CN103436855B - A kind of preparation method of mini milling cutter diamond composite coating - Google Patents
A kind of preparation method of mini milling cutter diamond composite coating Download PDFInfo
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Abstract
A preparation method for mini milling cutter diamond composite coating, relates to mini milling cutter.PCB mini milling cutter is loaded in frock, reinstalls deposition reaction indoor; Cvd reactive chamber is vacuumized, then passes into methane (CH to cvd reactive chamber
4), hydrogen and oxygen 3 kinds of gases; Direct current arc is passed into the heater strip being arranged on deposition reaction indoor; In cvd reactive chamber, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, and 5 stages adopt different vapor deposition conditions; Wherein, sub-micro crystals growth phase and superfine nano-crystalline generation capable of circulation in vegetative period, circulation frequency is N(N>=1) secondary, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating.The sharp of cutting edge can be kept for more time, obviously improve processing effect, tool life, reduce tool changing frequency, improve working (machining) efficiency, cut down finished cost.
Description
Technical field
The present invention relates to mini milling cutter, especially relate to the preparation method of a kind of mini milling cutter diamond composite coating being mainly used in printed circuit board (PCB).
Background technology
Printed circuit board (PCB) (PCB, PrintedCircuitBoard) is a kind of with printing or the circuit product of image transfer fabrication techniques.In the various product of modern society, arrive greatly computer, TV, little of mobile phone, IC-card, as long as have circuit in product, just there is the existence of printed circuit board (PCB).Along with European Union RoHS(electrically, in electronics restriction use the instruction of some objectionable impurities) enforcement, environment-friendly type PCB version there occurs great variety under the requirement of RoHS.The PCB industry in the whole world enters lead-free compatible and halogen environmental protection epoch, but in order to ensure the stability of size, the oxide fillers such as aluminium, barium, silicon, magnesium are often added in printed circuit board (PCB), add the difficulty of processing of printed circuit board (PCB), this just proposes new higher requirement to PCB mini milling cutter.General Wimet mini milling cutter is difficult to reach processing request, but coating milling cutter completely likely reaches.
Coated cutting tool is on tool matrix, apply one deck wear-resistant coating, and coating, as thermodynamic barrier and chemical barrier, can reduce phase mutual diffusion and the chemical reaction of cutter and workpiece material element, the frictional coefficient both simultaneously reducing, thus improves cutting-tool's used life.Diamond coatings has the advantages such as high rigidity, high heat conductance, low-friction coefficient, low-expansion coefficient and high chemical stability, is the ideal material as abrasion resistant coating layer of cutter.The preparation technology of cvd diamond coated cutting tool is simple, cost is lower, and during cutting, comparable non-cutting tool coated with hard alloy improves more than 3 ~ 5 times of life-spans, improves 20% ~ 70% cutting speed.The real advantage of cvd diamond coating technology is the Application and Development at complicated shape diamond-coated tools, but the domestic research for complicated shape diamond-coated tools is still in the starting stage at present, and some problems are not also well solved.On the one hand, the sticking power of diamond coatings on matrix is poor, does not play diamond coatings wear resisting property; On the other hand, diamond coatings crystal grain is thicker, and surface smoothness is bad, does not reach work pieces process requirement.
Chinese patent CN102650053A discloses the preparation method of a kind of complicated shape cvd diamond/diamond-like composite coating cutter.Adopt filament CVD to deposit one deck MCD film at tool surface, in deposition process, adopt negative bias to produce ion bombardment ensure that MCD film has smooth surface; Continue deposition one deck DLC film subsequently, in the starting stage, with positive negative pulse stuffing ion power supply, ion bombardment is carried out to the tool surface being coated with MCD film, to remove the impurity of tool surface, and the crystal grain corner angle that decoating surface is sharp-pointed, increase coating planeness, improve coatingsurface active, reach the effect strengthening ply adhesion strength.Adopt the preparation method of this invention can obtain the cvd diamond/diamond-like composite coating with excellent film-Ji adhesion strength, surface abrasion resistance antifriction and self-lubricating property in the monoblock type carbide tool surface deposition with surfaces of complex shape, this compound coating also has the features such as internal stress is low, smooth surface is smooth, thickness is even.
