CN219260271U - Seed crystal position fixing device for mass production of diamonds - Google Patents
Seed crystal position fixing device for mass production of diamonds Download PDFInfo
- Publication number
- CN219260271U CN219260271U CN202223202795.3U CN202223202795U CN219260271U CN 219260271 U CN219260271 U CN 219260271U CN 202223202795 U CN202223202795 U CN 202223202795U CN 219260271 U CN219260271 U CN 219260271U
- Authority
- CN
- China
- Prior art keywords
- diamond
- grooves
- seed crystal
- fixing device
- carbon source
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model discloses a seed crystal position fixing device for mass production of diamonds, which comprises a substrate and a plurality of grooves formed in the upper surface of the substrate, wherein single crystal diamonds are in clearance fit with the corresponding grooves, and the depth of the grooves is smaller than the thickness of the single crystal diamonds at the corresponding positions; the depth of the grooves from the central groove to the grooves on the two sides sequentially becomes shallow, and the grooves from the central groove to the grooves on the two sides are arranged in a step shape; the method comprises the following steps: seed crystal pretreatment is selected; etching; diamond growth: shut down O 2 After the gas is stabilized, introducing carbon source gasAnd mixed gas, carbon source and H 2 The percentage of the carbon source is controlled to be 1-12 percent, after the growth is completed, the carbon source is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed; the mixed gas is Ar gas and oxygen, and the oxygen content is not more than 1% of the hydrogen content; the utility model realizes batch stability and can produce diamond in batches.
Description
Technical Field
The utility model relates to the technical field of diamond growth, in particular to a seed crystal position fixing device for mass production of diamond.
Background
Diamond has attracted attention due to its extremely excellent physicochemical properties. Natural diamond reserves are limited, however, and various synthetic diamond methods have been developed, such as high temperature High Pressure (HPHT) and hot wire chemical vapor deposition (HJCVD). The microwave plasma chemical vapor deposition method (Microwave plasma chemical vapor deposition) can synthesize diamond with high quality and large area because no impurity is introduced. A flow chart of the microwave plasma chemical vapor deposition method for synthesizing diamond is shown in fig. 1.
The quality of the synthesized diamond by the MPCVD method is related to various factors, including the concentration of carbon source, the gas flow, the temperature, the height of the substrate table, the microwave power, the synthesis temperature, and the synthesis temperature have great relations to the quality of the synthesized diamond. However, during the batch diamond synthesis, the seed crystal position is shifted during the temperature rising process, which greatly hinders the measurement of the seed crystal temperature and the setting of the target parameters, and further affects the quality of the final synthesized product.
The reason for the drift of the seed crystal is mainly the following: (1) in the heating process, the substrate and the diamond generate a gassing phenomenon, so that the friction force between the seed crystals and the substrate is reduced, (2) gaps exist between the substrate and the seed crystals, namely, the processing level of a contact surface is limited, and the main reasons are that when the laser is used for cutting, the profile of the laser is caused, and the surface profile meter test shows that the drifting seeds all find that the surface is protruded; (3) when in ventilation, the air flow is too large, turbulence occurs in the air flow, and certain turbulence is caused to the seed crystal; (4) turbulence or turbulence caused by uneven distribution of plasma species, density, temperature, etc.
In order to solve the above technical problems, there are various solutions for fixing single diamond in the prior art. For example, the substrate and the single crystal diamond are fixed on the surface of the substrate by welding; a specific molybdenum holder design, etc.; in the work of Mokuno et al, a seed holder made of two metallic Mo was also specifically designed (see fig. 2). Such designs are intended to generate a higher density plasma to achieve high-speed growth; and two different seed holders will produce different substrate temperatures. In Mao Heguang et al, a complex seed holder made of metallic Mo (as shown in fig. 3) is used, and in this design, they mechanically fix the diamond seed to the Mo holder by means of clamps, sheaths, etc. in order to maintain the diamond seed at a uniform temperature during growth.
