CN107268078A - A kind of artificial synthesis of Gem Grade colorless diamond - Google Patents
A kind of artificial synthesis of Gem Grade colorless diamond Download PDFInfo
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- CN107268078A CN107268078A CN201710478166.8A CN201710478166A CN107268078A CN 107268078 A CN107268078 A CN 107268078A CN 201710478166 A CN201710478166 A CN 201710478166A CN 107268078 A CN107268078 A CN 107268078A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/12—Single-crystal growth directly from the solid state by pressure treatment during the growth
Abstract
The invention discloses a kind of artificial synthesis of Gem Grade colorless diamond, this method is compressed to diamond growth layer first with Fe Base Metals catalyst, high purity graphite, trace element；By diamond growth layer and denitrogenate metal level with different arrangement modes be placed on high-purity magnesium oxide cup in formed synthesizing post；Heating carbon pipe, pressure transmission salt pipe, composite pyrophyllite are set gradually outside synthesizing post, and sets heating carbon plate and conducting metal circle to be combined as synthesizing block at two ends；Synthesizing block is placed in high temperature press operation 24~300 hours under the conditions of 1300~1500 DEG C, 5.5~6.5GPa after passing through vacuum drying treatment, and colorless diamond is made in HTHP synthesis.Rational in infrastructure used in this method, preparation manipulation is simple, cost is low, and gained colorless diamond crystal formation is completely consistent, epigranular, pure color, high conversion rate, can effectively solve existing colorless diamond synthesis cycle length, the problem such as output capacity is low, uniformity is poor.
Description
Technical field
Changed colour technical field the present invention relates to artificial lens synthesis and crystal, more particularly to a kind of Gem Grade colorless diamond
Artificial synthesis.
Technical background
Colorless diamond is II a (nitrogen content) type diamond, and electronics, space flight, laser are widely used in its unique performance
The fields such as transmitter, Diamond Jewelry, with combination properties such as excellent light, electricity, thermal conductivities, are with a wide range of applications；It is existing
Known colorless diamond is mainly derived from rough diamond ore deposit, and the formation of rough diamond needs more than one hundred million years, and yield is rare, and price is held high
Expensive, long-term exploitation can then cause the exhaustion of rough diamond resource, and cost is high.Therefore it is badly in need of the research of artificial synthetic diamond
With development.
At present, the method for artificial synthetic diamond has been studied, and its method is main based on CVD and temperature differential method, but temperature differential method
Because carbon source by the temperature difference is influenceed the skewness in catalyst, therefore cause carbon atom that inside and outside diamond receives in growth not
Equilibrium, therefore crystal formation differs；And CVD, due to being influenceed by its growing principle, carbon atom deposit thickness is partially thin, more based on sheet.
And one or less several can only be synthesized using above method single, synthesis cycle is longer, and cost is higher and crystal formation is difficult
Control.Uniformity is poor, greatly limit the development and application of artificial synthesized colorless diamond.Application No. 201610683882.5
A kind of people of " Synthetic block and its synthetic method of artificial synthesized jewellery colorless diamond " disclosure of the invention described in patent of invention
The Synthetic block and its synthetic method of work synthesis jewellery colorless diamond, its Synthetic block include the empty block of pyrophyllite and are disposed therein the heart
Multi-layered osmotic structure stem, the stem includes the dolomite being cascading by the empty block first end of pyrophyllite to the second end
Piece, carbon source, catalyst sheet, Cu paper tinsels and catalyst sheet composite bed and brilliant bed.This method passes through overlapped way based on temperature differential method principle
Carbon atom is set to be deposited at high temperature by catalyst layer on brilliant bed and realize and grow, this method is due to by structure and growing principle
Limitation, growing space is limited, and single synthesis yield is not high, and synthesis granule size is influenceed larger by catalyst layer thickness, therefore
It is difficult to the synthesis of megadiamond and high yield.
Based on this, for the rare situation of current Gem Grade colorless diamond, for the artificial diamond of exploitation high yield, high-quality
Synthetic method, as field technical problem urgently to be resolved hurrily at present.
The content of the invention
In order to solve the above problems, the invention provides a kind of artificial synthesis of Gem Grade colorless diamond.This method
Design synthetic cavity structure, different diamond growths layer separated with denitrogenating metal level and carries out beneficial combination, it is ensured that high-quality without
The growth of color diamond crystal, reduces growth and interfering for changing colour, while by process and technology controlling and process, realizing Gao Pin
The long-time synthesising stability of level diamond, substantially increases gem-quality crystal output capacity.
The present invention is achieved by the following technical solutions
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take Fe Base Metals catalyst, high purity graphite and trace element through three-dimensional ball milling mixing, isostatic pressed, granulate, be suppressed into
Cylindric diamond growth layer, by obtained cylindric diamond growth layer by after high vacuum reduction treatment, being naturally cooling to room
Temperature, Vacuum Package is standby；The vacuum of high vacuum described in the step is 2.0~8.0 × 10-3pa；
(2) preparation of synthesizing post：
High-purity magnesium oxide cup is taken, the diamond growth layer for denitrogenating metal level and step (1) preparation is put into high-purity magnesium oxide
In cup, obtaining synthesizing post, (wherein synthesizing post is：Diamond growth layer is placed in a high-purity magnesium oxide cup and is denitrogenated
After metal level, another identical high-purity magnesium oxide cup is fastened with opening direction)；
(3) preparation of synthesizing block：
Heating carbon pipe, pressure transmission salt pipe and composite leaf wax stone block are set gradually in the synthesizing post periphery described in step (2),
Its upper end sets heating carbon plate and conducting metal circle, lower end to be also equipped with heating carbon plate and conducting metal circle, heating carbon plate and hair
Hot carbon pipe is connected, forming closed heater；Described pressure transmission salt pipe is concordant with the height for the carbon pipe that generates heat, composite pyrophyllite and two
The conductive plug at end is concordant；Combinations thereof obtains synthesizing block after completing；
(4) processing of colorless diamond Synthetic block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum 22~35min it
Temperature in interior, drying box is by room temperature to maximum temperature；When dry the temperature inside the box rises to maximum temperature by room temperature, keep
Temperature 5min, is then passed through pressure of the argon gas into vacuum drying chamber for 0.02-0.03Mpa, then into vacuum drying chamber
Heat-insulation pressure keeping 4~6 hours under this condition, applying argon gas are to normal pressure when insulation end is cooled to less than 50 degree, and synthesizing block goes out
Baking oven, carries out high temperature press synthesis；
(5) synthesis of colorless diamond Synthetic block：
Synthesizing block after step (4) described processing is put into high temperature press and synthesized, 1300~1500
DEG C, run 24~300 hours under the conditions of 5.5~6.5GPa, synthesized under HTHP and colorless diamond be made；
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle after electrolysis, purification processes.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, the three-dimensional ball milling described in step (1) is mixed into be mixed at room temperature
Close 12~18 hours；Described hydrostatic pressure is 240~300MPa, and it is the spherical of 4-6mm that particle diameter is obtained after the granulation
Particle；Reduction temperature of the cylindric diamond growth layer in high vacuum reduction process is 750~980 DEG C, vacuum is
2.0-8.0×10-3The pa recovery times are 24~48 hours.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, the composition and matter of the Fe Base Metal catalyst described in step (1)
Measure percentage composition as follows：Fe：50~70%, Ni：25~50%, Co：0~20%, the granularity of the metal solvent is 2~50 μm；
High purity graphite described in step (1) is the native graphite or Delanium that granularity is 2~40 μm, wherein the purity of graphite >=
99.99%；Minor metallic element described in step (1) for any of Al, Cu, Ti and Zr or appoint it is several, wherein Al, Cu,
Ti and Zr purity is >=99.9%；In diamond growth layer during the minor metallic element addition diamond growth layer, after addition
In every kind of element shared weight/mass percentage composition is Al respectively：0.05~1.5%, Cu：0.5~3%, Ti：0.06~3.0%,
Zr：0.05~1.0%；The weight that Fe metal solvents, high purity graphite and minor metallic element mixing described in the step are added
Than for (50~90)：(50~10)：(0.05~1).
