CN109621843A - A kind of diamond synthesizing column of gradient function and preparation method thereof - Google Patents
A kind of diamond synthesizing column of gradient function and preparation method thereof Download PDFInfo
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- CN109621843A CN109621843A CN201910066606.8A CN201910066606A CN109621843A CN 109621843 A CN109621843 A CN 109621843A CN 201910066606 A CN201910066606 A CN 201910066606A CN 109621843 A CN109621843 A CN 109621843A
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Abstract
The invention discloses diamond synthesizing columns of a kind of gradient function and preparation method thereof.The synthesis column is formed by stacking by three layers of graphite powder and metal solvent powder mixed block layer level, three block layer diameters are equal, the height of intermediate mixed block layer is greater than the height of upper and lower ends mixed block layer, and graphite and the mass ratio of catalyst powder are 0.5~1.0 times of the two mass ratio in two end block layers in intermediate mixed block layer.This method uniformly mixes graphite powder with catalyst powder by special mixing device, eliminates the generation of mixing segregation phenomena, avoids influence of the mixing segregation to synthesis diamond quality.The synthesis column passes through different masses layer height and the wherein control of graphite and catalyst powder quality, the temperature difference and pressure difference in device diamond synthesizing cavity are substantially reduced, is avoided during diamond synthesizing since the temperature difference is big, the phenomenon of the low caused diamond quality difference of internal temperature.The synthesis column prepare it is simple to operation, in diamond synthesizing synthesize column inside and outside the temperature difference reduction have the function of it is apparent.
Description
Technical field
The invention belongs to technical field of diamond preparation, and in particular to a kind of diamond synthesizing column of gradient function and its
Preparation method.
Background technique
The synthesis of diamond is to be suitable for gold for column is synthesized made of graphite powder and the compacting of metal solvent powder mixture
Under the high-temperature and high-pressure conditions of hard rock growth, then carbon atom continuous nucleation and growth process in fused solution catalyst powder is converted by graphite
For the process of diamond.In the synthesis process of diamond, the synthesis quality and yield of diamond are removed by temperature, pressure, conjunction
Outside influence at technological parameters such as times, also depend greatly on synthesis column preparation quality, especially graphite powder with
The control precision of mixing uniformity, synthesis column cylinder pressing weight between metal solvent powder and size.In the preparation of synthesis column
In the process, synthesize graphite powder and metal solvent powder in column must be uniformly mixed with guarantee between the two being mixed it is abundant,
In favor of the diamond nucleation core for forming sufficient amount in synthetic cavity during diamond synthesizing and being evenly distributed, and it is
The growth of nucleation of diamond provides sufficient carbon source, to guarantee that graphite powder is converted into the synthetic yield and quality of diamond.
As shown in the above, synthesizing the mixing uniformity in column between graphite powder and metal solvent powder is to guarantee diamond
Synthesize the necessary condition of quality and yield.But in the synthesis process, due to the difference in specific gravity between graphite powder and metal solvent powder
It is different that (specific gravity of graphite powder is 2.25g/cm greatly3, Fe70Ni30The specific gravity of catalyst powder is 8.15g/cm3), in mixed process easily
There is the difference agglomeration of the different material of specific gravity, causes mixing to be segregated, greatly reduce the synthesis quality of diamond, also drop
The low synthesis yield of diamond.Meanwhile the particle shape of graphite powder and metal solvent powder, surface characteristic difference are also very big, stone
Coefficient of friction very little, the lubricity of ink are good, keep its mutual " engagement " between metal solvent powder particle less able, and synthesis produces
Amount is decreased obviously, it is easier to lead to material segregation aggregation.
In actual production, in order to enable mixing is uniform, usually certain particle size and the graphite powder of weight ratio, metal are touched
Matchmaker's powder and bonding agent are mixed 8 hours or more in three-dimensional material mixer at room temperature, by the extension of mixing time to increase
The uniformity of mixing.But during being somebody's turn to do, although the time of mixing is long, since the difference of specific gravity of graphite and metal solvent is big,
There can be the tendency that heavy metal sinks, light graphite floats always in entire mixing process, still will appear the segregation of material
Phenomenon, so that the synthesis quality and yield of diamond have biggish fluctuation.Therefore, how preferable mixing, make it not
Phenomena such as segregation, reunite occur becomes the diamond synthesizing process technical issues that need to address.
In addition, being to pass through the heating of synthesis column outer periphery using indirect heating method during diamond synthesizing
After body heat production, from synthetic cavity edge to synthetic cavity internal heat transfer, in this case, there is deviation in synthetic cavity always:
Outer edge area temperature is high, the temperature of intermediate region is low (its axial temperature difference is up to 80 DEG C), the diamond for causing intermediate region to synthesize
Quality is deteriorated, and (even glomerocryst is more, inside impurity is more, poor transparency, intensity are low, particularly difference between TI and TTI is larger, >
10%, the requirement of high quality diamond is not achieved).And the synthesis column that industry uses at present is graphite and metal solvent powder point
The synthesis column that fixed component and performance are integrated is matched, synthesis column can not adjust synthesis chamber by the variation of cylinder itself
The internal difference in temperature of body, and the yield of monolithic synthesis column is usually 250~270 carats, yield is lower.
