CN105349965B - A kind of composite polycrystal-diamond and preparation method thereof - Google Patents
A kind of composite polycrystal-diamond and preparation method thereof Download PDFInfo
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- CN105349965B CN105349965B CN201510734565.7A CN201510734565A CN105349965B CN 105349965 B CN105349965 B CN 105349965B CN 201510734565 A CN201510734565 A CN 201510734565A CN 105349965 B CN105349965 B CN 105349965B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/271—Diamond only using hot filaments
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Abstract
A kind of composite polycrystal-diamond and preparation method thereof, the composite sheet includes columned composite sheet matrix and operative end surface, the polycrystalline diamond layer that the composite sheet matrix includes cemented carbide substrate and cemented carbide substrate upper surface covers, operative end surface is located at the upper surface of polycrystalline diamond layer, the operative end surface is equipped with multi-layer nano diamond layer, and every layer of nano-diamond layer includes the different nano-crystalline layers of two layers of average grain size.Its preparation method is：（1）Prepare composite sheet matrix；（2）Pre-treatment；（3）CVD plated films；（4）To the polishing treatment of Nano diamond layer surface to obtain the final product.In the outer layer coated with multiple layer nano-diamond layer of composite sheet, the wearability of composite polycrystal-diamond is improved, impact resistance, toughness extends the service life of composite sheet；Method using the present invention is prepared for a kind of with good wearability, heat-resisting quantity and shock resistance composite polycrystal-diamond.
Description
Technical field
Present invention relates particularly to a kind of composite polycrystal-diamonds and preparation method thereof.
Background technology
Composite polycrystal-diamond（Polycrystalline Diamond Compact, lower abbreviation PDC composite sheets）It is one
Plant the composite material for being covered in cemented carbide substrate surfaces by polycrystalline diamond layer and being formed.It has had both polycrystalline diamond layer
The advantages that high-wearing feature and the toughness of hard alloy, solderability, therefore as efficient cutting tool material and excellent wear-resisting
Material, and it is widely used in oil and the fields such as geological drilling and mechanical processing.
In practical applications, due to composite polycrystal-diamond（PDC）Catalyst containing Co, Ni, Fe etc., the presence of Co makes
Composite sheet is not resistant to 700 DEG C of high temperature under normal pressure, also, Co is present in the interface of diamond DD keys, Co and diamond
The coefficient of expansion it is different, thermal stress can be generated, so as to cause the stress damage of composite sheet.
At present, high-end composite sheet improves wearability, the heat-resisting quantity of composite sheet by taking off cobalt processing, but de- cobalt processing is only
Surface can be made to take off Co, internal layer Co still has, and after certain abrasion, new wear surface occurs, the presence of Co still into
The reason for reduce the comprehensive mechanical performance of composite sheet.Studies have found that：Composite polycrystal-diamond containing Co is taken off into Co processing
Afterwards, composite sheet surface is present with substantial amounts of small holes, and then reduces the wearability of composite sheet.
Separately there is research to point out：Use chemical deposition（CVD）PDC surfaces or the internal millimetre-sized Buddha's warrior attendant of deposition after de- Co
Stone film or thick film form diamond nucleation, can promote the wearability of composite sheet.However this method still has following deficiency：
I.e. since the Co inside composite polycrystal-diamond is still remained, and CVD temperature is generally at 800~1000 DEG C, when temperature is higher than
At 400 DEG C, Co starts to expand between diamond crystals, and Co volumes become larger, and thermal stress causes it abnormal with diamond contact position
Change can increase, and occur substantial amounts of thermal defect inside polycrystalline diamond, cause hydraulic performance decline.
Also research is pointed out：Composite polycrystal-diamond uses the binding agent without Co, although eliminating remaining Co to poly-
The influence of the thermal stability of diamond composite sheet, but this composite polycrystal-diamond for DD bond close, composite sheet it is wear-resisting
Property be deteriorated.
The content of the invention
Present invention aims at a kind of composite polycrystal-diamond of offer, while provide the system of the composite polycrystal-diamond
Preparation Method is second goal of the invention of the present invention.