The artificial synthesis of above-mentioned Gem Grade colorless diamond, described in step (2) denitrogenate metal level for Al, Cu, Ti and
Any of Zr or appoint it is several, described metal Al, Cu, Ti and Zr purity are all higher than 99%；Described metal level of denitrogenating is
It is stamped to form by the metal tape containing above-mentioned metal ingredient, what punching press was obtained denitrogenates metal level by 30~60min of ultrasonic cleaning, then
Carry out alkali oil removal treatment, the then vacuum drying under the conditions of 200 DEG C, and be naturally cooling to be used after room temperature；Step (4) institute
Maximum temperature in the vacuum drying chamber stated is 180~200 DEG C, i.e., be first heated to by room temperature after 180~200 DEG C, keep this most
High-temperature 5min, then applying argon gas.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, the synthesizing post described in step (2) is opened together comprising two
The high-purity magnesium oxide cup of mouth direction fastening and the synthesizing layer that setting is arranged under the overlay in the high-purity magnesium oxide cup of fastening, institute
The synthesizing layer stated is comprising the diamond growth layer for carrying out cross-superimposed arrangement in parallel and denitrogenates metal level (wherein in oxygen
Change the first layer placed in magnesium cup be diamond growth layer, upper layer to denitrogenate metal level, then upper layer be diamond growth layer,
Again upwards to denitrogenate metal level, so cross-superimposed horizontal parallel arrangement), described diamond growth layer and denitrogenate metal level and be
Cylinder and diameter are consistent, as shown in Figure 1 and Figure 2.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, the thickness of step (2) diamond growth layer for 5~
10mm, the thickness for denitrogenating metal level is 0.5~4mm.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, step (2) the synthesizing post includes two same openings
High-purity magnesium oxide cup and the integrative-structure being arranged in high-purity magnesium oxide glass that direction is fastened, described integrative-structure is by diamond
Grown layer and cup-shaped are denitrogenated metal layer combination and formed, and described cup-shaped denitrogenates the periphery that metal level bag is located at diamond growth layer, such as
Shown in Fig. 3, Fig. 4, Fig. 5.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, integrative-structure described in step (2) by diamond growth layer and
Cup-shaped denitrogenates the diamond growth layer that metal layer combination is formed and diamond growth layer is placed for two superpositions, and described cup-shaped is denitrogenated
Metal level bag is also equipped with denitrogenating metal level (described between the periphery of two diamond growths layer and two diamond growths layers
Metal level diameter of denitrogenating between two diamond growth layers and two diamond growth layers is consistent), such as Fig. 3, Fig. 4, Fig. 6 institute
Show.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, the thickness of step (2) diamond growth layer for 5~
25mm, the thickness of denitrogenating metal level of the bag located at diamond growth layer periphery is 0.5~4mm, described to be arranged at two diamonds
The thickness for denitrogenating metal level between grown layer is 0.5~3.5mm.
The artificial synthesis of above-mentioned Gem Grade colorless diamond, step (5) the colorless diamond Synthetic block is in high temperature press
In synthesis technique comprise the following steps：
A. pressure change process is：When starting synthetic work, pressure boosts to 55~60MPa in 50s~60s by 0MPa,
Then 60~80min is kept under the pressure condition；Keep after completing, pressure is boosted in 25s~30s by 55~60MPa
65~70MPa, and holding 1000s~1800s under the pressure condition；Keep after completing, pressure 25s~30s by 65~
70MPa boosts to 80~85MPa, after boosting is completed, then in 24~300 hours pressure boost to 95 by 80~85MPa~
100MPa；
B. temperature changing process is：Start synthetic work when, temperature 9min~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is risen in 110s~120s by 1000~1050 DEG C
Temperature keeps 2000s~3000s at such a temperature to 1300~1350 DEG C；After the completion of holding, temperature is in 20s~30s by 1300
~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 24~300 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of synthesizing block；Control pressure curve and control temperature curve such as Fig. 7 during this
It is shown.
In the preparation process of above-mentioned Gem Grade colorless diamond, the high-purity magnesium oxide cup described in step (2) is using conventional
Method prepares gained, using the magnesia of purity >=99.8%, is made after being handled 12-24 hours under 1100 DEG C of high temperature after compacting
；Two identical magnesia cups are prepared, after diamond growth layer is placed with denitrogenating metal level, two magnesia cups are with same
Opening direction fastens the diamond growth rod structure described in composition；
Pressure transmission salt pipe described in step (3) is to prepare gained using conventional method, is existed using the NaCl of purity >=99.6%
It is made after being toasted 10-12 hours under the conditions of 300 DEG C.
Compared with prior art, the present invention has following positive beneficial effect：
(1) present invention is in the preparation process of diamond growth layer, by the diamond growth being pressed into layer using low temperature long-time
Reduce, while being protected with high vacuum, the entrance of initial nitrogen is effectively controlled, in the starting stage without using denitrogenating examination
Agent and operation can reach removing nitrogen, the effect except color, and the synthesis of colorless diamond is improved under conditions of operation is simplified
Quality；
(2) present invention is except nitrogen layer and grown layer are using mixing, superposition and cladding multiple combinations method, can be to synthesis during
The nitrogen of generation is fully absorbed, and prevents nitrogen in diamond growth from participating in, so as to realize the uniform excellent of colorless diamond
Matter is synthesized；
(3) in the structure of synthesizing post of the present invention and synthesis post diamond growth layer with denitrogenating the combination of metal level
Mode, can be achieved the three-dimension type growth of diamond, bores raw growing space and greatly improves, single yield, up to 80--150ct, is current
8~10 times of colorless diamond method therefor yield are prepared in the prior art；
(4) synthetic cavity structure of the present invention, periphery set temperature in multi-layer heat preserving and pressure transfer, synthetic cavity,
Pressure uniformity, synthesizing diamond crystal formation concordance rate is up to more than 80%；It ensure that the long-time synthesis of high grade diamond is steady simultaneously
It is qualitative, provide powerful guarantee for the synthesis of megadiamond；
(5) synthesizing block of the present invention is heated using baking oven first before HTHP synthesis and is passed through argon
Gas, it is therefore prevented that the entrance of extraneous nitrogen, effectively reduces influence of the nitrogen to synthesizing diamond, i.e., synthesizes it in synthesizing block
Before avoid influence of the nitrogen for diamond color, further increase the synthesis quality of diamond；
(6) material used in preparation process of the present invention is easy to make, and simple for structure, year-on-year temperature differential method eliminates crystalline substance
The APPENDIX MATERIALSThes such as bed, insulation sheet, while expanding the contact area except nitrogen layer and grown layer, denitrogenate efficiency raising, monolithic is integrated
Cost declines more than 30%；
(7) colorless diamond synthesized using method of the present invention, crystal formation is consistent, pure color, crystal water white transparency,
Rough diamond can be substituted completely, with the stronger market advantage.