However, the existing scheme can only solve the problem of fixing a single diamond, but for mass production of diamond products, a good effect cannot be achieved because of the natural defect of the oval shape of the plasma fireball, so that the surface temperature of the diamond seed crystal cannot reach a consistent state.
Disclosure of Invention
The utility model aims to provide a seed crystal position fixing device for mass production of diamond, which solves the problem that the existing scheme only can solve the problem that the fixing scheme of single diamond can not achieve good effect for mass production of diamond products.
The utility model is realized in such a way, a seed crystal position fixing device for mass production of diamond, the fixing device comprises a substrate and a plurality of grooves formed on the upper surface of the substrate, the monocrystalline diamond is in clearance fit with the corresponding grooves, and the depth of the grooves is smaller than the thickness of the monocrystalline diamond at the corresponding positions;
the grooves are arranged on the substrate from the center to the periphery at equal intervals, the depths of the grooves from the center to the periphery are sequentially shallower, and the grooves from the center to the periphery are arranged in a step shape.
Aiming at the current seed crystal fixing mode, the utility model provides a solution for the co-growth of a plurality of diamond, which not only can play a role in fixing the diamond seed crystal, but also can make up for the natural defect of the oval shape of the plasma fireball, so that the surface temperature of the diamond seed crystal is in a consistent state as far as possible; specifically, on the upper surface of the substrate, a groove is precisely machined according to the geometric shape and the size of diamond, and the diamond is sequentially placed into the groove, so that the purpose of fixing diamond seed crystals is achieved. The depth of the groove from the center to the periphery is sequentially shallower and takes the shape of a step, so that the defect of nonuniform heating caused by elliptical plasma fireball is overcome.
According to the utility model, the central groove is arranged in the center of the substrate, the peripheral grooves are arranged along the periphery of the central groove, the positions of the diamonds are fixed, the limited space can be utilized to grow a plurality of diamonds to the maximum extent, the common growth of the plurality of diamonds is realized, the plurality of diamonds are synthesized as much as possible, and the cost is reduced.
The utility model further adopts the technical scheme that: and the peripheral grooves in the grooves are symmetrically arranged by taking the central groove as the center. And after the positions of the diamonds are fixed by further utilizing the space, the co-growth of a plurality of diamonds is realized, and the batch production of the diamonds is realized.
The utility model further adopts the technical scheme that: the clearance of the clearance fit is 0.1-0.5mm.
The utility model further adopts the technical scheme that: the depth of the groove is 0.1-0.3mm smaller than the thickness of the single crystal diamond at the corresponding position. The diamond is convenient to take and put.
The utility model further adopts the technical scheme that: the substrate is made of a material which is high in temperature resistance and thermal conductivity and does not generate buckling deformation.
The utility model further adopts the technical scheme that: the material is molybdenum or tungsten.
The utility model further adopts the technical scheme that: the depth of the grooves sequentially becomes shallow from the center to the periphery, and the depth difference between two adjacent grooves on the horizontal section is smaller than 0.1mm.
The utility model further adopts the technical scheme that: the depth difference between two adjacent grooves on the horizontal section is 0.02mm. The depth difference is optimal.
The utility model further adopts the technical scheme that: the cross section of the groove is round, square or rectangular. In particular to a diamond seed crystal. The whole shape is in a ladder shape, and the processing positions of the grooves are in the most densely arranged mode, so that the aims of maximizing the synthesis quantity and reducing the cost are fulfilled. And the arrangement can be changed according to actual conditions, such as circular arc arrangement.
The utility model also provides a method for mass production of diamond, which is based on the fixing device and comprises the following steps:
step one, seed crystals are selected for pretreatment;
step two, etching treatment: putting seed crystal into corresponding groove of fixing device, introducing hydrogen, controlling hydrogen introducing condition to generate plasma, gradually increasing pressure and power until seed crystal temperature of diamond is stable at 850-950 ℃, and introducing O 2 Then etching for 15-60min in the environment;
step three, diamond growth: shut down O 2 Gas is kept to be introduced with H 2 After the gas is stabilized, introducing carbon source gas and mixed gas, and introducing the carbon source gas and H 2 The volume percentage of the carbon source gas is controlled to be 1-12 percent until the seed crystal grows to a set thickness, the carbon source gas is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed; the mixed gas is Ar gas and oxygen, and the volume content of the oxygen is not more than 1% of the hydrogen content.
