CN117733662B - Diamond polishing method based on plasma etching and modification effects - Google Patents
Diamond polishing method based on plasma etching and modification effects Download PDFInfo
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Abstract
The invention provides a diamond polishing method based on plasma etching and modification, which comprises the following steps: placing diamond to be polished above the rigid polishing disc through a clamp; the rigid polishing disk is provided with a plurality of through holes which are communicated up and down; controlling the diamond and the rigid polishing disk to rotate in opposite directions; heating the diamond by an atmospheric inductively coupled plasma comprising oxygen radicals and hydroxyl radicals; when the instant temperature is heated to exceed the critical transition temperature corresponding to the surface atomic differential etching, the atomic selective etching and modification effect are generated, and the polishing of the diamond is completed. According to the invention, the atmospheric inductively coupled plasma containing high-concentration high-activity oxygen free radicals and hydroxyl free radicals is used in the diamond polishing method, and the planarization treatment of the diamond surface is realized by combining the atomic selective etching removal and the hydroxyl modified polishing removal, so that the polishing efficiency of the diamond is improved, and meanwhile, the polishing device is simplified.
Description
Technical Field
The invention relates to the technical field of diamond polishing, in particular to a diamond polishing method based on plasma etching and modification.
Background
The special crystal structure and the strong carbon-carbon bond effect of the single crystal diamond enable the single crystal diamond to have extreme chemical inertness and excellent physical properties, and the single crystal diamond is a key basic material in the modern industry. The rapid development of the microwave plasma chemical vapor deposition technology also enables the mass production of large-size high-quality artificial diamond, breaks through the limit of the price, the number and the size of the traditional natural diamond, and enables the wide application of the diamond in the high and new technical fields of optics, heat and semiconductors and the like to be possible. In addition, the single-crystal diamond is also commonly applied to single-point diamond cutters of ultra-precise lathes and biological implantable devices by virtue of ultra-high hardness, chemical inertness and biocompatibility, and has extremely high application value.
The diamond surface with low damage, ultra-smooth and high precision characteristics is a precondition for realizing various excellent performances of the diamond, but as a typical difficult-to-process material, the extremely high hardness and extremely strong chemical stability of the diamond severely limit the planarization process of the diamond, and become one of key problems restricting the industrial application of wafer-level single crystal diamond.
Most of the existing diamond polishing methods adopt a capacitively coupled plasma source, so that hydroxyl active particles with higher concentration are difficult to generate, and the polishing efficiency is low; and the excitation mode of the capacitive coupling plasma needs to utilize a vacuum cavity to restrain the reaction gas, so that the processing equipment is complex and has high cost.
Disclosure of Invention
In view of the above, the invention provides a diamond polishing method based on plasma etching and modification, which comprises the following specific scheme:
a diamond polishing method based on plasma etching and modification, comprising:
placing diamond to be polished above the rigid polishing disc through a clamp; the rigid polishing disk is provided with a plurality of through holes which penetrate through the rigid polishing disk up and down;
controlling the diamond to rotate in a first direction through the clamp, and controlling the rigid polishing disk to rotate in a second direction; the first direction is opposite to the second direction;
ejecting an atmospheric inductively coupled plasma containing oxygen radicals and hydroxyl radicals over the rigid polishing disk, such that the atmospheric inductively coupled plasma heats the diamond through the through hole;
and when the instantaneous temperature is heated to exceed the critical transition temperature corresponding to the surface atomic differential etching, performing atomic selective etching on the diamond by oxygen free radicals in the atmosphere inductively coupled plasma, and simultaneously performing modification on the diamond by hydroxyl free radicals in the atmosphere inductively coupled plasma to finish polishing of the diamond.
In a specific embodiment, the method further comprises: and controlling the diamond to reciprocate at a preset speed along the radial direction of the rigid polishing disk through the clamp.
In a specific embodiment, the fixture includes a rotation control portion that controls the diamond to rotate in the first direction and a reciprocation control portion that controls the diamond to reciprocate at the preset speed in the radial direction of the rigid polishing disk.
In a specific embodiment, a plurality of through holes are uniformly formed above the rigid polishing disk; the through holes with the same distance from the center of the rigid polishing disk are communicated through a flow channel; and a plurality of through holes positioned in the same radial direction on the rigid polishing disk are communicated through radial grooves.
In one embodiment, the atmospheric inductively coupled plasma is ejected through the torch body;
the torch body comprises an inner torch tube and an outer torch tube;
the torch body ejects the atmospheric inductively coupled plasma through the outer torch tube and/or the inner torch tube;
when the atmosphere inductively coupled plasma is ejected, the mixed gas is introduced into the inner torch tube as an excitation gas to generate active free radicals, and argon is introduced into the outer torch tube as a cooling gas.
