阅读说明：本技术 一种大颗粒金刚石的制备装置及其制备方法 (Preparation device and preparation method of large-particle diamond ) 是由 王忠强 丁雄傑 王�琦 张国义 于 2019-10-31 设计创作，主要内容包括：本发明涉及金刚石制备技术领域,具体涉及一种大颗粒金刚石的制备装置及其制备方法,本发明的大颗粒金刚石的制备装置包括沉积腔体,还包括吹气单元、排气单元和等离子体单元,吹气单元设有进气管路,进气管路伸入沉积腔体一端设为喇叭状开口,并在喇叭状开口处设有若干个吹气小孔,本发明通过设置于喇叭状开口处的若干个吹气小孔吹出气流,使得进气管路内的气压大于沉积腔体内的气压,两者的压力差使得金刚石籽晶悬浮在进气管路喇叭状开口处上方并三维旋转,从而实现籽晶可以在三维方向均衡生长；本发明的制备方法,其工艺简单,制备效率高,且制得的大颗粒金刚石质量好,满足工业化的生产制造。(The invention relates to the technical field of diamond preparation, in particular to a preparation device of large-particle diamond and a preparation method thereof, wherein the preparation device of large-particle diamond comprises a deposition cavity, an air blowing unit, an exhaust unit and a plasma unit, wherein the air blowing unit is provided with an air inlet pipeline, one end of the air inlet pipeline, which extends into the deposition cavity, is provided with a horn-shaped opening, and a plurality of small air blowing holes are arranged at the horn-shaped opening; the preparation method has the advantages of simple process and high preparation efficiency, and the prepared large-particle diamond has good quality and meets the requirement of industrialized production.)

1. The utility model provides a preparation facilities of large granule diamond, including the deposit cavity, a serial communication port, still including the unit of blowing, exhaust unit and plasma unit, the unit of blowing is equipped with the air inlet pipeline, air inlet pipeline one end stretches into deposit cavity bottom and communicates with the deposit cavity, air inlet pipeline stretches into deposit cavity one end and establishes to loudspeaker form opening to be equipped with a plurality of aperture of blowing at loudspeaker form opening part, the exhaust unit is equipped with exhaust pipe, exhaust pipe and deposit cavity top intercommunication, the plasma unit is connected with the deposit cavity.

2. The apparatus for preparing a large granular diamond according to claim 1, further comprising an air blowing adjusting means connected to the air blowing unit.

3. The apparatus of claim 1, further comprising a vacuum regulator, wherein the vacuum regulator is installed in an exhaust line.

4. The apparatus for preparing a large granular diamond according to claim 1, further comprising an exhaust regulating valve installed in an exhaust line.

5. The apparatus according to claim 2, further comprising a circulation unit, wherein the circulation unit is provided with a circulation air duct, and the two ends of the circulation air duct are respectively communicated with the blowing adjustment device and the exhaust pipeline.

6. The apparatus for preparing a large granular diamond according to claim 5, wherein the circulation unit is further provided with a heat exchange device and a circulation regulating valve, and the heat exchange device and the circulation regulating valve are respectively installed on a circulation air duct.

7. The apparatus of claim 1, wherein the plasma unit is provided with a microwave plasma generator, and the microwave plasma generator is connected to the deposition chamber.

8. The apparatus of claim 1, further comprising an observation window, wherein the observation window is installed on a wall of the deposition chamber.

9. The method for preparing a large granular diamond according to any one of claims 1 to 8, comprising the steps of:

the method comprises the following steps: placing the diamond seed crystal into a deposition cavity, and blowing air flow from a plurality of air blowing small holes arranged at the horn-shaped opening, so that the diamond seed crystal is suspended above the horn-shaped opening of the air inlet pipeline and rotates in three dimensions;

step two: coating the plasma generated by the plasma unit above the diamond seed crystal;

step three: controlling the growth condition of the crystal to prepare the large-particle diamond.

