CN102583362A - Method for manually prefabricating large-particle diamond by using recrystallization method - Google Patents
Method for manually prefabricating large-particle diamond by using recrystallization method Download PDFInfo
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- CN102583362A CN102583362A CN2012100725115A CN201210072511A CN102583362A CN 102583362 A CN102583362 A CN 102583362A CN 2012100725115 A CN2012100725115 A CN 2012100725115A CN 201210072511 A CN201210072511 A CN 201210072511A CN 102583362 A CN102583362 A CN 102583362A
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Abstract
The invention discloses a method for manually prefabricating large-particle diamond by using a recrystallization method, which comprises (1) adopting pyrophyllite to manufacture a rectangular pyrophyllite cup with a cylindrical cavity; (2) horizontally placing a first accelerant alloy metal sheet at the bottom of the pyrophyllite cup and horizontally laying a carbon nano tube powder layer; (3) adopting filling hoppers to lay a carbon nano tube powder gridding layer on the carbon nano tube powder layer and alternately laying a small-particle artificially-synthesized diamond single crystalline layer in the gridding; (4) continuously laying a carbon nano tube powder layer; (5) horizontally placing the accelerant alloy metal sheet; (6) placing a cylindrical electrode; (7) enabling the pyrophyllite cup with materials laid well to be placed in a press machine for electrification and pressurization; and (8) taking out and washing pyrophyllite, removing the metal sheet and residual carbon nano tube, and finally obtaining the large-particle diamond. The method solves the problem that the existing method for synthesizing the large-particle diamond in the world at present is disorder in method, high in cost, low in efficiency and inaccurate in technical direction.
Description
Technical field
The invention belongs to crystal recrystallize and molecular material and learn field, particularly a kind of method of making bulky diamond with recrystallize legal person worker.
Background technology
Technology with graphite artificially synthesizing diamond under HTHP is very ripe, and is widely used in industrial scale production.But; The particle of artificially synthesizing diamond is little at present, and the field of application is very limited, is the application of industry basically; Particularly manual work can't other bulky diamond of synthesis of natural jewel level; This major cause is that adamantine crystallization condition is harsh, poor growth, and people also do not find the technique means of recrystallize.
Therefore; For the rare situation of other bulky diamond of natural gemstone level on the our times; For solving the our times economic problems; Open up the world economy new growth point significant opportunity is provided, provide a kind of and make other bulky diamond method of jewel level, become the technical problem that this area needs to be resolved hurrily at present with recrystallize legal person worker.
Summary of the invention
The purpose of this invention is to provide the method that a kind of recrystallize legal person worker makes bulky diamond; The method that has solved synthetic in the world bulky diamond existence at present through the synthetic bulky diamond is mixed and disorderly; Cost is high, and efficient is extremely low, the inaccurate problems of technique direction.
Technical scheme of the present invention realizes through following technical proposals.
Recrystallize legal person worker makes the method for bulky diamond, and this method comprises the steps:
1) taking agalmatolite is that material is processed a rectangular parallelepiped, and the rectangular parallelepiped inner chamber is a right cylinder, constitutes an agalmatolite cup thus;
2) horizontal positioned first catalyst alloy belongs to thin slice at the bottom of the agalmatolite cup, and then level is laid one deck first carbon nanotube powder layer;
3) in step 2) take to fill funnel on the first carbon nanotube powder layer and lay the carbon nanotube powder clathrum that constitutes by carbon nanotube powder and the small-particle artificially synthesizing diamond single crystalline layer of alternate laying in this grid;
4) in step 3) carbon nanotube powder clathrum, continue on the small-particle artificially synthesizing diamond single crystalline layer of alternate laying to lay one deck second carbon nanotube powder layer, this second carbon nanotube powder layer contacts with the carbon nanotube powder clathrum;
5) horizontal positioned second catalyst alloy belongs to thin slice then;
6) belong at second catalyst alloy and place cylindrical electrode on the thin slice, whole agalmatolite cup is laid and is accomplished;
7) put the agalmatolite cup of the good above-mentioned materials of lay the interior energising of into 6 * 800 tons of man-made diamond six top surfaces of CS-1 type pressure machine and be forced into 5～7GPa, 1200 ℃～2000 ℃ temperature, continue 10～15 minutes;
8) take out the agalmatolite cup that process is processed, with commercially available hydrofluoric acid flush away agalmatolite, electrolytic process is removed sheet metal, removes the residual carbon nanotube with commercially available permanganic acid, finally obtains bulky diamond.
Further aspect of the present invention is:
The length of said rectangular parallelepiped agalmatolite cup * wide * height=4cm * 4cm * 6cm, the cylinder diameter of rectangular parallelepiped inner chamber are 3cm, the high 5cm of being, agalmatolite cup bottom thickness is 1cm.