The temperature occurred during diamond synthesizing is not almost can avoid using the heating method internally to be conducted heat by outer rim
Degree difference phenomenon takes in the industry many kinds of measures and is continuously improved, to further increase Buddha's warrior attendant to reduce temperature difference
The synthesis quality and monolithic yield of stone.The application documents of Publication No. CN207221875U describe a kind of " diamond conjunction
At assembling block structure ", using double group conductive plugs, heat generating component etc. in this document, pass through the heat source items increased outside synthesis column
Part improves the internal temperature of synthetic cavity, reduces the temperature difference, improves diamond synthesizing quality and yield, but the technological means group
Assembling structure is complicated, assembles that difficulty is larger, little for the improvement of synthesis column temperature difference integrated in cavity, is unfavorable for industry
Large-scale production can not still be effectively improved the temperature difference problem of synthetic cavity.The application documents of Publication No. CN106270484A
It describes " preparation method that graphite stem is used in a kind of diamond synthesis ", this document preset cementite in synthesis column, with
Cementite is forming core core, adjusts the number of nuclei of diamond by controlling the adding proportion of cementite to regulate and control diamond and close
At granularity and quality, but this mode is more suited to the synthesis of coarse diamond, is unable to improve the temperature difference problem of synthesis.It is open
It number is described " manufacture craft that a kind of novel diamond synthesizes column " for the application documents of CN108144554A, this document is by metal
Catalyst is pressed into 10 or so (often in the graphite powder mixing of the form and certain mass ratio of quality arithmetic progression (│=0.1 │ d)
Piece is with a thickness of 2~5mm), layering assembling then is carried out to compressed tablets in such a way that catalyst weight successively reduces from top to bottom again, with
Phase is upper and lower caused by catalyst sinks because melting in synthesis process to improve by adjusting the content of synthesis column upper and lower side catalyst powder
The problem of end catalyst is unevenly distributed.But each lamellar spacing made by the technology is very thin, and the shaping strength of compacting is low, fragile
It is broken, be difficult suppress major diameter specification lamella, also therefore and be difficult to use in major diameter (such as Φ 55mm) synthesis column production；And
It takes the mode film-making of │=0.1 arithmetic progression │ d, synthesizes the catalyst maximum weight difference of column upper and lower side monolithic in 1g or so, such as
The effect of poor quality that the temperature difference is adjusted in prolonged synthesis process of this small catalyst is weaker；Meanwhile multilayer assembling procedure is very big
Reduce production efficiency and the piece of multiple very thin thickness is assembled, efficiency is very low, assembly precision deviation is big, in practical life
Application in production is by larger limitation, it is difficult to meet the needs of large-scale production.Therefore, expedient measure how is taken to improve and close
At the temperature difference in cavity, the synthesis quality and yield of diamond are improved, it is anxious to be still industrial scale production diamond
Realistic problem to be solved.
Summary of the invention
The present invention for the technical issues of be: in the prior art for the mixing efficiency of graphite powder and metal solvent powder
It is low, uneven, it is easy to appear segregation phenomena, seriously affects the quality and yield for preparing diamond.Meanwhile existing diamond preparation
In the process, since heating method causes diamond synthesizing column edge and internal uneven heating even, exist always in synthetic cavity inclined
Difference, the diamond quality for causing intermediate region to synthesize are deteriorated, and due to the indirect heating method of diamond synthesizing process, so that reducing
The temperature difference in synthetic cavity becomes existing technical problem.
In view of the above-mentioned problems, the present invention provides a kind of diamond synthesizing column, diamond synthesizing column is divided into not by the present invention
Same block layer, each piece of layer, by diamond synthesizing column edge and internal raw material dosage difference, to change chamber central and side
The temperature difference of edge.It is simple and efficient to handle, and the internal and external temperature deviation of cavity is efficiently reduced, it substantially change in practical applications
The quality of diamond synthesis.
The present invention also provides one kind during diamond synthesis, the mixing device of graphite powder and metal solvent powder,
The device enables to the graphite powder for preparing diamond synthesizing column to be uniformly mixed with metal solvent powder.In the apparatus, than
The biggish material of heavy phase difference can will be expected in the disk blender of tilt rotation by the frictional force of feed bin inner wall and storeroom
Storehouse bottoms material turns to fall after mentioning to certain altitude, and the period is reciprocal, and material eliminates heavy in the feed bin of rotation as a result,
Material sinking segregation phenomenon, storeroom can be effectively uniformly mixed.
The present invention also provides the preparation methods of above-mentioned diamond synthesizing column.
The present invention is achieved by the following technical solutions a kind of diamond synthesizing column of gradient function, the synthesis column packet
Graphite and the first mixed layer of catalyst powder block (1) are included, the graphite and catalyst powder second being arranged in parallel on the first mixed layer block (1) are mixed
It closes layer block (2), and the graphite and catalyst powder third mixed layer block (3) that are arranged in parallel on the second mixed layer block (2)；Described
The diameter of one mixed layer block (1), the second mixed layer block (2) and third mixed layer block (3) is equal.
The diamond synthesizing column of the gradient function, the graphite and the first mixed layer of catalyst powder block (1) and graphite
It is equal with the height of catalyst powder third mixed layer block (3), and it is lower than the height of graphite and the second mixed layer of catalyst powder block (2).
The diamond synthesizing column of the gradient function, the height of the graphite and the second mixed layer of catalyst powder block (2)
It is 2.2~2.5 times of graphite and the first mixed layer of catalyst powder block (1),
Preferably, the height of the graphite and the second mixed layer of catalyst powder block (2) is graphite and the first mixed layer of catalyst powder
2.4 times of block (1).
The diamond synthesizing column of the gradient function, the graphite and the first mixed layer of catalyst powder block (1) and graphite
And graphite is identical as the mass ratio of catalyst powder in catalyst powder third mixed layer block (3)；The graphite and the second mixed layer of catalyst powder
Graphite and the mass ratio of catalyst powder are graphite and catalyst powder mass ratio in graphite and the first mixed layer of catalyst powder block (1) in block (2)
0.5~1.0 times.