Brief description of the drawings
Fig. 1 is one of structural representation of synthesizing block,
Fig. 2 is the diamond growth layer described in Fig. 1 and denitrogenates metal level schematic diagram,
The meaning that symbol is represented in figure is：1 represents conducting metal circle, and 2 represent carbon fever tablet, and 3 represent high-purity magnesium oxide cup,
4 represent heating carbon pipe, and 5 represent pressure transmission salt pipe, and 6 represent composite pyrophyllite, and 7 represent to denitrogenate metal level, and 8 represent diamond growth layer；
Fig. 3 is the two of the structural representation of synthesizing block,
Fig. 4 is the synthesizing post schematic diagram in the synthesizing block described in Fig. 3,
Fig. 5 be Fig. 3 described in synthesizing block in diamond growth layer with denitrogenate metal level arrangement mode schematic diagram it
One,
Fig. 6 be Fig. 3 described in synthesizing block in diamond growth layer with denitrogenate metal level arrangement mode schematic diagram it
Two,
The meaning that symbol is represented in figure is：1 represents conducting metal circle, and 2 represent carbon fever tablet, and 3 represent high-purity magnesium oxide cup,
4 represent heating carbon pipe, and 5 represent pressure transmission salt pipe, and 6 represent composite pyrophyllite, and 10 represent synthesizing post, and 11 represent diamond growth
Layer, 12 expression cup-shapeds denitrogenate metal level；
Fig. 7 is the schematic diagram of control pressure curve and temperature curve in synthesizing block building-up process；
One of colorless diamond sample drawing that Fig. 8-1 is prepared for the present invention；
The two of the colorless diamond sample drawing that Fig. 8-2 is prepared for the present invention；
The three of the colorless diamond sample drawing that Fig. 8-3 is prepared for the present invention.
Embodiment
The present invention is described in more details below by embodiment, but is not intended to limit the invention
Protection domain.
Embodiment 1
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take the Fe Base Metal catalyst Fe that granularity is 10~50 μm65Ni30Co5, granularity be 5~40 μm of native graphite (purity
>=99.99%) and trace element Cu (purity >=99.9%) according to mass ratio be 50:50:0.5 ratio is mixed, so
Above-mentioned compound is added afterwards and mixed at room temperature 12 hours in three-dimensional material mixer, isostatic pressed 240Mpa is carried out, (particle diameter is 4 for granulation
~6mm), it is 10mm, a diameter of 40mm cylindric diamond growth layer to be pressed into thickness；After the completion of compacting, by the diamond of preparation
Grown layer high vacuum reductase 12 4 hours under conditions of temperature is 850 DEG C, reduction is naturally cooling to room temperature, Ran Houzhen after completing
Sky encapsulation is standby；
(2) preparation of synthesizing post：
1. prepares high-purity magnesium oxide cup using conventional method, using the magnesia of purity >=99.8%, 1100 after compacting
Processing is made after 12 hours under DEG C high temperature, prepares two thickness and is 2.0mm, is highly 24mm high-purity magnesium oxide cup；
2. the Ti alloy sheets that takes purity to be 99.9%, which are washed into disk and denitrogenate metal level, (denitrogenates metal level diameter and diamond
Grown layer diameter is consistent, denitrogenate the thickness of metal level for 1mm)；With being cleaned by ultrasonic 30min and carrying out alkali oil removal treatment, handle
After under the conditions of 200 DEG C vacuum drying, be then naturally cooling to room temperature and obtain and step (1) diamond growth layer diameter one
What is caused denitrogenates metal level；
3. the metal that the obtained diamond growth layer and step (2) for preparing step (1) are 2. prepared is except nitrogen layer is put into step
(2) in the high-purity magnesium oxide cup 1. prepared, one layer of diamond growth layer and then this layer of diamond are first placed at a magnesia cup cup bottom
Grown layer is placed above one layer and denitrogenates metal level, places diamond growth layer again, i.e. diamond growth layer removes nitrogen layer with parallel with metal
Mode carry out it is cross-superimposed be placed in high-purity magnesium oxide cup in, as shown in Figure 2；Laying is reached after setting height 44mm, is detained
Another upper high-purity magnesium oxide cup obtains synthesizing post into closing insulated column；
(3) preparation of synthesizing block：
The synthesizing post periphery prepared in step (2) sets gradually heating carbon pipe, pressure transmission salt pipe and is combined from inside to outside
Pyrophillite, and the conducting steel ring that the heating carbon plate that thickness is 1.5mm and height are 10mm is respectively placed in upper and lower ends, wherein
Heating carbon plate is connected to form closed heater with heating carbon pipe, and concordant with the height of carbon heat-generating pipe, the compound leaf of pressure transmission salt pipe is cured
Stone is concordant with two ends conductive plug, obtains synthesizing block, as shown in Figure 1 and Figure 2；
(4) processing of synthesizing block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then the temperature in drying box 22~
By room temperature to 180 DEG C in 25min；When temperature rises to 180 DEG C, temperature 5min is kept, then into vacuum drying chamber
It is 0.02-0.03Mpa to be passed through pressure in argon gas to vacuum drying chamber, then heat-insulation pressure keeping 4 hours under this condition, keeps knot
Less than 50 degree and applying argon gas are cooled to after beam to normal pressure, the synthesizing block after processing goes out baking oven, carry out high temperature press conjunction
Into；
(5) synthesis technique of synthesizing block：
Synthesizing block of the step (4) after handled is placed on synthetic gem level nothing in high temperature press (cavity is 40)
Color diamond block, concrete technology step is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55 by 0MPa in 55s~60s~
60MPa, then keeps 60~80min under the pressure condition；Keep after completing, pressure in 25s~30s by 55~
60MPa boosts to 65~70MPa, and 1000~1800s of holding under the pressure condition；Keep complete after, pressure 25s~
80~85MPa is boosted to by 65~70MPa in 30s, after boosting is completed, then in 95~97 hours pressure by 80~85MPa
Boost to 95~100MPa；
B. temperature changing process is：Start synthetic work when, temperature in 9~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C
1300~1350 DEG C are warming up to, and keeps 2000~3000s at such a temperature；After the completion of holding, temperature in 20~30s by
1300~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 96 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of colorless diamond；
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle, such as through electrolysis, purification processes after the completion of processing
Fig. 8-1, Fig. 8-2, shown in Fig. 8-3.