It is that 3cm, thickness are 0.1cm that said first catalyst alloy belongs to the diameter that thin slice and second catalyst alloy belong to thin slice.
The said first carbon nanotube powder layer and the second carbon nanotube powder layer thickness are 0.5cm.
Said cylindrical electrode diameter is 3cm, and height is 2cm.
The single crystal diameter of said small-particle man-made diamond is 0.1～1mm.
Said carbon nanotube powder is the multi-walled carbon nano-tubes black powder.
Saidly take to fill that funnel is laid the grid that is made up of the multi-walled carbon nano-tubes black powder and the artificially synthesizing diamond single crystalline layer method of alternate laying is:
The cylindrical shell height that uses sheet iron to make a cylindrical structure is 2cm, and in the cylindrical shell cavity, adopts sheet iron to make the funnel along the vertical up/down perforation of right cylinder cylindrical shell, and the cross section of this funnel is latticed, and the length of grid * wide is 0.5cm * 0.4cm; And the grid grid is the perforation layer in 0.1～0.15cm gap; Said multi-walled carbon nano-tubes black powder is filled along the grid grid, after the artificially synthesizing diamond monocrystalline is filled along grid, vertically slowly takes out and fills funnel, and weighting material is just natural under action of gravity to be laid according to design requirements.
The present invention puts together the small-particle diamond of large-scale industrial production at present, through HTHP recrystallize method once more, just can obtain the bulky diamond crystal, and its quality can reach the level of other diamond crystal of natural gemstone level fully.
The each side effect that the present invention can reach is extremely remarkable.At first, diamond crystal has very high use value and wealth symbol as " blank " of the jewelry diamond of rare Industrial materials and costliness.Make a breakthrough if the artificially synthesizing diamond crystal reaches the level of natural gemstone rank diamond crystal, will become the current world economy new growth point, will drive a large amount of employment and related industries development, promote progress of human society.Secondly, the present invention has taked the method for the recrystallize that natural diamond forms, and has utilized " the crystallization inertia " of crystal recrystallize, for the theoretical developments of Materials science plays important pushing effect.
Description of drawings
Fig. 1 is the agalmatolite cup schematic appearance that is used for the synthetic bulky diamond;
Fig. 2 is small-particle diamond of the present invention and carbon nanotube powder packing layer distribution schematic diagram;
Fig. 3 is a filling carbon nano-pipe powder funnel grid sections synoptic diagram of the present invention.
Among the figure: 1, first catalyst alloy belongs to thin slice; 2, the first carbon nanotube powder layer; 3, carbon nanotube powder clathrum; 4, artificially synthesizing diamond single crystalline layer; 5, the second carbon nanotube powder layer; 6, second catalyst alloy belongs to thin slice; 7, cylindrical electrode; A is the multi-walled carbon nano-tubes grid grid of being made by sheet iron; B is the filling funnel grid of being made by sheet iron, is used to fill the small-particle diamond single crystal.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Like Fig. 1, shown in Figure 2, recrystallize legal person worker of the present invention makes the method for bulky diamond, comprises the steps:
1) taking agalmatolite is the rectangular parallelepiped that material is processed a long * wide * height=4cm * 4cm * 6cm, and the rectangular parallelepiped inner chamber is the right cylinder of a diameter 3cm, high 5cm, constitutes an agalmatolite cup thus, and agalmatolite cup bottom thickness is 1cm;
2) horizontal positioned diameter 3cm, the first circular catalyst alloy of thickness 0.1cm belong to thin slice 1 at the bottom of the agalmatolite cup, and then level is laid the first carbon nanotube powder layer 2 of a layer thickness 0.5cm, and this carbon nanotube powder is taked the multi-walled carbon nano-tubes black powder;
3) in step 2) take to fill that funnel is laid the carbon nanotube powder clathrum 3 that is made up of the multi-walled carbon nano-tubes black powder and the diameter of alternate laying in this grid is 0.1～1 on the first carbon nanotube powder layer 2
MmArtificially synthesizing diamond single crystalline layer 4;
Lay the first carbon nanotube powder layer 2 and lay carbon nanotube powder clathrum 3 and will use " professional funnel " (seeing filling funnel shown in Figure 3); " professional funnel " is to make with sheet iron; The cylindrical shell that is made into a cylindrical structure is high to be 2cm, and in the cylindrical shell cavity, adopts sheet iron to make the funnel along the vertical up/down perforation of right cylinder cylindrical shell, and the cross section of this funnel is latticed; The length of grid * wide is 0.5cm * 0.4cm, sees shown in Fig. 3 arrow B; And the grid grid is the perforation layer in 0.1～0.15cm gap, sees shown in Fig. 3 arrow A; Filling funnel with above-mentioned cylindrical tube structure after having laid 2 layers on carbon nanotube powder layer is inserted in along in the agalmatolite cup; Shown in accompanying drawing 3; The multi-walled carbon nano-tubes black powder is filled along the multi-walled carbon nano-tubes grid grid A that is made by sheet iron, and diameter is 0.1～1
MmThe artificially synthesizing diamond monocrystalline fill along the filling funnel grid B that makes by sheet iron, fill finish after, vertical slowly the taking-up filled funnel; Weighting material just natural laying according to design requirements under action of gravity finishes.