In one embodiment, the atmospheric inductively coupled plasma is obtained by vaporizing/volatilizing a mixture of a reactive liquid, oxygen and argon.
In a specific embodiment, controlling the flow of each of the gases used to generate the atmospheric inductively coupled plasma by a flow meter; different ones of the gases correspond to different ones of the flowmeters;
and controlling the mixed gas to generate the atmosphere inductively coupled plasma through a spark generator and a radio frequency coil.
In a specific embodiment, the method further comprises:
and controlling the reaction rate of the atomic selective etching by controlling the flow rate of the oxygen, wherein the higher the flow rate of the oxygen is, the faster the reaction rate of the atomic selective etching is.
In a specific embodiment, the time for the atmospheric inductively coupled plasma to irradiate the surface of the diamond sample through the through hole ranges from 8min to 12min.
In a specific embodiment, the critical transition temperature ranges from 1250 ℃ to 1300 ℃.
The beneficial effects are that:
according to the invention, a plasma source in the diamond polishing method based on plasma etching and modification is selected as the atmospheric inductively coupled plasma containing high-concentration high-activity oxygen free radicals and hydroxyl free radicals, and the planarization treatment on the diamond surface is realized by combining atomic selective etching removal and hydroxyl modified polishing removal, so that the polishing efficiency of the diamond is improved, the polishing device is simplified, the polishing cost is reduced, and the production efficiency is improved.
Drawings
FIG. 1 is a flow chart of a diamond polishing method based on plasma etching and modification in accordance with an embodiment of the present invention;
FIG. 2 is a schematic diagram of a diamond polishing method based on plasma etching and modification according to an embodiment of the present invention;
FIG. 3 is a schematic view of a polishing apparatus for diamond according to an embodiment of the present invention;
FIG. 4 is a graph showing oxygen flow rate versus instantaneous temperature and material removal rate for an embodiment of the present invention;
FIG. 5 is a schematic diagram of etching phenomena of different types of plasmas according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of a characteristic spectrum excited by different types of plasmas according to an embodiment of the present invention;
FIG. 7 is a graph showing the relationship between the instantaneous temperature of the diamond surface and the power of the RF power source and the surface roughness according to the embodiment of the present invention;
FIG. 8 is a schematic diagram of a characteristic spectrum excited by a plasma containing a reaction solution according to an embodiment of the present invention;
FIG. 9 is a schematic diagram showing the intensity of hydroxyl reactive particles at different RF power source powers for a plasma containing a reactive liquid according to an embodiment of the present invention.
Reference numerals: 1-a clamp; 2-diamond; 3-a rigid polishing disc; 4-through holes; 5-atmosphere inductively coupled plasma; 6-flow passage; 7-radial grooves; 8-a torch body; 81-an inner torch tube; 82-an outer torch tube; 9-a flow meter; 10-spark generator; 11-radio frequency coil.
Detailed Description
Hereinafter, various embodiments of the present disclosure will be more fully described. The present disclosure is capable of various embodiments and its modifications and variations are possible in light of the above teachings. However, it should be understood that: there is no intention to limit the various embodiments of the present disclosure to the specific embodiments disclosed herein, but rather the present disclosure is to be understood to cover all modifications, equivalents, and/or alternatives falling within the spirit and scope of the various embodiments of the present disclosure.
The terminology used in the various embodiments of the disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the various embodiments of the disclosure. As used herein, the singular is intended to include the plural as well, unless the context clearly indicates otherwise. Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which various embodiments of the present disclosure belong. The terms (such as those defined in commonly used dictionaries) will be interpreted as having a meaning that is identical to the meaning of the context in the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein in the various embodiments of the disclosure.
Example 1
According to the invention, a plasma source in the diamond polishing method based on plasma etching and modification is selected as the atmospheric inductively coupled plasma containing high-concentration high-activity oxygen free radicals and hydroxyl free radicals, and the planarization treatment on the diamond surface is realized by combining atomic selective etching removal and hydroxyl modified polishing removal, so that the polishing efficiency of the diamond is improved, the polishing device is simplified, the polishing cost is reduced, and the production efficiency is improved. The specific flow is shown in figure 1 of the specification. The specific scheme is as follows:
the method of polishing diamond based on plasma etching and modification according to this embodiment includes, as shown in fig. 1 to 3:
101. placing diamond 2 to be polished above a rigid polishing disc 3 by a clamp 1; the rigid polishing disk 3 is provided with a plurality of through holes 4 which penetrate up and down;
102. the diamond 2 is controlled to rotate in a first direction by the fixture 1, and the rigid polishing disk 3 is controlled to rotate in a second direction; the first direction is opposite to the second direction;
103. ejecting an atmospheric inductively coupled plasma 5 containing oxygen radicals and hydroxyl radicals above the rigid polishing disk 3 so that the atmospheric inductively coupled plasma 5 passes through the through hole 4 to heat the diamond 2;
104. when the instantaneous temperature is heated to exceed the critical transition temperature corresponding to the surface atomic differential etching, the atomic selective etching is carried out on the diamond 2 through oxygen free radicals in the atmosphere inductively coupled plasma 5, and simultaneously, the modification effect is carried out on the diamond 2 through hydroxyl free radicals in the atmosphere inductively coupled plasma 5, so that the polishing of the diamond 2 is completed.