After the diamond position is fixed, the co-growth of a plurality of diamonds is realized through the adjustment of the technological parameters such as power, air pressure and the like, the plurality of diamonds are synthesized as much as possible, the cost is reduced, the batch stability is realized, and the yield is improved to more than 95%.
The utility model further adopts the technical scheme that: in the second step H 2 The gas flow is 100-1000sccm, when the gas pressure is 2-20mbar, 300-1500W is introduced to start to generate plasma, the pressure increasing rate is controlled to be 1-10mbar per minute, the power increasing rate is controlled to be 10-300W per minute, and O is introduced 2 ：H 2 The volume percentage of the metal oxide is controlled to be 0.2-10 percent, and then the metal oxide is etched for 15-60 minutes in the environment.
The utility model further adopts the technical scheme that: in the third step, the carbon source gas is methane, CH 4 And H is 2 The volume percentage of the mixed gas is controlled between 1 and 12 percent, wherein: h 2 The volume ratio of the seed crystal is between 0.1 and 50 percent, the temperature is between 800 and 1250 ℃, the power is 3000 to 6000W, the gas pressure is 120 to 300mbar, the ratio coefficient of the power to the gas pressure is 20 to 40, the carbon source is closed until the seed crystal grows to a set thickness (the growth rate of the seed crystal is controllable, the time of the growth to the set thickness can be calculated), the power and the pressure are gradually reduced, and the shutdown operation is completed.
The utility model further adopts the technical scheme that: the carbon source gas may be carbon-containing gas such as ethanol and acetylene.
The utility model further adopts the technical scheme that: firstly, selecting seed crystals with flat surfaces, wherein the thickness of the seed crystals is 0.3-4mm, polishing, pickling and cleaning the seed crystals, enabling the growth surface to be a (100) surface, polishing the seed crystals, washing organic matters on the seed crystal surface by using acetone or absolute ethyl alcohol, pickling by using prepared piranha solution, removing metal impurities on the seed crystal surface, washing acid liquor by using deionized water, drying, and placing the seed crystals into a cavity for growth.
The utility model has the beneficial effects that:
the utility model not only can play a role of fixing diamond seed crystals, but also can make up for the natural defect of the oval shape of the plasma fireball, so that the surface temperature of the diamond seed crystals reaches a consistent state as far as possible; specifically, on the upper surface of the substrate, a groove is precisely machined according to the geometric shape and the size of diamond, and the diamond is sequentially placed into the groove, so that the purpose of fixing diamond seed crystals is achieved. The depth of the groove from the center to the periphery is sequentially shallower and takes the shape of a step, so that the defect of nonuniform heating caused by elliptical plasma fireball is overcome;
according to the utility model, the central groove is arranged in the center of the substrate, the peripheral groove is arranged along the periphery of the central groove, the positions of the diamonds are fixed, the limited space can be utilized to grow a plurality of diamonds to the maximum extent, the common growth of the plurality of diamonds is realized, the plurality of diamonds are synthesized as far as possible, and the cost is reduced;
after the diamond positions are fixed, the fixing device provided by the utility model is matched with the method disclosed by the utility model, so that the co-growth of a plurality of diamonds is realized, the plurality of diamonds are synthesized as much as possible, the cost is reduced, the batch stability is realized, and the yield is improved to more than 95%.
Drawings
FIG. 1 is a flow chart of a microwave plasma chemical vapor deposition process for synthesizing diamond;
FIG. 2 is a schematic diagram of a seed holder made of two metallic Mo designed in the work of Mokuno et al;
FIG. 3 is a schematic view of a seed holder of Mao Heguang design;
FIG. 4 is a top view of a fastening device according to a first embodiment of the present utility model;
FIG. 5 is a cross-sectional view A-A provided by the present utility model;
FIG. 6 is a Raman spectrum of diamond prepared in example II;
FIG. 7 is a Raman spectrum of diamond prepared in comparative example I provided by the utility model;
fig. 8 is a top view of a fixture provided by the present utility model.