Chinese patent CN101824618A discloses a kind of superhard quasi-diamond (DLC) base nano-composite coating printed circuit board (PCB) (PCB) micro-brill and preparation method thereof, and the micro-brill of PCB is generated by column target electric arc discharge means the multi-gradient nano-composite coating be made up of successively Ti/TiCN/TiCN-DLC/TiC-DLC.Compound coating prepared by this invention and tool matrix have good bonding force, very high hardness (42GPa) and good wear-resisting and lubricity (frictional coefficient is less than 0.15).To overcome in PCB micro-brill course of processing the problem that causes chip removal not smooth because tool surface lubrication is poor, solve the cutting force that in the course of processing, edge wear seriously causes and increase the micro-brill breakage problem caused, the life-span of the micro-brill of PCB and the working (machining) efficiency of PCB can be increased substantially, there is good prospects for commercial application.
Summary of the invention
The object of the invention is to the processing difficult problem in order to overcome difficult-to-machine material, and overcome the deficiency of existing complicated shape diamond-coated tools, there is provided the coating preparative layer that the internal layer of formed diamond composite coating is wear-resisting sub-micro crystal coating, table cuts the diamond composite coating PCB mini milling cutter of difficult-to-machine material to be meticulous nanocrystalline coating, thus make the preparation method of a kind of mini milling cutter diamond composite coating that the processing characteristics of this diamond composite coating PCB mini milling cutter is better, the processing life-span is longer.
The present invention includes following steps:
1) PCB mini milling cutter is loaded in frock, reinstall deposition reaction indoor;
2) cvd reactive chamber is vacuumized, then pass into methane (CH to cvd reactive chamber
4), hydrogen and oxygen 3 kinds of gases;
3) direct current arc is passed into the heater strip being arranged on deposition reaction indoor;
4) in cvd reactive chamber, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, and 5 stages adopt different vapor deposition conditions; Wherein, sub-micro crystals growth phase and superfine nano-crystalline generation capable of circulation in vegetative period, circulation frequency is N(N >=1) secondary, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating.
In step 1), described PCB mini milling cutter can adopt WC-Co hard alloy PCB mini milling cutter, and the sword footpath scope of described PCB mini milling cutter can be 0.01 ~ 3.175mm.
In step 2) in, the volume percent of described methane, hydrogen and oxygen can be (0.01% ~ 20%): (70% ~ 99.99%): (0 ~ 20%).
In step 3), described heater strip can be selected from tungsten filament or tantalum wire etc., and the temperature of heater strip can be 1500 ~ 2400 DEG C; The electric current of described direct current arc can be 100 ~ 200A.
In step 4), described different vapor deposition conditions is as follows:
Heating period: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 10%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 25 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 3h;
The forming core phase: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 10%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 600 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 5h;
The sub-micro crystals growth phase: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 20%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 600 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 20h;
Superfine nano-crystalline vegetative period: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 20%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 600 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 20h;
Grow latter stage: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 20%, hot tungsten filament temperature 2700 ~ 1000 DEG C, flame current 200 ~ 50A, deposition chamber temperatures 1000 ~ 100 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 3h;
The average crystal grain size of described sub-micro crystalline substance can be 0.5 ~ 10 μm;
The average crystal grain size of described superfine nano-crystalline is less than 0.5 μm;
Described diamond sub-micro is brilliant to be made up of sub-micro crystalline substance and superfine nano diamond coating with superfine nano-crystalline compound coating, and described diamond sub-micro is brilliant is at least 2 layers with the number of plies of superfine nano-crystalline compound coating.
The present invention utilizes tungsten filament to heat, and reactant gases is under the activation of hot filament, and produce carbon-containing group, oversaturated atomic hydrogen and atomic oxygen or hydroxyl etc., under certain depositing temperature, carbon-containing group flows to mini milling cutter matrix surface, with SP
3carry out dehydrogenation and key and become diamond lattic structure and be converted into diamond crystals.
The invention has the beneficial effects as follows, the present invention is to mini milling cutter matrix surface temperature, carbon-source gas concentration, the coating process state modulator such as deposition reaction chamber pressure within limits, multiple deposition method is adopted to produce diamond composite coating, this compound coating internal layer is the coating of sub-micro crystal structure, sub-micro crystal coating effectively can improve the wear resistance of cutter, surface is the coating of superfine nano crystal structure, what nanocrystalline coating can improve mini milling cutter shows smooth finish, improve workpiece processing quality, and compound coating effectively can delay the generation of crackle, adding man-hour, the sharp of cutting edge can be kept for more time, obviously improve processing effect, tool life, reduce tool changing frequency, improve working (machining) efficiency, cut down finished cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of the diamond coatings equipment that the embodiment of the present invention uses.