10. The method of claim 9, wherein the large particle diamond is selected from the group consisting of diamond particles,

in the first step, putting diamond seed crystals into a deposition cavity through an observation window;

in the third step, the growth temperature and pressure of the crystal are controlled by controlling the power of the microwave plasma generator and adjusting the temperature of the gas in the circulating gas inlet pipeline through the circulating unit, and the vacuum degree in the deposition cavity is adjusted through the vacuum adjusting device.

Technical Field

The invention relates to diamond preparation, in particular to a preparation device and a preparation method of large-particle diamond.

Background

The single crystal diamond has excellent physical and chemical properties, has important application value in the fields of machinery, electronics, jewelry and the like, and needs to be prepared into large-particle diamond in order to expand the application.

Among various diamond preparation methods, the microwave plasma chemical vapor deposition method is the preferred method for preparing high-quality diamond due to the characteristics of high plasma power density, no electrode discharge pollution, stable performance and the like, in the process of producing large-particle monocrystalline diamond by the current method, the diamond seed crystal is generally fixed on a deposition table, the temperature of the seed crystal is controlled by cooling the deposition table, unidirectional growth is carried out on the side of the seed crystal facing to plasma, polycrystalline or amorphous carbonization is often caused at the edge due to the difference of growth environments of the side edge and the center of the crystal, dislocation is more and more spread to the growth surface, the growth surface of the single crystal is smaller and smaller, the crystal needs to be repeatedly cleaned and cut and then grows again or grows in a splicing manner, and the production efficiency and the product quality are seriously influenced.

In view of the above technical problems, there is a need for a new diamond manufacturing apparatus and a new diamond manufacturing method to better solve the above technical problems.

Disclosure of Invention

In order to solve the problems, the invention provides a preparation device and a preparation method of large-particle diamond, and the preparation device provided by the invention has the advantages of simple structure, reasonable design and convenience for preparing large-particle diamond; the preparation method provided by the invention has simple process, can effectively control the temperature in the growth process of the diamond seed crystal, and the prepared diamond product has high quality.

The technical scheme adopted by the invention is as follows:

the utility model provides a preparation facilities of large granule diamond, including the deposit cavity, still include the unit of blowing, exhaust unit and plasma unit, the unit of blowing is equipped with the air inlet pipeline, air inlet pipeline one end stretches into deposit cavity bottom and communicates with the deposit cavity, air inlet pipeline stretches into deposit cavity one end and establishes to loudspeaker form opening to be equipped with a plurality of small hole of blowing at loudspeaker form opening part, the exhaust unit is equipped with exhaust pipe, exhaust pipe and deposit cavity top intercommunication, the plasma unit is connected with the deposit cavity.

The technical scheme is further improved by further comprising an air blowing adjusting device, and the air blowing adjusting device is connected with the air blowing unit.

The further improvement of the technical proposal is that the device also comprises a vacuum adjusting device which is arranged on the exhaust pipeline.

The further improvement of the technical scheme is that the exhaust gas regulating valve is further included and is arranged in an exhaust pipeline.

The technical scheme is further improved by further comprising a circulating unit, wherein the circulating unit is provided with a circulating air pipe, and two ends of the circulating air pipe are respectively communicated with an air blowing adjusting device and an exhaust pipeline.

The technical scheme is further improved in that the circulating unit is further provided with a heat exchange device and a circulating regulating valve, and the heat exchange device and the circulating regulating valve are respectively arranged on the circulating air pipe.

The plasma unit is further improved by being provided with a microwave plasma generator which is connected with the deposition cavity.

The further improvement of the technical scheme is that the device further comprises an observation window, and the observation window is arranged on the wall of the deposition cavity.

The method for preparing the large-particle diamond by adopting the preparation device of the large-particle diamond comprises the following steps:

the method comprises the following steps: placing the diamond seed crystal into a deposition cavity, and blowing air flow from a plurality of air blowing small holes arranged at the horn-shaped opening, so that the diamond seed crystal is suspended above the horn-shaped opening of the air inlet pipeline and rotates in three dimensions;

step two: coating the plasma generated by the plasma unit above the diamond seed crystal;

step three: controlling the growth condition of the crystal to prepare the large-particle diamond.