The diamond polishing method of the present embodiment is applicable to various fields including, but not limited to, glass products, semiconductor manufacturing or high precision machining fields. The diamond polishing method of the present embodiment may be applied to a manufacturing process, for example, in a glass factory, a semiconductor production line, or a high-precision machine tool, in order to provide a higher quality and more accurate article.
101. Placing diamond 2 to be polished above a rigid polishing disc 3 by a clamp 1; the rigid polishing disk 3 is provided with a plurality of through holes 4 penetrating up and down.
The diamond polishing method mentioned in this embodiment is a high-efficiency and accurate processing technology, and can be widely applied to the manufacturing process of diamond products. In this diamond polishing method, the use of the jig 1 plays a key role, and it can stably fix the diamond 2 to be polished and ensure its correct position. By placing the diamond 2 over the rigid polishing disc 3, the subsequent polishing process can be made more convenient and accurate. The through holes 4 penetrating up and down are provided in the rigid polishing disk 3 for introducing the atmospheric inductively coupled plasma 5. The plasma 5 contains oxygen radicals and hydroxyl radicals, which penetrate through the rigid polishing disk 3 via the through holes 4, and heat the surface of the diamond 2 to realize the atomic selective etching and modification of the diamond 2.
102. The diamond 2 is controlled to rotate in a first direction by the fixture 1, and the rigid polishing disk 3 is controlled to rotate in a second direction; the first direction is opposite to the second direction.
The diamond 2 may be rotated in a first direction by control of the clamp 1. The jig 1 stably holds the diamond 2 and ensures that it maintains the correct position and angle during rotation. This rotation allows each area of the surface of the diamond 2 to be uniformly contacted with the polishing pad 3, thereby achieving an overall uniform polishing effect.
Meanwhile, during polishing, rotation is performed in the second direction by controlling the rigid polishing disk 3. This opposite direction of rotation, as opposed to the direction of rotation of the diamond 2, helps to create a mechanical shearing force to achieve uniform polishing of the diamond 2 surface. In this embodiment, the jig 1 controls the diamond 2 to rotate clockwise, and the rigid polishing disk 3 rotates counterclockwise. This opposite direction of rotation causes a lateral shear force to be created between the surface of the diamond 2 and the rigid polishing disk 3. Such transverse shear forces can remove surface irregularities and imperfections and improve surface flatness and finish.
The diamond 2 and the rigid polishing disk 3 are controlled to rotate in opposite directions by the fixture 1, so that defects and uneven parts on the surface of the diamond 2 can be removed more uniformly, and the surface of the diamond is smoother and smoother.
103. An atmospheric inductively coupled plasma 5 containing oxygen radicals and hydroxyl radicals is ejected above the rigid polishing disk 3 such that the atmospheric inductively coupled plasma 5 heats the diamond 2 through the through hole 4.
The atmospheric inductively coupled plasma 5 containing oxygen free radicals and hydroxyl free radicals penetrates through the through holes 4 on the rigid polishing disk 3 and contacts the surface of the diamond 2, and the diamond 2 is heated, so that the atomic selective etching and modification effects on the diamond 2 are realized.
During polishing, the atmospheric inductively coupled plasma 5 is ejected, and oxygen radicals therein generate different etching priorities, i.e., atomic selective etching, according to the number of carbon dangling bonds at different positions on the surface of the diamond 2. Atomic selective etching can eliminate the carbon atom differential formation bond state of the etched area of the diamond 2 surface, remove subsurface damage and an amorphous layer, and construct an atomic-level smooth surface (the roughness Sa is less than 0.5 nm).
Meanwhile, the high-activity hydroxyl radical is attached to the diamond 2 and the rigid polishing disk 3 and forms a bond with carbon atoms of the diamond 2 and specific atoms of the rigid polishing disk 3 to generate a modification effect, and then a hydroxyl dehydration condensation reaction CD-OH+M-OH- & gt CD-O-M+H2O (CD refers to carbon atoms of which the surface of the diamond is modified by hydroxyl groups and M refers to atoms of which the surface of the polishing disk is modified by hydroxyl groups) can be generated at the interface, so that a new bond CD-O-M is formed at the interface, and the surface C-CD of the diamond is broken under the action of mechanical shearing, thereby generating impurity removal of the surface of the diamond 2. Since the raised areas on the surface of the diamond 2 are more prone to capture hydroxyl radicals, and have a higher material removal rate, the surface planarity thereof will eventually approach that of the rigid polishing disk 3, thereby achieving global planarization (planarity less than 0.5 μm) of the diamond 2.