Reference numerals: 1. substrate, 2. Groove.
Detailed Description
Other advantages and effects of the present utility model will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present utility model with reference to specific examples. The utility model may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present utility model.
It should be noted that, the structures, proportions, sizes and the like shown in the drawings attached to the present specification are used for understanding and reading only in conjunction with the disclosure of the present specification, and are not intended to limit the applicable limitations of the present utility model, so that any modification of the structures, variation of proportions or adjustment of sizes of the structures, proportions and the like should not be construed as essential to the present utility model, and should still fall within the scope of the disclosure of the present utility model without affecting the efficacy and achievement of the present utility model. Also, the terms such as "upper," "lower," "left," "right," "middle," and "a" and the like recited in the present specification are merely for descriptive purposes and are not intended to limit the scope of the utility model, but are intended to provide relative positional changes or modifications without materially altering the technical context in which the utility model may be practiced.
Embodiment one:
fig. 4 to 5 show a seed crystal position fixing device for mass-producing diamond, the fixing device comprises a substrate 1 and a plurality of grooves 2 formed on the upper surface of the substrate 1, the single crystal diamond is in clearance fit with the corresponding grooves 2, and the depth of the grooves 2 is smaller than the thickness of the single crystal diamond at the corresponding positions;
the depth of the grooves 2 from the central groove to the peripheral groove sequentially becomes shallow, and the grooves 2 from the central groove to the peripheral groove are arranged in a step shape.
In this embodiment, the peripheral grooves among the plurality of grooves 2 are symmetrically arranged with the central groove as the center. After the diamond position is fixed in the maximized utilization space, the co-growth of a plurality of diamonds is realized through the adjustment of the technological parameters such as power, air pressure and the like, the batch stability is realized, and the yield is improved to more than 95%.
In this embodiment, the grooves are five and are arranged in a row.
In this embodiment, the gap of the clearance fit is 0.1-0.5mm.
In this embodiment, the depth of the groove 2 is 0.1-0.3mm smaller than the thickness of the single crystal diamond at the corresponding position. The diamond is convenient to take and put.
In this embodiment, the substrate 1 is made of a material that is resistant to high temperature, has high thermal conductivity, and does not undergo warp deformation.
In this embodiment, the material is molybdenum.
In this embodiment, the depths of the plurality of grooves become shallower from the center to the periphery in sequence, and the depth difference between two adjacent grooves is less than 0.1mm.
In this embodiment, the cross section of the groove 2 is circular. As other embodiments, the recess may be square or rectangular. In particular to a diamond seed crystal. The whole shape is in a ladder shape, and the processing positions of the grooves are in the most densely arranged mode, so that the aims of maximizing the synthesis quantity and reducing the cost are fulfilled. And the arrangement can be changed according to actual conditions, such as circular arc arrangement.
The working principle of the embodiment is as follows: aiming at the current seed crystal fixing mode, the utility model provides a solution for the co-growth of a plurality of diamond, which not only can play a role in fixing the diamond seed crystal, but also can make up for the natural defect of the oval shape of the plasma fireball, so that the surface temperature of the diamond seed crystal is in a consistent state as far as possible; specifically, on the upper surface of the substrate, a groove is precisely machined according to the geometric shape and the size of diamond, and the diamond is sequentially placed into the groove, so that the purpose of fixing diamond seed crystals is achieved. The depth of the groove from the center to the periphery is sequentially shallower and takes the shape of a step, so that the defect of nonuniform heating caused by elliptical plasma fireball is overcome. According to the utility model, the central groove is arranged in the center of the substrate, the peripheral grooves are arranged along the periphery of the central groove, the positions of the diamonds are fixed, the limited space can be utilized to grow a plurality of diamonds to the maximum extent, the common growth of the plurality of diamonds is realized, the plurality of diamonds are synthesized as much as possible, and the cost is reduced.