4) in the carbon nanotube powder clathrum 3 that step 3) is made up of the multi-walled carbon nano-tubes black powder, continuing on the artificially synthesizing diamond single crystalline layer 4 of alternate laying to lay a layer thickness is the second carbon nanotube powder layer 5 of 0.5cm, and this second carbon nanotube powder layer 5 contacts with carbon nanotube powder clathrum 3; This carbon nanotube powder is taked the multi-walled carbon nano-tubes black powder;
5) the horizontal positioned diameter is that 3cm, thickness are that the second circular catalyst alloy of 0.1cm belongs to thin slice 6 then;
6) second catalyst alloy in circle belongs to the cylindrical electrode 7 of placing diameter 3cm, high 2cm on the thin slice 6, and whole agalmatolite cup is laid and accomplished;
7) put the agalmatolite cup of the good above-mentioned materials of lay the interior energising of into 6 * 800 tons of man-made diamond six top surfaces of CS-1 type pressure machine and be forced into 5～7GPa, 1200 ℃～2000 ℃ temperature;
According to the characteristics of diamond recrystallize required time, such energising pressurization must keep 10 to 15 minutes, then naturally cooling.In pressurized, heated and refrigerative process, the atom of carbon nanotube can carry out orderly combination and arrangement according to the structure of diamond atom;
Under HTHP, small-particle diamond atomic structure is arranged main body and is not changed, and still, " edge is active " of its atomic arrangement strengthens.Because it is that lattice can be consistent in order that there is " inertia " in crystal structure.To form macrobead according to a definite sequence " voluntarily " recrystallize between each small-particle diamond at interval; " the broken atomic structure " that perhaps, formed by HTHP through carbon nanotube carried out recrystallize as certain " bridge tie " and formed macrobead; Thereby produce macrobead man-made diamond crystal; The produced man-made diamond crystalline particle of this method can reach 1～20 carat, even crystalline particle is bigger.
8) take out the agalmatolite cup that process is processed; With commercially available hydrofluoric acid flush away agalmatolite; Electrolytic process removes that first catalyst alloy belongs to thin slice 1 and second catalyst alloy belongs to thin slice 6, removes the residual carbon nanotube with commercially available permanganic acid, finally obtains the bulky diamond that overall target reaches natural grades; After simple cutting, each particulate weight is at 1 carat～20 carats.
If want synthetic colour diamond crystal, so, the nano material of adding respective element is followed the prescribed rules and is got final product.
The above; Be merely the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field is in the technical scope that the present invention discloses; The variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (8)
1. recrystallize legal person worker makes the method for bulky diamond, it is characterized in that, this method comprises the steps:
1) taking agalmatolite is that material is processed a rectangular parallelepiped, and the rectangular parallelepiped inner chamber is a right cylinder, constitutes an agalmatolite cup thus;
2) horizontal positioned first catalyst alloy belongs to thin slice at the bottom of the agalmatolite cup, and then level is laid one deck first carbon nanotube powder layer;
3) in step 2) take to fill funnel on the first carbon nanotube powder layer and lay the carbon nanotube powder clathrum that constitutes by carbon nanotube powder and the small-particle artificially synthesizing diamond single crystalline layer of alternate laying in this grid;
4) in step 3) carbon nanotube powder clathrum, continue on the small-particle artificially synthesizing diamond single crystalline layer of alternate laying to lay one deck second carbon nanotube powder layer, this second carbon nanotube powder layer contacts with the carbon nanotube powder clathrum;
5) horizontal positioned second catalyst alloy belongs to thin slice then;
6) belong at second catalyst alloy and place cylindrical electrode on the thin slice, whole agalmatolite cup is laid and is accomplished;
7) put the agalmatolite cup of the good above-mentioned materials of lay the interior energising of into 6 * 800 tons of man-made diamond six top surfaces of CS-1 type pressure machine and be forced into 5～7GPa, 1200 ℃～2000 ℃ temperature, continue 10～15 minutes;
8) take out the agalmatolite cup that process is processed, with commercially available hydrofluoric acid flush away agalmatolite, electrolytic process is removed sheet metal, removes the residual carbon nanotube with commercially available permanganic acid, finally obtains bulky diamond.
2. a kind of recrystallize legal person worker according to claim 1 makes the method for bulky diamond; It is characterized in that; The length of said rectangular parallelepiped agalmatolite cup * wide * height=4cm * 4cm * 6cm, the cylinder diameter of rectangular parallelepiped inner chamber are 3cm, the high 5cm of being, agalmatolite cup bottom thickness is 1cm.