Through the polishing process of the above steps, the surface of the diamond 2 is sufficiently dressed and improved. This method not only removes surface defects and impurities, but also improves the overall quality and performance of the diamond 2. Therefore, the polishing method has important application value in the manufacturing process of diamond products.
104. When the instantaneous temperature is heated to exceed the critical transition temperature corresponding to the surface atomic differential etching, the atomic selective etching is carried out on the diamond 2 through oxygen free radicals in the atmosphere inductively coupled plasma 5, and simultaneously, the modification effect is carried out on the diamond 2 through hydroxyl free radicals in the atmosphere inductively coupled plasma 5, so that the polishing of the diamond 2 is completed.
When the diamond 2 is heated to a temperature exceeding the critical transition temperature corresponding to the differential etching of surface atoms, oxygen radicals and hydroxyl radicals released from the atmospheric inductively coupled plasma 5 start to act, completing the polishing of the diamond 2. In this embodiment, the critical transition temperature is 1270 ℃ (it should be noted that, the instantaneous temperature of the surface of the diamond 2 is measured by the infrared thermal imager, and the measurement result is related to the measurement distance, the position, the imaging focal length, the corrected sample emissivity and other factors, so that the critical transition temperature will be different under different experimental conditions, and the correction is specifically performed according to the experimental phenomena.
First, oxygen radicals produce an atomic selective etching action at the surface of the diamond 2. When the instantaneous temperature of the surface of the diamond 2 exceeds the critical transition temperature corresponding to the differential etching of surface atoms, oxygen free radicals can generate different etching priorities according to the different numbers of the dangling bonds of carbon atoms at different positions of the surface of the diamond, and the carbon atoms with more dangling bonds can be removed preferentially.
Meanwhile, the hydroxyl radical can also modify the surface of the diamond 2 during the heating process. The hydroxyl radical has certain chemical activity, can react with atoms on the surface of the diamond 2 and form chemical bonds. This chemical reaction changes the surface chemistry and structure of the diamond 2, resulting in better polishing performance and surface flatness.
Specifically, regarding the atomic selective etching mentioned in this example, an etching particle screening experiment was performed, as shown in fig. 4-7, using a radio frequency power supply of 1000W, respectively performing the etching particle screening experiment on pure argon plasma (18 slm argon cooling gas, 1.5 slm argon carrier gas), oxygen-containing plasma (18 slm argon cooling gas, 1.5 slm argon carrier gas, 20 seem oxygen reaction gas), fluorine-containing plasma (18 slm argon cooling gas, 1.5 slm argon carrier gas, 20 seem carbon tetrafluoride reaction gas), irradiation duration was 10min, and the instantaneous temperature after the diamond 2 surface was stabilized was collected and the surface morphology and roughness was detected in the process. In the etching particle screening experiment, three different plasmas can ensure that the stable instantaneous temperature of the diamond surface is above 1350 ℃, but only oxygen-containing plasmas can reduce the roughness of the diamond surface from the original submicron level to 0.502nm. The special oxygen free radical in the oxygen-containing plasma is a main reason for generating the selective etching of the atoms on the surface of the diamond, and other plasmas containing different free radicals can not generate the selective etching phenomenon of the atoms, so that the high-efficiency smoothness of the diamond can not be realized.
Further, in this embodiment, an atom selective etching experiment is performed by using oxygen-containing plasma (the gas flow is unchanged) to explore the critical transition temperature, the irradiation duration of the plasma is 10min, and the instantaneous temperature, the surface morphology and the roughness of the diamond 2 after the surface stabilization under different radio frequency power supply powers are collected in the process. In the experiment of atomic selective etching, with the increase of the power of the radio frequency power supply, the stable instantaneous temperature of the diamond 2 surface is increased from 965 ℃ to 1398 ℃, different etching phenomena are generated on the diamond 2 surface under different power conditions, and only when the power of the radio frequency power supply is increased to 900W and the temperature of the diamond surface reaches 1270 ℃, atomic selective etching reaction can be generated by oxygen plasma, so that the diamond surface is efficiently smoothed. When the instantaneous temperature is further increased, the surface roughness is still stabilized at about 0.5 and nm, which still corresponds to the atomic selective etching reaction, so that the critical switching temperature corresponding to the atomic differential etching of the diamond surface is defined as 1270 ℃.