Based on above-mentioned purpose, the present invention adopts the following technical scheme that：A kind of composite polycrystal-diamond, including columned
Composite sheet matrix and operative end surface, the composite sheet matrix are covered including cemented carbide substrate and cemented carbide substrate upper surface
Polycrystalline diamond layer, the operative end surface are located at the upper surface of polycrystalline diamond layer, and the operative end surface is equipped with multi-layer nano
Diamond layer, every layer of nano-diamond layer include the different nano-crystalline layers of two layers of average grain size.
Multi-layer nano diamond layer is equipped on the side of the polycrystalline diamond layer or the side of composite sheet matrix.
The average grain size for two layers of nano-crystalline layers that every layer of nano-diamond layer includes be respectively 20~40nm and 60~
80nm；The thickness of every layer of nano-crystalline layers is 0.3~0.5 μm.If the study found that when the crystalline size of crystal layer is larger, reach micro-
During the crystalline size of meter level, brittleness is larger, and is also easy to produce cleavage surface cleavage, and microcrystalline region easily cracks, can not be effective
Crackle is prevented to reach hard alloy substrate from crystal boundaries.
The overall thickness of multi-layer nano diamond layer is 6 ~ 20 μm.
A kind of preparation method of composite polycrystal-diamond, comprises the following steps：
（1）Prepare composite sheet matrix：The composite sheet matrix includes cemented carbide substrate and cemented carbide substrate upper surface
The polycrystalline diamond layer of covering, the upper surface of the polycrystalline diamond layer are machined with operative end surface；
（2）Pre-treatment：After the polishing of composite sheet matrix surface, oil removing, cleaning and drying, 2~5s or use are acidified through chloroazotic acid
After sand-blasting machine is to its surface sand-blasting, then enter filming process after surface degreasing, cleaning, drying；
（3）CVD plated films：Composite sheet matrix after pre-treatment is placed on the chip bench of CVD heated filament Diamond Equipments,
Multi-layer nano diamond layer is deposited in the operative end surface of composite sheet matrix, every layer of nano-diamond layer includes two layers of average crystal grain ruler
Very little different nano-crystalline layers；
（4）To Nano diamond layer surface polishing treatment up to composite polycrystal-diamond.
Step（3）In, while the operative end surface to composite sheet matrix deposits multi-layer nano diamond layer, to glomerocryst gold
Multi-layer nano diamond layer is deposited on the side of hard rock layer or the side of composite sheet matrix.
The concrete operations for preparing composite sheet matrix are：Bortz powder and binding agent are mixed, with hard aluminium alloy matrix 5
~5.5GPa, 3~8min of sintering obtains cemented carbide substrate upper surface covered with polycrystalline diamond layer at 1400~1600 DEG C
Composite sheet matrix blank, by composite sheet matrix blank by obtaining the upper end of polycrystalline diamond layer after grinding processing, finishing processing
Face is machined with the composite sheet matrix of operative end surface；With volume percentage, the bortz powder is 45~90%, binding agent 10
~55%；The binding agent is superhard refractory ceramics nitride material；The bortz powder is prepared by volumes below number：55
~60 parts, 2~4 μm of bortz powders, 30~40 parts, 6~8 μm 5~20 parts of bortz powders.
The binding agent is one kind in the nitride of IVB, VIB, IIIA, IVA element in the periodic table of chemical element
Or two or more combination.
The binding agent is the mixture of the three kinds or more in TiN, ZrN, CrN, AlN and SiN.
CVD plated films specifically include following steps：
a）Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, is evacuated to 0.6~0.8Pa heating
Substrate temperature is passed through CH to 700~900 DEG C4And H2, vacuum degree to 0.1~0.3Pa, composite sheet matrix surface forming core, simultaneously lead to
Enter inert gas shielding, 0.1~0.5Pa of air pressure of inert gas；
b）Hot-wire temperature is adjusted, one layer of 0.3~0.5 μ m-thick of deposition is nanocrystalline in the operative end surface of composite sheet matrix
Layer, the average grain size of the nano-crystalline layers is 20~40nm；
c）Hot-wire temperature is adjusted, the nanometer of redeposited one layer of 0.3~0.5 μ m-thick on the nano-crystalline layers formed in previous step
Crystal layer, the average grain size of the nano-crystalline layers is 60~80nm；
d）Repeat step b）And c）Until plated film terminates.