The diamond synthesizing column of the gradient function, the graphite and the first mixed layer of catalyst powder block (1) and graphite
It is 62~70:30~38 with graphite in catalyst powder third mixed layer block (3) and the mass ratio of catalyst powder；The graphite and catalyst powder
Graphite and the mass ratio of catalyst powder are 60~55:40~45 in second mixed layer block (2).
The diamond synthesizing column of the gradient function, the graphite are high purity graphite powder (purity >=99.99%),
Partial size is 300 mesh；
The catalyst powder includes the raw material of following parts by weight: Fe68.15%, Ni30%, Co1.5%, Mn0.3% and
La0.05%；Its partial size is 400 mesh numbers.
A kind of diamond synthesizing column mixing device preparing above-mentioned gradient function, which includes electric control gear
(100), cabinet (200), motor (300) in cabinet (200) and setting are set in the hopper of cabinet (200) outer upper ends
Support rod (400), one end of the hopper support bar (400) is connect with cabinet, other end end is offered for hopper
(500) the first hopper fixation hole (401)；
The device further includes the blending bunker (600) being connected by axis (700) with motor (300), and blending bunker (600) is in electricity
It is rotated under the drive of machine (300)；Blending bunker (600) wall is equipped with feed inlet (601), when being in feed state, institute
State the underface that feed inlet (601) is located at the discharge port of hopper (500)；
The electric control gear (100) is connected with motor (300).
The diamond synthesizing column mixing device for preparing gradient function, hopper support bar (400) packet
Include the first hopper support bar (402) being vertically arranged and horizontally disposed second hopper support bar (403), the first hopper support bar
(402) one end end is detachably connected with cabinet, the other end end of the first hopper support bar (402) and the second hopper support
One end end of bar (403) is hinged, and the second hopper support bar (403) is rotated up and down relative to the first hopper support bar (402), the
The other end end of two hopper support bars (403) is provided with the first hopper fixation hole (401) for hopper (500).
The diamond synthesizing column mixing device for preparing gradient function, on the blending bunker feed inlet (601)
It is additionally provided with corresponding sealing cover (602)；Centre bore (603), institute are additionally provided on the mixing bulkhead, at centre rotational axis
The centre bore stated is additionally provided with corresponding port lid (604).
The diamond synthesizing column mixing device for preparing gradient function, the axis (700) periphery are additionally provided with
Axle sleeve (701)；It is additionally provided with cloche (800) outside the disk blender, cloche (800) is equipped under hopper
The through-hole (801) in portion.
The diamond synthesizing column mixing device for preparing gradient function, the blending bunker (600) is ellipse
The blending bunker of shape, oval long axis length are 800~1000mm, and oval minor axis length is 220~250mm；Ellipse
Blending bunker carries out rotation mixing using short axle as center rotary shaft, and the angle of long axis and vertical direction is 15~20 °；The mixing
The wall body in storehouse is 304 stainless steel plates with a thickness of 1.5~2.0mm.
A kind of preparation method of the diamond synthesizing column of above-mentioned gradient function, this method include mixing, granulation, also original place
Reason, cold moudling；Specific step is as follows:
(1) preparation of graphite and catalyst powder the first mixed layer block and graphite and catalyst powder third mixed layer block:
A. by required raw graphite powder, catalyst powder and ethylene glycol be added in mixing device as claimed in claim 7 into
Row mixing；
B. the mixed material of step a is subjected to granulation processing, obtains feed particles；
C. feed particles step b obtained carry out reduction treatment, obtain reduction particle；
D. cold moudling is carried out to the reduction particle that step c is obtained, graphite and catalyst powder is obtained after the completion of cold moudling
First mixed layer block；
E. step a, b, c, d are repeated, graphite and catalyst powder third mixed layer block is prepared；
(2) preparation of graphite and the second mixed layer of catalyst powder block:
Graphite and the second mixed layer of catalyst powder block are prepared according to step described in step (1)；
(3) graphite and the first mixed layer of catalyst powder, graphite and catalyst powder second prepared step (1) and step (2) is mixed
It closes layer block, block, graphite and catalyst powder third mixed layer block to stack according to sequential parallel from bottom to top, the ladder can be obtained
Spend the diamond synthesizing column of functionalization.
The preparation method of the diamond synthesizing column of the gradient function, graphite powder, catalyst powder and second two described in step a
The mass ratio of alcohol is 62~70:30~38:0.12；In step (2) graphite and the second mixed layer of catalyst powder block preparation process,
The mass ratio of graphite powder, metal solvent powder and ethylene glycol are as follows: 60~55:40~45:0.12.
The method of the preparation method of the diamond synthesizing column of the gradient function, mixing described in step a is specific as follows:
The graphite powder of preparation is placed in mixing device, ethylene glycol is then added and is uniformly mixed, shuts down, catalyst powder, booting mixing is added
Uniformly to get arrive uniform mixture.
The preparation method of the diamond synthesizing column of the gradient function, the graphite powder and ethylene glycol are in mixing device
Middle mixing time is 15~25min, and the mixing time after catalyst powder is added is 20~30min；When mixing power of motor be 15~
20kW, motor speed are 0~50rpm.
The preparation method of the diamond synthesizing column of the gradient function is granulated in Doubleroller compaction granulator described in step b
It carries out, the working speed of pelletizer is 42 turns/min, and the partial size that feed particles are obtained after the completion of being granulated is 2mm.
