CN105156037A - Thermostable polycrystalline diamond composite piece and preparation method thereof - Google Patents
Thermostable polycrystalline diamond composite piece and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a thermostable polycrystalline diamond composite piece and a preparation method thereof. The thermostable polycrystalline diamond composite piece is prepared through the following steps of: coating a plastic layer on the surface of a hard alloy matrix of a polycrystalline diamond composite body compounded through high temperature and high pressure; and then immersing the coated polycrystalline diamond composite body into acid liquor so as to perform acid cooking. According to the thermostable polycrystalline diamond composite piece disclosed by the invention, the plastic layer is coated on the surface of the hard alloy matrix of the polycrystalline diamond composite body during preparing the thermostable polycrystalline diamond composite piece, and only the surface of a polycrystalline diamond layer is exposed into the acid liquor when the acid cooking is performed so as to prevent the hard alloy matrix and joints between the polycrystalline diamond layer and the hard alloy matrix from being damaged by the acid liquor. Compared with a conventional polycrystalline diamond composite piece, the thermostable polycrystalline diamond composite piece disclosed by the invention has excellent synthesized mechanical properties, particularly has high heat stability and a good abrasion resistant property, is suitable for the application fields of oil drilling, geological drilling, coal mining and the like, and has a high social value and high economic benefits.
Description
Technical field
The invention belongs to composite polycrystal-diamond technical field, be specifically related to a kind of thermostable type composite polycrystal-diamond, also relate to a kind of preparation method of thermostable type composite polycrystal-diamond simultaneously.
Background technology
Composite polycrystal-diamond (Polycrystallinediamondcompact, PDC) be added by diamond dust after certain catalyzer and hard alloy substrate fit together, on special diamond hydraulic press, under superhigh-temperature and-pressure condition, sintering is obtained.It is made up of polycrystalline diamond layer and hard alloy substrate, and because polycrystalline diamond layer hardness is high, abrasion resistance is good, adds excellent toughness and the solderability of hard alloy substrate, makes it be used widely in oil drilling, geological drilling and coal mining application.
In making PDC process, generally adopt cobalt, nickel, iron to make high wearable PDC as bonding agent or adopt silicon to be that bonding agent makes heat resistant type PDC.Adopt the PDC that makes as bonding agent of silicon, due to thing phase and the adamantine similar thermal expansion coefficient such as SiC of Si bonding agent and formation, thermal stress is less; And Si does not exist under the high temperature conditions to adamantine anticaltalysis effect yet, the PDC that therefore silicon bonding agent makes has higher heat stability.But directly combine owing to not formed between diamond particles, but form D-M-D structure (diamond-mesophase spherule-diamond), so the PDC abrasion resistance of this kind of structure is poor.
Cobalt, nickel, iron is adopted to make PDC as bonding agent, due to the catalytic action of cobalt, between diamond particles, mutual direct sintering forms D-D integrated structure (diamond-diamond combines) together, and the microscopic structure of the polycrystalline diamond layer of this structure is made up of " little island " Metal Phase of the diamond phase and Dispersed precipitate with connected cage construction.Because combine fully between diamond particles, so generally adopt cobalt, nickel, iron to have very high abrasion resistance as the composite sheet that bonding agent makes.
But, as impelling graphite to change adamantine bonding agent under high pressure, under metallic cobalt, nickel, iron normal pressure, also can promote that diamond is to the transformation of graphite, reducing the intensity of polycrystalline diamond layer; On the other hand, the coefficient of thermal expansion of metallic cobalt is nearly adamantine 10 times, when operating temperature is very high, easily produces thermal stress, destroys diamond framework, makes polycrystalline diamond occur crackle, cause stress to damage.Therefore, the heat stability that the Metal Phase in polycrystalline diamond layer can reduce PDC to a certain extent because operating point temperature is different.