The synthetic effect of the present embodiment, per unit area yield 75ct, granularmetric composition is as shown in the table, note：(1ct=100 points)
| Granularity | <9 points | 9-19 points | 20-39 points | 40-59 points | 60-79 points | >79 points |
| Content % | 3.5% | 16% | 43.5% | 23% | 10% | 4% |
Color：E, F, cleanliness：SI1、VS
Embodiment 2
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take the Fe Base Metal catalyst Fe that granularity is 2~40 μm65Ni30Co5, granularity for 2~40 μm high purity graphite (purity >=
99.99%) and trace element Cu (purity >=99.9%) according to mass ratio be 70:30:1 ratio is mixed, and then will
Above-mentioned compound is added in three-dimensional material mixer and mixed 12 hours under normal temperature, carry out isostatic pressed 240Mpa, granulation (particle diameter is 4~
6mm), it is 8mm, a diameter of 40mm cylindric diamond growth layer to be pressed into thickness；After the completion of compacting, by the diamond growth of preparation
Layer high vacuum reductase 12 4 hour under conditions of temperature is 800 DEG C, reduction is naturally cooling to room temperature after completing, then vacuum seal
Equipment is used；
(2) preparation of synthesizing post：
1. prepares high-purity magnesium oxide cup using conventional method, using the magnesia of purity >=99.8%, 1100 after compacting
Processing is made after 12 hours under DEG C high temperature, prepares two thickness and is 2.0mm, is highly 24.5mm high-purity magnesium oxide cup；
2. the Ti alloy sheets that takes purity to be 99.9%, which are washed into disk and denitrogenate metal level, (denitrogenates metal level diameter and diamond
Grown layer diameter is consistent, denitrogenate the thickness of metal level for 1mm)；With being cleaned by ultrasonic 30min and carrying out alkali oil removal treatment, handle
After under the conditions of 200 DEG C vacuum drying, be then naturally cooling to room temperature and obtain and step (1) diamond growth layer diameter one
What is caused denitrogenates metal level；
3. the metal that the obtained diamond growth layer and step (2) for preparing step (1) are 2. prepared is except nitrogen layer is put into step
(2) in the high-purity magnesium oxide cup 1. prepared, one layer of diamond growth layer and then this layer of diamond are first placed at a magnesia cup cup bottom
Grown layer is placed above layer of metal and removes nitrogen layer, places diamond growth layer again, i.e. diamond growth layer removes nitrogen layer with parallel with metal
Mode carry out it is cross-superimposed be placed in high-purity magnesium oxide cup in, as shown in Figure 2；Laying is reached after setting height 45mm, is detained
Another upper magnesia cup obtains synthesizing post into closing insulated column；
(3) preparation of synthesizing block：
The synthesizing post periphery prepared in step (2) sets gradually heating carbon pipe, pressure transmission salt pipe and is combined from inside to outside
Pyrophillite, and the conducting steel ring that the heating carbon plate that thickness is 1.5mm and height are 10mm is respectively placed in upper and lower ends, wherein
Heating carbon plate is connected to form closed heater with heating carbon pipe, and concordant with the height of carbon heat-generating pipe, the compound leaf of pressure transmission salt pipe is cured
Stone is concordant with two ends conductive plug, obtains synthesizing block, as shown in Figure 1 and Figure 2；
(4) processing of synthesizing block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum in drying box
Temperature is in 32~35min by room temperature to 200 DEG C；When temperature rises to 200 DEG C, temperature 5min is kept, then to true
It is 0.02-0.03Mpa that pressure is passed through in argon gas to case in empty drying box, then heat-insulation pressure keeping 4 hours under this condition, keeps knot
Shu Hou, is cooled to less than 50 degree and applying argon gas to normal pressure, and the synthesizing block after processing goes out baking oven, carries out high temperature press conjunction
Into；
(5) synthesis technique of synthesizing block：
Synthesizing block of the step (4) after handled is placed on synthetic gem level nothing in high temperature press (cavity is 40)
Color diamond block, concrete technology step is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55 by 0MPa in 55s~60s~
60MPa, then keeps 60~80min under the pressure condition；Keep after completing, pressure in 25s~30s by 55~
60MPa boosts to 65~70MPa, and 1000~1800s of holding under the pressure condition；Keep complete after, pressure 25s~
80~85MPa is boosted to by 65~70MPa in 30s, after boosting is completed, then in 99~101 hours pressure by 80~85MPa
Boost to 95~100MPa；
B. temperature changing process is：Start synthetic work when, temperature in 9~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C
1300~1350 DEG C are warming up to, and keeps 2000~3000s at such a temperature；After the completion of holding, temperature in 20~30s by
1300~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 100 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of colorless diamond；
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle, such as through electrolysis, purification processes after the completion of processing
Fig. 8-1, Fig. 8-2, shown in Fig. 8-3.
The synthetic effect of the present embodiment, per unit area yield 83ct, granularmetric composition is as shown in the table, note：(1ct=100 points)
| Granularity | <9 points | 9-19 points | 20-39 points | 40-59 points | 60-79 points | >79 points |
| Content % | 2.5% | 13% | 41% | 22% | 17% | 4.5% |
Color：F, G, cleanliness：SI1、VS
Embodiment 3
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take the Fe Base Metal catalyst Fe that granularity is 2~50 μm70Ni29Co1, granularity for 2~40 μm native graphite (purity >=
99.99%) and microelement Ti (purity >=99.9%) according to mass ratio be 50:50:0.5 ratio is mixed, then
Above-mentioned compound is added and mixed at room temperature 16 hours in three-dimensional material mixer, carry out isostatic pressed 300Mpa, granulation (particle diameter is 4~
6mm), it is 25mm, a diameter of 35mm cylindric diamond growth layer to be pressed into height；After the completion of compacting, the diamond of preparation is given birth to
Long layer high vacuum under conditions of temperature is 900 DEG C is reduced 30 hours, and reduction is naturally cooling to room temperature after completing, then vacuum
Encapsulation is standby；
(2) preparation of synthesizing post：
1. prepares high-purity magnesium oxide cup using conventional method, using the magnesia of purity >=99.8%, 1100 after compacting
Processing is made after 12 hours under DEG C high temperature, prepares two thickness and is 1.5mm, is highly 15mm high-purity magnesium oxide
Cup；
2. the Ti alloy sheets that takes purity to be 99.9% are washed into wall thickness and are 1.0mm, are highly 13.5mm cup-shaped and denitrogenate
(external diameter that cup-shaped denitrogenates metal level is consistent with the internal diameter of high-purity magnesium oxide cup, and cup-shaped denitrogenates the internal diameter of metal level for metal level two
It is consistent with the diameter of diamond growth layer)；Then with being cleaned by ultrasonic 60min and carrying out alkali oil removal treatment, at 200 DEG C after the completion of processing
Under the conditions of vacuum drying, be then naturally cooling to room temperature and obtain cup-shaped to denitrogenate metal level, as shown in Figure 4, Figure 5；
3. the cup-shaped that the obtained diamond growth layer and step (2) for preparing step (1) are 2. prepared is denitrogenated metal level and is put into
In high-purity magnesium oxide that step (2) is 1. prepared cup, wherein diamond growth layer is first placed on the cup-shaped of make-up and denitrogenates in metal level (two
Individual cup-shaped is denitrogenated metal level and fastened with opening direction) and then cup-shaped is denitrogenated into metal level be put into high-purity magnesium oxide cup, such as
Shown in Fig. 3, Fig. 4, Fig. 5；Another high-purity magnesium oxide cup is buckled into closing insulated column, that is, obtains synthesizing post；
(3) preparation of synthesizing block：
The synthesizing post periphery prepared in step (2) sets gradually heating carbon pipe, pressure transmission salt pipe and is combined from inside to outside
Pyrophillite, and the conducting steel ring that the heating carbon plate that thickness is 1.5mm and height are 13mm is respectively placed in upper and lower ends, wherein
Heating carbon plate is connected to form closed heater with heating carbon pipe, and concordant with the height of carbon heat-generating pipe, the compound leaf of pressure transmission salt pipe is cured
Stone is concordant with two ends conductive plug, obtains synthesizing block, as shown in Figure 3；
(4) processing of synthesizing block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum in drying box
Temperature is in 32~35min by room temperature to 200 DEG C；When temperature rises to 200 DEG C, temperature 5min is kept, then to true
It is 0.02-0.03Mpa that pressure in argon gas to case is passed through in empty drying box, and heat-insulation pressure keeping 6 hours, keep terminating under this condition
Afterwards, less than 50 degree, applying argon gas to normal pressure are cooled to, the synthesizing block after processing goes out baking oven, carry out high temperature press synthesis；
(5) synthesis technique of synthesizing block：
Synthesizing block after step (4) described processing is placed on synthetic gem level colorless diamond in high temperature press,
Concrete technology step is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55 by 0MPa in 55s~60s~
60MPa, then keeps 60~80min under the pressure condition；Keep after completing, pressure in 25s~30s by 55~
60MPa boosts to 65~70MPa, and 1000~1800s of holding under the pressure condition；Keep complete after, pressure 25s~
80~85MPa is boosted to by 65~70MPa in 30s, after boosting is completed, then in 119~121 hours pressure by 80~
85MPa boosts to 95~100MPa；
B. temperature changing process is：Start synthetic work when, temperature in 9~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C
1300~1350 DEG C are warming up to, and keeps 2000~3000s at such a temperature；After the completion of holding, temperature in 20~30s by
1300~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 120 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of colorless diamond.