The preparation method of the diamond synthesizing column of the gradient function, reduction treatment described in step c is in hydrogen reducing
It is carried out in furnace, temperature when feed particles restore is 1000~1100 DEG C, the recovery time is 6~8 hours.
The preparation method of the diamond synthesizing column of the gradient function, cold moudling described in step d is in automatic hydraulic
Processing is pressed in machine, the operating pressure of automatic hydraulic press is 40Mpa.
Compared with prior art, the present invention has following positive beneficial effect
Under existing technology condition, stablizing and improving the necessary condition of diamond synthesizing quality is to first have to guarantee
The mixing uniformity of graphite and catalyst powder in column is synthesized, furthermore is the stability for maintaining the temperature difference and pressure difference of synthetic cavity.
The present invention is mixed graphite powder with metal solvent powder using disk blender, mixed using the disk with certain gradient
Graphite powder and bonding agent are sufficiently mixed by glassware first, then by with bonding agent graphite powder and metal solvent powder into
Row is sufficiently mixed, and in mixed process, mixing passes through under gravity under the rotation of inclined plate, after reaching a certain height
It falls, is sufficiently mixed, the blender mixing is full and uniform, the time is short, in a relatively short period of time can be abundant mixed between complete raw material
It closes, the time is short, high-efficient, and production cost can be greatly lowered；Meanwhile the device effectively prevents graphite powder and metal solvent powder
Due to difference in specific gravity it is larger caused by segregation phenomena, can effectively avoid existing three-dimensional material mixer exist always material segregation show
As substantially eliminating the traditional persistent ailment for leading to diamond synthesizing quality shakiness because synthesizing the segregation of column material, being obviously improved diamond
Synthesis quality, have a good application prospect.
During existing indirect heating method diamond synthesizing, influencing maximum factor to diamond synthesizing quality is to close
At the temperature difference and pressure difference of cavity, influenced by synthesis package assembly and top hammer heat dissipation, the synthesis column outer rim of indirect heating method
There are the biggish temperature difference with inside, have seriously affected the quality and yield of diamond synthesis.The present invention is well-mixed in raw material
Under the conditions of, diamond synthesizing column is divided into three layers, wherein the ratio of graphite powder is higher than middle layer block in two layer blocks up and down,
On the one hand heat input provided by external heating source can be promoted, the direct fever of graphite itself on the other hand can also be increased
Amount improves the temperature of synthesis column central area to effectively improve synthesis heat input of the column both ends to intermediate region, improves and closes
The axial temperature difference of Cheng Zhu effectively prevents during diamond synthesizing since the temperature difference is big, the low caused diamond of internal temperature
Ropy technical problem.The synthesis column prepare it is simple to operation, for synthesizing the temperature difference inside and outside column during diamond synthesizing
Reduction has the function of apparent.
Practical composite result is shown, is significantly improved using the diamond quality that the synthesis column synthesizes, is further demonstrated this
Diamond synthesizing column has the function of the reduction temperature difference outstanding.
Detailed description of the invention
Fig. 1 shows diamond synthesizing column one of the mixing device schematic diagrames for preparing gradient function；
Fig. 2 expression prepares the diamond synthesizing column of gradient function with the two of mixing device schematic diagram；
Fig. 3 expression prepares the diamond synthesizing column of gradient function with the three of mixing device schematic diagram；
Fig. 4 expression prepares the hopper support bar schematic diagram of the diamond synthesizing column mixing device of gradient function；
The diamond synthesizing column schematic diagram of Fig. 5 expression gradient function；
The meaning that symbol indicates in figure are as follows: 1 indicates graphite and the first mixed layer of catalyst powder block, and 2 indicate graphite and catalyst powder
Second mixed layer block, 3 indicate graphite and catalyst powder third mixed layer block；
100 indicate electric control gear, and 200 indicate cabinet, and 300 indicate motor, and 400 indicate hopper support bar, and 401 indicate first
Hopper fixation hole, 402 indicate the first hopper support bar, and 403 indicate the second hopper support bar, and 500 indicate hopper, and 600 indicate mixed
Feed bin, 601 indicate the feed inlet of blending bunker, and 602 indicate the corresponding sealing cover of feed inlet, and 603 indicate the centre bore of blending bunker,
604 indicate the corresponding port lid of centre bore, and 700 indicate the axis of connection motor and blending bunker, and 701 indicate axle sleeve, and 800 indicate glass
Cover, 801 indicate the through-hole on cloche.
Specific embodiment
The present invention is described in more details below by specific embodiment, but is not intended to restrict the invention
Protection scope.
Diamond catalyst powder used in following embodiment, using entitled " the synthesis ultra-fine iron of high self-sharpening diamond
The method recorded in the patent of invention of base catalyst powder, preparation method and applications " is prepared.Described in following embodiment
Diamond catalyst powder use following parts by weight raw material Fe 68.15%, Ni 30%, Co 1.5%, Mn 0.3% and La
0.05%, it is prepared by water-gas combined atomizing device, the granularity of gained diamond catalyst powder is 400 mesh.
Equipment therefor Doubleroller compaction granulator is produced purchased from Zhengzhou Yuan Chuan Machinery Co., Ltd., and Full Automatic Liquid press is precious purchased from Changzhou
Press mechanical pressing Manufacturing Co., Ltd, ethylene glycol are that analysis is pure.
