CN109589870A - A kind of graphene reinforcing polycrystalline diamond preparation method - Google Patents
A kind of graphene reinforcing polycrystalline diamond preparation method Download PDFInfo
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- CN109589870A CN109589870A CN201910029344.8A CN201910029344A CN109589870A CN 109589870 A CN109589870 A CN 109589870A CN 201910029344 A CN201910029344 A CN 201910029344A CN 109589870 A CN109589870 A CN 109589870A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
- B01J3/067—Presses using a plurality of pressing members working in different directions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
Abstract
A kind of graphene strengthens the preparation method of polycrystalline diamond, utilize six or eight press of walker type, sample cavity is that regular octahedron composed by one jiao of tungsten carbide cubic block is clipped as eight, six or eight press of Walker type can reach higher chamber pressure, can satisfy the requirement for strengthening polycrystalline diamond experiment condition to graphene.Good " lubrication " characteristic of graphene, so that then the friction between diamond particles is sharply reduced, the mobility of particle increases, it can cause further to be compacted, and the addition of graphene, in sintering process, graphene is full of between diamond particles, a uniform pressure field is formd in inside, when pressure reaches the stable region of diamond precipitation, carbon in solvent-carbon system will be precipitated in these gaps in the form of diamond, so that fine grained micro mist is grown up, it overlaps with neighboring particles, reduce the surface free energy of particle, it is formed and stablizes fine and close plycrystalline diamond sintered body, and it is finally completed polycrystalline diamond sintering.
Description
Technical field
The present invention relates to a kind of polycrystalline diamonds, and in particular to and a kind of graphene strengthens the preparation method of polycrystalline diamond,
Belong to materialogy field.
Background technique
Polycrystalline diamond-Ka Bangnaduo (Carbonado) in nature causes material circle because of its excellent performance
Note that people begin one's study, preparation has the man-made polycrystalline diamond material of similar performance.Containing micro in " Ka Bangnaduo "
Metal and nonmetallic inclusion are made of countless tiny diamond particles, they are in disorderly arranged, also without cleavage surface, but
With high intensity, hardness and wearability.These performance characteristics are superior to natural bulky diamond monocrystalline.These are better than
The performance of single-crystalline diamond, the idealization requirement for making it very meet people to particularity wear resistant cutters.Artificial diamond
Stone material (Polycrystalline Diamond, abbreviation PCD) polycrystalline diamond, is that diadust is burnt under high pressure
It ties, the capital equipment currently used for synthesizing polycrystalline diamond is cubic hydraulic press and two faces top hydraulic press, and the country is main
With cubic hydraulic press, and external then generally use two faces top hydraulic press compacting polycrystalline diamond.This novel superhard material of PCD
Material is widely used among the Geological Engineerings operation such as geological core drilling and oil exploitation probing, in oil and gas well drilling
It is also the continuous emphasis studied and break through with fields such as Geological Engineering explorations, but it is applied under the conditions of certain extreme operating environments
The effect is unsatisfactory.
Country's polycrystalline diamond synthesis at present, since the original bulk density of diamond particles is low, hole is more, in high temperature height
Pressure, particle are contacted with another particle, and diamond belongs in conjunction with strong bond between diamond particles, and crystal grain, which contacts with each other, locates pressure
Height makes diamond particles itself fragmentation, and the fragmentation diamond particles that fragmentation generates largely still are concentrated in situ, are not had
It is filled into the larger gap of coarse-grain intergranular formation, and is not also filled out by binder all between the crystal boundary of the diamond of fragmentation
It fills.Being uniformly distributed for binder phase is thus affected, so that eventually leading to the wearability of PCD reduces.
Simultaneously in the inside of high temperature and pressure diamond synthesis plycrystalline diamond, pressure be not it is uniform, hydrostatic pressing is a kind of reason
Think state.When the certain pressure of external application, pressure is transmitted simply by the contact point of diamond, and between particles
Gap, do not contact between diamond particles, surface does not stress, these diamond surfaces are in low-voltage high-temperature area, causes
The graphited generation of grain, eventually leads to PDC sintered body strength reduction.
This project proposed adoption graphene strengthens polycrystalline diamond and corresponding preparation means further increase its intensity, densification
Property, wearability are to cope with various complex stratigraphic drillings.