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle, such as through electrolysis, purification processes after the completion of processing
Fig. 8-1, Fig. 8-2, shown in Fig. 8-3.
The synthetic effect of the present embodiment, per unit area yield 70ct, granularmetric composition is as shown in the table, note：(1ct=100 points)
| Granularity | <9 points | 9-19 points | 20-39 points | 40-59 points | 60-79 points | >79 points |
| Content % | 4% | 17.5% | 45% | 21% | 10% | 2.5% |
Color：E, F, cleanliness：SI1、VS
Embodiment 4
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take the Fe Base Metal catalyst Fe that granularity is 2~50 μm70Ni29Co1, granularity for 2~40 μm native graphite (purity >=
99.99%) and microelement Ti (purity >=99.9%) according to mass ratio be 70:30:1.0 ratio is mixed, then
Above-mentioned compound is added in three-dimensional material mixer and mixed 12 hours, isostatic pressed 300Mpa, granulation (particle diameter is 4~6mm), pressure is carried out
It is 30mm, a diameter of 35mm cylindric diamond growth layer that height, which is made,；After the completion of compacting, by the diamond growth layer of preparation in temperature
Spend and reduced 30 hours for high vacuum under conditions of 850 DEG C, reduction is naturally cooling to room temperature after completing, and then Vacuum Package is standby
With；
(2) preparation of synthesizing post：
1. prepares high-purity magnesium oxide cup using conventional method, using the magnesia of purity >=99.8%, 1100 after compacting
Processing is made after 12 hours under DEG C high temperature, prepares two thickness and is 1.5mm, is highly 17mm high-purity magnesium oxide
Cup；
2. the Ti alloy sheets that takes purity to be 99.9% are washed into wall thickness and are 0.5mm, are highly 15.5mm cup-shaped and denitrogenate
(external diameter that cup-shaped denitrogenates metal level is consistent with the internal diameter of high-purity magnesium oxide cup, and cup-shaped denitrogenates the internal diameter of metal level for metal level two
It is consistent with the diameter of diamond growth layer)；Then with being cleaned by ultrasonic 60min and carrying out alkali oil removal treatment, at 200 DEG C after the completion of processing
Under the conditions of vacuum drying, be then naturally cooling to room temperature and obtain cup-shaped to denitrogenate metal level, as shown in Figure 4, Figure 5；
3. the cup-shaped that the obtained diamond growth layer and step (2) for preparing step (1) are 2. prepared is denitrogenated metal level and is put into
In high-purity magnesium oxide that step (2) is 1. prepared cup, wherein diamond growth layer is first placed on the cup-shaped of make-up and denitrogenates in metal level (two
Individual cup-shaped is denitrogenated metal level and fastened with opening direction) and then cup-shaped is denitrogenated into metal level be put into high-purity magnesium oxide cup, such as
Shown in Fig. 3, Fig. 4, Fig. 5；Another magnesia cup is buckled into closing insulated column, that is, obtains synthesizing post；
(3) preparation of synthesizing block：
The synthesizing post periphery prepared in step (2) sets gradually heating carbon pipe, pressure transmission salt pipe and is combined from inside to outside
Pyrophillite, and the conducting steel ring that the heating carbon plate that thickness is 1.5mm and height are 13mm is respectively placed in upper and lower ends, wherein
Heating carbon plate is connected to form closed heater with heating carbon pipe, and concordant with the height of carbon heat-generating pipe, the compound leaf of pressure transmission salt pipe is cured
Stone is concordant with two ends conductive plug, obtains synthesizing block, as shown in Figure 3；
(4) processing of synthesizing block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum in drying box
Temperature is in 28~30min by room temperature to 190 DEG C；When temperature rises to 190 DEG C, temperature 5min is kept, then to true
It is 0.02-0.03Mpa that pressure in argon gas to case is passed through in empty drying box, and heat-insulation pressure keeping 5 hours, keep terminating under this condition
Afterwards, less than 50 degree, applying argon gas to normal pressure are cooled to, the synthesizing block after processing goes out baking oven, carry out high temperature press synthesis；
(5) synthesis technique of synthesizing block：
Synthesizing block after step (4) described processing is placed on synthetic gem level colorless diamond in high temperature press,
Concrete technology step is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55 by 0MPa in 55s~60s~
60MPa, then keeps 60~80min under the pressure condition；Keep after completing, pressure in 25s~30s by 55~
60MPa boosts to 65~70MPa, and 1000~1800s of holding under the pressure condition；Keep complete after, pressure 25s~
80~85MPa is boosted to by 65~70MPa in 30s, after boosting is completed, then in 119~121 hours pressure by 80~
85MPa boosts to 95~100MPa；
B. temperature changing process is：Start synthetic work when, temperature in 9~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C
1300~1350 DEG C are warming up to, and keeps 2000~3000s at such a temperature；After the completion of holding, temperature in 20~30s by
1300~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 200 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of colorless diamond.
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle, such as through electrolysis, purification processes after the completion of processing
Fig. 8-1, Fig. 8-2, shown in Fig. 8-3.