Embodiment 1
A kind of diamond synthesizing column of gradient function, as shown in figure 5, the synthesis column includes that graphite and catalyst powder first are mixed
Layer block 1 is closed, graphite on the first mixed layer block and the second mixed layer of catalyst powder block 2 are arranged in parallel in, and is arranged in parallel in the
Graphite and catalyst powder third mixed layer block 3 on two mixed layer blocks；The height and third mixed layer block of the first mixed layer block 1
3 height is equal and is below the height of the second mixed layer block 2, the first mixed layer block 1, the second mixed layer block 2 and third
The diameter of mixed layer block 3 is equal.
Further, the graphite mixes for graphite with catalyst powder first with the height of catalyst powder the second mixed layer block (2)
2.2~2.5 times of layer block (1).
The present invention also provides another embodiment, the height of the graphite and catalyst powder the second mixed layer block (2) is
2.4 times of graphite and the first mixed layer of catalyst powder block (1)；
Preferably, the height of the first mixed layer block and the height of third mixed layer block are 10 ± 0.1mm, and second is mixed
The height for closing layer block is 24 ± 0.1mm.
The present invention also provides another embodiment, the first mixed layer block 1, the second mixed layer block 2 and third are mixed
The diameter for closing layer block 3 is 55 ± 0.1mm.
The present invention also provides another embodiment, the graphite and the first mixed layer of catalyst powder block (1) and graphite with
Graphite is identical as the mass ratio of catalyst powder in catalyst powder third mixed layer block (3)；The graphite and the second mixed layer of catalyst powder block
(2) graphite and the mass ratio of catalyst powder are graphite and catalyst powder mass ratio in graphite and the first mixed layer of catalyst powder block (1) in
0.5~1.0 times.
The present invention also provides another preferred embodiment, in the first mixed layer block 1 and third mixed layer block 3
The mass ratio of graphite powder and metal solvent powder is 65~70:35~30；Graphite powder and metal solvent in the second mixed layer block
The mass ratio of powder is 60~55:40~45；
Preferably, the mass ratio of graphite powder and metal solvent powder is in the first mixed layer block 1 and third mixed layer block 3
65:35, the mass ratio of graphite powder and metal solvent powder is 60:40 in the second mixed layer block.
The present invention also provides another preferred embodiment, the graphite powder is high purity graphite powder, and purity is
>=99.99%, the average grain diameter of graphite powder is 300 mesh；The metal solvent powder by following parts by weight raw material: Fe
68.15%, Ni 30%, Co 1.5%, Mn 0.3% and La 0.05% are prepared using water-aerosolization combined unit；
Its partial size is 400 mesh.
Embodiment 2
This embodiment offers a kind of diamond synthesizing column mixing devices for preparing above-mentioned gradient function, such as Fig. 1, figure
3, shown in Fig. 4, which includes electric control gear 100, cabinet 200, the motor 300 being arranged in cabinet and is arranged outside cabinet
One end of the hopper support bar 400 of portion upper end, the hopper support bar 400 is connect with cabinet 200, and other end end offers
The first hopper fixation hole 401 for hopper 500；
The device further includes the blending bunker 600 being connect by axis 700 (axis periphery is equipped with axle sleeve 701) with motor 300, mixing
Storehouse 600 rotates under motor drive；600 wall of blending bunker is equipped with feed inlet 601, when the device is in feed state
When, the feed inlet 601 is located at the underface of 500 discharge port of material mouth, and the feed inlet 601 is equipped with corresponding sealing cover
602；On the mixing bulkhead, centre bore 603 is additionally provided at centre rotational axis, the centre bore 603, which is equipped with, to be corresponded to
Port lid 604.After throat-fed therein passes through hopper feed, lid is sealed, blending bunker rotation, material therein is mixed
Top is reached by bottom with the rotation of blender in feed bin, bottom is then fallen by top again, is adequately mixed, is mixed
Mixture is discharged by feed inlet after the completion.And the centre bore by being arranged on mixing bulkhead carries out sufficiently the intracorporal material of mixing chamber
Discharge and the cleaning to mixing cavity；
The blending bunker 600 is the blending bunker of ellipse, and oval long axis length is 800~1000mm, ellipse
Minor axis length be 220~250mm；Oval blending bunker is using short axle as center rotary shaft, the angle of long axis and vertical direction
It is 15~20 °.
Further, the hopper support bar 400 includes the first hopper support bar 402 being vertically arranged and horizontal direction
The second hopper support bar 403 being arranged；Wherein one end end of the first hopper support bar 402 detachably connects with cabinet outer upper ends
It connects, the other end end of the first hopper support bar 402 and one end end of second support bar 403 are hinged, the second hopper support bar
403 are rotated up and down relative to the first hopper support bar 402, and the other end end of second support bar 403, which is equipped with, is used for hopper
The first hopper fixation hole.
Further, the wall body of the blending bunker is 304 stainless steel plates with a thickness of 1.5~2.0mm.
Further, as shown in Fig. 2, being additionally provided with cloche 800 outside the blender of the device, the cloche 800 is set
There is the through-hole 801 for passing through hopper lower part.The cloche further avoids during charging and in mixing process, raw material powder
Influence of the dirt to working environment avoids harm and the influence caused by environment caused by staff, and can be certain
The recycling and reusing to raw material is realized in degree.
Therefore, the mixing device through the invention, can be realized the mixing to raw material, and mixing is equal in a short time
It is even, it can effectively avoid the generation of segregation phenomena.Time is short, high-efficient, and compounding effect is good.