Further, in this embodiment, a material removal experiment was performed under an oxygen-containing plasma with a radio frequency power of 1000W to explore factors affecting the material removal rate, and the plasma irradiation period was 10min, and the instantaneous temperature and the material removal rate after the diamond 2 surface was stabilized at different oxygen flow rates were collected during the process. In the material removal experiment, the stable instantaneous temperature change of the diamond surface is less than 30 ℃, and the influence of the temperature change on the material removal rate is negligible. When the oxygen flow rate is 0, the material removal rate is 0, and the material removal rate of the diamond surface linearly increases along with the increase of the oxygen flow rate, and the maximum material removal rate can reach 56.53 mu m/min in the experimental range. (it should be noted that, the result of the diamond material removal rate has a large correlation with the size of the sample used, so that the sample material removal rates of different sizes will be different, but always conform to the law that the material removal rate is approximately proportional to the oxygen flow rate.)
Therefore, high-activity oxygen free radicals generated by atmospheric inductively coupled plasma can induce the surface of the diamond 2 to generate atomic selective etching, so that the diamond 2 is polished efficiently and ultra-smoothly. It should be noted that, the selective etching of the surface atoms of diamond 2 requires that both conditions of high concentration oxygen radicals and critical conversion temperature be satisfied. In addition, the critical transition temperature may shift with the size of the processed diamond, the time of application, and the operating conditions (sample holder thermal conductivity, gas flow, processing environment) among other factors. In practical applications, careful selection of process parameters is necessary to meet different processing requirements, and the experimental results and the variation trend in fig. 4-7 can provide theoretical basis for process parameter selection.
Meanwhile, as shown in fig. 8 to 9, experiments for exploring the induction of hydroxyl active particles were conducted with respect to the modification effect mentioned in this example. The method comprises the steps of exploring a hydroxyl active particle induction experiment by adopting radio frequency power from 300 to 1000W and adopting reaction liquid (H2O 2) -containing plasma (18 slm argon cooling gas, 1.5 slm argon carrier gas and 20 seem reaction liquid-containing argon), and acquiring optical excitation spectrums of the plasma under different experimental conditions in the process to determine the strength of the hydroxyl active particles. In the hydroxyl active particle induction experiment, the strength of the hydroxyl active particles in the plasma is obviously enhanced along with the increase of the power of the radio frequency power supply, the enhancement amplitude is increased along with the increase of the power, the 900W radio frequency power supply power can already obtain the hydroxyl active particles with larger strength in the experimental interval range, and when the radio frequency power supply power reaches 1000W, the strength of the hydroxyl active particles in the plasma containing the reaction liquid is the largest. This suggests that highly reactive hydroxyl radicals can be simultaneously generated for hydroxyl modification under conditions that meet the atomic selectivity etch.
The excitation intensity measured by the hydroxyl active particles is closely related to the orientation and distance of the detection probe with respect to the plasma, and the induction of the active particles may be generated by ionization of substances that generate hydroxyl groups, including but not limited to hydrogen peroxide, water vapor, and the like.
In summary, through the atomic selective etching and modification of the diamond 2 by oxygen free radicals and hydroxyl free radicals in the atmospheric inductively coupled plasma 5, microscopic control of the surface of the diamond 2 can be achieved in the polishing process. This method can remove defects and unevenness of the surface of the diamond 2 while improving the quality and finish of the surface thereof. Finally, the polishing of the diamond 2 is completed to achieve the required accuracy and quality requirements.
In a specific embodiment, the method further comprises: the diamond to be polished 2 is controlled by the jig 1 to reciprocate at a preset speed in the radial direction of the rigid polishing disk 3.
In the present embodiment, in addition to the diamond 2 and the rigid polishing disk 3 rotating in opposite directions, it is also included to control the diamond 2 to be polished to reciprocate at a preset speed in the radial direction of the rigid polishing disk 3 by the jig 1. By controlling the movement of the diamond 2, a more uniform and comprehensive polishing effect can be achieved. The diamond 2 is in full contact with the rigid polishing disk 3 during the reciprocating motion, further promoting the etching and modifying effect. Meanwhile, the reciprocating motion can also prevent the diamond 2 from being locally overheated or overloaded in the polishing process, and the polishing stability and reliability are ensured.
Therefore, in the present embodiment, by controlling the reciprocating motion of the diamond 2 to be polished in the radial direction of the rigid polishing disk 3 at a preset speed by the jig 1, the polishing effect can be further improved, so that the surface of the diamond 2 is smoother, smoother and more accurate.
In one embodiment, the jig 1 includes a rotation control portion that controls the diamond 2 to rotate in a first direction, and a reciprocation control portion that controls the diamond 2 to reciprocate at a preset speed in a radial direction of the rigid polishing disk 3.
In this embodiment, the fixture 1 is composed of two parts, and the main task of the rotation control part is to control the rotation of the diamond 2 in the first direction, and the fixture 1 can adjust the rotation speed according to the requirement to meet the polishing requirements of different materials. By controlling the rotation direction of the diamond 2 against the rigid polishing disc 3, this helps to create a mechanical shearing force to achieve uniform polishing of the diamond 2 surface. The function of the reciprocation control section is to control the reciprocation of the diamond 2 in the radial direction of the rigid polishing disk 3, thereby achieving a uniform and high-quality polishing effect.