Embodiment two:
a method of mass producing diamond based on the fixture of embodiment one, the method comprising the steps of:
step one: seed crystals are selected for pretreatment;
step two: etching: putting seed crystal into corresponding groove of fixing device, introducing hydrogen, controlling hydrogen introducing condition to generate plasma, gradually increasing pressure and power until the temperature of diamond seed crystal is 900 deg.C stable, and introducing O 2 Then etching for 30min in the environment;
step three: diamond growth: shut down O 2 Gas is kept to be introduced with H 2 After the gas is stabilized, introducing carbon source gas and mixed gas, and introducing the carbon source gas and H 2 The percentage of the carbon source is controlled to be 10 percent of the volume percentage until the seed crystal grows to the set thickness, the carbon source is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed; the mixed gas is Ar gas and oxygen, and the oxygen content is not more than 1% of the hydrogen content.
In this embodiment, H in the second step 2 The gas flow rate is 500sccm, when the gas pressure is 10mbar, 1000W is introduced to start, plasma is generated, and the pressure increasing rate is controlled at 5mbar per minuteThe rate of power increase was controlled at 100W per minute, O was let in 2 ：H 2 Is controlled to be 5% by volume and then etched for 30 minutes in this environment.
In this embodiment, the carbon source gas in the third step is methane, CH 4 And H is 2 Wherein the volume percentage of the mixed gas is controlled at 10 percent: h 2 The volume ratio of the catalyst is 20%, the temperature is 1000 ℃, the power is 5000W, the gas pressure is 200mbar, the ratio coefficient of the power to the gas pressure is 25, until seed crystals grow to a set thickness, the carbon source is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed.
As other examples, the carbon source gas may be carbon-containing gas such as ethanol or acetylene.
Firstly, selecting seed crystals with a flat surface, wherein the thickness of the seed crystals is 2mm, polishing, pickling and cleaning, the growth surface is a (100) surface, polishing, washing away organic matters on the surface of the seed crystals by using acetone or absolute ethyl alcohol, pickling by using prepared piranha solution, removing metal impurities on the surface of the seed crystals, washing away acid liquor by using deionized water, and then drying and placing the seed crystals into a cavity for growth.
The raman spectrum test was performed on either of the diamonds obtained in example two, and the results are shown in fig. 6. Using Ar and O 2 As a result of raman spectrum test after the growth of the mixed gas, the prepared sample Raman characteristic peak and the natural diamond first-order characteristic Raman peak (1332 cm -1 ) Very close, indicating that the grown single crystal diamond sample has no non-diamond phase generation, and the Raman shift offset is 0.06cm -1 。
Embodiment III:
a method of mass producing diamond based on the fixture of embodiment one, the method comprising the steps of:
step one: seed crystals are selected for pretreatment;
step two: etching: putting seed crystal into corresponding groove of fixing device, introducing hydrogen, controlling hydrogen introducing condition to generate plasma, thenGradually increasing pressure and power until the seed crystal temperature of diamond is stable at 850 ℃, and then introducing O 2 Then etching for 15min in the environment;
step three: diamond growth: shut down O 2 Gas is kept to be introduced with H 2 After the gas is stabilized, introducing carbon source gas and mixed gas, and introducing the carbon source gas and H 2 The percentage of the carbon source is controlled to be 1 percent by volume until seed crystals grow to a set thickness, the carbon source is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed; the mixed gas is Ar gas and oxygen, and the oxygen content is not more than 1% of the hydrogen content.
In this embodiment, H in the second step 2 The gas flow rate is 100sccm, when the gas pressure is 2mbar, 500W is introduced to start, plasma is generated, the pressure increasing rate is controlled to be 1mbar per minute, the power increasing rate is controlled to be 10W per minute, and O is introduced 2 ：H 2 Is controlled to be 0.2 percent by volume and then etched for 15 minutes in the environment.
