deposition of diamond needs to have proper surface energy on the molybdenum carrying disc 1, the adsorption, decomposition and deposition of carbon atoms can be facilitated, the surface energy of the stainless steel ring 2 has larger phase difference with diamond deposition materials, so that the carbon atoms cannot be stably attached, the temperature field in a preset diamond deposition target area is more uniform, the defect of the microwave system applied in the diamond growth process is overcome, and the quality of polycrystalline diamond generated by the microwave plasma chemical vapor deposition technology is improved;
the stainless steel ring 2 and the diamond have larger lattice matching phase difference, a continuous and uniform crystal structure cannot be formed on the stainless steel ring 2, the situation that the polycrystalline diamond grows on the side edge of the molybdenum carrying disc 1, and the wafer cannot be separated or the wafer is broken in the separation process is avoided, and the possibility that the polycrystalline diamond grown on the molybdenum carrying disc 1 is broken in the taking-out stage is reduced;
The surface of the stainless steel ring 2 is easy to form an oxide layer, the oxide layer plays a role of a diaphragm to prevent carbon atoms and the surface of the stainless steel ring 2 from depositing, and the possibility of product growth on the outer side of the molybdenum carrier disc 1 is extremely low;
in conclusion, when the stainless steel ring 2 is used as a traction ring in the MPCVD polycrystalline deposition process, graphite-like amorphous carbon substances are formed on the surface of the stainless steel ring 2 and cannot adhere to target polycrystalline diamond, so that the problem of cracking caused by sidewall adhesion in the diamond growth and detachment process is solved.
Step seven, cooling and furnace withdrawal, namely firstly, gas injection is carried out to stop working, and the supply of methane, nitrogen and oxygen is closed successively;
Setting the cooling, pressure relief and microwave power reduction time to be 300 minutes, so that the parameters such as the ambient air pressure, the temperature, the electric field and the like of the polycrystalline diamond are slowly changed, the situation that the polycrystalline diamond is cracked due to the change of the thermal stress of the material caused by rapid cooling is avoided, the situation that the polycrystalline diamond chip formed on the molybdenum carrying disc 1 is cracked is reduced, and the occurrence of cracks of the diamond chip can be effectively reduced;
As the molybdenum carrying disc 1 is used as a growth platform of polycrystalline diamond, and the main constituent materials of the molybdenum carrying disc 1, namely molybdenum and diamond have certain difference in thermal expansion coefficients, the difference in shrinkage degree of the surface of the molybdenum carrying disc 1 and diamond slowly occurs along with the slow reduction of the temperature in an MPCVD cavity, the stress difference is generated at the interface between the molybdenum carrying disc 1 and a polycrystalline diamond sheet, the stress difference can lead to weakening of the bonding force between the molybdenum carrying disc 1 and the polycrystalline diamond sheet, finally the polycrystalline diamond sheet is separated from the molybdenum carrying disc 1, the later process is not needed to finish the separation of the molybdenum carrying disc 1 and the polycrystalline diamond sheet, the processing period of polycrystalline diamond can be shortened, the time cost and the material cost are reduced, and the environmental pollution caused by the processing of the polycrystalline diamond is reduced by the application of chemical materials.
And then carrying out furnace withdrawal operation, and when the cavity pressure in the MPCVD cavity reaches 3Torr, the microwave power reaches 1000W and the wafer temperature is 60-90 degrees, turning off the microwave power supply.
Step eight, separating the polycrystalline diamond sheet:
Firstly, cooling, closing hydrogen, and waiting for cooling the wafer for 15 minutes;
Then, exhausting, opening a mechanical pump, and pumping out residual reaction gas in the cavity, so that the cavity pressure in the MPCVD cavity reaches 0.01Torr;
Then, performing air pressure control, namely injecting nitrogen into the MPCVD cavity, separating the MPCVD cavity from a vacuum environment, enabling the cavity pressure in the MPCVD cavity to reach atmospheric pressure, and injecting nitrogen after the crystal diamond is formed, so that the possibility of chemical reaction of the crystal diamond sheet is reduced;
And finally, withdrawing the substrate combination, taking out the polycrystalline diamond, and cleaning the substrate combination.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
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| CN101220464A (en) * | 2008-01-25 | 2008-07-16 | 南京航空航天大学 | High thermal resistance hollow substrate workbench capable of depositing CVD diamond film on multiple surfaces and its application |
| CN114561698A (en) * | 2022-03-02 | 2022-05-31 | 河南天璇半导体科技有限责任公司 | Method for batch production of diamond single crystals by MPCVD (multi-phase chemical vapor deposition) method and molybdenum substrate table |
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| US7060130B2 (en) * | 2002-08-27 | 2006-06-13 | Board Of Trustees Of Michigan State University | Heteroepitaxial diamond and diamond nuclei precursors |
| JP2007261846A (en) * | 2006-03-28 | 2007-10-11 | Ｓｕｍｃｏ Ｔｅｃｈｘｉｖ株式会社 | Method for manufacturing defect-free silicon single crystal |
| CN115558902A (en) * | 2022-10-26 | 2023-01-03 | 武汉莱格晶钻科技有限公司 | Substrate table suitable for diamond growth and use method thereof |
| CN221501303U (en) * | 2023-12-28 | 2024-08-09 | 济南金刚石科技有限公司 | Novel MPCVD (multi-point chemical vapor deposition) growth device applied to preparation of large-size-grade polycrystalline diamond |
| CN118668191A (en) * | 2024-05-31 | 2024-09-20 | 北京北方华创微电子装备有限公司 | Substrate table system and MPCVD equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101220464A (en) * | 2008-01-25 | 2008-07-16 | 南京航空航天大学 | High thermal resistance hollow substrate workbench capable of depositing CVD diamond film on multiple surfaces and its application |
| CN114561698A (en) * | 2022-03-02 | 2022-05-31 | 河南天璇半导体科技有限责任公司 | Method for batch production of diamond single crystals by MPCVD (multi-phase chemical vapor deposition) method and molybdenum substrate table |
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