CN103436855A - Preparation method of diamond composite coating of micro milling cutter - Google Patents
Preparation method of diamond composite coating of micro milling cutter Download PDFInfo
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Abstract
The invention discloses a preparation method of a diamond composite coating of a micro milling cutter, and relates to the micro milling cutter. The preparation method comprises the following steps of: placing a PCB (Printed Circuit Board) micro milling cutter into a tool and then placing into a deposition reaction chamber; evacuating the deposition reaction chamber, and introducing methane (CH4), hydrogen gas and oxygen gas into the deposition reaction chamber; applying direct-current electric arc to a heating wire which is installed in the deposition reaction chamber, wherein a deposition process in the deposition reaction chamber is divided into five stages including a heating stage, a nucleation stage, a submicrocrystal growth stage, a superfine nanocrystalline growth stage and a final growth stage, different gas-phase deposition conditions are adopted in the five stages, the submicrocrystal growth stage and the superfine nanocrystalline growth stage can be generated in a circulating manner to form a diamond submicrocrystal and superfine nanocrystalline composite coating, and the circulating generation number is N (N is not less than 1). The prepared diamond composite coating of the micro milling cutter can be used for keeping the cutting edge to be sharp for a longer time, obviously improving the machining effect, prolonging the service life of the cutter, reducing the cutter changing frequency, improving the machining efficiency and lowering the machining 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 that is mainly used in printed circuit board (PCB).
Background technology
Printed circuit board (PCB) (PCB, Printed Circuit Board) is a kind of circuit product with printing or image transfer fabrication techniques.In the various product of modern society, arrive greatly computer, TV, little of mobile phone, IC-card, as long as in product, circuit is arranged, the existence of printed circuit board (PCB) is just arranged.The instruction of be accompanied by that the RoHS(of European Union is electric, some objectionable impurities being used in restriction in electronics) enforcement, great variety has occurred in environment-friendly type PCB version under the requirement of RoHS.The PCB industry in the whole world has entered lead-free compatible and halogen environmental protection epoch, but in order to guarantee the stability of size, often add the oxide fillers such as aluminium, barium, silicon, magnesium in printed circuit board (PCB), increased the difficulty of processing of printed circuit board (PCB), this has just proposed new higher requirement to the PCB mini milling cutter.General Wimet mini milling cutter is difficult to reach processing request, but the coating milling cutter fully likely reaches.
Coated cutting tool is coating one deck wear-resistant coating on tool matrix, and coating, as thermodynamic barrier and chemical barrier, can reduce phase mutual diffusion and the chemical reaction of cutter and workpiece material element, reduces the frictional coefficient of the two simultaneously, thereby improves the work-ing life of cutter.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 tools is simple, cost is lower, and during cutting, comparable not cutting tool coated with hard alloy improves 3～5 times more than the life-span, improves 20%～70% cutting speed.The real advantage of CVD diamond coatings technology is the Application and Development at the complicated shape diamond-coated tools, and still the domestic research for the complicated shape diamond-coated tools at present is still in the starting stage, and some problems also are not well solved.On the one hand, the sticking power of diamond coatings on matrix is poor, does not bring into play the diamond coatings wear resisting property; On the other hand, diamond coatings crystal grain is thicker, and surface smoothness is bad, does not reach the workpiece processing request.
Chinese patent CN102650053A discloses the preparation method of a kind of complicated shape CVD diamond/diamond-like composite coating cutter.Adopt filament CVD at tool surface deposition one deck MCD film, in deposition process, adopt negative bias to produce ion bombardment and guarantee that the MCD film has smooth surface; Continue subsequently deposition one deck DLC film, in the starting stage, with the positive negative pulse stuffing ion power supply, the tool surface that has applied the MCD film is carried out to ion bombardment, to remove the impurity of tool surface, and the sharp-pointed crystal grain corner angle in decoating surface, increase the coating planeness, improve the coatingsurface activity, reach the effect that strengthens ply adhesion strength.Adopt the preparation method of this invention to 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 characteristics such as internal stress is low, smooth surface is smooth, even thickness.
Chinese patent CN101824618A discloses micro-brill of a kind of superhard quasi-diamond (DLC) base nano-composite coating printed circuit board (PCB) (PCB) and preparation method thereof, on the micro-brill of PCB, by the column target electric arc discharge means, generates the multi-gradient nano-composite coating consisted of successively Ti/TiCN/TiCN-DLC/TiC-DLC is arranged.The compound coating of this invention preparation and tool matrix have good bonding force, very high hardness (42GPa) and good wear-resisting and lubricity (frictional coefficient is less than 0.15).Overcome in the micro-brill course of processing of PCB due to the lubricated poor not smooth problem of chip removal that causes of tool surface, the cutting force that has solved blade serious wear in the course of processing and caused increases the micro-brill breakage problem caused, can increase substantially the life-span of the micro-brill of PCB and the working (machining) efficiency of PCB, there is good prospects for commercial application.