Compared with the prior art, beneficial effects of the present invention are：
1）The outer layer of composite sheet provided by the present invention is equipped with multi-layer nano diamond layer, with cemented carbide substrate and glomerocryst
Diamond layer coordinates, and improves the wearability of composite polycrystal-diamond product, impact resistance and toughness, extends composite sheet
Service life；
2）The multi-layer nano diamond layer of the present invention is using 20~40nm and the different average grain sizes of two kinds of 60~80nm
Nano-crystalline layers be arranged alternately, be integrally formed protection film layer, on the one hand, be conducive to hinder by the way of this be arranged alternately
The extension of crackle is kept off, makes the crackle that part is sponged at the big nano-crystalline layers of crystallite dimension, further increases composite sheet
Impact resistance and toughness；On the other hand, the study found that when crystalline size is larger, when reaching micro-crystal, brittleness is larger, and easily
Cleavage surface cleavage is generated, microcrystalline region easily cracks, and crackle can not effectively be prevented to reach matrix from crystal boundaries.Therefore
The average grain size of nano-crystalline layers of the present invention is controlled in nano-scale range, and the total surface area of sedimentary diamond increases,
Extraneous crackle is extended along crystal boundary, the increase of diamond total surface area, the process that crackle has been delayed to be extended to the depths of diamond,
Composite sheet shock resistance and stress effect anti-coating shedding ability also therefore enhance, can greatly enhance extend it is compound
The service life of piece；
In addition, multi-layer nano diamond layer is arranged alternately convenient for coating, while it is also beneficial to control multi-layer nano diamond
The thickness of layer coating, is conveniently operated；
Finally, after being processed by shot blasting to the surface later stage of nano-diamond layer, the light on process surface can be increased
Cleanliness；
3）Binding agent in the present invention in polycrystalline diamond is had higher hard using superhard high temperature resistant nitride material
Degree, and can make PDC composite sheets obtained that not only there is higher hardness with the high-temperature process of resistance to CVD, and can be with resistance to
The high-temperature process of CVD；In preparation process, after being processed by shot blasting to the nano-diamond layer of outer layer, the finish on surface increases
Add, reduce the heat that drill bit is generated with rock frictional test, so as to delay the service life of drill bit；
4）The raw material bortz powder of polycrystalline diamond layer is further screened in the present invention, is found using the different gold of grain size
The effect that hard rock micro mist reaches when being compounded is best, i.e. evades bulky diamond, using fine-grained diamond as not
The main phase of one-size proportioning, specific surface increase, and activity increase promotes diamond and the interface diffusion of solid phase binding agent, increases
Add the bond strength of diamond and bonding agent, improve the sintered density and uniformity of sintering reaction.
Description of the drawings
Fig. 1 is the structure diagram of composite polycrystal-diamond in embodiment 1；
Fig. 2 is the structure diagram of composite polycrystal-diamond in embodiment 2；
Fig. 3 is the structure diagram of composite polycrystal-diamond in embodiment 3；
Fig. 4 is the structure diagram of nano-diamond layer in embodiment 1.
Specific embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
A kind of composite polycrystal-diamond, as shown in Figure 1 and Figure 4, including columned composite sheet matrix and operative end surface
3, the polycrystalline diamond layer 2 that composite sheet matrix includes cemented carbide substrate 1 and 1 upper surface of cemented carbide substrate covers, hard closes
Auri layer 1 and polycrystalline diamond layer 2 are sintered into one by high temperature and pressure；Operative end surface 3 is located at the upper end of polycrystalline diamond layer 2
Face, coated with multi-layer nano diamond layer 4 in operative end surface 3, the overall thickness of multi-layer nano diamond layer 4 is 6 μm.
Nano-crystalline layers 5 and average grain size 60nm of the every layer of nano-diamond layer 4 including average grain size 20nm
Nano-crystalline layers 6.The thickness of every layer of nano-crystalline layers is 0.3um.
