CN105921076A - Preparation method for green artificial diamond - Google Patents
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- CN105921076A CN105921076A CN201610386904.1A CN201610386904A CN105921076A CN 105921076 A CN105921076 A CN 105921076A CN 201610386904 A CN201610386904 A CN 201610386904A CN 105921076 A CN105921076 A CN 105921076A
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- 239000010432 diamond Substances 0.000 title claims abstract description 96
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 62
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 51
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims abstract description 41
- 230000003197 catalytic effect Effects 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000010941 cobalt Substances 0.000 claims abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 32
- 239000011572 manganese Substances 0.000 claims description 20
- 229910052748 manganese Inorganic materials 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 150000002739 metals Chemical class 0.000 claims description 7
- 238000009692 water atomization Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 238000010306 acid treatment Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 68
- 239000013078 crystal Substances 0.000 abstract description 40
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 34
- 239000000654 additive Substances 0.000 abstract description 22
- 230000000996 additive effect Effects 0.000 abstract description 21
- 239000012535 impurity Substances 0.000 abstract description 20
- 238000005303 weighing Methods 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- -1 manganese metal nitride Chemical class 0.000 abstract 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 20
- 239000002245 particle Substances 0.000 description 14
- 235000013339 cereals Nutrition 0.000 description 12
- 239000008187 granular material Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 7
- 241000233855 Orchidaceae Species 0.000 description 6
- 238000000889 atomisation Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910020056 Mg3N2 Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 230000002411 adverse Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910000531 Co alloy Inorganic materials 0.000 description 1
- 229910002555 FeNi Inorganic materials 0.000 description 1
- 229910005800 NiMnCo Inorganic materials 0.000 description 1
- RBVYPNHAAJQXIW-UHFFFAOYSA-N azanylidynemanganese Chemical compound [N].[Mn] RBVYPNHAAJQXIW-UHFFFAOYSA-N 0.000 description 1
- 150000001540 azides Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical group [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
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Abstract
The invention discloses a preparation method for a green artificial diamond. The method comprises the following steps: A, preparation of catalytic alloy powder: weighing manganese, cobalt and nickel to prepare the catalytic alloy powder; B, preparation of modified graphite powder: weighting and uniformly mixing graphite powder and manganese metal nitride powder to obtain the modified graphite powder; C, preparation of a synthesis column: weighing the catalytic alloy powder and the modified graphite powder to obtain the synthesis column; D, synthesis of the diamond: performing synthesis to implement synthesis of the green artificial diamond according to a high-temperature and high-pressure method; E, subsequent treatment: treating the converted synthesis column, washing insoluble matters to neutral with clear water, and performing drying to obtain the green artificial diamond. The method is easy, simple and convenient to operate, safe and low in cost, a crystal is high in integrity and nitrogen content and uniform in granularity, the defect that in the prior art, other impurities are inevitably entrained into an additive is overcome, and the negative influence of the impurities on diamond synthesis is avoided.
Description
Technical field
The present invention relates to diamond synthesis field, be more particularly to the preparation method of a kind of green man-made diamond.
Background technology
Diamond, also known as diamond, the mineral being made up of carbon, is the allotrope of carbon.Diamond is material the hardest during find on earth at present numerous naturally occur, the purposes of diamond widely, such as: the cutting tool in artware, industry.
Research finds, why diamond has different colors, and it is primarily due in diamond contain what a certain amount of impurity element caused, and some impurity element can also change some performance of diamond simultaneously.Among numerous impurity elements, nitrogen is topmost impurity element in diamond, and the physical property such as diamond mechanics, optics, calorifics and electricity all can change because of the existence of nitrogen impurity.Therefore, according to the existence form in lattice of the nitrogen impurity in diamond, generally diamond is divided into four types: I a, I b, II a and II b.Wherein, I type diamond nitrogen content is high, and II type nitrogen content is low.Common naturally colorless diamond broadly falls into -a-type mostly, and nitrogen element forms tetrahedral geometry assemble with the gathering of atom pair form or four nitrogen-atoms and a room, and nitrogen content is at about 2000ppm.And the diamond of industrial synthesis is belonging to I b type mostly, nitrogen element exists with single substitution atoms form, and along with the increase of nitrogen content, the color of diamond is revealed as colourless-light yellow-yellow-buff-light green color-green-bottle green-blackish green the most successively, its nitrogen content of common carbonado is at about 300ppm, for light yellow, yellow or buff.In nature, the green diamond naturally occurred is the most rare, and price is colourless more more expensive than common, and therefore people always strive to synthesize this green diamond.