Embodiment 3
A kind of preparation method of the diamond synthesizing column of above-mentioned gradient function, method includes the following steps:
(1) the metal solvent powder and ethylene glycol for preparing graphite powder, being prepared；
(2) preparation of graphite and the first mixed layer of catalyst powder block
A. prepare raw material: metal solvent powder 7Kg prepared by high purity graphite powder 13Kg, ethylene glycol 120g, step (1)；
B. the graphite powder of preparation is added in the mixing cavity of disk blender by hopper, ethylene glycol is then added,
Mixing device mixing 15min is opened, graphite powder and the uniform mixture of ethylene glycol are obtained, is shut down, then passes through hopper and feed inlet
The metal solvent powder of preparation is added into mixing cavity, opens mixing device mixing 30min, graphite and metal solvent powder can be obtained
Uniform mixture；
Power of mixing device work is 18kW, in the course of work during this, and the revolving speed of disk blender is 24rpm；
C. the obtained mixture of step b is placed in Doubleroller compaction granulator and is granulated, working speed is 42 turns/min, is made
Grain is completed to obtain feed particles, and the partial size of gained feed particles is 2mm；
D. the obtained feed particles of step c are placed in hydrogen reducing furnace, reduction 6 is small under the conditions of temperature is 1060 DEG C
When, complete the feed particles of reduction treatment；
E. the feed particles of reduction treatment are placed in full-automatic automatic hydraulic press and are suppressed, compressor operation pressure is
40Mpa obtains diameter and is 55mm, is highly the graphite and catalyst powder the first mixed layer block of 10mm；
(3) preparation of graphite and catalyst powder third mixed layer block
The step of repeating step (2), is prepared the preparation of graphite Yu catalyst powder third mixed layer block.
(4) preparation of graphite and the second mixed layer of catalyst powder block
A. prepare raw material: metal solvent powder 8Kg prepared by high purity graphite powder 12Kg, ethylene glycol 120g, step (1)；
B. the graphite powder of preparation is added in the mixing cavity of disk blender by hopper, ethylene glycol is then added,
Mixing device mixing 18min is opened, graphite powder and the uniform mixture of ethylene glycol are obtained, is shut down, then passes through hopper and feed inlet
The metal solvent powder of preparation is added into mixing cavity, opens mixing device mixing 25min, graphite and metal solvent powder can be obtained
Uniform mixture；
Power of mixing device work is 18kW, in the course of work during this, and the revolving speed of disk blender is 24rpm；
C. the obtained mixture of step b is placed in Doubleroller compaction granulator and is granulated, revolving speed is 42 turns/min, has been granulated
At feed particles are obtained, the partial size of gained feed particles is 2mm；
D. the obtained feed particles of step c are placed in hydrogen reducing furnace, reduction 7 is small under the conditions of temperature is 1050 DEG C
When, complete the feed particles of reduction treatment；
E. the feed particles of reduction treatment are placed in full-automatic automatic hydraulic press and are suppressed, compressor operation pressure is
40Mpa obtains diameter and is 55mm, is highly the graphite and catalyst powder the first mixed layer block of 24mm；
(5) preparation of diamond synthesizing column
By the graphite being prepared and the first mixed layer of catalyst powder block, graphite and catalyst powder the second mixed layer block and graphite with
Successively the gradient function diamond synthesizing column can be obtained in parallel superposition to catalyst powder third mixed layer block from bottom to top.
Embodiment 4
A kind of preparation method of the diamond synthesizing column of above-mentioned gradient function, method includes the following steps:
(1) the metal solvent powder that partial size is 400 mesh is prepared according to the preparation method recorded in patent of invention " ", prepares the gold
Belong to the raw materials and consumption of catalyst powder than specific as follows: 68.15%Fe, 30%Ni, 1.5%Co, 0.3%Mn, 0.05%La；
(2) preparation of graphite and the first mixed layer of catalyst powder block
A. prepare raw material: metal solvent powder 7.5Kg prepared by high purity graphite powder 12.5Kg, ethylene glycol 120g, step (1)；
B. the graphite powder of preparation is added in the mixing cavity of disk blender by hopper, ethylene glycol is then added,
Mixing device mixing 25min is opened, graphite powder and the uniform mixture of ethylene glycol are obtained, is shut down, then passes through hopper and feed inlet
The metal solvent powder of preparation is added into mixing cavity, opens mixing device mixing 25min, graphite and metal solvent powder can be obtained
Uniform mixture；
Power of mixing device work is 18kW, in the course of work during this, and the revolving speed of disk blender is 24rpm；
C. the obtained mixture of step b is placed in Doubleroller compaction granulator and is granulated, revolving speed is 42 turns/min, has been granulated
At feed particles are obtained, the partial size of gained feed particles is 2mm；
D. the obtained feed particles of step c are placed in hydrogen reducing furnace, reduction 7 is small under the conditions of temperature is 1060 DEG C
When, complete the feed particles of reduction treatment；
E. the feed particles of reduction treatment are placed in full-automatic automatic hydraulic press and are suppressed, compressor operation pressure is
40Mpa obtains diameter and is 55mm, is highly the graphite and catalyst powder the first mixed layer block of 10mm；
(3) preparation of graphite and catalyst powder third mixed layer block
The step of repeating step (2), is prepared the preparation of graphite Yu catalyst powder third mixed layer block.
(4) preparation of graphite and the second mixed layer of catalyst powder block
A. prepare raw material: metal solvent powder 8Kg prepared by high purity graphite powder 12Kg, ethylene glycol 120g, step (1)；
B. the graphite powder of preparation is added in the mixing cavity of disk blender by hopper, ethylene glycol is then added,
Mixing device mixing 25min is opened, graphite powder and the uniform mixture of ethylene glycol are obtained, is shut down, then passes through hopper and feed inlet
The metal solvent powder of preparation is added into mixing cavity, opens mixing device mixing 25min, graphite and metal solvent powder can be obtained
Uniform mixture；
Power of mixing device work is 18kW, in the course of work during this, and the revolving speed of disk blender is 24rpm；
C. the obtained mixture of step b is placed in Doubleroller compaction granulator and is granulated, revolving speed is 42 turns/min, has been granulated
At feed particles are obtained, the partial size of gained feed particles is 2mm；
D. the obtained feed particles of step c are placed in hydrogen reducing furnace, reduction 7 is small under the conditions of temperature is 1060 DEG C
When, complete the feed particles of reduction treatment；
E. the feed particles of reduction treatment are placed in full-automatic automatic hydraulic press and are suppressed, compressor operation pressure is
40Mpa obtains diameter and is 55mm, is highly the graphite and catalyst powder the first mixed layer block of 24mm；
(5) preparation of diamond synthesizing column
By the graphite being prepared and the first mixed layer of catalyst powder block, graphite and catalyst powder the second mixed layer block and graphite with
Successively the gradient function diamond synthesizing column can be obtained in parallel superposition to catalyst powder third mixed layer block from bottom to top.
Below by concrete application embodiment, gradient function diamond synthesizing column prepared by the present invention is used for diamond
Preparation, it is specific as follows:
Application Example 1
By the gradient function diamond synthesizing column being prepared in above-described embodiment be placed in D800 type cubic hinge press into
Row synthesizes the high grade that main granularity is 35/40, the synthetic diamond single crystal of high self-sharpening.
It is primary to suspend pressure 52MPa, secondary pause pressure 65MPa in synthesis technology (being conventionally synthesized technique), synthesize final pressure
78MPa, total heating time are 45min, and the yield that monolithic synthesizes column is 286 carats, is relatively conventionally synthesized the synthesis output increased of column
5% or so；High-quality ratio >=52% is synthesized, it is 82 that wherein the TI value of HD-9880 monocrystalline, which is 86, TTI value,.
Application Example 2
The gradient function diamond synthesizing column being prepared in above-described embodiment is placed in D800 type cubic hinge press
Synthesize the synthetic diamond single crystal of high grade, high self-sharpening that main granularity is 40/45.
It is primary to suspend pressure 52MPa, secondary pause pressure 65MPa in synthesis technology (being conventionally synthesized technique), synthesize final pressure
77MPa, total heating time are 40min, and the yield that monolithic synthesizes column is 295 carats, and the synthesis yield compared with conventional catalyst mentions
It is high by 10%；High-quality ratio >=55% is synthesized, it is 81 that wherein the TI value of HD-9880 monocrystalline, which is 84, TTI value,.
Application Example 3
The gradient function diamond synthesizing column being prepared in above-described embodiment is placed in D800 type cubic hinge press
Synthesize the synthetic diamond single crystal of high grade, high self-sharpening that main granularity is 45/50.
It is primary to suspend pressure 52MPa, secondary pause pressure 65MPa in synthesis technology, final pressure 77MPa is synthesized, always when heating
Between be 40min, monolithic synthesize column yield be 298 carats, compared with the synthesis output increased 10% of conventional catalyst；It synthesizes high-quality
Than >=53%, it is 81 that wherein the TI value of HD-9860 monocrystalline, which is 85, TTI value,.
Can be obtained by above content: the present invention is using preferable mixing device and reasonably probes into design, makes gained gradient function
The diamond synthesizing column of energyization can significantly improve the quality and yield of diamond synthesis in diamond synthesizing, close in diamond
Cheng Zhong, high grade diamond, the synthesis quality of especially high grade high self-sharpening diamond and output increased difficulty are all very big, this
Invention significantly improves high grade, the yield of high self-sharpening diamond using the diamond synthesizing column of gradient function, obtains
Diamond yield is high, high-quality, has a good application prospect.
Claims (10)
1. a kind of diamond synthesizing column of gradient function, which is characterized in that the synthesis column includes that graphite and catalyst powder first are mixed
It closes layer block (1), the graphite and the second mixed layer of catalyst powder block (2) being arranged in parallel on the first mixed layer block (1), and sets in parallel
Set graphite and catalyst powder third mixed layer block (3) on the second mixed layer block (2)；The first mixed layer block (1), second mix
The diameter for closing layer block (2) and third mixed layer block (3) is equal.
2. the diamond synthesizing column of gradient function according to claim 1, which is characterized in that the graphite and catalyst powder
First mixed layer block (1) and graphite are equal with the height of catalyst powder third mixed layer block (3), and lower than graphite and catalyst powder second
The height of mixed layer block (2)；
The height of the graphite and the second mixed layer of catalyst powder block (2) be graphite and the first mixed layer of catalyst powder block (1) 2.2~
2.5 again.
3. according to claim 1 or the diamond synthesizing column of 2 described in any item gradient functions, which is characterized in that the stone
The mass ratio of ink and graphite and catalyst powder in the first mixed layer of catalyst powder block (1) and graphite and catalyst powder third mixed layer block (3)
It is identical；Graphite and the mass ratio of catalyst powder are graphite and catalyst powder first in the graphite and the second mixed layer of catalyst powder block (2)
0.5~1.0 times of graphite and catalyst powder mass ratio in mixed layer block (1).
4. the diamond synthesizing column of gradient function according to claim 3, which is characterized in that the graphite and catalyst powder
Graphite and the mass ratio of catalyst powder are 62~70:30 in first mixed layer block (1) and graphite and catalyst powder third mixed layer block (3)
~38；Graphite and the mass ratio of catalyst powder are 60~55:40~45 in the graphite and the second mixed layer of catalyst powder block (2)；
Wherein, the graphite is high purity graphite powder, and partial size is 300 mesh；
The catalyst powder includes the raw material of following parts by weight: Fe 68.15%, Ni 30%, Co 1.5%, Mn 0.3% and La
0.05%；Its partial size is 400 mesh.
5. a kind of diamond synthesizing column mixing device for preparing gradient function described in claim 1, which is characterized in that the dress
It sets including electric control gear (100), cabinet (200), the motor (300) being arranged in cabinet (200) and is arranged in cabinet (200)
The hopper support bar (400) of outer upper ends, one end of the hopper support bar (400) connect with cabinet (200), other end end
Offer the first hopper fixation hole (401) for hopper (500)；
The device further includes the blending bunker (600) being connected by axis (700) with motor (300)；Described blending bunker (600) wall
It is equipped with feed inlet (601), when being in feed state, the feed inlet (601) is located at the underface of hopper (500)；
The electric control gear (100) is connected with motor (300).
6. the diamond synthesizing column mixing device according to claim 5 for preparing gradient function, which is characterized in that institute
The hopper support bar (400) stated includes the first hopper support bar (402) and horizontally disposed second hopper support being vertically arranged
One end end of bar (403), the first hopper support bar (402) is detachably connected with cabinet, the first hopper support bar (402) it is another
One end end and one end end of the second hopper support bar (403) are hinged, and the other end end of the second hopper support bar (403) is set
It is equipped with the first hopper fixation hole (401) for hopper (500)；
Corresponding sealing cover (602) is additionally provided on the blending bunker feed inlet (601)；On the mixing bulkhead, it is located at center
It is additionally provided at rotary shaft centre bore (603), the centre bore is additionally provided with corresponding port lid (604).
7. the diamond synthesizing column mixing device according to claim 5 for preparing gradient function, which is characterized in that institute
Axis (700) periphery stated is additionally provided with axle sleeve (701)；Cloche (800), cloche are additionally provided with outside the disk blender
(800) it is equipped with for the through-hole (801) across hopper lower part.
8. special according to the described in any item diamond synthesizing column mixing devices for preparing gradient function of claim 5~7
Sign is that the blending bunker (600) is the blending bunker of ellipse, and oval long axis length is 800~1000mm, ellipse
Minor axis length be 220~250mm；Oval blending bunker is using short axle as center rotary shaft, the angle of long axis and vertical direction
It is 15~20 °；The wall body of the blending bunker is 304 stainless steel plates with a thickness of 1.5~2.0mm.
9. a kind of preparation method of the diamond synthesizing column of gradient function described in claim 1, this method includes mixing, makes
Grain, reduction treatment, cold moudling；It is characterized in that, specific step is as follows:
(1) preparation of graphite and catalyst powder the first mixed layer block and graphite and catalyst powder third mixed layer block:
A. required raw graphite powder, catalyst powder and ethylene glycol are added in mixing device as claimed in claim 7 and are mixed
It closes；
B. the mixed material of step a is subjected to granulation processing, obtains feed particles；
C. feed particles step b obtained carry out reduction treatment, obtain reduction particle；
D. cold moudling is carried out to the reduction particle that step c is obtained, graphite and catalyst powder first is obtained after the completion of cold moudling
Mixed layer block；
E. step a, b, c, d are repeated, graphite and catalyst powder third mixed layer block is prepared；
(2) preparation of graphite and the second mixed layer of catalyst powder block:
Graphite and the second mixed layer of catalyst powder block are prepared according to step described in step (1)；
(3) graphite and the second mixed layer of the first mixed layer of catalyst powder, graphite and catalyst powder for preparing step (1) and step (2)
Block, block, graphite and catalyst powder third mixed layer block are stacked according to sequential parallel from bottom to top, and the gradient function can be obtained
The diamond synthesizing column of energyization.
10. the preparation method of the diamond synthesizing column of gradient function according to claim 9, which is characterized in that step a
The mass ratio of the graphite powder, catalyst powder and ethylene glycol is 62~70:30~38:0.12；Step (2) graphite and catalyst powder
In second mixed layer block preparation process, the mass ratio of graphite powder, metal solvent powder and ethylene glycol are as follows: 60~55:40~45:
0.12；
The method of mixing described in step a is specific as follows: the graphite powder of preparation being placed in mixing device, it is mixed that ethylene glycol is then added
It closes uniformly, shuts down, catalyst powder is added, booting is uniformly mixed to arrive uniform mixture；
The graphite powder and the ethylene glycol mixing time in mixing device are 15~25min, the mixing time after catalyst powder is added
For 20~30min；Power of motor is 15~20kW when mixing, motor speed is 0~50rpm；
Granulation described in step b carries out in Doubleroller compaction granulator, and the working speed of pelletizer is 42 turns/min, obtains after the completion of being granulated
The partial size of feed particles is 2mm；
Reduction treatment described in step c carries out in hydrogen reducing furnace, and temperature when feed particles restore is 1000~1100 DEG C, goes back
The former time is 6~8 hours；
Processing is pressed in cold moudling described in step d in automatic hydraulic press, and the operating pressure of automatic hydraulic press is
40MPa。
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| CN115337866A (en) * | 2022-08-26 | 2022-11-15 | 中南钻石有限公司 | Seed crystal seed distribution method for synthesizing colorless diamond by powder catalyst constant temperature method |
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