In a specific embodiment, a plurality of through holes 4 are uniformly formed above the rigid polishing disk 3; the through holes 4 with the same distance from the center of the rigid polishing disk 3 are communicated through a flow channel 6; the through holes 4 of the rigid polishing disk 3 located in the same radial direction are communicated through radial grooves 7.
In this embodiment, a plurality of through holes 4 are uniformly formed above the rigid polishing disk 3, and the through holes 4 are used for enabling the atmospheric inductively coupled plasma 5 containing oxygen free radicals and hydroxyl free radicals to penetrate through the through holes 4 on the rigid polishing disk 3, contact the surface of the diamond 2, and heat the diamond 2 so as to realize the selective etching and modification effects on atoms of the diamond 2.
Meanwhile, in order to better control the flow and distribution of the gas, through holes equidistantly arranged from the center point of the rigid polishing disk 3 are communicated through the flow channel 6, so that the gas can flow uniformly over the entire surface. Furthermore, radial grooves 7 are provided between the plurality of through holes 4 in the same radial direction on the surface of the rigid polishing disk 3 to further enhance the flow and distribution of the gas. These radial grooves 7 can direct gas from one through hole 4 to another through hole 4, thereby achieving a large gas flow and distribution over the surface of the rigid polishing disc 3.
By this arrangement, a uniform gas flow and distribution can be formed between the plurality of through holes 4 on the surface of the rigid polishing disk 3, thereby making the polishing process more stable and uniform. Meanwhile, the design can also reduce the surface temperature and friction heat, thereby avoiding damage to materials such as diamond 2 and the like.
In one embodiment, the atmospheric inductively coupled plasma 5 is ejected through the torch body 8;
the torch body 8 includes an inner torch tube 81 and an outer torch tube 82;
the torch body 8 ejects the atmospheric inductively coupled plasma 5 through the outer torch tube 82, and/or the inner torch tube 81;
when the atmospheric induction coupled plasma 5 is ejected, a mixed gas is introduced into the inner torch tube 81 as an excitation gas to generate active radicals, and argon gas is introduced into the outer torch tube 82 as a cooling gas.
In this embodiment, the atmospheric inductively coupled plasma 5 is ejected through the torch body 8. The torch body 8 is composed of an inner torch tube 81 and an outer torch tube 82. In this embodiment, the inner torch tube 81 and the outer torch tube 82 are simultaneously responsible for ejecting the atmospheric inductively coupled plasma 5, and active radicals are generated by introducing a mixture gas as an excitation gas into the inner torch tube 81, and argon gas is used as a cooling gas into the outer torch tube 82, so as to ensure that the ejected plasma 5 does not overheat.
Specifically, the inner torch tube 81 regulates the species of reactive species in the atmospheric inductively coupled plasma 5 by controlling the species of reactant gas introduced to meet the requirements of a particular application.
At the same time, argon gas is introduced as a cooling gas through the outer torch tube 82 during the ejection of the plasma 5. The argon can absorb the heat released by the plasma, and plays roles in cooling down and cooling down. This effectively prevents overheating of the plasma while protecting the torch body 8 from excessive temperatures. When the atmospheric induction coupled plasma 5 is discharged, argon gas is introduced into the outer torch tube 82 as a cooling gas, so that plasma stability and control can be ensured. The flow of cooling gas can carry away heat around the torch body 8, prevent problems caused by overheating, and extend the useful life of the torch body 8.
In one embodiment, the atmospheric inductively coupled plasma 5 is obtained by vaporizing/volatilizing a mixture of a reaction liquid, oxygen and argon.
In this embodiment, the atmospheric inductively coupled plasma 5 is obtained by evaporating/volatilizing a mixed gas of a reaction liquid, oxygen and argon. Wherein the reaction liquid evaporates/volatilizes gas and oxygen gas as the reaction gas, and argon gas serves as the carrier gas.
The reaction liquid is vaporized/volatilized to be a gas capable of generating hydroxyl groups under the excitation of plasma. The reaction solution may be converted into a gaseous reactant by heating the reaction solution and evaporating or volatilizing it into a gaseous state. The gaseous reactants may be mixed with other gases (e.g., oxygen) to form a mixed gas having a specified composition. Oxygen is then involved in the chemical reaction as a reactant gas. Oxygen is an essential oxidant in many chemical reactions and can promote the oxidation process of substances. It can react with chemical species in the evaporating/volatilizing gases of the reaction solution, initiating a series of oxidation reactions, thereby promoting the formation of the plasma 5.