In prior art, CN104532016A discloses a kind of de-cobalt method of the de-cobalt Compound-acid based on man-made polycrystalline diamond composite sheet, be that organic acid and two or more inorganic acid are mixed and made into Compound-acid solution, then be dipping 48 ~ 72h in the Compound-acid solution of 25 ~ 90 DEG C in temperature by man-made polycrystalline diamond composite sheet.The method that the method utilizes Compound-acid to flood makes composite polycrystal-diamond take off cobalt, thus diamond is closed with D-D bond, reduces the possibility of Co vein shape distribution between diamond crystals, thus improves the abrasion resistance of composite polycrystal-diamond.But, whole composite polycrystal-diamond is needed to be immersed in Compound-acid solution during acidleach, acid solution inevitably damages the junction of hard alloy substrate itself and polycrystalline diamond layer and hard alloy substrate, reduce the mechanical property of hard alloy substrate and the bond strength of polycrystalline diamond layer and hard alloy substrate, thus the quality of composite polycrystal-diamond and anti-wear performance are caused have a strong impact on.
Summary of the invention
The object of this invention is to provide a kind of thermostable type composite polycrystal-diamond, solve existing acidleach and take off the problem that cobalt reduces the mechanical property of composite polycrystal-diamond hard alloy substrate and the bond strength of polycrystalline diamond layer and hard alloy substrate.
Second object of the present invention is to provide a kind of preparation method of thermostable type composite polycrystal-diamond.
In order to realize above object, the technical solution adopted in the present invention is:
A kind of thermostable type composite polycrystal-diamond is by after the cemented carbide substrate surfaces of the polycrystalline diamond complex of HP-HT synthesize parcel plastic layer, then polycrystalline diamond complex is immersed in acid solution that to carry out sour boiling standby.
Plastic layer is wrapped in cemented carbide substrate surfaces on polycrystalline diamond complex, only have when acid is boiled polycrystalline diamond layer surface to expose to the open air in acid solution, prevent the junction of acid solution to hard alloy substrate itself and polycrystalline diamond layer and hard alloy substrate from damaging.
Described thermostable type composite polycrystal-diamond, specifically prepared by the method comprised the following steps:
1) get diadust, metallic catalyst, hard alloy substrate be assembled into assembled block, after vacuum heat is carried out to assembled block, then carry out HP-HT synthesize, obtain polycrystalline diamond complex;
2) in step 1) after the cemented carbide substrate surfaces parcel plastic layer of the polycrystalline diamond complex of gained, then polycrystalline diamond complex is immersed in acid solution and carry out acid and boil, obtain described thermostable type composite polycrystal-diamond.
Wherein, in the method for the cemented carbide substrate surfaces parcel plastic layer of polycrystalline diamond complex be: after polycrystalline diamond complex surface injection moulding forms one deck plastic layer, then the plastic layer on polycrystalline diamond layer surface on polycrystalline diamond complex is peeled off.
Allly may be used for injection mo(u)lding and the plastic material with certain acid resistance is all available; Preferably, the material of described plastic layer is epoxy resin, polyethylene, polypropylene or polyvinyl chloride.
The metallic catalyst part of diamond particles gap location in polycrystalline diamond layer or close acid of all removing all can be can be used as acid and boil acid solution used; Preferably, the mixture of mixture that acid solution used is nitric acid and hydrofluoric acid or nitric acid and hydrochloric acid is boiled in acid.Wherein, the mass concentration of described nitric acid is 65% ~ 68%, and the mass concentration of described hydrofluoric acid is 40%, and the concentration of described hydrochloric acid is 36% ~ 38%.In order to improve the removal effect of metallic catalyst, further preferably, it be the volume ratio of nitric acid and hydrofluoric acid is the mixture of 1:1 that acid solution used is boiled in acid, or the volume ratio of nitric acid and hydrochloric acid is the mixture of 1:3.
It is pure that described nitric acid, hydrofluoric acid, hydrochloric acid are commercially available analysis.