The further improvement of the technical proposal is that,

in the first step, putting diamond seed crystals into a deposition cavity through an observation window;

in the third step, the growth temperature and pressure of the crystal are controlled by controlling the power of the microwave plasma generator and adjusting the temperature of the gas in the circulating gas inlet pipeline through the circulating unit, and the vacuum degree in the deposition cavity is adjusted through the vacuum adjusting device.

The invention has the following beneficial effects:

1. the invention comprises a deposition cavity, a blowing unit, an exhaust unit and a plasma unit, wherein the blowing unit is provided with an air inlet pipeline, one end of the air inlet pipeline extends into the bottom end of the deposition cavity and is communicated with the deposition cavity, one end of the air inlet pipeline extending into the deposition cavity is provided with a horn-shaped opening, a plurality of blowing small holes are arranged at the horn-shaped opening, the exhaust unit is provided with an exhaust pipeline communicated with the top end of the deposition cavity, the plasma unit is connected with the deposition cavity, the invention has simple structure and reasonable design, process gas enters from the air inlet pipeline, the process gas is blown into the deposition cavity by the blowing small holes, air flow is blown out through the blowing small holes arranged at the horn-shaped opening, the air pressure in the air inlet pipeline is larger than the air pressure in the deposition cavity, and diamond seed crystals are suspended above the horn-shaped opening of the, in the rotation process of the diamond seed crystal, the plasma in the deposition cavity is coated above the suspended diamond seed crystal, the crystal growth temperature is controlled by controlling the power of the plasma unit and the temperature of the gas in the gas inlet pipeline, the temperature is controlled uniformly, and the high-quality large-particle diamond can be prepared.

2. The preparation method has simple process, meets the industrial production requirement, simultaneously controls the growth temperature of the diamond seed crystal accurately in the preparation process, and has high preparation efficiency and good quality of the prepared large-particle diamond.

Drawings

FIG. 1 is a schematic structural view of the present invention;

description of reference numerals: 1. the device comprises an air inlet pipeline, 2 blowing small holes, 3 deposition cavities, 4 blowing adjusting devices, 5 diamond seed crystals, 6 plasma units, 7 observation windows, 8 microwave plasma generators, 9 vacuum adjusting devices, 10 exhaust adjusting valves, 11 circulating pipelines, 12 heat exchange devices, 13 circulating adjusting valves and 14 exhaust units.

Detailed Description

The invention will be further described with reference to the accompanying drawings.

As shown in fig. 1, the device for preparing large-particle diamond of this embodiment includes a deposition chamber 3, and further includes an air blowing unit, an air exhaust unit and a plasma unit 6, the air blowing unit is provided with an air inlet pipeline 1, one end of the air inlet pipeline 1 extends into the bottom end of the deposition chamber 3 and is communicated with the deposition chamber 3, one end of the air inlet pipeline 1 extending into the deposition chamber 3 is provided with a horn-shaped opening, and is provided with a plurality of air blowing pores 2 at the horn-shaped opening, the air exhaust unit is provided with a circulation pipeline 11, the circulation pipeline 11 is communicated with the top end of the deposition chamber 3, and the plasma unit 6 is located in the deposition chamber 3, the device of the invention has simple structure and reasonable design, process gas enters from the air inlet pipeline 1, blows out air through the plurality of air blowing pores 2 arranged at the horn-shaped opening, so that the air pressure in the air inlet pipeline 1 is greater than the air pressure in the deposition chamber 3, in this embodiment, the one end that air inlet pipe way 1 was equipped with the aperture of blowing 2 is established to tubaeform opening, through setting up tubaeform opening, can increase the area of air inlet pipe way 1 air blow mouth, and then can set up more apertures of blowing 2, can blow aperture 2 through a plurality of, better control and distribution air current of aperture of blowing 2, and then better control diamond seed crystal 5 is rotatory, in diamond seed crystal 5 rotation process, make the cladding of the plasma in the deposit chamber in the diamond seed crystal 5 top of suspension, power through control microwave plasma generator 8, the temperature of air inlet pipe way 1 and circulation pipeline 11 internal gas controls crystal growth temperature, temperature control is even, thereby realize that the seed crystal can be in three-dimensional direction equilibrium growth.

In some specific embodiments, the diamond seed crystal growth device further comprises an air blowing adjusting device 4, the air blowing adjusting device 4 is connected with an air blowing unit, and the condition of air flow blown out from the air blowing small holes 2 can be further adjusted and distributed by arranging the adjusting device 4, so that suspension and three-dimensional rotation of the diamond seed crystal 5 can be better controlled, growth of the diamond seed crystal 5 in all directions is more balanced, and large-particle diamond with better quality is prepared.

In some embodiments, the deposition chamber further comprises a vacuum adjusting device 9, the vacuum adjusting device 9 is connected to the circulation pipeline 11, and specifically, the vacuum adjusting device in this embodiment is a vacuum pump, and the vacuum pump is equipped to control the process vacuum degree in the deposition chamber 3, so as to better control the growth conditions of the diamond seed crystal 5 in the deposition chamber 3.

In some optional embodiments, the exhaust gas regulating valve 10 is further included, and the exhaust gas regulating valve 10 is installed in the exhaust unit 14, so that the exhaust gas emission can be effectively controlled through the exhaust gas regulating valve 10, and the subsequent exhaust gas treatment is facilitated.

In other specific embodiments, the diamond seed crystal growth device further comprises an exhaust unit 14, the exhaust unit 14 is provided with a circulation pipeline 11, two ends of the circulation pipeline 11 are respectively communicated with the air blowing adjusting device 4 and the vacuum adjusting device 9, the circulation pipeline 11 is further provided with a heat exchanging device 12 and a circulation adjusting valve 13, the heat exchanging device 12 and the circulation adjusting valve 13 are respectively installed on the circulation pipeline 11, specifically, the heat exchanging device 12 in the embodiment is a heat exchanger, a circulation air pipe is arranged to improve the utilization efficiency of process gas and energy, the circulation air pipe adjusts the circulation inlet air temperature through the heat exchanger, and adjusts the pressure of the circulation gas through the circulation adjusting valve 13, so that the temperature and pressure conditions required by the growth of the diamond seed crystal 5 are better met.

Microwave plasma generator 8 is connected with deposition cavity 3, controls plasma unit 6 through the power that sets up microwave plasma generator 8, and then controls diamond seed crystal 5's growth temperature, and control is convenient and accurate.

In other specific examples, the device further comprises an observation window 7, wherein the observation window 7 is arranged on the wall of the deposition cavity 3, the diamond seed crystal 5 can be conveniently placed into the deposition cavity 3 by arranging the observation window 7, the prepared large-particle diamond can be conveniently taken out of the deposition cavity 3, in the preparation process, the growth process can be observed through the observation window 7, and the growth condition of the diamond seed crystal 5 in the deposition cavity 3 can be conveniently regulated and controlled in time.

The method for preparing the large-particle diamond by using the preparation device comprises the following steps:

the method comprises the following steps: placing the diamond seed crystal 5 into a deposition cavity 3, and blowing air flow out of a plurality of small air blowing holes 2 arranged at the horn-shaped opening, so that the diamond seed crystal 5 is suspended above the horn-shaped opening of the air inlet pipeline 1 and rotates in three dimensions;

step two: the plasma generated by the plasma unit 6 is coated above the diamond seed crystal 5;

step three: controlling the growth condition of the crystal to prepare the large-particle diamond.

In the first step, putting the diamond seed crystal 5 into the deposition cavity 3 through the observation window 7;

in the third step, the growth temperature and pressure of the crystal are controlled by controlling the power of the microwave plasma generator 8 and adjusting the temperature of the gas in the circulating inlet gas temperature inlet pipeline 1 through the circulating unit 11, and the vacuum degree in the deposition cavity 3 is adjusted through the vacuum adjusting device.

The preparation method has simple process, meets the requirement of industrial preparation production, can obtain equal growth opportunities and growth conditions in all directions by suspending the diamond seed crystal 5 in the plasma deposition cavity and controllably rotating under the blowing of gas in the process of preparing the large-particle diamond, can obtain large-size single crystal diamond by the balanced growth of crystals in three-dimensional directions, and has high preparation efficiency and good quality of the prepared diamond.

The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.