The addition of certain proportion graphene can between diamond particles in play good lubricating action, in high-pressure section
Intergranular frictional resistance is reduced under part, promotes the filling in fragmentation diamond gap, promotes being uniformly distributed for binder phase, is increased
Small grains, to make to form more fine and close, uniform structure in polycrystalline diamond.It is divided into the process for preparing polycrystalline diamond
The process that is precipitated after phase transition process and the diamond dissolution of carbon atom, in sintering process, graphene is full of between diamond particles,
When inside forms a uniform pressure field, and pressure reaches the stable region of diamond precipitation, in solvent-carbon system
Carbon will be precipitated in these gaps in the form of diamond so that fine grained micro mist is grown up, overlap with neighboring particles,
The surface free energy of particle is reduced, is formed and stablizes fine and close plycrystalline diamond sintered body, improve the intensity and wearability of polycrystalline diamond.
Summary of the invention
The object of the present invention is to provide the preparation methods that a kind of graphene strengthens polycrystalline diamond.
Its main feature is that Walker type two-stage pressurizing device, sample cavity is clipped by eight using six or eight press of walker type
Regular octahedron composed by one jiao of tungsten carbide cubic block, since the pressure of domestic hinge type cubic apparatus being often used at present is usual
In 6GPa hereinafter, six or eight press of Walker type, which is compared, can reach higher chamber pressure, energy for more domestic cubic hinge press
Enough meet us and strengthens the requirement of polycrystalline diamond experiment condition to graphene.Good " lubrication " characteristic of graphene, so that then
Friction between diamond particles is sharply reduced, and the mobility of particle increases, and can cause further to be compacted, and centainly match
The addition of graphene, in sintering process, graphene is full of between diamond particles, forms a uniform pressure in inside
, when pressure reaches the stable region of diamond precipitation, the carbon in solvent-carbon system will be in the form of diamond at these
It is precipitated in gap, so that fine grained micro mist is grown up, overlaps with neighboring particles, reduce the surface free energy of particle, shape
At stable fine and close plycrystalline diamond sintered body, and it is finally completed polycrystalline diamond sintering.
A kind of graphene strengthens the preparation method of polycrystalline diamond.This method is:
According to material composition and the diadust of quality proportioning addition graphene, according to assemble sequence, in Walker type
The process curve sintering that six or eight press are set obtains a kind of graphene reinforcing polycrystalline diamond, compared with not adding graphene,
Its intensity, wearability improve.
It is six or eight swaging machine of walker type that the graphene, which strengthens polycrystalline diamond agglomerating plant,.
The pressure P, temperature T, sintering duration t that the sintering uses, pressure P are 7~9GPa, and temperature T is 1400 DEG C,
Sintering duration t is 15min.
The material composition and quality proportioning: diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-
0.3wt%;
The diadust is 30-50um;
The bonding agent silicon powder partial size is less than 5um;
The graphene nanometer sheet thickness 6-8nm, it is 5 μm wide.
Polycrystalline diamond preparation method of the invention comprising the following specific steps
One, diadust is surface-treated, then carries out high temperature and pressure sintering, and the strength of materials and wearability of acquisition are very
It is high.The purifying treatment method used is put into long-neck for chemical method, by 1 part of diadust and 4~5 parts of solids NaOH or KOH
In silver or nickel crucible, it is heated to 870K or so, stops heating after making lye pinkiness, is poured on stainless steel before lye does not solidify
On plate, then condensation block is put into container and is dissolved with water, neutralized after removing solution with acid, remove remaining pyrophillite in sample
Equal impurity;Kish impurity is cooked off with chloroazotic acid or other acid heating, distillation is washed to neutrality, is put into drying receptacle after dry
It is spare.
Two, by diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-0.3wt% is weighed, wherein in stone
Polyvinylpyrrolidone dispersing agent is added in black alkene and passes through ultrasonic disperse in ethanol, removes solvent, and sufficiently drying is dispersed
Good graphene powder.By diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-0.3wt% is in ball mill
Lower uniformly to be mixed, ball milling uses ratio of grinding media to material 1:1, and mixing material quality is 0.5-2g, dehydrated alcohol 10ml, revolving speed 600r/
Min, bulb diameter 2mm.Alcohol is added every 30min in mechanical milling process, ball milling stopped ball milling after 48 hours.Open ball grinder
Afterwards, dry to vaporized alcohol, the diamond powder of mixed incorporation adhesive is initially charged in graphite cup, it then will be charged
Graphite cup, which is placed in vacuum drying oven, carries out vacuum heat treatment, removes oxygen, the vapor of powder adsorption, and make its surface have compared with
Good reactivity.During heating, maximum temperature is 650 DEG C in vacuum drying oven, and vacuum degree is 3 × 10-3Pa.