In this embodiment, the carbon source gas in the third step is methane, CH 4 And H is 2 Wherein the volume percentage of the mixed gas is controlled at 1 percent: h 2 The volume ratio of the catalyst is 0.1%, the temperature is 800 ℃, the power is 3000W, the gas pressure is 150mbar, the ratio coefficient of the power to the gas pressure is 20, until seed crystal grows to a set thickness, the carbon source is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed.
As other examples, the carbon source gas may be carbon-containing gas such as ethanol or acetylene.
Firstly, selecting seed crystals with a flat surface, wherein the thickness of the seed crystals is 2mm, polishing, pickling and cleaning, the growth surface is a (100) surface, polishing, washing away organic matters on the surface of the seed crystals by using acetone or absolute ethyl alcohol, pickling by using prepared piranha solution, removing metal impurities on the surface of the seed crystals, washing away acid liquor by using deionized water, and then drying and placing the seed crystals into a cavity for growth.
The 5 diamonds obtained in example three were subjected to raman spectroscopy. The results are shown in Table 1
Table 1 raman spectral detection data for diamond products in five grooves
Using Ar and O 2 Raman spectrum test result after mixed gas growth, and natural diamond first-order characteristic Raman peak (1332 cm -1 ) Quite close, it was demonstrated that no non-diamond phase was generated for the grown single crystal diamond samples.
Embodiment four:
a method of mass producing diamond based on the fixture of embodiment one, the method comprising the steps of:
step one: seed crystals are selected for pretreatment;
step two: etching: putting seed crystal into corresponding groove of fixing device, introducing hydrogen, controlling hydrogen introducing condition to generate plasma, gradually increasing pressure and power until the temperature of diamond seed crystal is stable at 950 deg.C, and introducing O 2 Then etching for 60min in the environment;
step three: diamond growth: shut down O 2 Gas is kept to be introduced with H 2 After the gas is stabilized, introducing carbon source gas and mixed gas, and introducing the carbon source gas and H 2 The percentage of the carbon source is controlled to be 12 percent of the volume percentage until the seed crystal grows to the set thickness, the carbon source is closed, the power and the pressure are gradually reduced, and the shutdown operation is completed; the mixed gas is Ar gas and oxygen, and the oxygen content is not more than 1% of the hydrogen content.
In this embodiment, H in the second step 2 The gas flow is 1000sccm, when the gas pressure is 20mbar, 1500W is introduced to start plasma, the pressure increasing rate is controlled at 10mbar per minute, and the power increasing rate is controlledAt 300W per minute, let-in O 2 ：H 2 Is controlled to be 10 percent by volume and then etched for 60 minutes in the environment.
In this embodiment, the carbon source gas in the third step is methane, CH 4 And H is 2 Wherein the volume percentage of the mixed gas is controlled at 12 percent: h 2 The volume ratio of the catalyst is 50%, the temperature is 1250 ℃, the power is 6000W, the gas pressure is 300mbar, the ratio coefficient of the power to the gas pressure is 20, the catalyst is closed until the seed crystal grows to a set thickness, the power and the pressure are gradually reduced, and the shutdown operation is completed.
As other examples, the carbon source gas may be carbon-containing gas such as ethanol or acetylene.
Firstly, selecting seed crystals with a flat surface, wherein the thickness of the seed crystals is 2mm, polishing, pickling and cleaning, the growth surface is a (100) surface, polishing, washing away organic matters on the surface of the seed crystals by using acetone or absolute ethyl alcohol, pickling by using prepared piranha solution, removing metal impurities on the surface of the seed crystals, washing away acid liquor by using deionized water, and then drying and placing the seed crystals into a cavity for growth.
The 5 diamonds obtained in example four were subjected to raman spectroscopy. The results are shown in Table 2
Table 2 raman spectral detection data for diamond products in five grooves
| Sequence number | Peak value/cm -1 | Peak width at half maximum (FWHM)/cm -1 | Impurity peak/ |
| 1 | 1332.28 | 3.28 | Without any means for |
| 2 | 1332.38 | 3.59 | Without any means for |
| 3 | 1332.10 | 3.71 | Without any means for |
| 4 | 1332.23 | 3.08 | Without any means for |
| 5 | 1332.26 | 3.46 | Without any means for |
Using Ar and O 2 Raman spectrum test result after mixed gas growth, and natural diamond first-order characteristic Raman peak (1332 cm -1 ) Quite close, it was demonstrated that no non-diamond phase was generated for the grown single crystal diamond samples.