The time that described acid is boiled is 6 ~ 60h.
Step 1) in, described diadust is the composite mixture of the diamond single crystal of Monosized powder or multiple grit diamond monocrystalline, and granularity extreme value is no more than 0.5 ~ 40 μm.When described diadust is the composite mixture of multiple grit diamond monocrystalline, after selected a kind of granularity, all the other sizes are selected within the scope of 1.5 ~ 5 times according to grain composition.
During synthesis polycrystalline diamond complex, the metallic catalyst for HP-HT synthesize composite polycrystal-diamond of this area routine is all available.In order to improve the performance of composite polycrystal-diamond, preferably, step 1) described in metallic catalyst be any one or multiple mixture in Co, Fe, Ni, V, Cr or alloy.The particle diameter of described metallic catalyst is 0.1 ~ 20 μm.
During synthesis polycrystalline diamond complex, the hard alloy substrate for HP-HT synthesize composite polycrystal-diamond of this area routine is all available.In order to improve the combination property of composite polycrystal-diamond, preferably, step 1) described in hard alloy substrate be tungsten-cobalt alloy, tungsten titanium-cobalt alloy or tungsten titanium tantalum alloy.
During assembling assembled block, first by having loaded in the metal cup of shielding action after diadust and metallic catalyst ball mill mixing, then put into hard alloy substrate.Described metal cup has included but are not limited to titanium cup, the tantalum cup and zirconium cup etc. of shielding action.
Step 1) in, assembled block is placed in vacuum drying oven and carries out vacuum heat.Vacuum≤1 × 10 of described vacuum heat
-2pa, temperature is 450 ~ 700 DEG C, and the processing time is 2 ~ 10h.
Step 1) in, carry out HP-HT synthesize after assembled block being put into transmission medium.The pressure of described HP-HT synthesize is 5.2 ~ 6.6GPa, and temperature is 1350 ~ 1700 DEG C, and temperature retention time is 3 ~ 30min.
A kind of preparation method of thermostable type composite polycrystal-diamond, comprise after the cemented carbide substrate surfaces of the polycrystalline diamond complex of HP-HT synthesize parcel plastic layer, polycrystalline diamond complex is immersed in acid solution again and carry out acid and boil, obtain described thermostable type composite polycrystal-diamond.
Thermostable type composite polycrystal-diamond of the present invention is by after the cemented carbide substrate surfaces of the polycrystalline diamond complex of HP-HT synthesize parcel plastic layer, then polycrystalline diamond complex is immersed in acid solution that to carry out sour boiling standby, plastic layer is wrapped in cemented carbide substrate surfaces on polycrystalline diamond complex, only have polycrystalline diamond layer surface to expose to the open air in acid solution when acid is boiled, prevent the junction of acid solution to hard alloy substrate itself and polycrystalline diamond layer and hard alloy substrate from damaging, thus under the prerequisite ensureing the mechanical property of hard alloy substrate and the bond strength of polycrystalline diamond layer and hard alloy substrate, boil by the metallic catalyst part of diamond particles gap location in polycrystalline diamond layer or close to all removing by acid, avoid expanding with heat and contract with cold because of metallic catalyst, be oxidized and cause composite polycrystal-diamond mechanical performance to decline to adamantine graphitization catalytic action, relative to existing composite polycrystal-diamond, thermostable type composite polycrystal-diamond of the present invention has excellent comprehensive mechanical performance, especially there is high heat stability and abrasion resistance, be applicable to the applications such as oil drilling, geological drilling and coal mining, there is very high social value and economic benefit.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of thermostable type composite polycrystal-diamond.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further illustrated.
Embodiment 1
The thermostable type composite polycrystal-diamond of the present embodiment, prepared (preparation flow is as shown in Figure 1) by following methods:
1) be the diadust of 6-12 μm and granularity by granularity be loaded in the metal cup (molybdenum cup) of shielding action after the metallic catalyst Co powder ball mill mixing of 1-3 μm, then tungsten-cobalt hard alloy matrix is put into, be assembled into assembled block (as shown in Fig. 1 (a), wherein 1 is hard alloy substrate, and 2 is the batch mixing of diadust and metallic catalyst); Assembled block is placed in vacuum drying oven, is 6.0 × 10 in vacuum
-3pa, temperature are carry out vacuum heat 2h under 500 DEG C of conditions;
By after the assembled block of vacuum heat puts into transmission medium, under sintering pressure 5.2GPa, sintering temperature 1400 DEG C of conditions, be incubated 10min carry out HP-HT synthesize, (preprocessing refers to and carries out Mechanical Grinding Process to the complex of synthesis in the demoulding preprocessing after synthesis, be processed into standard size), obtain polycrystalline diamond complex (as shown in Fig. 1 (b), wherein 3 is polycrystalline diamond layer);
2) in step 1) the surface injection moulding of the polycrystalline diamond complex of gained forms one deck epoxy resin plastics layer, then the plastic layer on polycrystalline diamond layer surface is peeled off, obtain the polycrystalline diamond complex (as shown in Fig. 1 (c), wherein 4 is plastic layer) of cemented carbide substrate surfaces parcel plastic layer;
Polycrystalline diamond complex cemented carbide substrate surfaces being wrapped up plastic layer immerses in acid solution and carries out acid and boil 6h, obtain described thermostable type composite polycrystal-diamond (as shown in Fig. 1 (d), wherein the top layer of polycrystalline diamond layer 3 forms the denitrating catalyst layer 3-1 of containing metal catalyzer hardly); Wherein said acid solution to be mass concentration be 65% nitric acid and mass concentration be 40% hydrofluoric acid be the mix acid liquor mixed of 1:1 according to volume ratio.
The transverse breakage toughness of the thermostable type composite polycrystal-diamond of the present embodiment gained is 1200MPa, and young's modulus of elasticity is 750GPa, and heat resisting temperature is 1100 DEG C.
Embodiment 2
The thermostable type composite polycrystal-diamond of the present embodiment, prepared (preparation flow is with embodiment 1) by following methods:
1) be the diadust of 15-25 μm and granularity by granularity be loaded in the metal cup (tantalum cup) of shielding action after the metallic catalyst dilval ball mill mixing of 1-3 μm, then put into tungsten titanium cobalt hard alloy matrix, be assembled into assembled block; Assembled block is placed in vacuum drying oven, is 6.0 × 10 in vacuum
-3pa, temperature are carry out vacuum heat 5h under 700 DEG C of conditions;
By after the assembled block of vacuum heat puts into transmission medium, under sintering pressure 5.5GPa, sintering temperature 1500 DEG C of conditions, be incubated 15min carry out HP-HT synthesize, synthesize the rear demoulding and preprocessing, obtain polycrystalline diamond complex;
2) in step 1) the surface injection moulding of the polycrystalline diamond complex of gained forms one deck epoxy resin plastics layer, and then the plastic layer on polycrystalline diamond layer surface is peeled off, obtain the polycrystalline diamond complex of cemented carbide substrate surfaces parcel plastic layer;
Polycrystalline diamond complex cemented carbide substrate surfaces being wrapped up plastic layer immerses in acid solution and carries out acid and boil 24h, obtains described thermostable type composite polycrystal-diamond; Wherein said acid solution to be mass concentration be 65% nitric acid and mass concentration be 38% hydrochloric acid be the mix acid liquor mixed of 1:3 according to volume ratio.
The transverse breakage toughness of the thermostable type composite polycrystal-diamond of the present embodiment gained is 1100MPa, and young's modulus of elasticity is 730GPa, and heat resisting temperature is 1100 DEG C.
Embodiment 3
The thermostable type composite polycrystal-diamond of the present embodiment, prepared (preparation flow is with embodiment 1) by following methods:
1) be 6-12 μm by granularity, granularity be the mixing diadust (mass ratio of two kinds of grit diamond micro mists is 1:1) of 15-25 μm and granularity is loaded in the metal cup (molybdenum cup) of shielding action after the metallic catalyst Co powder ball mill mixing of 1-3 μm, then put into tungsten titanium tantalum hard alloy substrate, be assembled into assembled block; Assembled block is placed in vacuum drying oven, is 6.0 × 10 in vacuum
-3pa, temperature are carry out vacuum heat 5h under 600 DEG C of conditions;
By after the assembled block of vacuum heat puts into transmission medium, under sintering pressure 5.8GPa, sintering temperature 1500 DEG C of conditions, be incubated 30min carry out HP-HT synthesize, synthesize the rear demoulding and preprocessing, obtain polycrystalline diamond complex;
2) in step 1) the surface injection moulding of the polycrystalline diamond complex of gained forms layer of polyethylene plastic layer, and then the plastic layer on polycrystalline diamond layer surface is peeled off, obtain the polycrystalline diamond complex of cemented carbide substrate surfaces parcel plastic layer;
Polycrystalline diamond complex cemented carbide substrate surfaces being wrapped up plastic layer immerses in acid solution and carries out acid and boil 36h, obtains described thermostable type composite polycrystal-diamond; Wherein said acid solution to be mass concentration be 65% nitric acid and mass concentration be 38% hydrochloric acid be the mix acid liquor mixed of 1:3 according to volume ratio.
The transverse breakage toughness of the thermostable type composite polycrystal-diamond of the present embodiment gained is 1400MPa, and young's modulus of elasticity is 800GPa, and heat resisting temperature is 1300 DEG C.
Embodiment 4
The thermostable type composite polycrystal-diamond of the present embodiment, prepared (preparation flow is with embodiment 1) by following methods:
1) be the diadust of 6-12 μm and granularity by granularity be loaded in the metal cup (molybdenum cup) of shielding action after the metallic catalyst cobalt-nickel alloy ball mill mixing of 3-5 μm, then put into tungsten titanium tantalum hard alloy substrate, be assembled into assembled block; Assembled block is placed in vacuum drying oven, is 1.0 × 10 in vacuum
-2pa, temperature are carry out vacuum heat 10h under 700 DEG C of conditions;
By after the assembled block of vacuum heat puts into transmission medium, under sintering pressure 5.6GPa, sintering temperature 1350 DEG C of conditions, be incubated 5min carry out HP-HT synthesize, synthesize the rear demoulding and preprocessing, obtain polycrystalline diamond complex;
2) in step 1) the surface injection moulding of the polycrystalline diamond complex of gained forms one deck polyvinyl chloride plastic bed of material, and then the plastic layer on polycrystalline diamond layer surface is peeled off, obtain the polycrystalline diamond complex of cemented carbide substrate surfaces parcel plastic layer;
Polycrystalline diamond complex cemented carbide substrate surfaces being wrapped up plastic layer immerses in acid solution and carries out acid and boil 60h, obtains described thermostable type composite polycrystal-diamond; Wherein said acid solution to be mass concentration be 65% nitric acid and mass concentration be 40% hydrofluoric acid be the mix acid liquor mixed of 1:1 according to volume ratio.
The transverse breakage toughness of the thermostable type composite polycrystal-diamond of the present embodiment gained is 1220MPa, and young's modulus of elasticity is 730GPa, and heat resisting temperature is 1150 DEG C.
Claims (10)
1. a thermostable type composite polycrystal-diamond, is characterized in that: be by after the cemented carbide substrate surfaces of the polycrystalline diamond complex of HP-HT synthesize parcel plastic layer, then polycrystalline diamond complex is immersed in acid solution that to carry out sour boiling standby.
2. thermostable type composite polycrystal-diamond according to claim 1, is characterized in that: specifically prepared by the method comprised the following steps:
1) get diadust, metallic catalyst, hard alloy substrate be assembled into assembled block, after vacuum heat is carried out to assembled block, then carry out HP-HT synthesize, obtain polycrystalline diamond complex;
2) in step 1) after the cemented carbide substrate surfaces parcel plastic layer of the polycrystalline diamond complex of gained, then polycrystalline diamond complex is immersed in acid solution and carry out acid and boil, obtain described thermostable type composite polycrystal-diamond.
3. thermostable type composite polycrystal-diamond according to claim 1 and 2, it is characterized in that: in the method for the cemented carbide substrate surfaces parcel plastic layer of polycrystalline diamond complex be: after polycrystalline diamond complex surface injection moulding forms one deck plastic layer, then the plastic layer on polycrystalline diamond layer surface on polycrystalline diamond complex is peeled off.
4. thermostable type composite polycrystal-diamond according to claim 3, is characterized in that: the material of described plastic layer is epoxy resin, polyethylene, polypropylene or polyvinyl chloride.
5. thermostable type composite polycrystal-diamond according to claim 1 and 2, is characterized in that: the mixture of mixture that acid solution used is nitric acid and hydrofluoric acid or nitric acid and hydrochloric acid is boiled in acid.
6. thermostable type composite polycrystal-diamond according to claim 2, it is characterized in that: step 1) in, described diadust is the composite mixture of the diamond single crystal of Monosized powder or multiple grit diamond monocrystalline, and granularity extreme value is no more than 0.5 ~ 40 μm.
7. thermostable type composite polycrystal-diamond according to claim 2, is characterized in that: step 1) in, described metallic catalyst is any one or multiple mixture in Co, Fe, Ni, V, Cr or alloy.
8. thermostable type composite polycrystal-diamond according to claim 2, is characterized in that: step 1) in, vacuum≤1 × 10 of described vacuum heat
-2pa, temperature is 450 ~ 700 DEG C, and the processing time is 2 ~ 10h.
9. thermostable type composite polycrystal-diamond according to claim 1 and 2, is characterized in that: the pressure of described HP-HT synthesize is 5.2 ~ 6.6GPa, and temperature is 1350 ~ 1700 DEG C, and temperature retention time is 3 ~ 30min.
10. the preparation method of a thermostable type composite polycrystal-diamond, it is characterized in that: comprise after the cemented carbide substrate surfaces of the polycrystalline diamond complex of HP-HT synthesize parcel plastic layer, polycrystalline diamond complex is immersed in acid solution again and carry out acid and boil, obtain described thermostable type composite polycrystal-diamond.
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| CN110056313A (en) * | 2018-01-18 | 2019-07-26 | 中石化石油工程技术服务有限公司 | The impregnated diamond composite block of PDC- |
| CN113004865A (en) * | 2021-03-05 | 2021-06-22 | 河南晶锐新材料股份有限公司 | Polycrystalline diamond compact vacuum packaging flow choking agent and flow choking structure |
| CN113084173A (en) * | 2021-03-19 | 2021-07-09 | 重庆北思卡新材料股份有限公司 | Polycrystalline diamond compact and synthesis method thereof |
| CN114774919A (en) * | 2021-01-22 | 2022-07-22 | 四川伽锐科技有限公司 | Sealed cobalt removal device, reagent, method and application |
| CN115740457A (en) * | 2022-11-24 | 2023-03-07 | 吉林大学 | Vanadium-enhanced polycrystalline diamond compact and preparation method thereof |
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| CN105798312A (en) * | 2016-03-16 | 2016-07-27 | 郑州新亚复合超硬材料有限公司 | Sintering process for diamond composite piece used for petroleum drill bit |
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| CN115740457A (en) * | 2022-11-24 | 2023-03-07 | 吉林大学 | Vanadium-enhanced polycrystalline diamond compact and preparation method thereof |
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Application publication date: 20151216 |