The synthetic effect of the present embodiment, per unit area yield 78ct, granularmetric composition is as shown in the table, note：(1ct=100 points)
| Granularity | <9 points | 9-19 points | 20-39 points | 40-59 points | 60-79 points | >79 points |
| Content % | 3% | 13.5% | 38.5% | 30% | 12% | 3% |
Color：F, G, cleanliness：SI1、VS
Embodiment 5
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take the Fe Base Metal catalyst Fe that granularity is 2~40 μm60Ni30Co10, granularity be 2~40 μm of native graphite (purity
>=99.99%) and trace element Al (purity >=99.9%) according to mass ratio be 50:50:0.5 ratio is mixed, so
Above-mentioned compound is added afterwards and mixed at room temperature 14 hours in three-dimensional material mixer, isostatic pressed 300Mpa is carried out, (particle diameter is 4 for granulation
~6mm), be pressed into two height be 15mm, diameter be 40mm cylindric diamond growth layer；After the completion of compacting, it will make
Standby diamond growth layer high vacuum under conditions of temperature is 750 DEG C is reduced 40 hours, and reduction is naturally cooling to room after completing
Temperature, then Vacuum Package is standby；
(2) preparation of synthesizing post：
1. prepares high-purity magnesium oxide cup using conventional method, using the magnesia of purity >=99.8%, 1100 after compacting
Processing is made after 12 hours under DEG C high temperature, prepares two thickness and is 1.5mm, is highly 18mm high-purity magnesium oxide
Cup；
2. the Al alloy sheets that takes purity to be 99.9% are washed into wall thickness and are 1.0mm, are highly 16.5mm cup-shaped and denitrogenate
(external diameter that cup-shaped denitrogenates metal level is consistent with the internal diameter of high-purity magnesium oxide cup, and cup-shaped denitrogenates the internal diameter of metal level for metal level two
It is consistent with the diameter of diamond growth layer)；Then it is that 1.0mm denitrogenates gold that the Al alloy sheets that are again 99.9% with purity, which are washed into thickness,
Belong to synusia, the diameter that this denitrogenates metal sheet is consistent with the diameter of the diamond growth layer of step (1) described synthesis, as 40mm；
Above-mentioned cup-shaped denitrogenates metal level and denitrogenates metal sheet with being cleaned by ultrasonic 60min and carrying out alkali oil removal treatment, and processing is completed
The vacuum drying under the conditions of 200 DEG C afterwards, then Temperature fall is room temperature, obtains cup-shaped and denitrogenate metal level and denitrogenate metal level (to set
Put and denitrogenate metal level between two diamond growth blocks), as shown in Fig. 4, Fig. 6；
3. the metal level of denitrogenating that the obtained diamond growth layer and step (2) for preparing step (1) are 2. prepared is put into step
(2) in the high-purity magnesium oxide cup 1. prepared；Metal level is denitrogenated between two of which diamond growth layer and two diamond growth layers
The cup-shaped for being first placed on make-up jointly denitrogenates in metal level (two cup-shapeds are denitrogenated metal level and fastened with opening direction) and then by cup
Shape is denitrogenated metal level and is put into a high-purity magnesium oxide cup, buckles another magnesia cup into closing insulated column, that is, is bored
Stone synthesizes post；As shown in Fig. 3, Fig. 4, Fig. 6；
(3) preparation of synthesizing block：
The synthesizing post periphery prepared in step (2) sets gradually heating carbon pipe, pressure transmission salt pipe and is combined from inside to outside
Pyrophillite, and the conducting steel ring that the heating carbon plate that thickness is 1.5mm and height are 13mm is respectively placed in upper and lower ends, wherein
Heating carbon plate is connected to form closed heater with heating carbon pipe, and concordant with the height of carbon heat-generating pipe, the compound leaf of pressure transmission salt pipe is cured
Stone is concordant with two ends conductive plug, obtains synthesizing block, as shown in Figure 3；
(4) processing of diamond growth block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum in drying box
Temperature is in 32~35min by room temperature to 200 DEG C；When temperature rises to 200 DEG C, temperature 5min is kept, then to true
It is 0.02-0.03Mpa that pressure in argon gas to case is passed through in empty drying box, and heat-insulation pressure keeping 6 hours, keep terminating under this condition
Afterwards, less than 50 degree, applying argon gas to normal pressure are cooled to, the synthesizing block after processing goes out baking oven, carry out high temperature press synthesis；
(5) synthesis technique of synthesizing block：
Synthesizing block after step (4) described processing is placed on synthetic gem level colorless diamond in high temperature press,
Concrete technology step is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55 by 0MPa in 55s~60s~
60MPa, then keeps 60~80min under the pressure condition；Keep after completing, pressure in 25s~30s by 55~
60MPa boosts to 65~70MPa, and 1000~1800s of holding under the pressure condition；Keep complete after, pressure 25s~
80~85MPa is boosted to by 65~70MPa in 30s, after boosting is completed, then in 95~97 hours pressure by 80~85MPa
Boost to 95~100MPa；
B. temperature changing process is：Start synthetic work when, temperature in 9~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C
1300~1350 DEG C are warming up to, and keeps 2000~3000s at such a temperature；After the completion of holding, temperature in 20~30s by
1300~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 96 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of colorless diamond.
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle, such as through electrolysis, purification processes after the completion of processing
Fig. 8-1, Fig. 8-2, shown in Fig. 8-3.
The synthetic effect of the present embodiment, per unit area yield 85ct, granularmetric composition is as shown in the table, note：(1ct=100 points)
| Granularity | <9 points | 9-19 points | 20-39 points | 40-59 points | 60-79 points | >79 points |
| Content % | 5% | 20% | 46% | 16.5% | 11% | 1.5% |
Color：E, F, cleanliness：SI1、VS
Embodiment 6
A kind of artificial synthesis of Gem Grade colorless diamond, comprises the following steps：
(1) preparation of diamond growth layer：
Take the Fe Base Metal catalyst Fe that granularity is 2~50 μm55Ni30Co15, granularity be 2~40 μm of native graphite (purity
>=99.99%) and trace element Al (purity >=99.9%) according to mass ratio be 50:50:1.0 ratio is mixed, so
Above-mentioned compound is added afterwards and mixed at room temperature 12 hours in three-dimensional material mixer, isostatic pressed 300Mpa is carried out, (particle diameter is 4 for granulation
~6mm), it is 15.5mm, a diameter of 40mm cylindric diamond growth layer to be pressed into height；After the completion of compacting, by the brill of preparation
Stone grown layer high vacuum under conditions of temperature is 750 DEG C is reduced 40 hours, and reduction is naturally cooling to room temperature after completing, then
Vacuum Package is standby；
(2) preparation of synthesizing post：
1. prepares high-purity magnesium oxide cup using conventional method, using the magnesia of purity >=99.8%, 1100 after compacting
Processing is made after 12 hours under DEG C high temperature, prepares two thickness and is 1.5mm, is highly 18mm high-purity magnesium oxide
Cup；
2. the Al alloy sheets that takes purity to be 99.9% are washed into wall thickness and are 0.5mm, are highly 16.5mm cup-shaped and denitrogenate
(external diameter that cup-shaped denitrogenates metal level is consistent with the internal diameter of high-purity magnesium oxide cup, and cup-shaped denitrogenates the internal diameter of metal level for metal level two
It is consistent with the diameter of diamond growth layer)；Then it is that 1.0mm denitrogenates gold that the Al alloy sheets that are again 99.9% with purity, which are washed into thickness,
Belong to synusia, the diameter that this denitrogenates metal sheet is consistent with the diameter of the diamond growth layer of step (1) described synthesis, as 40mm；
Above-mentioned cup-shaped denitrogenates metal level and denitrogenates metal sheet with being cleaned by ultrasonic 60min and carrying out alkali oil removal treatment, and processing is completed
The vacuum drying under the conditions of 200 DEG C afterwards, then Temperature fall is room temperature, obtains cup-shaped and denitrogenate metal level and denitrogenate metal level (to set
Put and denitrogenate metal level between two diamond growth layers), as shown in Fig. 4, Fig. 6；
3. the metal level of denitrogenating that the obtained diamond growth layer and step (2) for preparing step (1) are 2. prepared is put into step
(2) in the high-purity magnesium oxide cup 1. prepared；Metal level is denitrogenated between two of which diamond growth layer and two diamond growth layers
The cup-shaped for being first placed on make-up jointly denitrogenates in metal level (two cup-shapeds are denitrogenated metal level and fastened with opening direction) and then by cup
Shape is denitrogenated metal level and is put into a high-purity magnesium oxide cup, as shown in Fig. 3, Fig. 4, Fig. 6；Another magnesia cup is buckled into envelope
Insulated column is closed, that is, obtains synthesizing post；
(3) preparation of synthesizing block：
The synthesizing post periphery prepared in step (2) sets gradually heating carbon pipe, pressure transmission salt pipe and is combined from inside to outside
Pyrophillite, and the conducting steel ring that the heating carbon plate that thickness is 1.5mm and height are 13mm is respectively placed in upper and lower ends, wherein
Heating carbon plate is connected to form closed heater with heating carbon pipe, and concordant with the height of carbon heat-generating pipe, the compound leaf of pressure transmission salt pipe is cured
Stone is concordant with two ends conductive plug, obtains synthesizing block, as shown in Figure 3；
(4) processing of diamond growth block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum in drying box
Temperature is in 32~35min by room temperature to 200 DEG C；When temperature rises to 200 DEG C, temperature 5min is kept, then to true
It is 0.02-0.03Mpa that pressure in argon gas to case is passed through in empty drying box, and heat-insulation pressure keeping 4 hours, keep terminating under this condition
Afterwards, less than 50 degree are cooled to, pressure is normal pressure in applying argon gas to case, the diamond growth layer after processing goes out baking oven, carries out high temperature
Press is synthesized；
(5) synthesis technique of synthesizing block：
Synthesizing block after step (4) described processing is placed on synthetic gem level colorless diamond in high temperature press,
Concrete technology step is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55 by 0MPa in 55s~60s~
60MPa, then keeps 60~80min under the pressure condition；Keep after completing, pressure in 25s~30s by 55~
60MPa boosts to 65~70MPa, and 1000~1800s of holding under the pressure condition；Keep complete after, pressure 25s~
80~85MPa is boosted to by 65~70MPa in 30s, after boosting is completed, then in 119~121 hours pressure by 80~
85MPa boosts to 95~100MPa；
B. temperature changing process is：Start synthetic work when, temperature in 9~10min by room temperature to 1000~
1050 DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C
1300~1350 DEG C are warming up to, and keeps 2000~3000s at such a temperature；After the completion of holding, temperature in 20~30s by
1300~1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 120 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by highest in 20 ± 5min
Pressure is depressurized to 0MPa, completes the synthesis of synthesizing block.