Three, by the mixed-powder of step 2 using first cold-press moulding, the method for hot repressing sintering is obtained step 2 mixed
Dusty material is closed, compressing tablet process is carried out in swager, tabletting is put by magnesia octahedron block.
Four, six or eight swaging machine cavity packaging technology of walker type: the experiment of Walker type six or eight is 10- selected by the present invention
3 assemblings, sealing edge are made of MDX-540 model engraving machine, and sealing edge plays support and seal chamber in high temperature and pressure assembling
The effect of body, the quality of the shape and size of made sealing edge directly affect the sealing performance of high temperature and pressure cavity, determine
The stability of high-potting.It is rhenium metal used in heating tube.Sample loads in sequence.Sample loaded after by sealing edge
It is first assembled into eight cube tungsten carbide fritters in order with assembling block shown.The cube of eight cube fritters composition is put
It sets in the cube cavity being made of six converted steel wedge type blocks, 20h is raised to 400bar, is then heated, heating mode
It is to be heated by the input of power percentage, slow release after the completion of heating.
Five, sintering process are as follows: pressure P is 7~9GPa, and temperature T is 1400 DEG C, and sintering duration t is 15min.
Beneficial effects of the present invention:
The pressure that traditional cubic hinge press uses is usually in 6GPa hereinafter, and graphene strengthens the condition of polycrystalline diamond
It is required that being just able to achieve in 7GPa or more, the present invention is utilized at six or eight press two-stage pressurizing of Walker type and specific technique sintering
Reason realizes that graphene strengthens the preparation of polycrystalline diamond.The addition of certain proportion graphene can between diamond particles in rise
To good lubricating action, intergranular frictional resistance is reduced under high pressure, is promoted the filling in fragmentation diamond gap, is mentioned
Being uniformly distributed for binder phase is risen, increases small grains, to make to form more fine and close, uniform structure in polycrystalline diamond.
The process being precipitated after the process for preparing polycrystalline diamond is divided into the phase transition process of carbon atom and diamond dissolves, sintering process
In, graphene is full of between diamond particles, forms a uniform pressure field in inside, pressure reaches diamond precipitation
When stable region, the carbon in solvent-carbon system will be precipitated in these gaps in the form of diamond, so that fine grained is micro-
Powder is grown up, and is overlapped with neighboring particles, and the surface free energy of particle is reduced, and is formed and is stablized fine and close plycrystalline diamond sintered body,
Improve the intensity and wearability of polycrystalline diamond.
Detailed description of the invention
Fig. 1 is magnesia octahedron block assembling block structure schematic diagram.
Fig. 2 is the structure chart that graphene strengthens polycrystalline diamond.
Fig. 3 is that graphene strengthens polycrystalline diamond electron microscope.
Wherein: 1- magnesia;2- rhenium pipe;3- alumina ceramic tube;4- Lanthanum Chromite pipe;Tetra- porous aluminum oxide pipe of 5-;6- thermoelectricity
It is even;7- alumina wafer;8- sample;9- magnesia;10- zirconium oxide;11- graphene and binder;12- diamond crystal;13- gold
Hard rock-diamond is bonded.
Specific embodiment
A kind of graphene strengthens the preparation method of polycrystalline diamond.This method is:
According to material composition and the diadust of quality proportioning addition graphene, according to assemble sequence, in Walker type
The process curve sintering that six or eight press are set obtains a kind of graphene reinforcing polycrystalline diamond, compared with not adding graphene,
Its intensity and wearability improve.
It is six or eight swaging machine of walker type that the graphene, which strengthens polycrystalline diamond agglomerating plant,.
The pressure P, temperature T, sintering duration t that the sintering uses, pressure P are 7~9GPa, and temperature T is 1400 DEG C,
Sintering duration t is 15min.