Argon serves as carrier gas for diluting the reaction gas, adjusting the density and concentration of the plasma, and cooling to protect equipment. Argon is an inert gas which does not participate in chemical reactions, but can effectively dilute other gas components and control the concentration of plasma. At the same time, argon may also cool the reaction zone to prevent overheating and protect the equipment.
In one particular embodiment, the flow rates of the gases used to generate the atmospheric inductively coupled plasma 5 are controlled by a flow meter 9; different flow meters 9 are corresponding to different gases;
the mixed gas is controlled by a spark generator 10 and a radio frequency coil 11 to generate the atmospheric inductively coupled plasma 5.
In the present embodiment, the flow rates of the respective gases for generating the atmospheric inductively coupled plasma 5 are controlled by the flow meter 9. Different gases are associated with different flow meters 9 to ensure that the amount of each gas supplied is accurately controlled.
The flow meter 9 is an instrument for measuring the flow of gas, which can monitor the flow rate and volume of the gas by means of different sensors or mechanisms. By setting different types and parameters of flow meters 9, real-time monitoring and adjustment of different gas flows can be realized. In this way, it is ensured that the proportions and concentrations of the components in the mixed gas can meet the desired requirements, thereby generating a stable atmospheric inductively coupled plasma 5.
The mixed gas is controlled by the spark generator 10 and the radio frequency coil 11 to generate the atmospheric inductively coupled plasma 5. The spark generator 10 is a device for generating an electric spark, and excites the mixed gas into plasma by an electric discharge. The rf coil 11 further activates and maintains the steady state of the plasma by providing an rf electric field. The spark generator 10 and the radio frequency coil 11 are matched to realize the precise control of the plasma generated by the mixed gas. By adjusting the discharge parameters of the spark generator 10 and the operating frequency of the rf coil 11, the plasma density, temperature and stability can be adjusted to meet the needs of a particular application.
In a specific embodiment, the method further comprises:
the reaction rate of the atomic selective etching is controlled by controlling the flow rate of oxygen, and the higher the flow rate of oxygen is, the faster the reaction rate of the atomic selective etching is.
In this embodiment, as shown in fig. 4, the reaction rate of the atomic selective etching is controlled according to the flow rate of oxygen. When the oxygen flow rate is 0, the material removal rate is 0, and the material removal rate of the diamond surface linearly increases along with the increase of the oxygen flow rate, and the maximum material removal rate can reach 56.53 mu m/min in the experimental range. (it should be noted that, the result of the diamond material removal rate has a large correlation with the size of the sample used, so that the sample material removal rates of different sizes will be different, but always conform to the law that the material removal rate is approximately proportional to the oxygen flow rate.)
The higher the flow rate of oxygen, the higher the concentration of oxygen active free radicals in the atmospheric inductively coupled plasma 5, so that the higher the content of oxygen free radicals acting on the surface of the diamond 2, and the reaction rate of atomic selective etching is further accelerated. The method can provide more flexible and adjustable parameters so as to adapt to the requirements of different application scenes on the plasma properties. Meanwhile, the precise control of the diamond 2 polishing process can be realized by adjusting the flow rate of oxygen, so that the reaction efficiency and the product quality are optimized.
In one embodiment, the time for which the atmospheric inductively coupled plasma 5 irradiates the surface of the diamond 2 sample through the through hole 4 ranges from 8min to 12min.
In this embodiment, the time for the atmospheric inductively coupled plasma 5 to irradiate the surface of the diamond 2 sample through the through hole 4 is in the range of 8min to 12min. This time range is the experimentally derived optimal time period. In this time range, the atmospheric inductively coupled plasma 5 can sufficiently cover the surface of the diamond 2 sample and generate a sufficient chemical reaction, thereby realizing the polishing process of the diamond 2.
It should be noted that the irradiation time of the atmospheric inductively coupled plasma 5 is not only related to the properties of the sample and the purpose of the treatment, but also closely related to parameters such as the power and density of the plasma. Thus, in practice, fine tuning and control of the parameters of the plasma is required to ensure optimum plasma power and density over the desired process time.
In one particular embodiment, the critical transition temperature ranges from 1250 ℃ to 1300 ℃.
In this embodiment, the critical transition temperature is 1270 ℃ (it should be noted that, the instantaneous temperature of the surface of the diamond 2 is measured by the infrared thermal imager, and the measurement result is related to the measurement distance, the position, the imaging focal length, the corrected sample emissivity and other factors, so that the critical transition temperature will be different under different experimental conditions, and the correction is specifically performed according to the experimental phenomena.
According to the invention, a plasma source in the diamond polishing method based on plasma etching and modification is selected as the atmospheric inductively coupled plasma containing high-concentration high-activity oxygen free radicals and hydroxyl free radicals, and the planarization treatment on the diamond surface is realized by combining atomic selective etching removal and hydroxyl modified polishing removal, so that the polishing efficiency of the diamond is improved, the polishing device is simplified, the polishing cost is reduced, and the production efficiency is improved.
Those skilled in the art will appreciate that the drawing is merely a schematic illustration of a preferred implementation scenario and that the modules or flows in the drawing are not necessarily required to practice the invention. Those skilled in the art will appreciate that modules in an apparatus in an implementation scenario may be distributed in an apparatus in an implementation scenario according to an implementation scenario description, or that corresponding changes may be located in one or more apparatuses different from the implementation scenario.
Claims (10)
1. A diamond polishing method based on plasma etching and modification, comprising:
placing diamond to be polished above the rigid polishing disc through a clamp; the rigid polishing disk is provided with a plurality of through holes which penetrate through the rigid polishing disk up and down;
controlling the diamond to rotate in a first direction through the clamp, and controlling the rigid polishing disk to rotate in a second direction; the first direction is opposite to the second direction;
ejecting an atmospheric inductively coupled plasma containing oxygen radicals and hydroxyl radicals over the rigid polishing disk, such that the atmospheric inductively coupled plasma heats the diamond through the through hole;
and when the instantaneous temperature is heated to exceed the critical transition temperature corresponding to the surface atomic differential etching, performing atomic selective etching on the diamond by oxygen free radicals in the atmosphere inductively coupled plasma, and simultaneously performing modification on the diamond by hydroxyl free radicals in the atmosphere inductively coupled plasma to finish polishing of the diamond.
2. The method as recited in claim 1, further comprising: and controlling the diamond to reciprocate at a preset speed along the radial direction of the rigid polishing disk through the clamp.
3. The method of claim 2, wherein the jig includes a rotation control portion that controls the diamond to rotate in the first direction and a reciprocation control portion that controls the diamond to reciprocate at the preset speed in a radial direction of the rigid polishing disk.
4. The method according to claim 1, wherein a plurality of the through holes are uniformly provided above the rigid polishing disk; the through holes with the same distance from the center of the rigid polishing disk are communicated through a flow channel; and a plurality of through holes positioned in the same radial direction on the rigid polishing disk are communicated through radial grooves.
5. The method of claim 1, wherein the atmospheric inductively coupled plasma is ejected through the torch body;
the torch body comprises an inner torch tube and an outer torch tube;
the torch body ejects the atmospheric inductively coupled plasma through the outer torch tube and/or the inner torch tube;
when the atmosphere inductively coupled plasma is ejected, the mixed gas is introduced into the inner torch tube as an excitation gas to generate active free radicals, and argon is introduced into the outer torch tube as a cooling gas.
6. The method of claim 1 or 5, wherein the atmospheric inductively coupled plasma is obtained by evaporating/volatilizing a mixture of a reaction liquid, oxygen and argon.
7. The method of claim 6, wherein the flow rate of each of the gases used to generate the atmospheric inductively coupled plasma is controlled by a flow meter; different ones of the gases correspond to different ones of the flowmeters;
and controlling the mixed gas to generate the atmosphere inductively coupled plasma through a spark generator and a radio frequency coil.
8. The method as recited in claim 6, further comprising:
and controlling the reaction rate of the atomic selective etching by controlling the flow rate of the oxygen, wherein the higher the flow rate of the oxygen is, the faster the reaction rate of the atomic selective etching is.
9. The method of claim 1, wherein the atmospheric inductively coupled plasma is irradiated to the surface of the diamond through the through hole for a time ranging from 8min to 12min.
10. The method of claim 1, wherein the critical transition temperature ranges from 1250 ℃ to 1300 ℃.
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| CN111251133A (en) * | 2020-02-25 | 2020-06-09 | 中国地质大学（北京） | Diamond grinding and polishing processing equipment and processing method |
| CN113186510A (en) * | 2021-04-28 | 2021-07-30 | 昆明理工大学 | Metal reinforced porous diamond film and preparation method thereof |
| CN116716591A (en) * | 2023-05-31 | 2023-09-08 | 中国电子科技集团公司第十三研究所 | Molybdenum support structure and diamond preparation method |
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| EP0806267A1 (en) * | 1996-05-02 | 1997-11-12 | Applied Materials, Inc. | Cross-hatched polishing pad for polishing substrates in a chemical mechanical polishing system |
| WO1997044160A1 (en) * | 1996-05-21 | 1997-11-27 | Micron Technology, Inc. | Method for chemical-mechanical planarization of stop-on-feature semiconductor wafers |
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| WO1998049723A1 (en) * | 1997-04-30 | 1998-11-05 | Minnesota Mining And Manufacturing Company | Method of planarizing the upper surface of a semiconductor wafer |
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| CN111251133A (en) * | 2020-02-25 | 2020-06-09 | 中国地质大学（北京） | Diamond grinding and polishing processing equipment and processing method |
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