(6) preparation of colorless diamond particle：
The colorless diamond Synthetic block that step (5) is obtained obtains colorless diamond through electrolysis, purification processes after the completion of processing
Grain, as shown in Fig. 8-1, Fig. 8-2, Fig. 8-3.
The synthetic effect of the present embodiment, per unit area yield 81ct, granularmetric composition is as shown in the table, note：(1ct=100 points)
| Granularity | <9 points | 9-19 points | 20-39 points | 40-59 points | 60-79 points | >79 points |
| Content % | 4% | 15.5% | 43% | 25.5% | 9% | 3% |
Color：F, G, cleanliness：SI1、VS
Embodiment 7
One of synthesizing block structure used, its structural representation in above-mentioned Gem Grade colorless diamond artificial synthesis
As shown in Figure 1 and Figure 2.The synthesizing block is set gradually from inside to outside including synthesizing post and synthesizing post periphery
Generate heat carbon pipe, pressure transmission salt pipe and composite leaf wax stone block；Be additionally included in heating carbon plate that synthesizing post upper and lower ends are respectively provided with
Conducting metal circle, described heating carbon plate is connected forming closed structure, described pressure transmission salt pipe and heating with heating carbon pipe
Carbon pipe is highly flushed, described composite pyrophyllite tile height is highly flushed with conductive plug；
Described synthesizing post includes the synthesizing layer placed in high-purity magnesium oxide cup and high-purity magnesium oxide cup, described
Synthesizing layer include with horizontal parallel mode carry out it is cross-superimposed arrangement place diamond growth layer and denitrogenate metal level, institute
The diamond growth layer stated is with denitrogenating that metal level is cylinder and diameter is consistent；Wherein, diamond growth is placed in orlop
Layer；
Described high-purity magnesium oxide cup is two identical opening high-purity magnesium oxide cups, and described synthesizing layer is at one
After placement reaches requirement for height in high-purity magnesium oxide cup, another high-purity magnesium oxide cup is fastened with opening direction, that is, obtained
Synthesizing post.
In use, high-purity magnesium oxide cup, diamond growth layer, the thickness for denitrogenating metal level can be according to realities
Border situation prepares different required thickness.
Embodiment 8
The two of synthesizing block structure used, its structural representation in above-mentioned Gem Grade colorless diamond artificial synthesis
As shown in Fig. 3, Fig. 4, Fig. 5.The synthesizing block includes synthesizing post and synthesizing post periphery is set successively from inside to outside
Heating carbon pipe, pressure transmission salt pipe and the composite leaf wax stone block put；It is additionally included in the heating carbon that synthesizing post upper and lower ends are respectively provided with
Piece and conducting metal circle, described heating carbon plate are connected forming closed structure with heating carbon pipe, described pressure transmission salt pipe and
Carbon pipe is highly flushed, described composite pyrophyllite tile height is highly flushed with conductive plug for heating；
The integrative-structure that described synthesizing post includes high-purity magnesium oxide cup and is arranged in high-purity magnesium oxide cup, institute
The integrative-structure stated is denitrogenated metal layer combination with cup-shaped by diamond growth layer and formed, and described cup-shaped denitrogenates metal level bag located at brill
The periphery of stone grown layer, diameter and the cup-shaped of diamond growth layer denitrogenate the internal diameter of metal level always, and the cup-shaped denitrogenates gold
The external diameter for belonging to layer is consistent with the internal diameter of high-purity magnesium oxide cup；
Described cup-shaped denitrogenate metal level for two identicals by denitrogenating the cup-like structure that metal level is prepared from, it is described
High-purity magnesium oxide cup is two identical opening high-purity magnesium oxide cups；Described diamond growth layer is positioned over a cup-shaped and denitrogenates gold
Belong to layer in, then by another cup-shaped denitrogenate metal level with opening direction fasten obtain sealed integrative-structure, then by one
Body structure is placed in a high-purity magnesium oxide cup, and another high-purity magnesium oxide cup is fastened with opening direction obtains diamond conjunction
Cheng Zhu.
In use, high-purity magnesium oxide cup, diamond growth layer, cup-shaped denitrogenates the thickness of metal level can be according to reality
Border situation prepares different required thickness.
Embodiment 9
The three of synthesizing block structure used, its structural representation in above-mentioned Gem Grade colorless diamond artificial synthesis
As shown in Fig. 3, Fig. 4, Fig. 6.
Synthesizing block structure part same as Example 8 described in the embodiment is no longer repeated, and difference is：Institute
The integrative-structure stated denitrogenates removing between metal level, the diamond growth layer that two superpositions are placed and two diamond growth layers by cup-shaped
Nitrogen metal layer combination is formed；Described cup-shaped denitrogenates metal level bag located at two diamond growth layer peripheries, two diamond growth layers
Between it is consistent with the diameter of diamond growth layer provided with denitrogenating metal level and denitrogenating the diameter of metal level.
Claims (10)
1. a kind of artificial synthesis of Gem Grade colorless diamond, it is characterised in that this method comprises the following steps：
(1) preparation of diamond growth layer：
Take Fe Base Metals catalyst, high purity graphite and minor metallic element through three-dimensional ball milling mixing, isostatic pressed, granulate, be suppressed into
Cylindric diamond growth layer, by obtained cylindric diamond growth layer by after high vacuum reduction treatment, being naturally cooling to room
Temperature, Vacuum Package is standby；
(2) preparation of synthesizing post：
High-purity magnesium oxide cup is taken, the diamond growth layer for denitrogenating metal level and step (1) preparation is put into high-purity magnesium oxide cup,
Obtain synthesizing post；
(3) preparation of synthesizing block：
Heating carbon pipe, pressure transmission salt pipe and compound leaf are set gradually from inside to outside in the synthesizing post periphery described in step (2)
Cured stone, its top and bottom are respectively provided with heating carbon plate and conducting metal circle, described heating carbon plate and heating carbon pipe phase
Connection, forming closed heater；Synthesizing block is obtained after the completion of combinations thereof；
(4) processing of synthesizing block：
The synthesizing block that step (3) is obtained is put into vacuum drying chamber, then under vacuum within 20~35min,
Temperature in drying box is by room temperature to maximum temperature；When dry the temperature inside the box rises to maximum temperature by room temperature, keep being somebody's turn to do
Temperature 5min, is then passed through pressure of the argon gas into drying box for 0.02-0.03Mpa, then at this into vacuum drying chamber
Heat-insulation pressure keeping 4~6 hours under part, when insulation end is cooled to less than 50 degree, applying argon gas to normal pressure, synthesizing block goes out baking oven,
Upper high temperature press is synthesized；
(5) synthesis of colorless diamond：
Synthesizing block after step (4) described processing is put into high temperature press and synthesized, 1300~1500 DEG C,
Run 24~300 hours under the conditions of 5.5~6.5GPa, synthesized under HTHP and colorless diamond is made；
(6) preparation of colorless diamond particle：
The colorless diamond that step (5) is obtained obtains colorless diamond particle after electrolysis, purification processes.
2. the artificial synthesis of Gem Grade colorless diamond according to claim 1, it is characterised in that step (1) is described
Three-dimensional ball milling be mixed into and mix 12~18 hours at room temperature, the pressure of the isostatic pressed is 240~300MPa, the granulation it
The spheric granules that particle diameter is 4~6mm is obtained afterwards；Reduction temperature of the cylindric diamond growth layer in high vacuum reduction process
It it is 24~48 hours for 750~980 DEG C, recovery time.
3. the artificial synthesis of Gem Grade colorless diamond according to claim 1, it is characterised in that step (1) is described
Fe metal solvents granularity be 2~50 μm, its composition and weight/mass percentage composition are as follows：Fe：50~70%, Ni：25~50%,
Co：0~20%；High purity graphite described in step (1) is the native graphite or electrographite that granularity is 2~40 μm, wherein graphite
Purity >=99.99%；Minor metallic element described in step (1) for any of Al, Cu, Ti and Zr or appoint it is several, its
>=99.9%, when the minor metallic element adds diamond growth layer, it is in diamond growth for middle Al, Cu, Ti and Zr purity
Content in layer is respectively Al：0.05~1.5%, Cu：0.5~3%, Ti：0.06~3.0%, Zr：0.05~1.0%；Step
(1) the weight ratio of Fe Base Metals catalyst, high purity graphite and minor metallic element described in is：(50~90)：(50~10)：
(0.05~1).
4. the artificial synthesis of Gem Grade colorless diamond according to claim 1, it is characterised in that step (2) is described
Denitrogenate metal level for any of Al, Cu, Ti and Zr or appoint several, Al, Cu, Ti and Zr purity are all higher than 99%；Institute
The metal level of denitrogenating stated is stamped to form by the metal tape containing above-mentioned metal ingredient, and what punching press was obtained denitrogenates metal level by ultrasound
30~60min is cleaned, and carries out alkali oil removal treatment, the then vacuum drying under the conditions of 200 DEG C, and it is laggard to be naturally cooling to room temperature
Exercise and use；Maximum temperature in step (4) described vacuum drying chamber is 180~200 DEG C.
5. the artificial synthesis of Gem Grade colorless diamond according to claim 1, it is characterised in that step (2) is described
Synthesizing post the synthesizing layer of setting is arranged under the overlay comprising high-purity magnesium oxide cup and in high-purity magnesium oxide cup, it is described
Synthesizing layer comprising carry out in parallel cross-superimposed arrangement diamond growth layer and denitrogenate metal level, described diamond
Grown layer with denitrogenate that metal level is cylinder and diameter is consistent.
6. the artificial synthesis of Gem Grade colorless diamond according to claim 5, it is characterised in that the diamond growth
The thickness of layer is 5~10mm, and the thickness for denitrogenating metal level is 0.5~4mm.
7. the artificial synthesis of Gem Grade colorless diamond according to claim 1, it is characterised in that step (2) is described
Synthesizing post comprising high-purity magnesium oxide cup and be arranged at high-purity magnesium oxide cup in integrative-structure, described integrative-structure
Denitrogenated metal layer combination by diamond growth layer and cup-shaped and formed, described cup-shaped denitrogenates metal level bag located at the outer of diamond growth layer
Enclose.
8. the artificial synthesis of Gem Grade colorless diamond according to claim 7, it is characterised in that described one knot
Structure is denitrogenated metal layer combination by diamond growth layer and cup-shaped and formed and comprising two sizes consistent diamond growth layer, described cup
Shape is denitrogenated metal level bag and is also equipped with and diamond growth between the periphery of two diamond growth layers and two diamond growth layers
Layer diameter unanimously denitrogenate metal level.
9. the artificial synthesis of the Gem Grade colorless diamond according to claim 7 or 8, it is characterised in that described brill
The thickness of stone grown layer is 5~25mm, cup-shaped of the bag located at diamond growth layer periphery denitrogenate the thickness of metal level for 0.5~
4mm；The thickness for denitrogenating metal level being arranged between two diamond growth layers is 0.5~3.5mm.
10. the artificial synthesis of Gem Grade colorless diamond according to claim 1, it is characterised in that step (5) is described
The synthesis technique step that is synthesized in high temperature press of colorless diamond Synthetic block it is as follows：
A. pressure change process is：When starting synthetic work, pressure boosts to 55~60MPa in 55s~60s by 0MPa, so
60~80min is kept under the pressure condition afterwards；Keep after completing, pressure is boosted in 25s~30s by 55~60MPa
65~70MPa, and 1000~1800s of holding under the pressure condition；Keep after completing, pressure in 25s~30s by 65~
70MPa boosts to 80~85MPa, after boosting is completed, then pressure boosts to 95 by 80~85MPa within 24~300 hours
~100MPa；
B. temperature changing process is：When starting synthetic work, temperature is in 9min~10min by room temperature to 1000~1050
DEG C, and 60~80min is kept at such a temperature；After the completion of holding, temperature is in 110s~120s by 1000~1050 DEG C of heatings
To 1300~1350 DEG C, and 2000~3000s is kept at such a temperature；After the completion of holding, temperature in 20~30s by 1300~
1350 DEG C are cooled to 1250~1280 DEG C, and are kept for 24~300 hours at such a temperature；
C. the temperature described in step b stops heat after the completion of keeping, and stops starting release after hot 10min, by maximum pressure in 20 ± 5min
0MPa is depressurized to, the synthesis of synthesizing block is completed.
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| CN108722317A (en) * | 2018-06-14 | 2018-11-02 | 杨鹏宇 | A kind of gem grade diamond annular composite structure and its preparation method and application |
| CN109825741A (en) * | 2019-03-25 | 2019-05-31 | 河南省力量钻石股份有限公司 | A kind of Ni Base Metal catalyst and its method using catalyst preparation IC chip polishing pad finishing special type diamond |
| 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 |
| CN113912056A (en) * | 2021-11-04 | 2022-01-11 | 郑州中南杰特超硬材料有限公司 | Method for synthesizing multiple NPDs in one time |
| CN114790570A (en) * | 2022-05-18 | 2022-07-26 | 南平市亿泽磨料磨具科技有限公司 | Process for cultivating diamonds in laboratory and manufacturing equipment thereof |
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| CN108722317A (en) * | 2018-06-14 | 2018-11-02 | 杨鹏宇 | A kind of gem grade diamond annular composite structure and its preparation method and application |
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| CN113912056B (en) * | 2021-11-04 | 2023-03-14 | 郑州中南杰特超硬材料有限公司 | Method for synthesizing multiple NPDs in one time |
| CN114790570A (en) * | 2022-05-18 | 2022-07-26 | 南平市亿泽磨料磨具科技有限公司 | Process for cultivating diamonds in laboratory and manufacturing equipment thereof |
| CN114790570B (en) * | 2022-05-18 | 2024-02-27 | 南平市亿泽磨料磨具科技有限公司 | Process for cultivating diamond in laboratory and manufacturing equipment thereof |
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