Its preparation method comprises the following steps：
（1）The preparation of composite sheet matrix：Bortz powder and binding agent are mixed（Before being mixed with bortz powder, will first it bond
Agent is uniformly mixed）, 3min is sintered at 5.5GPa, 1600 DEG C obtain composite sheet matrix blank with hard aluminium alloy matrix, it will be multiple
It closes sheet matrix blank to process by grinding, cemented carbide substrate upper surface is obtained covered with polycrystalline diamond layer after finishing processing
Composite sheet matrix blank, with volume percentage, bortz powder 45%, binding agent 55%, the binding agent is CrN, AlN and SiN
Three kinds of mixture；The bortz powder is prepared by volumes below number：0.5~1 μm of bortz powder, 50 parts, 2~4 μm diamonds
30 parts, 6~8 μm 20 parts of bortz powders of powder.
（2）Pre-treatment：After the polishing of composite sheet matrix surface, oil removing, cleaning and drying, with sand-blasting machine to its surface sand-blasting
Afterwards, then after surface degreasing, cleaning, drying filming process is entered；
（3）CVD plated films：Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, in composite sheet matrix
Operative end surface deposits multi-layer nano diamond layer, and every layer of nano-diamond layer is by the different nano-crystalline layers of two layers of average grain size
Composition；
（4）To Nano diamond layer surface polishing treatment up to composite polycrystal-diamond.
Wherein CVD plated films concretely comprise the following steps：
a）Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, is evacuated to 0.8Pa heated substrate temperature
Degree is passed through CH to 900 DEG C4、H2, vacuum degree to 0.3Pa, composite sheet matrix surface forming core, while inert gas shielding is passed through, it is lazy
Property gas air pressure 0.5Pa, the inert gas be Kr；
b）Hot-wire temperature is adjusted, the nano-crystalline layers of one layer of 0.3 μ m-thick, the nanometer are deposited in the operative end surface of composite sheet matrix
The average grain size control of crystal layer is 20nm；
c）Hot-wire temperature is adjusted, the nano-crystalline layers of one layer of 0.3 μ m-thick, the nanometer are deposited in the operative end surface of composite sheet matrix
The average grain size control of crystal layer is 60nm；
d）Step b）And c）For one layer of nano-diamond layer, step b is repeated）And c）Until plated film terminates, overall thickness 6
μm。
Embodiment 2
As shown in Fig. 2, in the present embodiment, it is coated in the operative end surface of composite sheet matrix and the side of polycrystalline diamond layer
There is multi-layer nano diamond layer, the overall thickness of multi-layer nano diamond layer 4 is 16 μm, and every layer of nano-diamond layer 4 includes average
Crystallite dimension is respectively two layers of nano-crystalline layers of 40nm and 60nm.The thickness of every layer of nano-crystalline layers is 0.4um.Remaining same embodiment
1。
Its preparation method comprises the following steps：
（1）The preparation of composite sheet matrix：Bortz powder and binding agent are mixed, with hard aluminium alloy matrix 5.5GPa,
8min is sintered at 1400 DEG C and obtains composite sheet matrix blank, composite sheet matrix blank is processed by grinding, after finishing processing
To composite sheet matrix blank of the cemented carbide substrate upper surface covered with polycrystalline diamond layer, composite sheet matrix blank is passed through into mill
Processing, the upper surface that polycrystalline diamond layer is obtained after finishing processing are machined with the composite sheet matrix of operative end surface；With volume hundred
Divide than meter, bortz powder 70%, binding agent 30%, the binding agent is the mixture of tri- kinds of TiN, ZrN and CrN；The diamond
Powder is prepared by volumes below number：0.5~1 μm of 60 parts, 2~4 μm of bortz powder, 30 parts, 6~8 μm of bortz powder bortz powder 10
Part.
（2）Pre-treatment：After the polishing of composite sheet matrix surface, oil removing, cleaning and drying, 2s is acidified through chloroazotic acid, then through table
Enter filming process after face oil removing, cleaning, drying；
（3）CVD plated films：Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, in composite sheet matrix
Operative end surface and polycrystalline diamond layer side deposition multi-layer nano diamond layer, every layer of nano-diamond layer is by two layers of average crystal grain
The different nano-crystalline layers composition of size；
（4）To Nano diamond layer surface polishing treatment up to composite polycrystal-diamond.