The material composition and quality proportioning: diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-
0.3wt%;
The diadust is 30-50um;
The bonding agent silicon powder partial size is less than 5um;
The graphene nanometer sheet thickness 6-8nm, it is 5 μm wide.
Polycrystalline diamond preparation method of the invention comprising the following specific steps
One, diadust is surface-treated, then carries out high temperature and pressure sintering, and the strength of materials and wearability of acquisition are very
It is high.The purifying treatment method used is put into long-neck for chemical method, by 1 part of diadust and 4~5 parts of solids NaOH or KOH
In silver or nickel crucible, it is heated to 870K or so, stops heating after making lye pinkiness, is poured on stainless steel before lye does not solidify
On plate, then condensation block is put into container and is dissolved with water, neutralized after removing solution with acid, remove remaining pyrophillite in sample
Equal impurity;Kish impurity is cooked off with chloroazotic acid or other acid heating, distillation is washed to neutrality, is put into drying receptacle after dry
It is spare.
Two, by diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-0.3wt% is weighed, wherein in stone
Polyvinylpyrrolidone dispersing agent is added in black alkene and passes through ultrasonic disperse in ethanol, removes solvent, and sufficiently drying is dispersed
Good graphene powder.By diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-0.3wt% is in ball mill
Lower uniformly to be mixed, ball milling uses ratio of grinding media to material 1:1, and mixing material quality is 0.5-2g, dehydrated alcohol 10ml, revolving speed 600r/
Min, bulb diameter 2mm.Alcohol is added every 30min in mechanical milling process, ball milling stopped ball milling after 48 hours.Open ball grinder
Afterwards, dry to vaporized alcohol, the diamond powder of mixed incorporation adhesive is initially charged in graphite cup, it then will be charged
Graphite cup, which is placed in vacuum drying oven, carries out vacuum heat treatment, removes oxygen, the vapor of powder adsorption, and make its surface have compared with
Good reactivity.During heating, maximum temperature is 650 DEG C in vacuum drying oven, and vacuum degree is 3 × 10-3Pa.
Three, by the mixed-powder of step 2 using first cold-press moulding, the method for hot repressing sintering is obtained step 2 mixed
Dusty material is closed, compressing tablet process is carried out in swager, tabletting is put by magnesia octahedron block, magnesia octahedron block group
It is as shown in Fig. 1 to fill block, by magnesia 1, rhenium pipe 2, alumina ceramic tube 3, Lanthanum Chromite pipe 4, four porous aluminum oxide pipes 5, thermocouple
6, alumina wafer 7, sample 8, magnesia 9 and zirconium oxide 10 form.
Four, six or eight swaging machine cavity packaging technology of walker type: the experiment of Walker type six or eight is 10- selected by the present invention
3 assemblings, sealing edge are made of MDX-540 model engraving machine, and sealing edge plays support and seal chamber in high temperature and pressure assembling
The effect of body, the quality of the shape and size of made sealing edge directly affect the sealing performance of high temperature and pressure cavity, determine
The stability of high-potting.It is rhenium metal used in heating tube.Sample loads in sequence.Sample loaded after by sealing edge
It is first assembled into eight cube tungsten carbide fritters in order with magnesia octahedron block assembling block shown.Eight cube fritters
The cube of composition is placed in the cube cavity being made of six converted steel wedge type blocks, and 20h is raised to 400bar, is then carried out
Heating, heating mode are heated by the input of power percentage, and slow release is carried out after the completion of heating.
Five, sintering process are as follows: pressure P is 7~9GPa, and temperature T is 1400 DEG C, and sintering duration t is 15min.
Fig. 2 is the structure chart that graphene strengthens polycrystalline diamond, and internal structure includes graphene and binder 11, Buddha's warrior attendant
Stone crystal 12 and diamond-diamond bonded 13.
Fig. 3 is that graphene strengthens polycrystalline diamond electron microscope.
Claims (2)
1. the preparation method that a kind of graphene strengthens polycrystalline diamond, it is characterised in that: this method is:
According to material composition and the diadust of quality proportioning addition graphene, according to assemble sequence, in Walker type six or eight
The process curve sintering that press is set, obtains graphene and strengthens polycrystalline diamond;
It is six or eight press of walker type that the graphene, which strengthens polycrystalline diamond agglomerating plant,;
The pressure P, temperature T, sintering duration t that the sintering uses, pressure P are 7~9GPa, and temperature T is 1400 DEG C, sintering
Duration t is 15min;
The material composition and quality proportioning: diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-
0.3wt%;
The diadust is 30-50um;
The bonding agent silicon powder partial size is less than 5um;
The graphene nanometer sheet thickness 6-8nm, it is 5 μm wide.
2. the preparation method that a kind of graphene strengthens polycrystalline diamond, it is characterised in that: comprising the following specific steps
One, diadust is surface-treated, then carries out high temperature and pressure sintering, and the strength of materials and wearability of acquisition are very high;
The purifying treatment method used for chemical method, by 1 part of diadust and 4~5 parts of solids NaOH or KOH be put into long-neck silver or
In nickel crucible, it is heated to 870K or so, stops heating after making lye pinkiness, is poured on stainless steel plate before lye does not solidify
On, then condensation block is put into container and is dissolved with water, is neutralized after removing solution with acid, removes remaining pyrophillite etc. in sample
Impurity;Kish impurity is cooked off with chloroazotic acid or other acid heating, distillation is washed to neutrality, is put into after dry standby in drying receptacle
With;
Two, by diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-0.3wt% is weighed, wherein in graphene
Middle addition polyvinylpyrrolidone dispersing agent in ethanol, removes solvent by ultrasonic disperse, and sufficiently drying obtains scattered
Graphene powder.By diadust 85-95wt%, Si powder 5-10wt%, graphene 0.05-0.3wt% under ball mill into
Row uniformly mixing, ball milling use ratio of grinding media to material 1:1, mixing material quality be 0.5-2g, dehydrated alcohol 10ml, revolving speed 600r/min,
Bulb diameter is 2mm;Alcohol is added every 30min in mechanical milling process, ball milling stopped ball milling after 48 hours;After opening ball grinder,
It is dry to vaporized alcohol, the diamond powder of mixed incorporation adhesive is initially charged in graphite cup, then by charged stone
Ink cup, which is placed in vacuum drying oven, carries out vacuum heat treatment, removes oxygen, the vapor of powder adsorption, and it is preferable to have its surface
Reactivity;During heating, maximum temperature is 650 DEG C in vacuum drying oven, and vacuum degree is 3 × 10-3Pa;
Three, by the mixed-powder of step 2 using first cold-press moulding, the method for hot repressing sintering, the mixed powder that step 2 is obtained
Powder material carries out compressing tablet process in swager, tabletting is put by magnesia octahedron block;
Four, six or eight press cavity packaging technology of walker type: the experiment of Walker type six or eight of selection is 10-3 assembling, and sealing edge is
It is made of MDX-540 model engraving machine;It is rhenium metal used in heating tube;Sample loads in sequence;Sample will after having loaded
Sealing edge and magnesia octahedron block assembling block are first assembled into eight cube tungsten carbide fritters in order;Eight cubes are small
Block composition cube be placed in the cube cavity being made of six converted steel wedge type blocks, 20h is raised to 400bar, then into
Row heating, heating mode are heated by the input of power percentage, and slow release is carried out after the completion of heating;
Five, sintering process are as follows: pressure P is 7~9GPa, and temperature T is 1400 DEG C, and sintering duration t is 15min.
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CN110090963A (en) * | 2019-05-27 | 2019-08-06 | 吉林大学 | A kind of high tenacity conductivity type composite polycrystal-diamond and preparation method thereof |
CN110253024A (en) * | 2019-07-22 | 2019-09-20 | 吉林大学 | A kind of diamond compact and preparation method thereof containing graphene |
CN115338420A (en) * | 2022-08-24 | 2022-11-15 | 河南四方达超硬材料股份有限公司 | Polycrystalline diamond precursor material and preparation method thereof, polycrystalline diamond and preparation method thereof, and polycrystalline diamond composite material and preparation method thereof |
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CN115338420A (en) * | 2022-08-24 | 2022-11-15 | 河南四方达超硬材料股份有限公司 | Polycrystalline diamond precursor material and preparation method thereof, polycrystalline diamond and preparation method thereof, and polycrystalline diamond composite material and preparation method thereof |
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