Embodiment
The invention will be further described by reference to the accompanying drawings for following examples.
Embodiment 1
See Fig. 1, adopt diamond coatings equipment to make, during preparation, comprise the steps:
PCB mini milling cutter 1 loads in frock 2 by step a.;
The frock 2 that mini milling cutter 1 is housed loads in cvd reactive chamber 3 by step b.;
Cvd reactive chamber 3 is evacuated to vacuum state by step c vacuum pump 4;
Steps d. pass into methane (CH to cvd reactive chamber 3
4), hydrogen (H
2) and oxygen (O
2) 3 kinds of gases; Wherein, the volume ratio of the methane passed into, hydrogen and oxygen is (0.1% ~ 10%): (90% ~ 99.99%): (0% ~ 5%);
Step e. passes into direct current arc by power supply 5 to the heater strip be arranged in cvd reactive chamber 3; Wherein, heater strip is tungsten filament or tantalum wire; Heater strip temperature is 2000 ~ 2100 DEG C; The flame current applied is 180A;
Step f. is in cvd reactive chamber 3, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, 5 stages adopt different vapor deposition conditions, to reach different diamond composite coating states, sub-micro crystals growth phase and superfine nano-crystalline generation capable of circulation in vegetative period, circulation frequency is N(N >=1) secondary, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating; The pressure of cvd reactive chamber is 1 ~ 10mbar; Depositing time is 20h.
Concrete technology condition is as table 1.
Table 1
Embodiment 2
The preparation method of the diamond composite coating of a kind of PCB mini milling cutter of the present invention, similar to Example 1, its difference is:
Steps d. pass into methane CH to cvd reactive chamber
4, hydrogen H
2and oxygen O
2three kinds of gases; Wherein, the volume ratio of the methane passed into, hydrogen and oxygen is (0.1% ~ 10%): (90% ~ 99.99%): (0 ~ 6%);
Step e. passes into direct current arc to the tungsten filament being arranged on deposition reaction indoor; Wherein, heater strip temperature is 2100 ~ 2200 DEG C; The flame current applied is 185A;
Step f. is in cvd reactive chamber, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, 5 stages adopt different vapor deposition conditions, sub-micro crystals growth phase and superfine nano-crystalline generation capable of circulation in vegetative period, circulation frequency is N(N >=1) secondary, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating; The pressure of cvd reactive chamber is 1 ~ 10mbar; Depositing time is 16h.
Concrete technology condition is as table 2.
Table 2
Embodiment 3
The preparation method of the diamond composite coating of a kind of PCB mini milling cutter of the present invention, similar to Example 1, its difference is:
Steps d. pass into methane CH to cvd reactive chamber
4, hydrogen H
2and oxygen O
2three kinds of gases; Wherein, the volume ratio of the methane passed into, hydrogen and oxygen is (0.1% ~ 10%): (90% ~ 99.99%): (0 ~ 7%);
Step e. passes into direct current arc to the tungsten filament being arranged on deposition reaction indoor; Wherein, heating tungsten filament temperature is 2300 DEG C; The flame current applied is 190A;
Step f. is in cvd reactive chamber, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, 5 stages adopt different vapor phase deposition conditions, sub-micro crystals growth phase and superfine nano-crystalline generation capable of circulation in vegetative period, circulation frequency is N(N >=1) secondary, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating; The pressure of cvd reactive chamber is 1 ~ 10mbar; Depositing time is 30h.
Concrete technology condition is as table 3.
Table 3
Embodiment 4
The preparation method of the diamond composite coating of a kind of PCB mini milling cutter of the present invention, similar to Example 1, its difference is:
Steps d. pass into methane CH to cvd reactive chamber
4, hydrogen H
2and oxygen O
2three kinds of gases; Wherein, the volume ratio of the methane passed into, hydrogen and oxygen is (0.1% ~ 10%): (90% ~ 99.99%): (0 ~ 9%);
Step e. passes into direct current arc to the tungsten filament being arranged on deposition reaction indoor; Wherein, heating tungsten filament temperature is 2400 DEG C; The flame current applied is 195A;
Step f. is in cvd reactive chamber, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, 5 stages adopt different vapor deposition conditions, sub-micro crystals growth phase and superfine nano-crystalline generation capable of circulation in vegetative period, circulation frequency is N(N >=1) secondary, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating; The pressure of cvd reactive chamber is 1 ~ 10mbar; Depositing time is 40h.