Wherein CVD plated films specifically include following steps：
a）PDC composite sheets are placed on the chip bench of CVD heated filament Diamond Equipments, are evacuated to 0.8Pa heated substrate temperature
Degree is passed through CH to 700 DEG C4、H2, vacuum degree to 0.1Pa, composite sheet surface forming core, while inert gas shielding is passed through, indifferent gas
The air pressure 0.1Pa of body, the inert gas are Ar；
b）Hot-wire temperature is adjusted, one layer of 0.4 μ is deposited in the operative end surface of composite sheet matrix and the side of polycrystalline diamond layer
The nano-crystalline layers of m thickness, the average grain size control of the nano-crystalline layers is 40nm；
c）Hot-wire temperature is adjusted, one layer of 0.4 μ is deposited in the operative end surface of composite sheet matrix and the side of polycrystalline diamond layer
The nano-crystalline layers of m thickness, the average grain size control of the nano-crystalline layers is 60nm；
d）Step b）And c）For one layer of nano-diamond layer, step b is repeated）And c）Until plated film terminates, overall thickness is
16μm。
Embodiment 3
In the present embodiment, as shown in figure 3, being coated in the operative end surface of polycrystalline diamond layer and the side of composite sheet matrix
There is multi-layer nano diamond layer 4, the overall thickness of multi-layer nano diamond layer 4 is 20 μm.Every layer of nano-diamond layer 4 includes average
Crystallite dimension is respectively two layers of nano-crystalline layers of 40nm and 80nm.Remaining is the same as embodiment 1.
Its preparation method comprises the following steps：
（1）The preparation of composite sheet：Bortz powder and binding agent are mixed, with hard aluminium alloy matrix in 5.5GPa, 1550
6min is sintered at DEG C and obtains composite sheet matrix blank, composite sheet matrix blank by grinding is processed, is obtained after finishing processing hard
Composite sheet matrix blank of the matter alloy base upper surface covered with polycrystalline diamond layer adds composite sheet matrix blank by mill
Work, the upper surface that polycrystalline diamond layer is obtained after finishing processing are machined with operative end surface composite sheet matrix；With percent by volume
Meter, bortz powder 90%, binding agent 10%, the binding agent are the mixture of tri- kinds of ZrN, CrN and AlN；The bortz powder is pressed
Volumes below number is prepared：0.5~1 μm of 55 parts, 2~4 μm of bortz powder, 40 parts, 6~8 μm of bortz powder, 5 parts of bortz powder.
（2）Pre-treatment：After the polishing of composite sheet matrix surface, oil removing, cleaning and drying, 5s is acidified through chloroazotic acid, then through table
Enter filming process after face oil removing, cleaning, drying；
（3）CVD plated films：Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, in composite sheet matrix
Operative end surface and composite sheet matrix side deposition multi-layer nano diamond layer, every layer of nano-diamond layer is by two layers of average crystal grain ruler
Very little different nano-crystalline layers composition；
（4）To Nano diamond layer surface polishing treatment up to composite polycrystal-diamond.
Wherein CVD plated films specifically include following steps：
a）Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, is evacuated to 0.7Pa heated substrate temperature
Degree is passed through CH to 800 DEG C4、H2, vacuum degree to 0.2Pa, composite sheet matrix surface forming core, while inert gas shielding is passed through, it is lazy
Property gas 0.1~0.5Pa of air pressure, the inert gas be Ar；
b）Hot-wire temperature is adjusted, one layer of 0.5 μ m-thick is deposited in the operative end surface of composite sheet matrix and composite sheet matrix side
Nano-crystalline layers, the average grain size control of the nano-crystalline layers is 40nm；
c）Hot-wire temperature is adjusted, one layer of 0.5 μ m-thick is deposited in the operative end surface of composite sheet matrix and composite sheet matrix side
Nano-crystalline layers, the average grain size control of the nano-crystalline layers is 80nm；
d）Step b）And c）For one layer of nano-diamond layer, step b is repeated）And c）Until plated film terminates, overall thickness is
20μm。
Comparative example A：
Non- coating composite sheet A in this comparative example is not coated with nano-diamond layer in operative end surface, other are the same as embodiment 1.
Its preparation method, with reference to step in embodiment 1（1）The preparation of composite sheet.
Comparative example B：
Nanogold is not coated on the side of non-coating composite sheet B in this comparative example, operative end surface and polycrystalline diamond layer
Hard rock layer, other are the same as embodiment 1.
Its preparation method, with reference to step in embodiment 2（1）The preparation of composite sheet.
Comparative example C：
Non- coating composite sheet C in this comparative example, in the operative end surface and side of composite sheet matrix are not coated with a nanometer Buddha's warrior attendant
Rock layers, other are the same as embodiment 1.
Its preparation method, with reference to step in embodiment 3（1）The preparation of composite sheet.
Performance test
Hardness test is carried out to composite sheet made from embodiment 1-3 and comparative example A, B, C（It is tested using normal industry, dimension
Family name's hardometer carries out diamond penetrator impression test）, wear resistance ratio test and high temperature resistant test, the result is shown in shown in table 1.
Wherein, high temperature resistant test method is：Sample to be tested is put into Muffle furnace, air atmosphere, 10-15min can be kept the temperature,
It does not aoxidize after testing.
1 embodiment 1-3 of table and comparative example A, B, C composite sheet test result
As can be drawn from Table 1, compared with non-coating composite sheet, the composite sheet after coating（Embodiment 1-3）Overall performance is (hard
Degree and wear resistance ratio) it is improved, and heat resistance and heat resisting temperature are greatly improved, wherein embodiment 2 and 3 is suitable,
It is higher than embodiment 1.
In addition, each performance of embodiment 2 and 3 is better than embodiment 1, the performance of comparative example B and C are better than comparative example A, this
It is measured when being hardness test using Vickers, pressure head is larger, and hardness number is affected by matrix；I.e. hardness number is by glomerocryst
The result that the content of diamond is affected in diamond.In addition wear resistance ratio is proportional with hardness number, and hardness number is bigger, mill
Loss-rate is bigger.
Film thickness is tested and is combined power and tests
Film thickness test is carried out to the composite sheet that embodiment 1-3 is obtained respectively and combines power testing, specific method and result are such as
Under：
1 film thickness is tested：Ball hole instrument measurement film thickness is carried out to it, measures film thickness average, specific test result is shown in Table 2.
2, which combine power, tests：Sandblasting test is carried out with dry blasting machine：SiC abrasive materials, granularity carry out sandblasting knot at 120 microns
It tests with joint efforts, 15S sprays fall 5 microns for qualification.According to this criterion validation, the identical operative end surface of composite sheet of Statistics Implementation example 1-3
The time that the diamond coatings sandblasting in region is fallen, as shown in table 2.
The film thickness of the composite sheet of 2 embodiment 1-3 of table and combination power test result
It is learnt by upper table 2, the film thickness and combination power of the composite sheet of embodiment 1-3 are qualified, have reached requirement.
Claims (9)
1. a kind of composite polycrystal-diamond, including columned composite sheet matrix and operative end surface, the composite sheet matrix bag
The polycrystalline diamond layer of cemented carbide substrate and the covering of cemented carbide substrate upper surface is included, the operative end surface is located at glomerocryst Buddha's warrior attendant
The upper surface of rock layers, which is characterized in that the operative end surface is equipped with multi-layer nano diamond layer, every layer of nano-diamond layer bag
Include the different nano-crystalline layers of two layers of average grain size；
The concrete operations for preparing composite sheet matrix are：Bortz powder and binding agent are mixed, with hard aluminium alloy matrix 5~
5.5GPa, 3~8min of sintering obtains cemented carbide substrate upper surface answering covered with polycrystalline diamond layer at 1400~1600 DEG C
Sheet matrix blank is closed, by composite sheet matrix blank by obtaining the upper surface of polycrystalline diamond layer after grinding processing, finishing processing
It is machined with the composite sheet matrix of operative end surface；With volume percentage, the bortz powder is 45~90%, binding agent be 10~
55% ；The binding agent is superhard refractory ceramics nitride material；The bortz powder is prepared by volumes below number：0.5
~1 μm of 55~60 parts, 2~4 μm of bortz powder, 30~40 parts, 6~8 μm of bortz powder, 5~20 parts of bortz powder.