3. a kind of recrystallize legal person worker according to claim 1 makes the method for bulky diamond, it is characterized in that, it is that 3cm, thickness are 0.1cm that said first catalyst alloy belongs to the diameter that thin slice and second catalyst alloy belong to thin slice.
4. make the method for bulky diamond according to claim 1 or 3 described a kind of recrystallize legal person workers, it is characterized in that the said first carbon nanotube powder layer and the second carbon nanotube powder layer thickness are 0.5cm.
5. make the method for bulky diamond according to claim 1 or 3 described a kind of recrystallize legal person workers, it is characterized in that said cylindrical electrode diameter is 3cm, height is 2cm.
6. make the method for bulky diamond according to claim 1 or 3 described a kind of recrystallize legal person workers, it is characterized in that the single crystal diameter of said small-particle man-made diamond is 0.1～1mm.
7. a kind of recrystallize legal person worker according to claim 1 makes the method for bulky diamond, it is characterized in that, said carbon nanotube powder is the multi-walled carbon nano-tubes black powder.
8. make the method for bulky diamond according to claim 1 or 3 described a kind of recrystallize legal person workers; It is characterized in that, saidly take to fill that funnel is laid the grid that is made up of the multi-walled carbon nano-tubes black powder and the artificially synthesizing diamond single crystalline layer method of alternate laying is:
The cylindrical shell height that uses sheet iron to make a cylindrical structure is 2cm, and in the cylindrical shell cavity, adopts sheet iron to make the funnel along the vertical up/down perforation of right cylinder cylindrical shell, and the cross section of this funnel is latticed, and the length of grid * wide is 0.5cm * 0.4cm; And the grid grid is the perforation layer in 0.1～0.15cm gap; Said multi-walled carbon nano-tubes black powder is filled along the grid grid, after the artificially synthesizing diamond monocrystalline is filled along grid, vertically slowly takes out and fills funnel, and weighting material is just natural under action of gravity to be laid according to design requirements.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104064A (en) * | 1986-06-14 | 1987-12-23 | 中国科学院物理研究所 | A kind of composite sintered polycrystalline diamond with inclusion and its production and use |
| JP3128807B2 (en) * | 1990-07-17 | 2001-01-29 | 石川島播磨重工業株式会社 | Method for producing diamond particles |
| CN1511783A (en) * | 2002-12-30 | 2004-07-14 | 韩光泰 | Method for synthesizing artificial diamond |
| CN1654321A (en) * | 2004-12-22 | 2005-08-17 | 哈尔滨工业大学 | Method fro directly synthesizing diamond by sintering nanometer carbon tube under low-pressure |
| CN101327927A (en) * | 2008-07-11 | 2008-12-24 | 武汉大学 | Method for synthesizing diamond with carbon nanofiber |
| CN102268619A (en) * | 2011-06-03 | 2011-12-07 | 中南大学 | Preparation method of carbon-nanotube-reinforced polycrystalline diamond compact (PDC) material |
-
2012
- 2012-03-19 CN CN2012100725115A patent/CN102583362B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104064A (en) * | 1986-06-14 | 1987-12-23 | 中国科学院物理研究所 | A kind of composite sintered polycrystalline diamond with inclusion and its production and use |
| JP3128807B2 (en) * | 1990-07-17 | 2001-01-29 | 石川島播磨重工業株式会社 | Method for producing diamond particles |
| CN1511783A (en) * | 2002-12-30 | 2004-07-14 | 韩光泰 | Method for synthesizing artificial diamond |
| CN1654321A (en) * | 2004-12-22 | 2005-08-17 | 哈尔滨工业大学 | Method fro directly synthesizing diamond by sintering nanometer carbon tube under low-pressure |
| CN101327927A (en) * | 2008-07-11 | 2008-12-24 | 武汉大学 | Method for synthesizing diamond with carbon nanofiber |
| CN102268619A (en) * | 2011-06-03 | 2011-12-07 | 中南大学 | Preparation method of carbon-nanotube-reinforced polycrystalline diamond compact (PDC) material |
Non-Patent Citations (1)
| Title |
|---|
| 曹立民等: "高温高压下碳纳米管的相转变及金刚石的合成", 《高压物理学报》, vol. 14, no. 1, 31 March 2000 (2000-03-31), pages 33 - 36 * |
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Address after: 364000 No. 40 Heping Road, Xinluo District, Fujian, Longyan Patentee after: Li Haiyun Address before: 710075 3F, 58, three hi tech Development Zone, West hi tech Development Zone, Shaanxi, Xi'an Patentee before: Li Haiyun |
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Granted publication date: 20130612 Termination date: 20210319 |