Summary of the invention
The object of the invention is in order to overcome the processing difficult problem of difficult-to-machine material, and the deficiency that overcomes existing complicated shape diamond-coated tools, the internal layer that formed diamond composite coating is provided is that wear-resisting sub-micro crystal coating, the coating preparative layer that table cuts the diamond composite coating PCB mini milling cutter of difficult-to-machine material are meticulous nanocrystalline coating, thus the preparation method who makes the processing characteristics of this diamond composite coating PCB mini milling cutter better, processes longer a kind of mini milling cutter diamond composite coating of life-span.
The present invention includes following steps:
1) the PCB mini milling cutter is packed in frock, reinstall deposition reaction indoor;
2) cvd reactive chamber is vacuumized, then pass into methane (CH to cvd reactive chamber
4), hydrogen and 3 kinds of gases of oxygen;
3) pass into direct current arc to being arranged on the indoor heater strip of deposition reaction;
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, the circulation frequency is N(N >=1) inferior, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating.
In step 1), described PCB mini milling cutter can adopt WC-Co Wimet 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 ℃; 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 volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～10%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 25～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～3h;
The forming core phase: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～10%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 600～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～5h;
The sub-micro crystals growth phase: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～20%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 600～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～20h;
Superfine nano-crystalline vegetative period: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～20%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 600～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～20h;
Grow latter stage: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～20%, 2700～1000 ℃ of hot tungsten filament temperature, flame current 200～50A, 1000～100 ℃ of sediment chamber's temperature, 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 μ m;
The average crystal grain size of described superfine nano-crystalline is less than 0.5 μ m;
Described diamond sub-micro is brilliant to be comprised of sub-micro crystalline substance and superfine nano diamond coating with the superfine nano-crystalline compound coating, and the brilliant number of plies with the superfine nano-crystalline compound coating of described diamond sub-micro is at least 2 layers.
The present invention utilizes the tungsten filament heating, and reactant gases, under the activation of hot filament, produces carbon-containing group, oversaturated atomic hydrogen and atomic oxygen or hydroxyl etc., and under certain depositing temperature, carbon-containing group flows to the 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 parameters such as deposition reaction chamber pressure are controlled within limits, adopt the multistep deposition method to produce diamond composite coating, the coating that this compound coating internal layer is the sub-micro crystal structure, the sub-micro crystal coating can effectively improve the wear resistance of cutter, surface is the coating of superfine nano crystal structure, nanocrystalline coating can improve the smooth finish that shows of mini milling cutter, improve the workpiece processing quality, and compound coating can effectively delay the generation of crackle, adding man-hour, can keep for more time the sharp of cutting edge, obviously improve processing effect, tool life, reduce the tool changing frequency, improve working (machining) efficiency, cut down finished cost.
The accompanying drawing explanation
Fig. 1 is the structural representation of the diamond coatings equipment that uses of the embodiment of the present invention.
Embodiment
The invention will be further described by reference to the accompanying drawings for following examples.
Referring to Fig. 1, adopt diamond coatings equipment to be made, during preparation, comprise the steps:
Step a. packs PCB mini milling cutter 1 in frock 2;
The frock 2 that step b. will be equipped with mini milling cutter 1 is packed in cvd reactive chamber 3;
Step c is evacuated to vacuum state with vacuum pump 4 by cvd reactive chamber 3;
Steps d. pass into methane (CH to cvd reactive chamber 3
4), hydrogen (H
2) and oxygen (O
2) 3 kinds of gases; The volume ratio of the methane wherein, 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; The heater strip temperature is 2000～2100 ℃; 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, the circulation frequency is N(N >=1) inferior, 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.
The 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; The volume ratio of the methane wherein, passed into, hydrogen and oxygen is (0.1%～10%): (90%～99.99%): (0～6%);
Step e. passes into direct current arc to being arranged on the indoor tungsten filament of deposition reaction; Wherein, the heater strip temperature is 2100～2200 ℃; 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, the circulation frequency is N(N >=1) inferior, 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.
The concrete technology condition is as table 2.
Table 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; The volume ratio of the methane wherein, passed into, hydrogen and oxygen is (0.1%～10%): (90%～99.99%): (0～7%);
Step e. passes into direct current arc to being arranged on the indoor tungsten filament of deposition reaction; Wherein, heating tungsten filament temperature is 2300 ℃; 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, the circulation frequency is N(N >=1) inferior, 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.
The concrete technology condition is as table 3.
Table 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; The volume ratio of the methane wherein, passed into, hydrogen and oxygen is (0.1%～10%): (90%～99.99%): (0～9%);
Step e. passes into direct current arc to being arranged on the indoor tungsten filament of deposition reaction; Wherein, heating tungsten filament temperature is 2400 ℃; 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, the circulation frequency is N(N >=1) inferior, 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.
The 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, to the coating cvd reactive chamber, pass into methane CH
4, hydrogen H
2and oxygen O
2three kinds of gases, obtain diamond coatings on the mini milling cutter surface of hard alloy substrate.The processing parameters such as the temperature of the present invention by controlling sediment chamber, pressure, filament temperature, depositing time, reaction gas flow, obtain sub-micro crystalline substance and superfine nano-crystalline diamond composite coating, thereby allow the mini milling cutter of the hard alloy substrate that scribbles 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 costs.
Claims (10)
1. the preparation method of a mini milling cutter diamond composite coating, is characterized in that comprising the steps:
1) the PCB mini milling cutter is packed in frock, reinstall deposition reaction indoor;
2) cvd reactive chamber is vacuumized, then pass into methane, hydrogen and 3 kinds of gases of oxygen to cvd reactive chamber;
3) pass into direct current arc to being arranged on the indoor heater strip of deposition reaction;
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, the circulation frequency is N(N >=1) inferior, form diamond sub-micro crystalline substance and superfine nano-crystalline compound coating.
2. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 1), and described PCB mini milling cutter adopts WC-Co Wimet PCB mini milling cutter.
3. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 1), and the sword footpath scope of described PCB mini milling cutter is 0.01～3.175mm.
4. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 2) in, the volume percent of described methane, hydrogen and oxygen is (0.01%～20%): (70%～99.99%): (0～20%).
5. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 3), and described heater strip is selected from tungsten filament or tantalum wire, and the temperature of heater strip is 1500～2400 ℃.
6. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 3), and the electric current of described direct current arc is 100～200A.
7. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 4), and described different vapor deposition conditions is as follows:
Heating period: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～10%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 25～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～3h;
The forming core phase: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～10%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 600～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～5h;
The sub-micro crystals growth phase: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～20%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 600～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～20h;
Superfine nano-crystalline vegetative period: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～20%, 1500～2700 ℃ of hot tungsten filament temperature, flame current 100～200A, 600～1000 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～20h;
Grow latter stage: methane volume content 0.01%～20%, hydrogen flowing quantity volume content 70%～99.9%, oxygen flow volume content 0～20%, 2700～1000 ℃ of hot tungsten filament temperature, flame current 200～50A, 1000～100 ℃ of sediment chamber's temperature, chamber pressure 0.1～50mbar, depositing time 0.1～3h.
8. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 4), and the average crystal grain size of described sub-micro crystalline substance is 0.5～10 μ m.
9. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, is characterized in that in step 4), and the average crystal grain size of described superfine nano-crystalline is less than 0.5 μ m.
10. a kind of preparation method of mini milling cutter diamond composite coating as claimed in claim 1, it is characterized in that in step 4), described diamond sub-micro is brilliant to be comprised of sub-micro crystalline substance and superfine nano diamond coating with the superfine nano-crystalline compound coating, and the brilliant number of plies with the superfine nano-crystalline compound coating of described diamond sub-micro is at least 2 layers.
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| CN103741114A (en) * | 2013-12-29 | 2014-04-23 | 湖南中航超强金刚石膜高科技有限公司 | Preparation method of milling cutter with diamond coating for processing pure titanium porcelain teeth and zirconium dioxide false teeth |
| CN105216021A (en) * | 2014-06-24 | 2016-01-06 | 厦门金鹭特种合金有限公司 | A kind of composite processing diamond-coated tools and preparation method thereof |
| CN105483644A (en) * | 2016-01-15 | 2016-04-13 | 中国科学院深圳先进技术研究院 | Multilayer diamond coating, manufacturing method thereof and coating tool |
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| CN103741114B (en) * | 2013-12-29 | 2019-01-29 | 武汉世纪中航超强金刚石膜高科技有限公司 | It is a kind of for processing the preparation method of pure titanium baking-ceramic tooth, zirconium dioxide false tooth diamond coatings milling cutter |
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| JP2020099979A (en) * | 2018-12-25 | 2020-07-02 | ユニオンツール株式会社 | Diamond coating for cutting tool |
| CN110423994A (en) * | 2019-08-10 | 2019-11-08 | 上海妙壳新材料科技有限公司 | A kind of diamond-like coating moves back membrane treatment appts and its application method |
| CN111286718A (en) * | 2020-03-20 | 2020-06-16 | 廊坊西波尔钻石技术有限公司 | Impact-resistant CVD diamond self-supporting material and manufacturing method thereof |
| CN111394774A (en) * | 2020-04-09 | 2020-07-10 | 科汇纳米技术（深圳）有限公司 | Multilayer composite structure diamond coating applied to printed circuit board drill point |
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