In prior art, the synthesis of synthetic green diamond being also carried out certain research, such as, prior art (CN101224399A, publication date: on July 23rd, 2008) discloses the preparation method of green man-made diamond, and it is to be added with Mg3N2Graphite be raw material, make catalyst with FeNi or NiMnCo alloy, prepare green diamond, nitrogen content 1000-2000ppm at high temperature under high pressure.
The most such as prior art (CN101224400A, publication date: on July 23rd, 2008) also discloses that a kind of method preparing green diamond, and its method is similar with CN101224399A, and simply the additive in graphite is Li3N, nitrogen content 1000-2000ppm.
Simultaneously, prior art (" the High Temperature High Pressure synthesis of high nitrogen-containing Tabular gem-grade diamond " Jia Xiaopeng, Journal of Atomic and Molecular Physics, 26(4): 720-724, on April 20th, 2009) in also disclose that the preparation method of a kind of green high nitrogen Tabular gem-grade diamond, method is similar with above two, but additive is then Na3N。
Same, prior art (" the High Temperature High Pressure synthesis of high nitrogen carbonado ", in moist, Jilin University's Master's thesis, 2008) also discloses that the preparation method of a kind of bottle green high nitrogen-containing carbonado, and its additive is then Ba (N3)2, nitrogen content reaches as high as 2550ppm.
But, in the preparation method of existing green man-made diamond, all additives also exist the problem unavoidably bringing corresponding impurity element into, as added Mg3N2Mg impurity element, Li can be brought into3N can bring Li impurity element, Na into3N can bring Na impurity element, Ba (N into3)2Can bring Ba impurity element into, these impurity elements there is no benefit to diamond synthesizing, and except Mg3N2Outside, when other several nitride, azide industrially scales use, production cost is high, clashes into and easily explodes, there is certain potential safety hazard.
Summary of the invention
It is an object of the invention to there are provided the preparation method of a kind of green man-made diamond, easy to implement the method, easy and simple to handle, safe and with low cost, crystal perfection degree height, homogeneous grain diameter, nitrogen content are high, will not bring other impurity element into, solve additive in prior art and have to bring into the drawback of other impurity elements in the course of reaction of diamond is prepared in catalysis, avoiding the impurity element adverse effect to diamond synthesizing, the green diamond quality produced is more preferably.
In order to realize above-mentioned purpose, the present invention by the following technical solutions:
The preparation method of a kind of green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weight percent, weigh manganese (Mn) 24% ~ 26%, cobalt (Co) 4% ~ 6%, nickel (Ni) 68% ~ 72% respectively, above-mentioned three kinds of metals are prepared as catalytic alloy powder by the water atomization complete set of equipments preparation that then employing Handan orchid moral powder by atomization equipment company limited produces, and are the green man-made diamond synthesis catalytic alloy powder used by the present invention.
B, the preparation of modified graphite powder: weigh graphite powder (natural high purity graphite powder respectively, the weight/mass percentage composition more than 99.95% of carbon, purchase on market) and nitrogenization manganese metal powder (additive), graphite powder and nitrogenization manganese metal powder are graphite powder according to percentage by weight: nitrogenization manganese metal powder=1:0.005 ~ 0.025, ratio be sufficiently mixed, for green man-made diamond synthesis modified graphite powder after mix homogeneously.
C, the preparation of synthesis post: weigh catalytic alloy powder and modified graphite powder respectively, green man-made diamond synthesis catalytic alloy powder and modified graphite divide mass ratio to be catalytic alloy powder: modified graphite powder=(0.3-0.5): the ratio of 1, after being sufficiently mixed, again by the method (" research of the iron-based powder catalyst diamond synthesis mechanism of action " of compression molding, Zhao Wendong, Beijing Non-Ferrous Metal Research General Academy's thesis for the doctorate, 2010) become synthesis post.
D, the synthesis of diamond: use high temperature and high pressure method (" mixing synthesis and the research of diamond in S system under High Temperature High Pressure ", Chen Xiaozhou, Institutes Of Technology Of He'nan's Master's thesis, 2009) synthesize, the auxiliary that will synthesize post and corresponding synthesis carries out synthesis conversion on cubic hinge press, increasing temperature and pressure is for being warming up to 1550-2000K, and is forced into 4.0-5.0GPa, and the time of heat-insulation pressure keeping is 1-3min；Secondary pressurized the most again, secondary pressurized pressure is 5.5-6.0GPa, and the time of secondary heat-insulation pressure keeping is 15-20min, completes the synthesis of green man-made diamond.
E, subsequent treatment: use 10# mixed acid solution to process on the synthesis post after having converted.After acid treatment, insoluble matter use clear water washing the most neutral, at 105 DEG C of drying green man-made diamonds.
In the present invention, wherein Mn is added by two parts, and the overwhelming majority is added in ni mn co alloy mode, and trace adds with Mn simple substance form in nitrogenization manganese metal.
In the present invention, how much can the ratio that nitrogenization manganese metal powder be selected to account for raw material composition as additive and nitrogenization manganese metal powder be the key that form high-quality green man-made diamond.
The purity of described raw material Ni, Mn, Co is more than 99.9%.
Described nitrogenization manganese metal be middle nitrogen content be 8%-11%, Fe content is 89% ~ 92%.
Described catalyst is powder catalyst.
Described catalyst, the particle diameter of nitrogenization manganese metal are less than 45 μm (i.e. granule mesh number is more than 325 mesh).
By to the selection of catalyst particle diameter used and adjustment, so that catalyst of the present invention can preferably contact with metallic combination raw material, and making reaction fully to carry out.Meanwhile, select powder additive that additive can be made to be more fully mixed in graphite.
In the present invention, by catalyst and the further of raw graphite consumption are adjusted and optimize, so that raw material can fully react, also will not waste catalyst and additive simultaneously, reduce reaction cost.
In the present invention, by to the adjustment of the initial reaction conditions such as increasing temperature and pressure and optimization, thus further increase the efficiency of reaction, and make raw material be capable of preliminary conversion completely, adjusting further and optimizing by the further reaction condition to pressurization, thus further increase the efficiency of final catalytic conversion reaction.
Compared with prior art, the invention have the benefit that
(1) catalyst of the present invention will not bring other impurity element in the course of reaction prepare diamond in catalysis, thus solve the additive that in prior art, manufacture green man-made diamond uses and have to bring into the drawback of other impurity elements, avoiding the impurity element adverse effect to diamond synthesizing, the green diamond quality produced is more preferably.
(2) additive provided by the present invention is more safer than existing additive and with low cost in safety.
(3) green man-made diamond of the present invention is to be prepared by the inventive method, has that product diamond crystal formation is intact, inclusion enclave is few, crystal perfection degree height, homogeneous grain diameter, nitrogen content advantages of higher.
The diamond of gained is carried out range estimation detection, found that green man-made diamond crystal is good, structural integrity, transparency is good.The granularity peak value of crystal mainly at-40/+45(i.e. crystal particle diameter less than 40 mesh and more than 45 mesh) and-45/+50(i.e. crystal particle diameter less than 45 mesh and more than 50 mesh) between, the ratio of both grit diamond crystal can reach more than the 80% of diamond crystal sum, and nitrogen content is between 1350ppm ~ 2400ppm.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, it will be appreciated by those skilled in the art that the following example is merely to illustrate the present invention, and are not construed as limiting the scope of the present invention.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument unreceipted production firm person, being can be by the commercially available conventional products bought and obtain.
Embodiment
1
:
The preparation method of a kind of green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weight percent, Mn 24%, Co 4%, Ni 72%, weighing raw material Mn, Co, Ni that purity is 99.9%, above-mentioned three kinds of metals are prepared as catalytic alloy powder by the water atomization complete set of equipments preparation that then employing Handan orchid moral powder by atomization equipment company limited produces.Use ocular estimate to observe catalytic alloy powder out prepared by this formula to find, prepared catalyst grains size is the most uniform, can be by the ratio of the granule (i.e. grain diameter is less than 45 μm) of 325 eye mesh screens up to more than the 85% of obtained catalyst total amount, selecting granule is the catalytic alloy powder used by embodiment 1 less than 45 μm.
B, the preparation of modified graphite powder: additive nitrogenization manganese metal is sieved that (in nitrogenization manganese metal, nitrogen mass content is 8%, the content of residue manganese is 92%), and according to the graphite powder that graphite powder and nitrogenization manganese metal flour additive agent weight ratio are 1:0.005 and nitrogenization manganese metal powder, mix homogeneously, is the green man-made diamond synthesis modified graphite powder used by the present invention.
C, the preparation of synthesis post: weigh catalytic alloy powder and modified graphite powder according to catalytic alloy powder and modified graphite powder weight ratio 1:2, after being sufficiently mixed, then become synthesis post by the method for compression molding.
D, synthesis: use high temperature and high pressure method to synthesize, the auxiliary that will synthesize post and corresponding synthesis carries out synthesis conversion on cubic hinge press, increasing temperature and pressure is for being warming up to 1550 or 1650 or 180 or 1900 or-2000K, and it being forced into 4.0 or 4.5 or 5.0GPa, the time of heat-insulation pressure keeping is 1 or 2 or 3min；Secondary pressurized the most again, secondary pressurized pressure is 5.5 or 5.8 or 6.0GPa, and the time of secondary heat-insulation pressure keeping is 15 or 18 or 20min, completes the synthesis of green man-made diamond.
E, subsequent treatment: use 10# mixed acid solution to process on the synthesis post after having converted.After acid treatment, insoluble matter uses clear water washing to neutral, and dries (temperature is 105 DEG C) and i.e. obtain green man-made diamond.
The diamond of embodiment 1 is carried out range estimation detection, found that the green man-made diamond crystal transparency obtained by embodiment 1 is good, inclusion enclave is few, structural integrity.The granularity peak value of crystal mainly at-40/+45(i.e. crystal particle diameter less than 40 mesh and more than 45 mesh) and-45/+50(i.e. crystal particle diameter less than 45 mesh and more than 50 mesh) between, the ratio of both grit diamond crystal can reach the 83% of diamond crystal sum, testing its nitrogen content, its nitrogen content is 1400ppm.
Embodiment
2
:
The preparation method of a kind of green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weight percent, Mn 26%, Co 6%, Ni 68%, weighing Mn, Co, Ni that purity is 99.9%, above-mentioned three kinds of metals are prepared as catalytic alloy powder by the water atomization complete set of equipments preparation that then employing Handan orchid moral powder by atomization equipment company limited produces.Use ocular estimate to observe catalytic alloy powder out prepared by this formula to find, prepared catalyst grains size is the most uniform, the granule catalytic alloy powder used by embodiment 2 less than 45 μm can be selected by the ratio of the granule (i.e. grain diameter is less than 45 μm) of 325 eye mesh screens up to more than the 85% of obtained catalyst total amount.
C, the preparation of synthesis post: weigh catalytic alloy powder and modified graphite powder according to modified graphite powder weight ratio 3:10 of catalytic alloy powder Yu nitrogen manganese powder, after being sufficiently mixed, then become synthesis post by the method for compression molding.
It is same as in Example 1 that other implements step.
The diamond of embodiment 2 is carried out range estimation detection, found that the green man-made diamond quartz crystal transparency obtained by embodiment 2 is good, inclusion enclave is few, structural integrity.The granularity peak value of crystal mainly at-40/+45(i.e. crystal particle diameter less than 40 mesh and more than 45 mesh) and-45/+50(i.e. crystal particle diameter less than 45 mesh and more than 50 mesh) between, the ratio of both grit diamond crystal can reach the 85% of diamond crystal sum, testing its nitrogen content, its nitrogen content is 1350ppm.
Embodiment
3
:
The preparation method of a kind of green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weight percent, Mn 24%, Co 6%, Ni 70%, weighing Mn, Co, Ni that purity is 99.9%, above-mentioned three kinds of metals are prepared as catalytic alloy powder by the water atomization complete set of equipments preparation that then employing Handan orchid moral powder by atomization equipment company limited produces.Use ocular estimate to observe catalytic alloy powder out prepared by this formula to find, prepared catalyst grains size is the most uniform, the granule catalytic alloy powder used by embodiment 3 less than 45 μm can be selected by the ratio of the granule (i.e. grain diameter is less than 45 μm) of 325 eye mesh screens up to more than the 85% of obtained catalyst total amount.
B, the preparation of modified graphite powder: additive nitrogenization manganese metal is sieved (in nitrogenization manganese metal, nitrogen mass content is 8%, and the content of residue manganese is 92%).According to the graphite powder that graphite powder and nitrogenization manganese metal additive weight ratio are 1:0.025 and nitrogenization manganese metal powder, mix homogeneously, it is the green man-made diamond synthesis modified graphite powder used by the present invention.
It is same as in Example 1 that other implements step.
The diamond of embodiment 3 is carried out range estimation detection, found that the green man-made diamond quartz crystal transparency obtained by embodiment 3 is good, inclusion enclave is few, structural integrity.The granularity peak value of crystal mainly at-40/+45(i.e. crystal particle diameter less than 40 mesh and more than 45 mesh) and-45/+50(i.e. crystal particle diameter less than 45 mesh and more than 50 mesh) between, the ratio of both grit diamond crystal can reach the 86% of diamond crystal sum, testing its nitrogen content, its nitrogen content is 2100ppm.
Embodiment
4
:
The preparation method of a kind of green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weight percent, Mn 25%, Co 5%, Ni 70%, weighing Mn, Co, Ni that purity is 99.9%, above-mentioned three kinds of metals are prepared as catalytic alloy powder by the water atomization complete set of equipments preparation that then employing Handan orchid moral powder by atomization equipment company limited produces.Use ocular estimate to observe catalytic alloy powder out prepared by this formula to find, prepared catalyst grains size is the most uniform, the granule catalytic alloy powder used by embodiment 4 less than 45 μm can be selected by the ratio of the granule (i.e. grain diameter is less than 45 μm) of 325 eye mesh screens up to more than the 85% of obtained catalyst total amount.
B, the preparation of modified graphite powder: additive nitrogenization manganese metal is sieved that (in nitrogenization manganese metal, nitrogen mass content is 11%, the content of residue manganese is 89%), and according to the graphite powder that graphite powder and nitrogenization manganese metal additive weight ratio are 1:0.025 and nitrogenization manganese metal powder, mix homogeneously, is the green man-made diamond synthesis modified graphite powder used by the present invention.
It is same as in Example 1 that other implements step.
The diamond of embodiment 4 is carried out range estimation detection, found that the green man-made diamond crystal transparency obtained by embodiment 4 is good, inclusion enclave is few, structural integrity.The granularity peak value of crystal mainly at-40/+45(i.e. crystal particle diameter less than 40 mesh and more than 45 mesh) and-45/+50(i.e. crystal particle diameter less than 45 mesh and more than 50 mesh) between, the ratio of both grit diamond crystal can reach the 88% of diamond crystal sum, testing its nitrogen content, its nitrogen content is 2400ppm.
Embodiment
5
:
The preparation method of a kind of green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weight percent, Mn 26%, Co 6%, Ni 68%, weighing Mn, Co, Ni that purity is 99.9%, above-mentioned three kinds of metals are prepared as catalytic alloy powder by the water atomization complete set of equipments preparation that then employing Handan orchid moral powder by atomization equipment company limited produces.Use ocular estimate to observe catalytic alloy powder out prepared by this formula to find, prepared catalyst grains size is the most uniform, the granule catalytic alloy powder used by embodiment 5 less than 45 μm can be selected by the ratio of the granule (i.e. grain diameter is less than 45 μm) of 325 eye mesh screens up to more than the 85% of obtained catalyst total amount.
B, the preparation of modified graphite powder: additive nitrogenization manganese metal is sieved that (in nitrogenization manganese metal, nitrogen mass content is 11%, the content of residue manganese is 89%), and according to the graphite powder that graphite powder and nitrogenization manganese metal flour additive agent weight ratio are 1:0.025 and nitrogenization manganese metal powder, mix homogeneously, is the green man-made diamond synthesis modified graphite powder used by the present invention.
C, the preparation of synthesis post: weigh catalytic alloy powder and modified graphite powder according to catalytic alloy powder and modified graphite powder weight ratio 3:10, after being sufficiently mixed, then become synthesis post by the method for compression molding.
It is same as in Example 1 that other implements step.
The diamond of embodiment 5 is carried out range estimation detection, found that the green man-made diamond crystal transparency obtained by embodiment 5 is good, inclusion enclave is few, structural integrity.The granularity peak value of crystal mainly at-40/+45(i.e. crystal particle diameter less than 40 mesh and more than 45 mesh) and-45/+50(i.e. crystal particle diameter less than 45 mesh and more than 50 mesh) between, the ratio of both grit diamond crystal can reach the 83% of diamond crystal sum, testing its nitrogen content, its nitrogen content is 2000ppm.
Although illustrate and describing the present invention with specific embodiment, however it will be appreciated that may be made that without departing from the spirit and scope of the present invention many other change and amendment.It is, therefore, intended that include all such changes and modifications belonging in the scope of the invention in the following claims.
Claims (1)
1. a preparation method for green man-made diamond, the steps include:
A, prepare catalytic alloy powder: weigh manganese 24% ~ 26%, cobalt 4% ~ 6%, nickel 68% ~ 72% respectively, use the preparation of water atomization complete set of equipments above-mentioned three kinds of metals to be prepared as catalytic alloy powder, for green man-made diamond synthesis catalytic alloy powder；
B, the preparation of modified graphite powder: weigh graphite powder and nitrogenization manganese metal powder respectively, graphite powder mixes according to the ratio that percentage by weight is 1:0.005 ~ 0.025 with nitrogenization manganese metal powder, for green man-made diamond synthesis modified graphite powder after mix homogeneously；
C, the preparation of synthesis post: weigh catalytic alloy powder and modified graphite powder respectively, after the ratio that green man-made diamond synthesis catalytic alloy powder divides mass ratio to be 0.3-0.5:1 with modified graphite mixes, then become synthesis post by the method for compression molding；
D, the synthesis of diamond: use high temperature and high pressure method to synthesize, the auxiliary of synthesis post and corresponding synthesis is carried out on cubic hinge press synthesis convert, increasing temperature and pressure is for being warming up to 1550-2000K, and is forced into 4.0-5.0GPa, and the time of heat-insulation pressure keeping is 1-3min；Secondary pressurized the most again, secondary pressurized pressure is 5.5-6.0GPa, and the time of secondary heat-insulation pressure keeping is 15-20min, completes the synthesis of green man-made diamond；
E, subsequent treatment: use 10# mixed acid solution to process on the synthesis post after having converted, after acid treatment, use clear water washing the most neutral, at 105 DEG C of drying green man-made diamonds by insoluble matter.
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| CN201610386904.1A CN105921076A (en) | 2016-06-03 | 2016-06-03 | Preparation method for green artificial diamond |
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| CN201610386904.1A CN105921076A (en) | 2016-06-03 | 2016-06-03 | Preparation method for green artificial diamond |
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| CN201610386904.1A Pending CN105921076A (en) | 2016-06-03 | 2016-06-03 | Preparation method for green artificial diamond |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591943A (en) * | 2016-12-30 | 2017-04-26 | 郑州沃德超硬材料有限公司 | Boron-containing diamond and preparation method and application thereof |
| CN107324329A (en) * | 2017-08-10 | 2017-11-07 | 中南钻石有限公司 | A kind of preparation method of colorless diamond synthesis raw material stem |
| CN113797852A (en) * | 2021-10-20 | 2021-12-17 | 中南钻石有限公司 | Process for synthesizing colorless diamond by constant temperature method |
| CN114433124A (en) * | 2022-01-24 | 2022-05-06 | 辽宁新瑞碳材料科技有限公司 | Preparation method of high-temperature alloy catalyst for producing artificial diamond |
| CN115400691A (en) * | 2022-08-24 | 2022-11-29 | 内蒙古唐合科技有限公司 | Preparation method of artificial diamond |
| CN115634622A (en) * | 2022-09-15 | 2023-01-24 | 内蒙古唐合科技有限公司 | Synthesis process of high-grade artificial diamond |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52134889A (en) * | 1976-05-06 | 1977-11-11 | Sumitomo Electric Ind Ltd | Production of sintered material of diamond |
| EP0476352A1 (en) * | 1990-08-30 | 1992-03-25 | Hughes Tool Company | Earth boring drill bit with improved wear inserts |
| CN101224400A (en) * | 2007-10-11 | 2008-07-23 | 中国科学院长春光学精密机械与物理研究所 | A kind of method for preparing green diamond |
| CN101224399A (en) * | 2007-10-11 | 2008-07-23 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of green synthetic diamond |
| CN102580618A (en) * | 2012-01-13 | 2012-07-18 | 河南省联合磨料磨具有限公司 | Protogenic diamond fine particle for precisio machining and production method thereof |
-
2016
- 2016-06-03 CN CN201610386904.1A patent/CN105921076A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52134889A (en) * | 1976-05-06 | 1977-11-11 | Sumitomo Electric Ind Ltd | Production of sintered material of diamond |
| EP0476352A1 (en) * | 1990-08-30 | 1992-03-25 | Hughes Tool Company | Earth boring drill bit with improved wear inserts |
| CN101224400A (en) * | 2007-10-11 | 2008-07-23 | 中国科学院长春光学精密机械与物理研究所 | A kind of method for preparing green diamond |
| CN101224399A (en) * | 2007-10-11 | 2008-07-23 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of green synthetic diamond |
| CN102580618A (en) * | 2012-01-13 | 2012-07-18 | 河南省联合磨料磨具有限公司 | Protogenic diamond fine particle for precisio machining and production method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 张曙光等: "气雾化Ni-Mn-Co合金粉末触媒制备及其合成金刚石特性", 《粉末冶金技术》 * |
| 梁中翥等: "用含添加剂氮化物MxN的粉末触媒合成金刚石", 《金刚石与磨料磨具工程》 * |
| 沃凌鹏: "某些含氮化合物对合成的影响和在熔体中金刚石由溶体结晶的机理", 《磨料磨具与磨削》 * |
| 贾晓鹏: "高氮含量宝石级金刚石单晶的高温高压合成", 《原子与分子物理学报》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106591943A (en) * | 2016-12-30 | 2017-04-26 | 郑州沃德超硬材料有限公司 | Boron-containing diamond and preparation method and application thereof |
| CN106591943B (en) * | 2016-12-30 | 2019-03-26 | 郑州沃德超硬材料有限公司 | Boric diamond and its preparation method and application |
| CN107324329A (en) * | 2017-08-10 | 2017-11-07 | 中南钻石有限公司 | A kind of preparation method of colorless diamond synthesis raw material stem |
| CN107324329B (en) * | 2017-08-10 | 2019-03-29 | 中南钻石有限公司 | A kind of colorless diamond synthesis preparation method of raw material stem |
| CN113797852A (en) * | 2021-10-20 | 2021-12-17 | 中南钻石有限公司 | Process for synthesizing colorless diamond by constant temperature method |
| CN113797852B (en) * | 2021-10-20 | 2024-04-09 | 中南钻石有限公司 | Process for synthesizing colorless diamond by constant temperature method |
| CN114433124A (en) * | 2022-01-24 | 2022-05-06 | 辽宁新瑞碳材料科技有限公司 | Preparation method of high-temperature alloy catalyst for producing artificial diamond |
| CN115400691A (en) * | 2022-08-24 | 2022-11-29 | 内蒙古唐合科技有限公司 | Preparation method of artificial diamond |
| CN115400691B (en) * | 2022-08-24 | 2024-05-10 | 内蒙古唐合科技有限公司 | Method for preparing artificial diamond |
| CN115634622A (en) * | 2022-09-15 | 2023-01-24 | 内蒙古唐合科技有限公司 | Synthesis process of high-grade artificial diamond |
| CN115634622B (en) * | 2022-09-15 | 2024-02-06 | 内蒙古唐合科技有限公司 | Synthesis process of high-grade artificial diamond |
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