Comparative example one:
in contrast to the method described in example two, only step three is different, and in this comparative example, step three is: diamond growth: shut down O 2 After the gas is stabilized, introducing carbon source gas and Ar gas, and introducing the carbon source gas and H 2 The percentage of the carbon source is controlled to be 10 percent, after the growth is completed, the carbon source is closed, and the power and the pressure are gradually reduced to complete the closingThe machine is operated.
One of the diamonds obtained in comparative example one was randomly selected for raman spectroscopy and the results are shown in fig. 7. Not using Ar and O 2 Raman spectrum test results after mixed gas growth, and raman test on the grown diamond sheet sample, the results show that besides typical diamond raman peak, the sample is 513.09cm -1 、1576.02cm -1 There are impurity peaks in the vicinity, and these two correspond to silicon impurity peaks and G-band (graphite) impurity peaks, respectively.
Comparative example two:
the difference from the method described in the second embodiment is only that the fixing device structure adopted in this embodiment is: the substrate is provided with 5 grooves which are arranged in a row, the depths of the grooves are equal and are positioned on the same horizontal plane, the seed crystal adopting the fixing device is used for preparing the diamond by the method described in the second embodiment, and the difference between the maximum peak value and the minimum peak value in the obtained Raman spectrum results of 5 diamonds is 1.06cm -1 At the same time, the maximum difference of half peak width is 2.11cm -1 . The results of raman spectrum detection of the diamond products in the five grooves in the second embodiment of the present utility model are shown in table 3;
table 3 raman spectral detection data for diamond products in five grooves
| Sequence number | Peak value/cm -1 | Peak width at half maximum (FWHM)/cm -1 | Impurity peak/ |
| 1 | 1332.25 | 3.25 | Without any means for |
| 2 | 1332.33 | 3.54 | Without any means for |
| 3 | 1332.06 | 3.68 | Without any means for |
| 4 | 1332.19 | 3.05 | Without any means for |
| 5 | 1332.23 | 3.41 | Without any means for |
As can be seen from Table 3, the maximum peak value is 1332.33cm -1 The minimum peak value is 1332.06cm -1 When the fixing device in the first embodiment is combined with the method in the second embodiment for mass production, the growth quality is high, and the quality uniformity is good, so that the fixing device and the method are adopted, the diamond particles are heated uniformly in the growth process, the product quality can be obviously improved, and the mass production of diamond with batch stability is realized.
The foregoing description of the preferred embodiments of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the utility model.
Claims (8)
1. A seed crystal position fixing device of batch production diamond, its characterized in that: the fixing device comprises a substrate (1) and a plurality of grooves (2) formed in the upper surface of the substrate (1), wherein single crystal diamond is in clearance fit with the corresponding grooves (2), and the depth of the grooves (2) is smaller than the thickness of the single crystal diamond at the corresponding position;
the grooves are arranged on the substrate from the center to the periphery at equal intervals, the depths of the grooves (2) from the center to the periphery are sequentially shallower, and the grooves (2) from the center to the periphery are arranged in a step shape.
2. A seed crystal position fixing device for mass-production of diamond according to claim 1, wherein the peripheral grooves among the plurality of grooves (2) are symmetrically arranged centering on the central groove.
3. A mass-produced diamond seed crystal position fixing device according to claim 1 or 2, wherein the clearance fit is 0.1-0.5mm.
4. A seed crystal position fixing device for mass-produced diamond according to claim 1 or 2, wherein the depth of the groove (2) is 0.1-0.3mm smaller than the thickness of single crystal diamond at the corresponding position.