A kind of 2. composite polycrystal-diamond as described in claim 1, which is characterized in that the side of the polycrystalline diamond layer
Multi-layer nano diamond layer is equipped on face or the side of composite sheet matrix.
A kind of 3. composite polycrystal-diamond as described in claim 1 or 2, which is characterized in that every layer of nano-diamond layer
Including the average grain size of two layers of nano-crystalline layers be respectively 20~40nm and 60~80nm；The thickness of every layer of nano-crystalline layers
For 0.3~0.5um.
4. a kind of composite polycrystal-diamond as described in claim 3, which is characterized in that multi-layer nano diamond layer it is total
Thickness is 6~20 μm.
5. a kind of preparation method of composite polycrystal-diamond, which is characterized in that comprise the following steps：
（1）Prepare composite sheet matrix：The composite sheet matrix includes cemented carbide substrate and cemented carbide substrate upper surface covers
Polycrystalline diamond layer, the upper surface of the polycrystalline diamond layer is machined with operative end surface；
（2）Pre-treatment：After the polishing of composite sheet matrix surface, oil removing, cleaning and drying, through chloroazotic acid be acidified 2~5s or with spray
After sand machine is to its surface sand-blasting, then enter filming process after surface degreasing, cleaning, drying；
（3）CVD plated films：Composite sheet matrix after pre-treatment is placed on the chip bench of CVD heated filament Diamond Equipments,
The operative end surface deposition multi-layer nano diamond layer of composite sheet matrix, every layer of nano-diamond layer include two layers of average grain size
Different nano-crystalline layers；
（4）To Nano diamond layer surface polishing treatment up to composite polycrystal-diamond；
The concrete operations for preparing composite sheet matrix are：Bortz powder and binding agent are mixed, with hard aluminium alloy matrix 5~
5.5GPa, 3~8min of sintering obtains cemented carbide substrate upper surface covered with polycrystalline diamond layer at 1400~1600 DEG C
Composite sheet matrix blank, by composite sheet matrix blank by grind processing, finishing processing after obtain the upper of polycrystalline diamond layer
End face is machined with the composite sheet matrix of operative end surface；With volume percentage, the bortz powder is 45~90%, binding agent is
10~55%；The binding agent is superhard refractory ceramics nitride material；The bortz powder is prepared by volumes below number：
0.5~1 μm of 55~60 parts, 2~4 μm of bortz powder, 30~40 parts, 6~8 μm of bortz powder bortz powder 5~20
Part.
6. the preparation method of the composite polycrystal-diamond as described in claim 5, which is characterized in that step（3）In, right
While the operative end surface deposition multi-layer nano diamond layer of composite sheet matrix, side or compound chip base to polycrystalline diamond layer
Multi-layer nano diamond layer is deposited on the side of body.
7. the preparation method of the composite polycrystal-diamond as described in claim 6, which is characterized in that the binding agent is position
Combination in the periodic table of chemical element more than one or both of nitride of IVB, VIB, IIIA, IVA element.
8. the preparation method of the composite polycrystal-diamond as described in claim 7, which is characterized in that the binding agent is
The mixture of three kinds or more in TiN, ZrN, CrN, AlN and SiN.
9. the preparation method of the composite polycrystal-diamond as described in claim 5 or 6 or 7 or 8, which is characterized in that CVD
Plated film specifically includes following steps：
a）Composite sheet matrix is placed on the chip bench of CVD heated filament Diamond Equipments, is evacuated to 0.6~0.8Pa heating
Substrate temperature is passed through CH to 700~900 DEG C4And H2, vacuum degree to 0.1~0.3Pa, composite sheet matrix surface forming core, together
When be passed through inert gas shielding, 0.1~0.5Pa of air pressure of inert gas；b）Hot-wire temperature is adjusted, in composite sheet matrix
Deposit one layer of 0.3~0.5 μm of thick nano-crystalline layers in operative end surface, the average grain sizes of the nano-crystalline layers for 20~
40nm ；
c）Hot-wire temperature is adjusted, redeposited one layer of 0.3~0.5 μm of thick nanometer on the nano-crystalline layers formed in previous step
Crystal layer, the average grain size of the nano-crystalline layers is 60~80nm；
d）Repeat step b）And c）Until plated film terminates.
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| CN105665806B (en) * | 2016-04-26 | 2018-02-16 | 深圳市力博刀具技术有限公司 | A kind of PCD milling cutters and its processing method |
| DE102017002154A1 (en) * | 2017-03-06 | 2018-09-06 | Audi Ag | Cutting element for a chip processing tool and method for producing such a cutting element |
| CN109128192A (en) * | 2017-06-28 | 2019-01-04 | 深圳先进技术研究院 | Composite polycrystal-diamond and preparation method thereof |
| CN109848761A (en) * | 2019-01-18 | 2019-06-07 | 株洲金佰利硬质合金有限公司 | A kind of carbide surface treatment process |
| CN109869096B (en) * | 2019-03-25 | 2020-07-10 | 邹城兖矿泰德工贸有限公司 | Diamond film coating drill bit |
| CN111911082B (en) * | 2020-07-11 | 2022-03-22 | 长江大学 | Method for strengthening polycrystalline diamond compact |
| CN111850335B (en) * | 2020-07-27 | 2022-04-29 | 深圳市海明润超硬材料股份有限公司 | Diamond composite sheet easy to remove cobalt and preparation method thereof |
| CN112323144B (en) * | 2020-11-04 | 2021-10-29 | 吉林大学 | Surface-enhanced polycrystalline diamond compact and preparation method thereof |
| CN113088919A (en) * | 2021-04-02 | 2021-07-09 | 吉林大学 | Method for growing diamond film on surface of polycrystalline diamond compact |
| CN116121728A (en) * | 2023-01-30 | 2023-05-16 | 江苏开放大学（江苏城市职业学院） | Method for preparing novel diamond composite thick film cutter |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626853A (en) * | 2011-02-07 | 2012-08-08 | 三菱综合材料株式会社 | Cutting tool covered with diamond |
| CN102678057A (en) * | 2012-05-22 | 2012-09-19 | 株洲西迪硬质合金科技有限公司 | Diamond composite sheet and preparation method thereof |
| CN103100977A (en) * | 2013-01-29 | 2013-05-15 | 中国地质大学（北京） | Preparation method of high-strength diamond grinding wheel dressing pen |
| CN103331442A (en) * | 2013-07-16 | 2013-10-02 | 中南钻石股份有限公司 | Nanometer binding agent, diamond-containing composite cutting tooth made from nanometer binding agent and manufacturing method of diamond-containing composite cutting tooth |
| CN104563889A (en) * | 2013-11-25 | 2015-04-29 | 莱州市原野科技有限公司 | Pre-graphitized polycrystalline diamond compact |
| CN205128957U (en) * | 2015-11-03 | 2016-04-06 | 富耐克超硬材料股份有限公司 | Polycrystalline diamond composite sheet |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL198916A0 (en) * | 2009-05-25 | 2010-02-17 | Iscar Ltd | Cutting tool coated with a diamond-like carbon multilayer |
| US20140060937A1 (en) * | 2012-08-31 | 2014-03-06 | Diamond Innovations, Inc. | Polycrystalline diamond compact coated with high abrasion resistance diamond layers |
-
2015
- 2015-11-03 CN CN201510734565.7A patent/CN105349965B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626853A (en) * | 2011-02-07 | 2012-08-08 | 三菱综合材料株式会社 | Cutting tool covered with diamond |
| CN102678057A (en) * | 2012-05-22 | 2012-09-19 | 株洲西迪硬质合金科技有限公司 | Diamond composite sheet and preparation method thereof |
| CN103100977A (en) * | 2013-01-29 | 2013-05-15 | 中国地质大学（北京） | Preparation method of high-strength diamond grinding wheel dressing pen |
| CN103331442A (en) * | 2013-07-16 | 2013-10-02 | 中南钻石股份有限公司 | Nanometer binding agent, diamond-containing composite cutting tooth made from nanometer binding agent and manufacturing method of diamond-containing composite cutting tooth |
| CN104563889A (en) * | 2013-11-25 | 2015-04-29 | 莱州市原野科技有限公司 | Pre-graphitized polycrystalline diamond compact |
| CN205128957U (en) * | 2015-11-03 | 2016-04-06 | 富耐克超硬材料股份有限公司 | Polycrystalline diamond composite sheet |
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