Concrete technology condition is as table 4.
Table 4
The invention provides a kind of manufacture method of PCB mini milling cutter diamond composite coating of hard alloy substrate, adopt hot wire process, pass into methane CH to coating cvd reactive chamber
4, hydrogen H
2and oxygen O
2three kinds of gases, obtain diamond coatings on the mini milling cutter surface of hard alloy substrate.The present invention is by controlling the processing parameter such as temperature, pressure, filament temperature, depositing time, reaction gas flow of sediment chamber, obtain sub-micro crystalline substance and superfine nano-crystalline diamond composite coating, thus allow the mini milling cutter of the hard alloy substrate scribbling this diamond composite coating, the processing life-span is longer, processing quality is higher, reduce the tool changing frequency of the course of processing, enhance productivity, reduce production cost.
Claims (8)
1. a preparation method for mini milling cutter diamond composite coating, is characterized in that comprising the steps:
1) PCB mini milling cutter is loaded in frock, reinstall deposition reaction indoor;
2) cvd reactive chamber is vacuumized, then pass into methane, hydrogen and oxygen 3 kinds of gases to cvd reactive chamber; The volume percent of described methane, hydrogen and oxygen is (0.01% ~ 20%): (70% ~ 99.99%): (0 ~ 20%);
3) direct current arc is passed into the heater strip being arranged on deposition reaction indoor;
4) in cvd reactive chamber, deposition process is divided into heating period, nucleation period, sub-micro crystals growth phase, superfine nano-crystalline vegetative period, growth 5 stages of latter stage, and 5 stages adopt different vapor deposition conditions; Wherein, circulation frequency is N time, forms diamond sub-micro crystalline substance and superfine nano-crystalline compound coating, wherein N >=1; Form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating; Described different vapor deposition conditions is as follows:
Heating period: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 10%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 25 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 3h;
The forming core phase: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 10%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 600 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 5h;
The sub-micro crystals growth phase: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 20%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 600 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 20h;
Superfine nano-crystalline vegetative period: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 20%, hot tungsten filament temperature 1500 ~ 2700 DEG C, flame current 100 ~ 200A, deposition chamber temperatures 600 ~ 1000 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 20h;
Grow latter stage: methane volumetric content 0.01% ~ 20%, hydrogen flowing quantity volume content 70% ~ 99.9%, oxygen flow volume content 0 ~ 20%, hot tungsten filament temperature 2700 ~ 1000 DEG C, flame current 200 ~ 50A, deposition chamber temperatures 1000 ~ 100 DEG C, chamber pressure 0.1 ~ 50mbar, depositing time 0.1 ~ 3h.
2. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 1) in, described PCB mini milling cutter adopts WC-Co hard alloy PCB mini milling cutter.
3. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 1) in, the sword footpath scope of described PCB mini milling cutter is 0.01 ~ 3.175mm.
4. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 3) in, described heater strip is selected from tungsten filament or tantalum wire, and the temperature of heater strip is 1500 ~ 2400 DEG C.
5. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 3) in, the electric current of described direct current arc is 100 ~ 200A.
6. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 4) in, the average crystal grain size of described sub-micro crystalline substance is 0.5 ~ 10 μm.
7. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 4) in, the average crystal grain size of described superfine nano-crystalline is less than 0.5 μm.
8. the preparation method of a kind of mini milling cutter diamond composite coating as claimed in claim 1, it is characterized in that in step 4) in, described diamond sub-micro is brilliant to be made up of sub-micro crystalline substance and superfine nano diamond coating with superfine nano-crystalline compound coating, and described diamond sub-micro is brilliant is at least 2 layers with the number of plies of superfine nano-crystalline compound coating.
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|---|---|---|---|---|
| EP3674441A1 (en) * | 2018-12-25 | 2020-07-01 | Union Tool Co. | Diamond film for cutting tools |
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