5. A seed crystal position fixing device for mass-production of diamond according to claim 1 or 2, wherein the substrate (1) is made of a material which is resistant to high temperature, has high thermal conductivity and does not undergo warp deformation, and the material is molybdenum.
6. A seed crystal position fixing device for mass-production of diamond according to claim 1 or 2, wherein the substrate (1) is made of a material which is resistant to high temperature, has high thermal conductivity and does not undergo warp deformation, and is tungsten.
7. A mass-produced diamond seed crystal position fixing device according to claim 1 or 2, wherein the depths of a plurality of grooves become shallower from the center to the periphery in sequence, and the difference in depth between two adjacent grooves in horizontal section is less than 0.1mm.
8. A mass-produced diamond seed crystal position fixing device according to claim 7, wherein the depth difference between two adjacent grooves in the horizontal section is 0.02mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223202795.3U CN219260271U (en) | 2022-12-01 | 2022-12-01 | Seed crystal position fixing device for mass production of diamonds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223202795.3U CN219260271U (en) | 2022-12-01 | 2022-12-01 | Seed crystal position fixing device for mass production of diamonds |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN219260271U true CN219260271U (en) | 2023-06-27 |
Family
ID=86870746
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202223202795.3U Active CN219260271U (en) | 2022-12-01 | 2022-12-01 | Seed crystal position fixing device for mass production of diamonds |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN219260271U (en) |
-
2022
- 2022-12-01 CN CN202223202795.3U patent/CN219260271U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112877773B (en) | Non-air-flow MPCVD single crystal diamond growth method using solid carbon source | |
| US20140150713A1 (en) | Controlling doping of synthetic diamond material | |
| CN215560802U (en) | Substrate table bearing device for preparing single crystal diamond through MPCVD | |
| Weng et al. | Preparation of diamond films with controllable surface morphology, orientation and quality in an overmoded microwave plasma CVD chamber | |
| CN111778555B (en) | Low-stress diamond and preparation method thereof | |
| CN110565164A (en) | Method for preventing seed crystal from drifting in process of growing diamond by MPCVD and growing method | |
| CN101363118B (en) | Method for growing silicon carbide film on silicon substrate | |
| CN111153407A (en) | Reactor for producing polycrystalline silicon, apparatus for producing polycrystalline silicon, method for producing polycrystalline silicon, and polycrystalline silicon rod or polycrystalline silicon block | |
| CN219260271U (en) | Seed crystal position fixing device for mass production of diamonds | |
| CN100432287C (en) | Process for preparing diamond film under strong magnetic field | |
| CN114752916A (en) | Method for converting graphite phase in nano diamond film into diamond phase under low pressure | |
| CN115838967A (en) | Seed crystal position fixing device and method for batch production of diamonds | |
| CN108070842A (en) | The method for using MPCVD methods growth single-crystal diamond as carbon source based on hairline | |
| CN112063996A (en) | Microwave plasma reaction chamber and accommodating base thereof | |
| CN110938811A (en) | Method for rotatably growing diamond in microwave plasma chemical vapor deposition | |
| CN206751920U (en) | A kind of chip bench that diamond film is prepared for MPCVD method | |
| Nakamura et al. | High quality chemical vapor deposition diamond growth on iron and stainless steel substrates | |
| CN115710747A (en) | Device for preventing internal discharge of MPCVD equipment, MPCVD equipment and diamond preparation method | |
| CN114318529B (en) | Diamond and synthesis process thereof | |
| CN111676466A (en) | A water conservancy diversion formula sample holds in palm and system for MPCVD system | |
| CN113061871A (en) | Method for preparing vertical graphene film in high-quality, rapid and large-area mode | |
| CN115142039A (en) | CVD diamond, manufacturing method thereof and method for improving optical property of diamond | |
| CN113186597B (en) | Low-cost, large-size and high-quality single crystal diamond as well as preparation method and application thereof | |
| KR101320620B1 (en) | Apparatus for chemical vapor deposition for diamond film and method for synthesis of diamond film | |
| Yan et al. | Chemical vapor deposition of uniform and high-quality diamond films by bias-enhanced nucleation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |