CN103361615B - The equipment of diamond surface double cathode plasma deposition nano coating and technique - Google Patents
The equipment of diamond surface double cathode plasma deposition nano coating and technique Download PDFInfo
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- CN103361615B CN103361615B CN201310254624.1A CN201310254624A CN103361615B CN 103361615 B CN103361615 B CN 103361615B CN 201310254624 A CN201310254624 A CN 201310254624A CN 103361615 B CN103361615 B CN 103361615B
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- 239000010432 diamond Substances 0.000 title claims abstract description 69
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 66
- 239000002103 nanocoating Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims description 14
- 230000008021 deposition Effects 0.000 title claims description 13
- 239000002184 metal Substances 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 238000000151 deposition Methods 0.000 claims abstract description 28
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 238000002294 plasma sputter deposition Methods 0.000 claims abstract description 16
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001573 adamantine Inorganic materials 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 238000007747 plating Methods 0.000 description 15
- 239000000843 powder Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 230000010355 oscillation Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 239000007767 bonding agent Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000000462 isostatic pressing Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 229910000939 field's metal Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000005289 physical deposition Methods 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910020515 Co—W Inorganic materials 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of double cathode plasma sputter deposition means prepare nano coating equipment and its preparation technology at diamond surface.This equipment comprises vacuum chamber, double cathode structure, target device, charging tray, oscillator, inlet mouth and air outlet; Double cathode structure comprises two anodes and two negative electrodes, one of them negative electrode connects target device, another negative electrode connects charging tray, adopt double cathode plasma sputter deposition means, by regulating adamantine distance in target and charging tray voltage and target and charging tray, control depositing time and temperature, make target metal form coating at diamond surface.The present invention is by double cathode plasma sputter deposition means, and prepared coating and diamond have good bonding force.
Description
Technical field
The present invention relates to diamond surface processing technology field, particularly relate to a kind of double cathode plasma sputter deposition means prepare nano coating equipment and its preparation technology at diamond surface.
Background technology
The thermal conductivity of adamantine high rigidity, high-wearing feature, high compressive strength and excellence, makes it have application widely at metal and hard and fragile material machining tool, abrasive tool industry.As diamond saw blade, emery wheel, bistrique etc.The leading product of the widely used class of current diamond tool are metal powder sintered diamond tools, be mixed with the metal-powder as bonding agent by diamond, sinter made by.Owing to having very high interfacial energy between diamond and general metal or alloy, cause diamond surface can not infiltrate by general metal or alloy, and the at high temperature easy greying of diamond and oxidation, so be difficult to and metal generation metallurgical binding, diamond particles is only combined with bonding agent by physical force and cast setting.In instrument use procedure, stand cutting force that is high, interval, under the effect of grinding force, diamond abrasive grain very easily comes off, thus the work-ing life of grinding tool is had a greatly reduced quality.
The bonding strength improving diamond and metal adhesive improves the key of diamond tool working (machining) efficiency, work-ing life and adamantine utilization ratio.Adopting process for modifying surface, is improve bonding agent to the important means of diamond particles hold in diamond abrasive surface preparation coating.
Current Modified Diamond technology mainly contains the various ways such as electroless plating, chemical vapour deposition, thermal evaporation plating, magnetron sputtering, ion plating, the micro-evaporation plating of vacuum.But there is variety of problems in above-mentioned process for modifying surface:
(1) diamond surface Electroless Plating Ni, Co, Cu are not suitable for metallic bond instrument, even if the product of plating Ni-W, Co-W alloy can not be used for metallic bond instrument, its reason is Ni, Co is graphite element, can not play metallurgical binding effect.
(2) common physical vapor deposition comprises thermal evaporation plating, magnetron sputtering, ion plating etc., complex process, single plating amount are few, it is physical attachment between coating and diamond, do not form carbide with diamond surface, within the hot pressing short period of time that instrument manufactures, be difficult to large-area compound bonding, so result of use is not obvious.
(3) chemical vapour deposition (CVD) and salt bath plating technic, plating process diamond is heated and reaches more than 850 DEG C, and in high vacuum conditions, adamantine intensity obviously declines, and loses industrial application value.
(4) vacuum slowly vapor deposition technology more widely of applying at present needs higher depositing temperature equally, and the limitednumber of plating (being only limitted to plate Ti), containing certain easy contaminate environment of toxic element titanous chloride in the starting material used.
Summary of the invention
The present invention is directed to the deficiencies in the prior art; provide a kind of equipment of diamond surface double cathode plasma deposition nano coating; adopt double cathode plasma sputter deposition technique means; nano metal coating is prepared at diamond particles or powder surface; improve the bonding strength of diamond and metal adhesive, improve diamond tool working (machining) efficiency, work-ing life and adamantine utilization ratio.
An equipment for diamond surface double cathode plasma deposition nano coating, includes vacuum chamber, power supply, target, monitor component, and in described vacuum chamber, charging tray is arranged at the side of target, and positive plate is arranged at the opposite side of target; Described power supply is outside at vacuum chamber, and power supply includes two negative electrodes, one of them negative electrode is connected to target, and another negative electrode is connected to charging tray, and the anode of power supply is connected to positive plate, and target is also provided with monitor component.
Described monitor component is for monitoring depositing temperature.
Power supply can comprise an anode also can be two anodes, as long as be connected to by anode on the positive plate in vacuum chamber.The common power supply of power acquisition.
In use, charging tray can place diamond, it can be particulate state also can be Powdered.
As improvement, below charging tray, be provided with oscillator.Oscillator can make diamond particles or powder constantly stir in deposition, to ensure coating uniform, without plating leakage.Oscillator is preferably located at 3 centimeters below charging tray.
Oscillator can adopt ultrasonic oscillation amplitude transformer, its effect utilizes hyperacoustic high frequency sound wave to produce vibration, ultrasonic output frequency can according to different operating situation carry out fine setting ultrasonic generator have the function of frequency trim under different working conditions slightly adjustment make transverter always work in optimum regime under, conversion efficiency reaches maximum, can reach best effect under different operating mode.
As improvement, vacuum chamber is also provided with inlet mouth and air outlet.Its effect passes into rare gas element,
Above-mentioned monitor component can adopt thermopair.As improvement, thermopair distance charging tray 2 centimetres.The temperature under depositing operation near diamond surface monitored in real time by thermopair.
As improvement, the distance between target and diamond is 10-20mm, preferred 15mm.
As improvement, vacuum chamber sidewall is provided with porthole.
As improvement, double cathode anatomical connectivity has operator's console, for controlling electric current and the voltage of double cathode structure.
Present invention also offers a kind of technique of diamond surface depositing nano coating, adopt double cathode plasma sputter deposition means, by regulating adamantine distance in target and charging tray voltage and target and charging tray, pass into argon gas, control depositing time and temperature, make target metal form coating at diamond surface.
Specifically comprise the following steps: place target in a vacuum chamber, the charging tray of the side of target places diamond, the opposite side of target arranges positive plate; Target and charging tray are connected on a negative electrode of double cathode power supply, and positive plate is connected to the anode of power supply; Carry out double cathode plasma sputtering to target and charging tray, obtain the diamond of surface-coated nano coating, coating comprises skin and internal layer, outer for grain-size be the metal level of 10-100 nanometer, internal layer is the metal carbide layer of thickness 90-110 nanometer.
As preferably, deposition process parameters is as follows:
As preferably, deposition process parameters is as follows:
As preferably, described target is one or more of Ti, Cr, Mo, Nb, Zr.Be target with metal, without environmentally harmful element in target.
As preferably, rare gas element is argon gas, the preferred 35Pa of ar pressure.
Equipment of the present invention has following features: below the adamantine charging tray of placement, install oscillator, diamond particles or powder are constantly rolled in deposition, thus make target be deposited on diamond particles or powder uniformly, finally make the product that coating uniform performance is good; The diamond simultaneously wish deposited and the distance adjustment of oscillator, in rational position, can reach better deposition effect.Described equipment is through test, and primary depositing diamonds at least can reach 20 kilograms, and sedimentation effect reaches 500 and to receive m/h, and with existing deposition method as compared with PVD physical deposition method, sedimentation effect is greatly improved, and single can plated coating in enormous quantities.
Technique of the present invention has following features: first in the selection of target, take metal as target, without environmentally harmful element in target, avoid the problem of prior art contaminate environment while plated coating, can also according to the difference of metal adhesive, select the composition of different metal targets, metal targets and metal adhesive are cooperatively interacted, better improves the bonding strength between diamond and metal adhesive.This technique is by selecting suitable processing parameter, if control temperature is at 500-600 DEG C, avoid diamond under the catalysis of internal package body, intensity is caused to reduce because there is greying, and adjustment diamond and oscillator, distance between diamond and target, achieve the bilayer structure of coating, outer field metal level be conducive to improve in sintering process with the wetting property of metal adhesive, and shorten sintering time, and metal carbide layer formed by epitaxy, hold can be improved further.
The present invention by double cathode plasma sputter deposition means, thus prepares metallic coating at diamond surface, and does not limit metal types, all can prepare nano coating for any metal.Different from common physical deposition, the present invention forms layer of metal carbide transition layer by chemical reaction between metallic coating and diamond, realizes combination good between coating and diamond; And low temperature depositing ensure that adamantine intensity.Equipment of the present invention can meet the requirement of single plating in enormous quantities, coating uniform, without plating leakage, and the starting material used are free from environmental pollution.Described equipment can meet the requirement of single plating in enormous quantities, and primary depositing diamonds can reach more than 20 kilograms, and sedimentation effect to be received m/h up to 500.
Accompanying drawing explanation
Fig. 1 is the equipment schematic diagram of diamond surface double cathode plasma deposition nano coating.
Fig. 2 is the structural representation of deposited coating.
Wherein 1 be positive plate, 2 are operator's console, 3 are power supplys, 4 are air outlets, 5 are inlet mouths, 6 are portholes, 7 are vacuum chambers, 8 are charging trays, 9 are target devices, 10 are thermopairs, 11 are targets, 12 are ultrasonic oscillation amplitude transformers, 13 are metal carbide layer, 14 is metal levels.
Specific embodiments
Below in conjunction with accompanying drawing, the present invention is further described in detail.
A kind of equipment of diamond surface double cathode plasma deposition nano coating; for preparing nano metal coating at diamond (artificial or natural) particle or powder surface; this equipment includes power supply 3 and vacuum chamber 7; be located at the target device 9 of vacuum chamber 7 inside, charging tray 8, ultrasonic oscillation amplitude transformer 12, thermopair 10; be located at the inlet mouth 5 bottom vacuum chamber 7 and air outlet 4; argon gas enters vacuum chamber 7 by inlet mouth 5; vacuum chamber 7 sidewall is also provided with a porthole 6, for observing internal vacuum chamber situation.In described vacuum chamber, charging tray 8 is arranged at the side of target 11, and positive plate 1 is arranged at the opposite side of target 11; Described power supply 3 is outside at vacuum chamber 7, and power supply 3 includes two negative electrodes, one of them negative electrode is connected to target 11, and another negative electrode is connected to charging tray 8, and the anode of power supply 3 is connected to positive plate 1, and target 11 is also provided with thermopair 10.
Below charging tray 8,3 centimeters are provided with ultrasonic oscillation amplitude transformer 12, and ultrasonic oscillation amplitude transformer 12 controls diamond particles or powder constantly stirs; Be provided with thermopair 10 from charging tray 8 liang of centimeters, the temperature under depositing operation near diamond surface monitored by thermopair 10.Place diamond particles or powder in charging tray 8, target device 9 places target, and target can be metal or alloy, as Ti, Cr, Mo, Nb, Zr or the alloy that formed between them.
The voltage and current of double cathode structure can be regulated and controled by operator's console 2, and a negative electrode in double cathode structure connects target device 9, and another negative electrode connects charging tray 8, and charging tray 8 and target device 9 can arrange two.
Described equipment can meet the requirement of single plating in enormous quantities, and primary depositing diamonds can reach more than 20 kilograms, and sedimentation effect to be received m/h up to 500.
The technique of diamond surface depositing nano coating, adopt the equipment of above-mentioned double cathode plasma deposition nano coating, the charging tray of the side of target places diamond, and the opposite side of target arranges positive plate; Target and charging tray are connected on a negative electrode of double cathode power supply, and positive plate is connected to the anode of power supply; Double cathode plasma sputtering is carried out to target and charging tray, in vacuum chamber, passes into argon gas from inlet mouth, select the sputter deposition craft parameter of following table 1, carry out double cathode plasma sputter deposition.The coating of deposition is made up of the metal carbide layer 13 of outer field metal level 14 and internal layer.
Table 1 double cathode plasma sputter deposition processing parameter:
The diamond of the band coating in the above embodiments compares with the diamond of non-plating, by cutting experiment, wear resistance test and the strength trial to thermal shocking, tests respective efficiency.The results are shown in following table 2.
Table 2
Diamond particles or powder adopt three-dimensional microscope to observe its surface topography before and after the titanizing of double cathode plasma sputtering, and observations is as shown in table 3 below.
Diamond particles or powder adopt scanning electronic microscope to observe its surface topography before and after the titanizing of double cathode plasma sputtering, and observations is as shown in table 3 below.
Table 3
Isostatic pressing strength is tested:
The adamantine isostatic pressing strength testing non-plating is 31.2kg, and according to the double cathode plasma sputter deposition nano metal layer that embodiment 1 is obtained, test isostatic pressing strength is 33.4kg.
Due to double cathode plasma sputter deposition nano metal layer, depositing temperature is lower, avoids diamond under the catalysis of internal package body, causes intensity to reduce because there is greying.
Claims (1)
1. the technique of diamond surface double cathode plasma deposition nano coating, is characterized in that comprising the following steps:
Adopt the equipment of diamond surface double cathode plasma deposition nano coating, this equipment comprises vacuum chamber, power supply, target, monitor component, and in described vacuum chamber, charging tray is arranged at the side of target, and positive plate is arranged at the opposite side of target; Described power supply is outside at vacuum chamber, and power supply includes two negative electrodes, one of them negative electrode is connected to target, and another negative electrode is connected to charging tray, and the anode of power supply is connected to positive plate, and target is also provided with monitor component;
Place target in a vacuum chamber, the charging tray of the side of target places diamond, the opposite side of target arranges positive plate; Target and charging tray are connected on a negative electrode of double cathode power supply, and positive plate is connected to the anode of power supply; Carry out double cathode plasma sputtering to target and charging tray, obtain the diamond of surface-coated nano coating, coating comprises skin and internal layer, outer for grain-size be the metal level of 10-100 nanometer, internal layer is the metal carbide layer of thickness 90-110 nanometer;
Fill adamantine charging tray voltage: 800-1000 V,
Diamond voltage: 300-450 V,
Target and inter-particle spacing: 10-20 mm,
Ar pressure: 33-36Pa,
Depositing temperature: 500-600 DEG C,
Depositing time: 1.5h;
Described target is one or more of Ti, Cr, Mo, Nb, Zr.
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CN104762598A (en) * | 2015-03-26 | 2015-07-08 | 河南黄河旋风股份有限公司 | Manufacturing method of nonmagnetic metal layer plated on diamond surface |
CN104762591A (en) * | 2015-03-26 | 2015-07-08 | 河南黄河旋风股份有限公司 | Manufacturing method of silicon film on diamond surface by vacuum ion plating |
CN110666708A (en) * | 2019-09-27 | 2020-01-10 | 西安奕斯伟硅片技术有限公司 | Chamfer grinding wheel, preparation method thereof and wafer processing equipment |
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CN1103900A (en) * | 1994-10-19 | 1995-06-21 | 太原工业大学 | Synthesis of diamond film with double cathode glow discharge |
CN1412343A (en) * | 2002-03-18 | 2003-04-23 | 太原理工大学 | Bicathode-high frequency glow ion diffusion coating equipment and its process |
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